JP6184627B1 - Method for producing fragrance composition from roasted coffee beans and apparatus for collecting aroma from roasted coffee beans - Google Patents

Abstract

The present invention relates to a perfume composition from roasted coffee beans that can be put into practical use without burdens such as large capital investment and equipment by using a general crusher, and feels aroma generated when crushing roasted coffee beans. Providing a method for manufacturing goods. The method includes a step of pulverizing roasted coffee beans to obtain a coarsely pulverized roasted coffee bean containing fine powder and flakes, and a fine powder from a gas containing aroma compounds and fine powder and flakes generated during the pulverization of roasted coffee beans. And a step of removing flakes, an adsorption step of passing the gas from which fine powder and flakes have been removed to the adsorbent and adsorbing the aroma compound to the adsorbent, and collecting the aroma compound from the adsorbent and containing the aroma compound A roasted coffee bean, wherein the adsorbent is accommodated in an adsorbent accommodating portion in the aromatic compound adsorbing device, and the adsorbent accommodating portion has net lids at both ends in the gas aeration direction. For producing a perfume composition from [Selection] Figure 1

Description

  The present invention relates to a method for producing a fragrance composition from roasted coffee beans and an aroma recovery device from roasted coffee beans.

  The fragrance composition is used as a food fragrance (flavor) or a cosmetic fragrance (fragrance). Perfume compositions for food and drink can be prepared from natural fragrances, synthetic fragrances and / or blended fragrances that combine them. Recently, with the natural orientation of consumers, it is desirable that flavors have natural fragrances or natural flavours. Various manufacturing methods are being studied.

Various manufacturing methods are currently employed for coffee flavors. For example, various methods are known as a method for producing a fragrance composition from roasted coffee beans (see Patent Document 1).
Specifically, for example, a method for producing a coffee flavor that supplements a solution such as caramel with a volatile coffee flavor component-containing gas phase released into the crushed roasted coffee through water vapor and / or an inert gas, Method for fractionating condensed water obtained by distillation, method for extracting aroma component-containing distillate obtained by distilling fruit juice or coffee with a reverse-phase distribution type adsorbent, and then extracting with a solvent, steam distillation method A method for formulating a coffee flavor that has a flavor component and a flavor component in which the coffee flavor raw material obtained by the above method is contained in a water layer and the oil phase is coffee oil obtained by pressing oil extraction or supercritical fluid, etc. Patent Document 1 discloses a method for producing a tea leaf flavor in which a distillate obtained in this manner is brought into contact with tea leaves to remove a heated distillation odor.
According to Patent Document 1, the steam distillation method is a method in which water vapor is passed through the raw material, and the aromatic component distilled off accompanying the water vapor is condensed together with the water vapor. Further, it is described that any distillation means of atmospheric steam distillation or vacuum steam distillation can be employed.

  In addition, among coffee flavors, a flavor that can give a particularly freshly scented scent has been demanded for many years. Then, the method of using the fragrance which generate | occur | produces at the time of grinding | pulverizing roasted coffee beans is proposed (patent documents 2-6).

JP 2003-33137 A Patent 3719995 Japanese Patent No. 4182471 Japanese Patent No. 4308724 Japanese Patent No. 4745591 JP 2003-144053 A

In the methods described in Patent Documents 2 to 5, a fragrance composition is produced by introducing a gas (crushed gas) containing an aroma component generated during pulverization of roasted coffee beans into a solvent such as water or coffee oil as it is. It was.
In the method described in Patent Document 6, the pulverized gas of roasted coffee beans was compressed and stored in an aluminum container.

However, the fragrance composition obtained by the methods described in Patent Documents 2 to 6 has a low collection efficiency because the gas containing the fragrance compound is passed through the solvent, and has a fragrance when the roasted coffee beans are ground. It cannot be reproduced sufficiently.
In addition, the methods described in Patent Documents 2 to 6 use a special apparatus such as an inert gas, a sealed pulverizer, a passage to a solvent layer, a solvent layer, a thermostatic bath, etc. It was not easy to put into practical use.

The problem to be solved by the present invention is to use a general pulverizing apparatus and to put it into practical use without burdens such as a large capital investment and load on the apparatus. It is to provide a method for producing a fragrance composition from roasted coffee beans, which gives a scent when beans are ground.
In addition, the problem to be solved by the present invention is to feel the aroma generated when crushing roasted coffee beans that can be put to practical use without burdens such as large additional capital investment and equipment using a general crushing device. It is providing the fragrance | flavor collection apparatus from roasted coffee beans which can manufacture the fragrance | flavor composition to be made.

  As a result of diligent research to solve the above problems, the inventors of the present invention generated completely from roasted coffee beans during pulverization of roasted coffee beans as a method completely different from the methods described in Patent Documents 1-6. Fragrant compounds, chaff flakes or pulverized products, excessively fine crushed coffee beans, and flakes and pulverized products derived from other contaminants (hereinafter collectively referred to as “fine powder and flakes” in this specification), After the fine powder and flakes are removed from the gas containing the fragrance compound, the fragrance compound generated during the pulverization of the roasted coffee beans is adsorbed and recovered by the adsorbent, and the fragrance compound is efficiently recovered, and a general pulverizer (For example, conventional pulverizers) A natural fragrance composition can be efficiently produced that feels the fragrance generated during pulverization of roasted coffee beans without imposing a heavy load or additional capital investment on the conventional pulverizer. They found the door, which resulted in the completion of the present invention.

The present invention, which is a specific means for solving the above problems, and preferred embodiments thereof are as follows.
[1] A step of pulverizing roasted coffee beans to obtain a coarsely pulverized roasted coffee bean containing fine powder and flakes,
Removing the fine powder and flakes from the gas containing the aromatic compound and fine powder and flakes generated from the roasted coffee beans when the roasted coffee beans are crushed;
An adsorbing step in which the gas from which the fine powder and flakes have been removed is passed through an adsorbent to adsorb the aromatic compound to the adsorbent;
A recovery step of recovering the fragrance compound from the adsorbent and preparing a fragrance composition containing the fragrance compound;
Including
The adsorbent is accommodated in an adsorbent accommodating portion in an aromatic compound adsorbing device, and the adsorbent accommodating portion has net-like lids at both ends in the gas ventilation direction.
A method for producing a fragrance composition from roasted coffee beans.
[2] The step of removing the fine powder and flakes from the roasted coffee bean coarsely pulverized product is performed before the step of removing the fine powder and flakes from the gas. A method for producing a fragrance composition.
[3] The method for producing a fragrance composition from roasted coffee beans according to [1] or [2], wherein the step of removing the fine powder and flakes is performed with a fine powder flake remover.
[4] The method for producing a fragrance composition from roasted coffee beans according to any one of [1] to [3], wherein the gas flow is generated using an airflow generator.
[5] A gas flow path from which the fine powder and flakes have been removed is provided with an introduction path that branches from the flow path and communicates with the aromatic compound adsorption device.
The roasted coffee according to any one of [1] to [4], wherein only a part of the gas from which the fine powder and flakes have been removed is passed through the introduction path and the adsorbent to collect the aroma compound. A method for producing a fragrance composition from beans.
[6] The adsorbent is a styrene divinylbenzene copolymer, a copolymer of ethylvinylbenzene and divinylbenzene, a polymer of 2,6-diphenyl-9-phenyl oxide, a polycondensation polymer of methacrylic acid and a diol, and The method for producing a fragrance composition from roasted coffee beans according to any one of [1] to [5], which is one or more selected from modified silica gel.
[7] The method for producing a fragrance composition from roasted coffee beans according to any one of [1] to [6], wherein the aroma compound is desorbed from the adsorbent using an organic solvent in the recovery step. .
[8] The method for producing a fragrance composition from roasted coffee beans according to [7], wherein the organic solvent is ethanol or propylene glycol.
[9] From the roasted coffee beans according to any one of [1] to [8], wherein the linear velocity of the gas flowing into the adsorbent is in the range of 0.1 to 35.0 m / s. A method for producing a fragrance composition.
[10] The method for producing a fragrance composition from roasted coffee beans according to any one of [1] to [9], wherein the gas aeration direction is substantially opposite to the direction of gravity.
[11] The method for producing a fragrance composition from roasted coffee beans according to any one of [1] to [10], wherein the aroma compound adsorption device is a fluidized bed column in which the adsorbent is accommodated. .
[12] The method for producing a fragrance composition from roasted coffee beans according to any one of [1] to [11], comprising a step of adjusting a linear velocity of gas flowing into the adsorbent.
[13] The method for producing a fragrance composition from roasted coffee beans according to [12], wherein the linear velocity of the gas flowing into the adsorbent is adjusted using a blower or a suction pump.
[14] A food or drink containing a fragrance composition produced using the production method according to any one of [1] to [13].
[15] A device for crushing roasted coffee beans;
A first flow path that communicates with the pulverizing device and through which a gas containing aroma compounds and fine powder and flakes generated when the roasted coffee beans are crushed;
A fine powder flake removal device communicating with the first flow path to remove the fine powder and flakes;
A second flow path that communicates with the fine powder flake removal device and through which the gas from which the fine powder and flakes have been removed can pass;
An aroma compound adsorbing device in communication with the second flow path;
An airflow generator for generating a continuous airflow from the pulverizer to the aromatic compound adsorbing device;
With
The aroma compound adsorbing device has an adsorbent accommodating portion in which an adsorbent is accommodated, and the adsorbent accommodating portion has net lids at both ends in the gas flow direction, and an aroma recovery device from roasted coffee beans .
[16] The apparatus for recovering aroma from roasted coffee beans according to [15], further including an introduction path branched from the second flow path, the introduction path communicating with the aroma compound adsorption device.
[17] The apparatus for recovering aroma from roasted coffee beans according to [15] or [16], further comprising a fine powder flake preliminary removal device between the pulverization device and the first flow path.
[18]
The aroma recovery device for roasted coffee beans according to any one of [15] to [17], wherein the gas aeration direction of the adsorbent is substantially opposite to the direction of gravity.
[19]
The aroma recovery device for roasted coffee beans according to any one of [15] to [18], wherein the aroma compound adsorption device is a fluidized bed column in which the adsorbent is accommodated.
[20]
The fragrance recovery device from roasted coffee beans according to any one of [15] to [19], further comprising a linear velocity adjusting device that adjusts a linear velocity of the gas from which the fine powder and flakes have been removed.
[21]
The fragrance recovery device from roasted coffee beans according to any one of [15] to [20], wherein the linear velocity adjusting device is a blower or a suction pump.
[22]
The fragrance recovery device from roasted coffee beans according to any one of [15] to [21], wherein a cross-sectional diameter of the adsorbent portion accommodated in the adsorbent accommodating portion is 10 mm or more.
[23]
Aroma recovery from roasted coffee beans according to any one of [15] to [22], wherein the length of the adsorbent portion accommodated in the adsorbent accommodating portion is 1000 mm or less. apparatus.

According to the present invention, an aroma generated from roasted coffee beans when roasted coffee beans are crushed, that is, roasted roasted coffee beans by using a general pulverizing apparatus without burden such as a large additional capital investment and load on the apparatus. The manufacturing method of the fragrance | flavor composition from roasted coffee beans which makes the fragrance feel when coffee beans are ground can be provided. Although the fragrance composition of the present invention is a natural fragrance, it can enhance the top fragrance derived from roasted coffee beans.
In addition, according to the present invention, a fragrance composition that makes use of a general pulverization apparatus without burden such as a large additional capital investment and a load on the apparatus makes the fragrance composition feel the aroma generated when pulverizing roasted coffee beans. An apparatus for recovering aroma from roasted coffee beans that can be manufactured can be provided.

FIG. 1 is a schematic view showing an example of an aroma recovery device of the present invention. FIG. 2 is a schematic view showing another example of the aroma recovery device of the present invention. FIG. 3 is a schematic cross-sectional view of the adsorbent container of the present invention. FIG. 4 is a performance diagram of a general airflow generation device. FIG. 5 is an example of the total ion chromatogram of the fragrance composition of the product 1 of the present invention. FIG. 6 is an example of the total ion chromatogram of the fragrance composition of Comparative Product 3.

  Hereinafter, the present invention will be described in detail. The description of the constituent elements described below may be made based on representative embodiments and specific examples, but the present invention is not limited to such embodiments. In the present specification, a numerical range expressed using “to” means a range including numerical values described before and after “to” as a lower limit value and an upper limit value.

[Method for producing a fragrance composition from roasted coffee beans]
The method for producing a fragrance composition from roasted coffee beans of the present invention (also referred to as the production method of the present invention) is a step of pulverizing roasted coffee beans to obtain a roasted coffee bean coarsely pulverized product containing fine powder and flakes Including
Removing fine powder and flakes from the gas containing aroma compounds and fine powder and flakes generated during grinding of roasted coffee beans;
An adsorption process in which the gas from which fine powder and flakes have been removed is passed through the adsorbent, and the aroma compound is adsorbed on the adsorbent;
A recovery step of recovering the fragrance compound from the adsorbent and preparing a fragrance composition containing the fragrance compound;
Including
The adsorbent is accommodated in an adsorbent accommodating portion inside the aromatic compound adsorbing device, and this adsorbent accommodating portion has mesh lids at both ends in the gas aeration direction (see FIG. 3, The arrow indicates the gas flow direction).
Details of the mesh lid will be described later.
With the above configuration, a perfume composition from roasted coffee beans that makes it possible to feel the aroma generated during the crushing of roasted coffee beans by using a general crushing apparatus without significant additional capital investment and load on the apparatus. Can be manufactured.
Coffee beans (raw beans) are the seeds of coffee cherries, and a thin skin called silver skin is attached to the coffee beans. The roasted coffee beans are roasted with a silver skin and have a chaff that shows astringency. When roasted coffee beans are ground to the desired size, in addition to ground coffee beans ground to the desired size, chaff flakes and grounds, excessively fine ground coffee beans, or even other Flakes or pulverized products derived from impurities (generally referred to herein as “fine powder and flakes”) are generated, and the fine powder and flakes are scattered because they are light. In industrial pulverization of roasted coffee beans, at least a part of the fine powder and flakes are scattered and mixed with the exhaust stream of the airflow generated by the pulverizer. This exhaust stream was discharged out of the apparatus as it was after appropriately removing fine powder and flakes.
Here, unlike patent documents 2-6, this invention uses the adsorption agent accommodated in the aromatic compound adsorption | suction apparatus instead of a solvent (liquid) for collection of an aromatic compound. If an exhaust stream containing fine powder and flakes is passed through the adsorbent as it is, the fine powder and flakes may cause clogging of the mesh lid and clogging of fine pores between adsorbents and adsorbent particles. The flow becomes difficult to flow, and it is considered that a load (pressure) is applied to the exhaust system of the pulverizer (exhaust by an airflow generator described later in the present invention). On the other hand, in the production method of the present invention, after removing fine powder and flakes from the exhaust stream, the method employs a method in which the exhaust stream is passed through the adsorbent to adsorb the fragrance compound. The aroma compounds contained in the exhaust stream can be adsorbed without worrying about clogging and load on the apparatus. Further, by preventing this clogging, the aroma compound can be adsorbed efficiently.
Also, depending on the performance of the exhaust system of a general crushing device, if an adsorbent container is provided in the exhaust flow passage to accommodate the adsorbent, the load on the device exceeds the allowable range due to the resistance of the adsorbent to the exhaust flow. (In the present specification, it may be simply referred to as a load). Therefore, in the present invention, it is possible to employ means for suppressing the resistance due to the adsorbent. For example, in the direction of exhaust flow ventilation (also referred to as gas ventilation direction) of the portion occupied by the adsorbent accommodated in the adsorbent accommodating portion (hereinafter referred to as the adsorbent portion or the adsorbent portion accommodated in this specification) Examples thereof include suppressing the length, and providing a flow path containing an adsorbent that branches off from the flow path of the exhaust flow, and recovering the aroma compound from a part of the exhaust flow. Further, the resistance of the adsorbent may be suppressed by increasing the mobility of the adsorbent accommodated (eg, using a so-called “fluidized bed column”). Further, an air blower or a suction pump may be further provided to vent the adsorbent beyond the resistance of the adsorbent.
Hereinafter, the preferable aspect of the manufacturing method of this invention is demonstrated.

<Step of obtaining a coarsely pulverized roasted coffee bean>
The production method of the present invention includes a step of pulverizing roasted coffee beans to obtain a coarsely pulverized roasted coffee bean containing fine powder and flakes.
It is preferable to perform the step of pulverizing roasted coffee beans to obtain a coarsely pulverized roasted coffee bean before the other steps.
There is no restriction | limiting in particular as a method of grind | pulverizing roasted coffee beans, A well-known method can be used. For example, a known crushing device such as a roller mill, a jet mill, a hammer mill, a rotary mill, a vibration mill, or the like can be used.
The grinding speed of roasted coffee beans can be set to 1 to 500 kg / h, for example, but is not particularly limited.
The pulverized size of the roasted coffee beans is not particularly limited, and may be any of so-called fine grinding, medium grinding, and coarse grinding, and may be the same as a known preferable size range. For example, it can be set to about 0.2 to 3 mm.

(Roasted coffee beans)
There is no restriction | limiting in particular as roasted coffee beans used for the manufacturing method of this invention. Although not bound for any reason, it is presumed that the type of coffee beans and the degree of roasting of coffee mainly affect the amount ratio of aromatic compounds having a large molecular weight in the perfume composition. The fragrance generated when the fragrance composition is roasted coffee beans is the top fragrance (due to the fragrance compound with low molecular weight and easy to volatilize), so the influence of the type of coffee beans and the degree of roasting of coffee It is estimated that there are few. Therefore, the present invention can be used universally regardless of the type of coffee beans and the degree of roasting.
As the coffee beans used in the production method of the present invention, for example, any of Arabica, Robusta, and Riberica can be used, and any coffee bean can be used regardless of its type and production area. The coffee beans can be roasted in a conventional manner using a coffee roaster or the like. For example, it can be roasted by putting green coffee beans inside a rotating drum and heating the rotating drum from below with a gas burner or the like while rotating and stirring. The roasting degree of roasted coffee beans is usually represented by L value, Italian roast: 16-19, French roast: 19-21, full city roast: 21-23, city roast: 23-25, high roast: 25 to 27, medium roast: about 27 to 29. Shallow roasting is less commonly used in normal drinking. The L value is an index representing the degree of roasted coffee, and is a value obtained by measuring the lightness of the crushed coffee beans with a color difference meter. Black is represented by an L value of 0 and white is represented by an L value of 100. Accordingly, the deeper the roasted coffee beans, the lower the value and the shallower the value, the higher the value.
There are no particular restrictions on the type of coffee beans, the method of roasting coffee beans, and the method of treating roasted coffee beans. For example, the methods described in [0015] to [0027] of JP2013-252112A and [0021] to [0024] of JP2015-149950A can be employed, and the contents of these publications are as follows: Which is incorporated herein by reference.

(Rough roasted coffee beans)
It is preferable that the roasted coffee bean coarsely pulverized product includes the fine powder and the flakes, and the pulverized product of the roasted coffee bean body pulverized to a desired size.
The fines and flakes are preferably removed from the gas containing aroma compounds generated from the roasted coffee beans when the roasted coffee beans are ground. Specifically, it is preferable that the first flow path, which will be described in detail later, passes along with the gas and is removed from the gas by a fine powder flake removing device.

(Aroma compounds generated when grinding roasted coffee beans)
The aromatic compound generated from the roasted coffee beans when the roasted coffee beans are crushed is one or more compounds. Specifically, it is shown in the description of the fragrance composition.

<Preliminary removal step of fine powder and flakes>
In the manufacturing method of this invention, it is preferable to perform the process of removing the fine powder and flakes contained in the roasted coffee bean coarse pulverized product before the process of removing the fine powder and flakes from the gas. Part of the fine powder and flakes may be removed, but substantially all may be removed. Further, for example, fine powders and flakes derived from other than chaff may be mainly removed, and fine powders and flakes derived from chaff may be removed at least partially in this preliminary removal step, and hardly removed. Also good.
The process of removing fine powder and flakes contained in the roasted coffee beans coarsely pulverized product can be performed using a known fine powder flake remover such as a vibration sieve or a classifier such as an air classifier. The classifier used is preferable. For example, a fine particle and flakes smaller than the opening can be removed using a sieve having an arbitrary opening.

<Process for removing fine powder and flakes>
The production method of the present invention includes a step of removing fine powder and flakes from a gas containing aromatic compounds and fine powder and flakes generated from roast coffee beans when the roasted coffee beans are pulverized. Although some of the fine powder and flakes may remain without being removed, it is preferable that substantially all of the fine powder and flakes are removed. The fine powder and flakes removed in this removal step may occupy at least half of the fine powder and flakes derived from chaff, or may consist essentially of fine powder and flakes derived from chaff.
There is no restriction | limiting in particular as a process of removing a fine powder and a flake, A well-known method can be used.
In the manufacturing method of this invention, it is preferable to perform the process of removing a fine powder and a thin piece with the fine powder thin piece removal apparatus mentioned later.
The details of the fine powder flake removing device are shown in the description of the aroma recovery device of the present invention.

<Adsorption process>
The production method of the present invention includes an adsorption step in which the gas from which fine powder and flakes have been removed is passed through the adsorbent, and the aromatic compound contained in the gas is adsorbed on the adsorbent. Here, the adsorbent is accommodated in an adsorbent accommodating portion provided in the aromatic compound adsorbing device, and this adsorbent accommodating portion has mesh lids at both ends in the gas aeration direction.
The amount of adsorbent is not limited as long as it is an amount that can be accommodated in the adsorbent accommodating portion. The volume (bulk volume) of the adsorbent to be used may be the same as or smaller than the volume of the adsorbent accommodating portion. In other words, the adsorbent may be filled (roughly packed or densely packed) in the adsorbent container, or a space may exist in the adsorbent container that contains the adsorbent.
The gas ventilation direction may be at an arbitrary angle with respect to the installation surface of the fragrance collection device (or the ground contact surface when the fragrance collection device is installed on the ground), and may be parallel or vertical, for example. Moreover, the direction which approaches the installation surface of a fragrance | flavor collection | recovery apparatus, or the direction away from it may be sufficient. In other words, the gas ventilation direction of the adsorbent may be substantially opposite to or substantially the same as the direction of gravity, may be a right angle, or may have another angle. In addition, when the gas is allowed to flow into and flow through the adsorbent in a direction substantially opposite to the direction of gravity, the volume of adsorbent to be used (bulk volume) is made smaller than the volume of the adsorbent accommodating portion, so that the aromatic compound adsorbing device is a so-called fluidized bed. It can be a column, and the resistance of the adsorbent to the flow of gas to be vented can be suppressed.
In the production method of the present invention, it is preferable to generate an air flow using an air flow generation device and to vent the gas from which fine powder and flakes have been removed to the adsorbent. Further, the flow velocity adjusting device may be used in combination with the air flow generating device to increase the gas flow velocity and pressure. By this combination, gas can be vented beyond the resistance of the adsorbent to the gas flow.
The details of the airflow generation device and the flow rate adjustment device are shown in the description of the aroma recovery device of the present invention.

In the production method of the present invention, by providing an introduction path in which the adsorbent is arranged so as to branch from the flow path of the gas from which fine powder and flakes have been removed, one of the gases from which fine powder and flakes have been removed in the introduction path. It is preferable that only the part is allowed to flow in and pass, and the gas is passed through the adsorbent to recover the aroma compound.
The details of the introduction path are shown in the description of the aroma recovery device of the present invention.

(Adsorbent)
The adsorbent is not particularly limited. As the adsorbent, a synthetic adsorbent or other adsorbent such as activated carbon can be used. It is preferable to use a synthetic adsorbent from the viewpoint of easy desorption.
Adsorbent is selected from styrene divinyl benzene copolymer, ethyl vinyl benzene and divinyl benzene copolymer, 2,6-diphenyl-9-phenyl oxide polymer, polycondensation polymer of methacrylic acid and diol, and modified silica gel It is preferable that it is 1 or more. The modified silica gel refers to a chemically bonded silica gel in which, for example, alcohols, amines, silanes, and the like are chemically bonded to the silica gel surface using the reactivity of silanol groups. Among these, styrene divinylbenzene copolymer is preferable.
The adsorbent is preferably a porous polymer resin. For example, the surface area of the adsorbent is preferably about 300 m ² / g or more, and more preferably about 500 m ² / g or more. It is preferred that the pore distribution of the adsorbent is about 10 to about 500 cm.
The shape of the adsorbent is not particularly limited, but is preferably particulate. There is no restriction | limiting in particular in the average particle diameter in case an adsorbent is particulate form, Although it can illustrate in the range of 0.1-20 mm or 0.1-1 mm, It is not limited to these.
Examples of the porous polymer resin corresponding to the above conditions include HP resin (manufactured by Mitsubishi Chemical Corporation), SP resin (manufactured by Mitsubishi Chemical Corporation) which is a styrene divinylbenzene copolymer, and XAD-4 (ROHM).・ Manufactured by Lotus, etc., and can be easily obtained in the market. In addition, methacrylic ester resins can also be obtained as products such as XAD-7 and XAD-8 (Rohm Haas).
As SP resin, Sepa beads SP-70 and SP-207 can be preferably used.

Either a batch system or a column system can be adopted as a processing means for allowing the gas from which fine powder and flakes have been removed to pass through the adsorbent to adsorb the aromatic compound to the adsorbent. From the viewpoint of workability, the column method can be preferably employed. As a method of adsorbing by a column method, for example, an aromatic compound can be adsorbed by introducing a gas into a column filled with the above adsorbent. The inflow and ventilation directions of the gas to the adsorbent can be any direction with respect to the direction of gravity, and examples thereof include substantially the same direction and substantially the opposite direction with respect to the direction of gravity, but are not limited thereto.
Alternatively, a fluidized bed column may be obtained by adjusting the particle size and amount of the adsorbent so that a space is formed in the adsorbent accommodating portion, and further performing gas inflow and aeration in a direction substantially opposite to the direction of gravity.

  In order to suppress cracking, the adsorbent is preferably accommodated in the aromatic compound adsorbing device after absorbing pure water and before completely drying.

  There is no restriction | limiting in particular as an air flow rate at the time of ventilating the gas from which the fine powder and the flakes were removed, For example, it is preferable that it is 0.1 to 1000 times the air flow rate of an adsorbent.

The flow rate of the gas flowing into the adsorbent (the speed of the aeration gas) may be appropriately set according to the amount of the adsorbent, the length of the adsorbent portion in the gas aeration direction, and the performance of the airflow generation device and the flow rate adjustment device described later, There is no particular limitation. For example, the flow rate (aeration rate) of the gas flowing into the adsorbent is preferably 0.1 to 10.0 L / min, more preferably 0.5 to 7.0 L / min, and 1.0 -5.0 L / min is particularly preferable.
In addition, the gas aeration time to the pulverization and the adsorbent can be set in a preferable range from the aeration amount when the gas from which fine powder and flakes have been removed is aerated and the flow rate of the gas flowing into the adsorbent.

  In the production method of the present invention, the flow velocity (linear velocity) of the gas flowing into the adsorbent is the amount of the adsorbent, the length of the adsorbent portion in the gas flow direction, the inner diameter of the second flow path, which will be described later, and the air flow generator. And may be set as appropriate depending on the performance of the flow rate adjusting device, and there is no particular limitation. For example, it is preferably within a range of 1.0 to 35.0 m / s, more preferably within a range of 2.0 to 20.0 m / s, and a range of 3.0 to 10.0 m / s. It is particularly preferred that

<Process for adjusting the linear velocity of gas>
The manufacturing method of the present invention includes the step of adjusting the linear velocity of the gas flowing into the adsorbent, so that the adsorbent resistance can be reduced even when a large amount of adsorbent is accommodated (for example, filled) in the aromatic compound adsorbing device. It is preferable from the viewpoint that it is possible to perform adsorption more than that, and the burden on the airflow generator described later can be suppressed.
In the production method of the present invention, the linear velocity of the gas flowing into the adsorbent can be adjusted using any known airflow generator, such as a suction pump or a blower.
For example, the linear velocity of the gas flowing into the adsorbent may be an arbitrary ratio with respect to the linear velocity of the gas flowing in the second flow path, and the upper limit is 100%, 90% or more, 80% or more, 70% or more 60% or more, 50% or more, 40% or more, 30% or more, 20% or more, 10% or more, 5% or more, or 1% or more. Specifically, the ranges of 0.05 to 35 m / s, 0.08 to 20 m / s, 1.0 to 10 m / s, 1.0 to 5 m / s, and 1.0 to 2 m / s are exemplified. However, it is not limited to these.
For example, it is preferable to adjust the ratio of the linear velocity of the gas flowing into the adsorbent with respect to the linear velocity of the gas flowing in the second flow path in accordance with the performance of the airflow generation device described later. By such adjustment, the burden on the airflow generation device can be suppressed.

<Recovery process>
The production method of the present invention includes a recovery step of recovering a fragrance compound from an adsorbent and preparing a fragrance composition containing the fragrance compound.
In the production method of the present invention, it is preferable to recover by removing the aromatic compound from the adsorbent using an organic solvent in the recovery step.
The adsorbent may be washed with water before desorbing the aromatic compound from the adsorbent using an organic solvent.
Examples of the organic solvent include alcohols and fats and oils.

The alcohol used in the recovery step is not particularly limited, and is preferably ethanol or propylene glycol, and more preferably propylene glycol from the viewpoint of safety (difficult to ignite). Without being bound by any theory, propylene glycol can acetalize (PG acetalization) a part of the recovered aroma compound, and as a result, it can be expected to enhance the fragrance expression of the aroma compound.
A 50 to 100% by weight alcohol aqueous solution may be used. In the case of ethanol, it is preferable to use hydrous ethanol having an ethanol concentration of 50 to 95% by weight, and in the case of PG, 100% PG is preferably used.
When a column is used, the flow rate for passing alcohols is preferably a flow rate of SV = 0.1-20.
There is no restriction | limiting in particular as the quantity of alcohol, It is preferable that it is the liquid flow volume of 1 times-100 times of adsorption agent, It is more preferable that it is the liquid flow volume of 3 times-40 times, 5 times-20 times It is particularly preferable that the liquid flow rate is.
A water-soluble fragrance composition (fragrance concentrate) can be obtained by eluting the fragrance compound adsorbed on the adsorbent with alcohols.

  The fats and oils used for desorption are not particularly limited. For example, vegetable oils such as soybean oil, rice oil, sesame oil, peanut oil, corn oil, rapeseed oil, coconut oil, palm oil, and hardened oils thereof; beef fat, lard , Animal oils and fats such as fish oil, and hardened oils thereof; medium chain fatty acid triglycerides (hereinafter sometimes referred to as MCT), and the like. MCT is preferably exemplified in terms of the stability of the obtained fragrance composition. be able to. Examples of the MCT include triglycerides of medium chain fatty acids having 6 to 12 carbon atoms such as caproic acid triglyceride, caprylic acid triglyceride, capric acid triglyceride, lauric acid triglyceride and any mixture thereof. In particular, caprylic acid triglyceride and capric acid triglyceride and any mixture thereof can be preferably mentioned. These MCT mixtures are easily and inexpensively available on the market.

  The amount of fats and oils used varies depending on the type of raw material and the concentration of aroma components in the gas. Desorption can be performed in a stationary state, and the desorption temperature and desorption time can be appropriately selected. For example, the temperature range of 10 to 80 ° C. can be exemplified for 5 minutes to 2 hours. After desorption, the obtained desorption liquid is allowed to stand, and the oil layer portion and the water layer portion can be separated by a commonly used separation method such as decantation or centrifugation. By adding and extracting oils and fats to the water layer part, the aroma component can be efficiently recovered. The obtained oil layer part can be dehydrated with a dehydrating agent such as anhydrous sodium sulfate, for example, and can be made into an oil-soluble fragrance composition by a clear filtration means such as filtration with filter paper.

<Reuse and cleaning of adsorbent>
Compare the pressure of the adsorbent before and after desorption with an organic solvent, and if the pressure is the same (for example, 2 times or less), clogging is not occurring or negligible, and cleaning is performed. It can be judged that it can be reused without. The method for managing the fragrance recovery apparatus may include a step of comparing the adsorbent before and after desorption with an organic solvent and confirming that the pressure is equal by comparing the pressure of the solution. Specifically, after desorption and after desorption, after the replacement with ultrapure water, after measuring the pressure when flowing ultrapure water at about SV = 10, after desorption relative to the pressure before desorption It is preferable to calculate the pressure.
On the other hand, the production method of the present invention may include an adsorbent cleaning step. That is, the method for managing the fragrance recovery device may include an adsorbent cleaning step. In the production method of the present invention, fine powder and flakes are hardly adsorbed by the adsorbent, but other components (particularly polymerizable components) contained in the gas may be adsorbed by the adsorbent. A method for cleaning the adsorbent is known to those skilled in the art, and it is sufficient to pass several kinds of solvents having different polarities in succession. There is no particular limitation on the kind of the solvent. After passing through and desorbing, ethyl acetate and hexane are passed in order and washed, and when regenerating, ethyl acetate and water are passed in order.
The adsorbent is preferably reused until the adsorption and recovery are repeated 5 times or more, more preferably 10 times, while washing is performed after the aromatic compound is recovered as necessary.

<Confirmation process>
The production method of the present invention preferably includes a step of confirming that the fragrance composition satisfies the following conditions.
Retention in total ion chromatogram obtained by electron impact ionization method (EI mode) at 70 eV using a polar column using a gas chromatograph mass spectrometer (GC / MS) equipped with a quadrupole mass spectrometer The ratio of the total area of all peaks with an index of acetoin or less to the total area of all peaks with a retention index greater than acetoin is 30.0: 70.0 to 100: 0.
Furthermore, it is more preferable that the production method of the present invention includes a step of confirming that the fragrance compound satisfies a preferable range of the composition of the fragrance composition described below.
The kind of polar column is not particularly limited, and any available polar column can be used. Examples include, but are not limited to, InertCap-WAX series polar columns (manufactured by GL Sciences), such as InertCap-WAX.

[Perfume composition]
The fragrance composition produced by the production method of the present invention contains a fragrance compound generated when pulverizing roasted coffee beans, and makes the fragrance generated when pulverizing roasted coffee beans feel.
As the aroma generated when the roasted coffee beans are crushed, specifically, the aroma when the roasted coffee beans are ground is preferable, the aroma that is felt at the top is preferably strong, and the middle and later It is preferable that there is also a volume and a reverberation.

The fragrance composition is a total ion obtained by electron impact ionization (EI mode) at 70 eV using a polar column using a gas chromatograph mass spectrometer (GC / MS) equipped with a quadrupole mass spectrometer. In the chromatogram, the ratio of the total area of all peaks with a retention index below acetoin to the total area of all peaks with a retention index greater than acetoin is, for example, 100: 0 or 30.0: 70.0 to 99.9: 0.1, 40:60 to 99.5: 0.5, 50.0: 50.0 to 98.0: 2.0, 70.0: 30.0 to 97.0: 3. 0, 80.0: 20.0-95.0: 5.0, 85.0: 15.0-94.0: 6.0. Preferred ranges are 80.0: 20.0 to 99.9: 0.1, 85.0: 15.0 to 99.8: 0.2, 87.0: 13.0 to 99.5: 0. 5 and the like, but are not limited thereto. The total area of all peaks having a retention index of acetoin or less is preferably larger than the total area of all peaks having a retention index greater than acetoin, more than 1 time, 2 times or more, 3 times or more, 4 times or more, 5 Times more, 7 times or more, 8 times or more, 10 times or more, 12 times or more, 15 times or more, 20 times or more, 25 times or more, 30 times or more, 35 times or more, 40 times or more, 45 times or more, or 50 times That's all.
In the present specification, the calculation of the peak area value of the total ion chromatogram of the fragrance composition is obtained by excluding the peak attributed to the solvent of the fragrance composition (the solvent used in the recovery step). . For example, when the solvent used in the recovery step is propylene glycol, the calculation of the peak area value of the total ion chromatogram is obtained by excluding the peak attributed to propylene glycol.

In the total ion chromatogram, examples of compounds belonging to all peaks having a retention index of acetoin or lower are listed in order of increasing retention index including acetoin.
2-methylfuran;
2-methylbutyraldehyde:
isovaleraldehyde;
2-methylbutyraldehyde PG acetate;
isovaleraldehyde PG acetal;
acetoin (RI = 1294).

In the total ion chromatogram, examples of compounds belonging to all peaks having a retention index larger than acetoin are listed in ascending order of the retention index.
acetol (RI = 1321);
furfural;
2-acetyfuran;
furfuryl acetate.

In the perfume composition obtained by the production method of the present invention, in the total ion chromatogram, the ratio of the peak areas of 2-methylfuran, 2-methylbutyraldehyde and isovaleraldehyde is other than the total area of all peaks having a retention index of acetoin or less. It is preferable that it is characterized by being higher than the fragrance composition. The proportions are 0.1-5.0%, 5-25% and 5-25%; 0.2-4.0%, 7-20% and 7-20%; 0.2-2.0, respectively. %, 10-18% and 10-18%; or 0.3-0.7%, 11-16% and 11-16%.
It is preferable that the fragrance composition further contains 2-methylfuran PG acetal, 2-methylbutyraldehyde PG acetal and isovalardehydrate PG acetal from the viewpoint of enhancing the fragrance expression of the fragrance composition.

[Use of perfume composition produced by the production method of the present invention]
The fragrance composition produced by the method for producing the fragrance composition of the present invention can be added to various types of base materials such as foods and drinks, cosmetics, hygiene products, and pharmaceuticals to obtain a fragrance product. The fragrance composition produced by the method for producing a fragrance composition of the present invention is preferably used for a substrate exhibiting a coffee-like fragrance, and more preferably added to a food or drink exhibiting a coffee-like fragrance.

  The food / beverage product is preferably a product obtained by adding 0.01 to 10% by mass of the fragrance composition produced by the method for producing a fragrance composition of the present invention to the total mass of the food / beverage product. It is more preferable that 7% by mass is added.

The food or drink is preferably a container-packed food or drink, and more preferably a container-packed drink. Moreover, the fragrance composition manufactured with the manufacturing method of the fragrance | flavor composition of this invention has a strong fragrance of a top (component of low molecular weight). Therefore, the container-packed drink containing the fragrance composition produced by the production method of the present invention can strongly feel the aroma generated when the roasted coffee beans are crushed when the container is opened.
Examples of the packaged food include frozen confectionery such as ice cream, soft cream or sherbet; biscuits, cookies, rice crackers, buns, chocolate, cream-containing confectionery, bread and the like.
The container-packed beverage means a beverage (generally sterilized before or after filling into a container) obtained by filling the container with a concentration suitable for drinking.
The packaged beverage is preferably a packaged beverage filled in a PET bottle, can or paper container. Container-packed beverages include barley tea drinks, grain tea drinks, brown rice tea drinks, tea-based drinks such as so-called mixed tea drinks (blended tea drinks) that are a mixture of tea and roasted grains, green tea drinks, oolong tea drinks, Tea-based beverages such as tea beverages; coffee beverages; beer, sparkling liquor, so-called third beer, beer-flavored beverages such as non-alcohol beer-flavored beverages, and the like are included. Among these, it is preferable to be used for coffee.
There is no restriction | limiting in particular as an aspect of the coffee used as a base material. For example, the coffee described in JP-A-2013-252112 [0028] to [0039] and JP-A-2015-149950 [0037] to [0042] can be employed. Which is incorporated herein by reference.

The preferable aspect of the aroma product (food-drinks) before heat sterilization using coffee as a base material is demonstrated.
Using a gas chromatograph mass spectrometer (GC / MS) equipped with a quadrupole mass spectrometer, using a polar column, the food / beverage product before heat sterilization obtained by the electron impact ionization method (EI mode) at 70 eV In the total ion chromatogram, when the total area of all peaks where the retention index of the base material (sugar-free black coffee) before heat sterilization is acetoin is 100%, the food / beverage products (flavored product) before heat sterilization The total area of all peaks having a retention index of acetoin or less is preferably more than 100%, more preferably 102% or more, further preferably 103% or more, and more preferably 105% or more. Preferably, it is 107% or more, more preferably 110% or more, 11 More preferably at least% or, more preferably 120% or more, and particularly preferably 130% or more.
In the total ion chromatogram, when the 2-methylfuran peak area of the base material (sugar-free black coffee) before heat sterilization is 100%, the 2-methylfuran peak of the food and drink (scented product) before heat sterilization The area is preferably more than 100%, more preferably 105% or more, further preferably 110% or more, further preferably 115% or more, and further preferably 120% or more. Preferably, it is more preferably 125% or more, and particularly preferably 130% or more.
In the total ion chromatogram, when the 2-methylbutarydehyde peak area of the base material (sugar-free black coffee) before heat sterilization is 100%, the 2-methylbutyraldehyde peak of the food / beverage product (flavored product) before heat sterilization The area is preferably more than 100%, more preferably 105% or more, further preferably 110% or more, further preferably 115% or more, and further preferably 120% or more. Preferably, it is more preferably 125% or more, and particularly preferably 130% or more.
In the total ion chromatogram, when the peak area of the isovalardehyde of the base material (sugar-free black coffee) before heat sterilization is 100%, the peak area of the isovaleraldehyde of the food / beverage product (flavored product) before heat sterilization is 100%. %, More preferably 105% or more, still more preferably 110% or more, still more preferably 115% or more, still more preferably 120% or more, 125% More preferably, it is more preferably 130% or more.

  The food and drink may be heat sterilized. In the manufacture of packaged beverages and the like, retort sterilization (heat sterilization at 121 ° C. for about 10 minutes) and UHT sterilization (heat sterilization at 135 ° C. for about 1 minute) are performed. However, the usual top fragrance is easily lost by heating. Since the fragrance composition produced by the method for producing the fragrance composition of the present invention has a strong scent at the top, the fragrance at the top is not easily lost even when heated, and is preferably used for heat-sterilized food and drink. Therefore, it is also preferably used in foods and drinks that require heating before eating.

The preferable aspect of the food-drinks after heat sterilization using coffee as a base material is demonstrated.
Using a gas chromatograph mass spectrometer (GC / MS) equipped with a quadrupole mass spectrometer, using a polar column, the food / beverage product after heat sterilization obtained by the electron impact ionization method (EI mode) at 70 eV In the total ion chromatogram, when the total area of all peaks where the retention index of the base material (sugar-free black coffee) after heat sterilization is 100% or less of acetoin is 100%, The total area of all peaks having a retention index of acetoin or less is preferably more than 100%, more preferably 102% or more, further preferably 103% or more, and more preferably 105% or more. Preferably, it is 107% or more, more preferably 110% or more, 11 More preferably at least% or, more preferably 120% or more, and particularly preferably 130% or more.
In the total ion chromatogram, when the 2-methylfuran peak area of the base material (sugar-free black coffee) after heat sterilization is defined as 100%, the 2-methylfuran peak of the food / beverage product (flavored product) after heat sterilization The area is preferably more than 100%, more preferably 105% or more, further preferably 110% or more, further preferably 115% or more, and further preferably 120% or more. Preferably, it is more preferably 125% or more, and particularly preferably 130% or more.
In the total ion chromatogram, when the 2-methylbutarydehyde peak area of the base material (sugar-free black coffee) after heat sterilization is defined as 100%, the 2-methylbutarydehyde peak of the food / beverage product (flavored product) after heat sterilization The area is preferably more than 100%, more preferably 105% or more, further preferably 110% or more, further preferably 115% or more, and further preferably 120% or more. Preferably, it is more preferably 125% or more, and particularly preferably 130% or more.
In the total ion chromatogram, when the peak area of the isovalardehyde of the base material (sugar-free black coffee) after heat sterilization is 100%, the peak area of the isovaleraldehyde of the food and drink (scented product) after heat sterilization is 100. %, More preferably 105% or more, still more preferably 110% or more, still more preferably 115% or more, still more preferably 120% or more, 125% More preferably, it is more preferably 130% or more.

[Aroma recovery device from roasted coffee beans]
An apparatus for recovering fragrance from roasted coffee beans of the present invention (also referred to as fragrance recovery apparatus of the present invention) includes a pulverizer for roasted coffee beans,
A first flow path in communication with the pulverizer, through which a gas containing aroma compounds and fine powder and flakes generated from the roasted coffee beans when the roasted coffee beans are crushed;
A fine powder flake removal device that communicates with the first flow path to remove fine powder and flakes;
A second flow path that communicates with the fine powder flake removal device and allows the gas from which fine powder and flakes have been removed to pass through;
An aroma compound adsorption device in communication with the second flow path;
An airflow generator for generating a continuous airflow from the pulverizer to the aroma compound adsorption device;
The fragrance compound adsorbing device has an adsorbent accommodating portion in which an adsorbent is accommodated, and the adsorbent accommodating portion has mesh lids at both ends in the gas aeration direction.
Hereinafter, the preferable aspect of the fragrance | flavor collection apparatus of this invention is demonstrated.

<Overall configuration of fragrance collection device>
The overall configuration of the aroma recovery device will be described with reference to the drawings. FIG. 1 is a schematic view showing an example of an aroma recovery device of the present invention. FIG. 2 is a schematic view showing another example of the aroma recovery device of the present invention.
An example of the aroma recovery device of FIG. 1 includes a crushing device 11, a first flow channel 1, an airflow generation device 13, a fine powder flake removal device 14, a second flow channel 2, and an aroma compound adsorption device K. The aroma compound adsorption device K has an adsorbent accommodating portion Kb having mesh lids Ka1 and Ka2 (FIG. 3). Furthermore, although the example of the fragrance | flavor collection | recovery apparatus of FIG. 1 is provided with the introduction path 3 and the linear velocity adjustment apparatus 4, these are not essential structures.
1, the pulverizer having the pulverizer 11, the first channel 1, the air flow generator 13, the fine powder flake remover 14, and the second channel 2 is generally used. (See, for example, U.S. Pat. No. 1,649,781 (1927)), the present invention is provided with an aroma compound adsorbing device K in a general pulverizing apparatus having such a configuration, and the roasted coffee beans are crushed at the time of pulverizing the roasted coffee beans. The aromatic compound generated can be collected.
1, the roasted coffee beans are pulverized by the pulverizer 11 and the roasted coffee bean coarsely pulverized product is produced, so that the pulverizer 11 uses the airflow generated by the airflow generator 13. Thus, the gas containing the aroma compound 21 generated from the roasted coffee beans and the fine powder and flakes 22 contained in the roasted coffee bean coarsely pulverized product moves to the first flow path 1. The gas containing the aroma compound 21 and the fine powder and the flakes 22 is moved from the first flow path 1 to the fine flake flake removing device 14 along the airflow. In the fine powder flake removal device 14, the gas from which the fine powder and flakes have been removed (including the aroma compound 21) is removed to the second flow path 2, and the fine powder and flakes 22 are removed by the fine powder flake removal device 14 and out of the device. , Each moved. The gas from which the fine powder and flakes have been removed from the second flow path 2 by the air flow generated by the air flow generation device 13 (and the air flow generated by the linear velocity adjusting device 4 if necessary) Part) flows into the introduction path 3, flows into the adsorbent accommodated in the aroma compound adsorbing device K arranged in the introduction path 3, and the gas is vented to the adsorbent, and the adsorption The aroma compound 21 is adsorbed on the agent. The gas that has adsorbed the aroma compound 21 and passed through the adsorbent is moved again from the outlet 3B of the introduction path to the second flow path 2 and does not flow into the introduction path 3 but passes through the second flow path 2. And the gas from which the flakes have been removed merges and is discharged out of the apparatus as exhaust gas 24.
In the present invention, since the introduction path 3 is not an essential configuration as described above, the gas that flows through the second flow path without providing the introduction path 3 (including the aroma compound 21 and fine powder and flakes are removed). You may use not all but one part for inflow to aroma compound adsorption | suction apparatus K, and ventilation | gas_flowing. In that case, the aromatic compound adsorption device K may be disposed in the second flow path.

Other examples of the fragrance recovery device of FIG. 2 include a pulverizer 11, a fine powder preliminarily removing device 12, a first flow path 1, an airflow generating device 13, a fine powder thin piece removing device 14, a second flow path 2, and an aroma. A compound adsorption device K is provided. Furthermore, although an example of the fragrance | flavor collection | recovery apparatus of FIG. 2 is provided with the introduction path 3 and the linear velocity adjustment apparatus 4, these are not essential structures.
2, the roasted coffee beans coarsely pulverized product produced by pulverizing roasted coffee beans by the pulverizing device 11 moves to the fine powder flake preliminary removing device 12 by a transport mechanism (not shown). The fine powder flake pre-removal device 12 removes at least part of the fine powder and flakes 22 from the roasted coffee bean coarsely pulverized product, accommodates the fine powder and flakes 22 removed in a waste unit (not shown), and discharges them outside the device. . On the other hand, the gas containing fine powder and flakes 22 that have not been removed by the fragrance compound 21 and the fine powder flake preliminary removal device 12 is moved to the first flow path 1 by the air flow generated by the air flow generator 13. The flow of the aroma compound 21 and the fine powder and the flakes 22 after the first channel 1 is the same as that in FIG.
Hereinafter, each preferable aspect is demonstrated about each apparatus with which an fragrance | flavor collection apparatus is preferable.

<Crushing device>
The aroma recovery device of the present invention includes a roasted coffee bean crusher.
There is no restriction | limiting in particular as a grinder. For example, a roller mill can be used.
The gas generated by the pulverization in the pulverizer 11 is carried to the adsorbent by the airflow generated by the airflow generator, so that it is difficult to diverge, and the pulverizer does not necessarily need to be sealed. However, from the viewpoint of recovering the aroma compound more efficiently, the pulverization apparatus 11 may communicate with the first flow path 1 and pulverize with the other portions sealed.

<Fine powder pre-removal device>
The aroma recovery device of the present invention preferably further includes a fine powder flake preliminary removal device between the crushing device and the first flow path.
It is preferable that the fine powder flake preliminary removing device communicates with the grinder and removes at least a part of the fine powder and flakes from the coarsely pulverized roasted coffee beans obtained by crushing roasted coffee beans. In addition, the roasted coffee bean refined pulverized product from which fine powder and flakes have been removed (that is, the pulverized product of roasted coffee bean main body pulverized to a desired size) can be used for foods and drinks or the production thereof.
Part or most of the fines and flakes may be removed and discharged out of the device. The smaller the amount of fine powder and flakes moving from the fine powder flake preliminary removal device to the first flow path, the more the load on the downstream fine powder flake removal device can be reduced.
As the fine powder preliminarily removing device, a known device can be used, and it is preferable to use a classifier such as a vibration sieve or an air classifier.

<First channel>
The aroma recovery device of the present invention includes a first flow path that communicates with a crushing device and through which a gas containing aroma compounds and fine powder and flakes generated from roasted coffee beans when roasted coffee beans are crushed.
The first flow path may be in direct communication with the pulverizing device, or may be in communication with the pulverizing device via the fine powder flake preliminary removal device.
The diameter (inner diameter) of the first flow path is not particularly limited, but is preferably 30 mm or more from the viewpoint of allowing more gas to pass, more preferably 50 mm or more, and even more preferably 100 mm or more. , 200 mm or more is more preferable, and 300 mm or more is particularly preferable.
The fine powder flake preliminary removal device 12 may include a suction port for connection to the first flow path 1.

<Fine powder removal device>
The aroma recovery device of the present invention includes a fine powder flake removal device that communicates with the first flow path and removes fine powder and flakes.
As the fine powder flake removal device, a known device can be used, and it is preferable to use a cyclone type separation device (powder separation device).

<Second channel>
The fragrance recovery device of the present invention includes a second flow path that communicates with the fine powder flake removal device and through which the gas from which fine powder and flakes have been removed can pass.
In the fragrance recovery device of the present invention, the diameter (inner diameter) of the second flow path is not particularly limited, but is preferably 30 mm or more from the viewpoint of passing more gas, more preferably 50 mm or more, More preferably, it is 100 mm or more, more preferably 200 mm or more, and particularly preferably 300 mm or more. The second flow path can be arbitrarily arranged so that the direction of the gas flowing into the aromatic compound adsorbing device described later becomes a desired one.

<Aroma compound adsorption device>
The aroma recovery device of the present invention includes an aroma compound adsorption device that communicates with the second flow path.
The fragrance compound adsorbing device has an adsorbent accommodating portion in which an adsorbent is accommodated, and the adsorbent accommodating portion has net-like lids at both ends in the gas aeration direction. With this mesh lid, the adsorbent accommodated in the adsorbent accommodating portion can be prevented from leaking out of the aromatic compound adsorbing device, and gas can be passed through the adsorbent.
The mesh lid is in the form of a sheet having an arbitrary thickness, and the size thereof is not particularly limited, and can be arbitrarily selected as long as leakage of the adsorbent from the aromatic compound adsorption device can be prevented. From the viewpoint of ease of gas passage, the adsorbent accommodating portion preferably has an area equal to or larger than the cross-sectional area in the gas ventilation direction.
The net-like lid may be net-like or partly net-like. From the viewpoint of easy gas passage, it is preferable that the portion corresponding to the cross section of the aromatic compound adsorbing device or the adsorbent accommodating portion is net-like.
The mesh opening of the mesh lid can be arbitrarily selected as long as the adsorbent used does not pass through. Although it can illustrate within the range of 10 micrometers-20 mm, it is not limited to this.
In the present invention, the aromatic compound adsorbing device preferably includes a portion occupied by the adsorbent accommodated in the adsorbent accommodating portion, that is, an adsorbent portion.
In the present invention, the length of the adsorbent portion (gas aeration direction) is not particularly limited, but is preferably 1000 mm or less, more preferably 700 mm or less, and more preferably 500 mm from the viewpoint of reducing the resistance of the adsorbent. Or less, more preferably 400 mm or less, further preferably 300 mm or less, and particularly preferably 200 mm or less. For example, the length of the adsorbent portion may be in the range of 10 mm to 800 mm, 20 mm to 400 mm, 40 mm to 200 mm, or 50 mm to 100 mm.
The major axis or diameter of the surface of the adsorbent portion perpendicular to the gas flow direction (hereinafter generally referred to as the cross-sectional diameter) is not particularly limited, but is controlled according to the amount of adsorbent and the length of the adsorbent portion. It is preferable. The cross-sectional diameter of the adsorbent portion is preferably 10 mm or more, more preferably 30 mm or more, further preferably 50 mm or more, and more preferably 100 mm or more from the viewpoint of easy gas passage. More preferably, it is more preferably 200 mm or more, and particularly preferably 300 mm or more.
In order to increase the amount of adsorbent, it is preferable to increase the cross-sectional diameter of the adsorbent part to suppress the length of the adsorbent part (gas aeration direction) from the viewpoint of suppressing the resistance of the adsorbent to the flow of gas to be vented. .
The amount of adsorbent is not limited as long as it is an amount that can be accommodated in the adsorbent accommodating portion. The bulk volume of the adsorbent to be used may be the same as or smaller than the volume of the adsorbent accommodating portion. In other words, the adsorbent may be filled (roughly packed or densely packed) in the adsorbent accommodating portion, or a space may exist in the adsorbent accommodating portion in which the adsorbent is accommodated.
As for the arrangement of the aroma compound adsorption device, in FIGS. 1 and 2, the aroma compound adsorption device is provided so as to be parallel to the installation surface of the aroma recovery device (parallel to the grounding surface, that is, horizontal). They may be perpendicular to each other or provided at other angles. Further, the gas inflow and ventilation directions may be designed so as to be close to the installation surface of the fragrance recovery apparatus, or may be designed to be away from the installation surface. In other words, the inflow and the aeration direction of the gas to the aroma compound adsorbing device and the adsorbent are substantially opposite to the direction of gravity, substantially the same direction, or at right angles, but at other angles. Also good.
When the aromatic compound adsorbing device is a fluidized bed column, the volume of the adsorbent to be used should be less than the volume of the adsorbent accommodating portion, and gas should be allowed to flow in and through the adsorbent in a direction substantially opposite to the direction of gravity. Good. If the fluidized bed column is used, the resistance of the adsorbent to the gas flow to be vented can be suppressed.

  The aroma compound adsorption device may include a basket as an adsorbent accommodating portion. As the basket, there are known a normal type basket having holes in the side surface and a side wall type basket having no holes in the side surface. It is preferable to use a side wall type basket having no holes in the side surface from the viewpoint that the adsorbent passage distance of the gas to be vented can be increased without escape of the gas from which fine powder and flakes have been removed from the side surface.

<Airflow generator>
The fragrance recovery device of the present invention includes an airflow generation device that generates a continuous airflow from the pulverizer to the fragrance compound adsorption device. By this air flow generation device 13, the air flow continuous to the pulverization device 11, (fine powder flake preliminary removal device 12), first flow channel 1, fine powder flake removal device 14, second flow channel 2, and aroma compound adsorption device K Can be generated.
The airflow generation device may be a blower device or a suction device. An example of the suction device is a suction blower.

<Introduction path>
The fragrance recovery apparatus includes an introduction path 3 that branches from the flow path and communicates with the fragrance compound adsorption apparatus in the gas flow path (second flow path) from which fine powder and flakes have been removed. Further, it is preferable from the viewpoint of suppressing the resistance caused by the adsorbent by aeration of only a part of the gas from which fine powder and flakes have been removed through the adsorbent to recover the aroma compound. Thus, the aromatic compound adsorption device may communicate with the second flow path via the introduction path.
The diameter (inner diameter) of the introduction path is not particularly limited, but the inner diameter is preferably 5 mm or more from the viewpoint of allowing more gas to pass, more preferably 15 mm or more, and more preferably 30 mm or more. It is further preferably 50 mm or more, more preferably 70 mm or more, further preferably 100 mm or more, further preferably 150 mm or more, further preferably 200 mm or more, and 300 mm or more. Is particularly preferred.
The introduction path 3 may be formed integrally with the second flow path or may be detachably connected to the second flow path, and at least a part of the introduction path 3 is the second flow path. You may fix to the path 2 by arbitrary fixing means, such as an adhesive tape and a screw.
The inlet 3 </ b> A of the introduction path 3 may be branched from any position of the second flow path 2. For example, in FIG. 1, the second flow path 2 is provided at a position extending horizontally (left and right in the drawing), but the second extending from the air flow generation device 13 vertically upward (upward on the drawing). You may provide in the flow path 2.
The outlet 3B of the introduction path 3 is preferably connected to the second flow path 2 so that the gas after adsorbing the aromatic compound can be returned to the second flow path 2.
Further, the inlet 3A and the outlet 3B of the introduction path 3 may be connected to the second flow path 2 at any angle, and the introduction path 3 is bent at one or more locations, whether linear or curved. Also good.
Moreover, the material of the introduction path 3 is not limited, For example, you may be metal or resin.

<Linear speed adjustment device>
The aroma recovery device of the present invention preferably further includes a linear velocity adjusting device 4 that adjusts the linear velocity of the gas from which fine powder and flakes have been removed.
The linear velocity adjusting device may be a blower or a suction device. A blower and a suction pump can be cited as examples.
The position of the linear velocity adjusting device in the fragrance recovery device of the present invention is not particularly limited, and may be either upstream or downstream of the flow of gas to be aerated with respect to the fragrance compound adsorption device, and may be arbitrarily determined depending on the device to be used. For example, it may be upstream if it is a blower and downstream if it is a suction device.
As the suction device used as the linear velocity adjusting device 4, it is preferable to use a suction device having a pump performance higher than that of the airflow generation device 13 from the viewpoint of efficiently recovering the aroma compound.
The linear velocity adjusting device 4 is preferably arranged in the introduction path 3. The linear velocity adjusting device 4 may be arranged at the inlet 3A of the introduction path or at the outlet 3B of the introduction path.

  Hereinafter, the present invention will be described more specifically with reference to examples and comparative examples. The materials, amounts used, ratios, processing details, processing procedures, and the like shown in the following examples can be changed as appropriate without departing from the spirit of the present invention. Therefore, the scope of the present invention should not be construed as being limited by the specific examples shown below.

[Example 1]
In the present invention that uses the exhaust flow of the pulverizer, pressure is applied to the inlet of the fragrance compound adsorbing device by using an adsorbent, which causes a load on the airflow generator employed in the fragrance collecting device of the present invention. It is preferable to check whether.
Therefore, as Example 1, by changing the appropriate cross-sectional diameter and length of the adsorbent part of the fragrance compound adsorbing device K provided in the fragrance collecting device A of the present invention, air is ventilated to each fragrance compound adsorbing device K, and The presence or absence of a proper range was confirmed. Each aroma compound adsorption device has mesh lids Ka1 and Ka2 and an adsorbent accommodating part Kb (FIG. 3).

  SP-207 (styrene divinylbenzene copolymer-based synthetic adsorbent, manufactured by Mitsubishi Chemical Corporation) was used as the adsorbent accommodated in the aromatic compound adsorbing device K. As an adsorbent accommodating part that accommodates (roughly fills) the adsorbent, a cylindrical side wall type basket having no holes in the side part was used.

Next, a fragrance compound adsorbing device having the cross-sectional diameter and length of the adsorbent portion occupied by the adsorbent accommodated in the fragrance compound adsorbing device K as shown in Table 1 below is prepared. The suction pump provided in the section was operated to ventilate the adsorbent accommodated in the aromatic compound adsorption device K. And the pressure of the inlet_port | entrance of each aromatic compound adsorption | suction apparatus and the air volume of an exit were measured. In the present embodiment, the cross-sectional diameter of the adsorbent portion is the same as the cross-sectional diameter (inner diameter) of the basket described above in the air ventilation direction. In addition, the aromatic compound adsorption device K was disposed substantially perpendicular to the ground, and the air flow direction of the adsorbent was substantially the same as the gravity direction.
Next, it was calculated whether or not a performance curve (also referred to as an air flow-static pressure characteristic curve) (FIG. 4) of a general blower (air flow generator) deviated. This curve is a curve plotting the relationship between the pressure of the air flow generated by the blower and the air volume when the motor output of the blower is 1.5 to 10 kW. If it does not deviate from the performance curve range shown in FIG. 4, for this blower, the blower performance exceeds the adsorbent resistance in the motor output range, and the air flow generated by the blower passes through the adsorbent. Suggest that you can. On the other hand, if the curve deviates to the left of the thick line, the outlet air volume cannot be obtained satisfactorily even with high pressure, that is, the adsorbent resistance exceeds the blower performance, and the blower is loaded. To suggest.
The obtained results are shown in Table 1 below.

From Table 1 above, it was confirmed that the length of the adsorbent portion (gas aeration direction) is preferably not more than a certain value because of the resistance of the adsorbent to the gas flow.
It is confirmed that the recovery of the aroma compound preferably includes a step of optimizing the length of the adsorbent part (gas aeration direction) according to the performance of the airflow generator employed in the aroma recovery device of the present invention. It was done. In addition, when it is desired to increase the amount of adsorbent, it is preferable not to increase the length of the adsorbent part, but to increase the cross-sectional diameter of the adsorbent part to suppress the length of the adsorbent part (gas aeration direction). It was also confirmed.
As is clear from the test results, if an adsorbent portion having a certain length is employed, if it deviates to the left from the performance curve of the airflow generation device scheduled to be used, it will be in the vicinity of the aromatic compound adsorption device K. Further, a linear velocity adjusting device 4 such as a blower (blower) or a suction pump is further arranged to generate an air flow, and the pressure of the air flow generated by the air flow generation device 13 is supplementarily increased, so that the adsorbent is sufficient. Gas can be vented.
In addition, a means for suppressing the resistance caused by the adsorbent, for example, the aroma compound adsorbing device is an adsorbing device in which the adsorbent such as a fluidized bed column is movable, and a part of the airflow generated by the airflow generating device 13 is branched. It is obvious that the adsorbent can be sufficiently ventilated only by a normal blower without the linear velocity adjusting device 4 even if the branched airflow is passed through the adsorbent.
As described above, in the present invention, the length of the adsorbent portion in the gas flow direction, the presence or absence of airflow branching, the mobility of the adsorbent, and the like are appropriately set in accordance with the airflow generator of the general pulverizer to be used. By adjusting, the burden on a more general pulverizer can be suppressed.

[Example 2]
The collection of aroma compounds at the time of pulverizing roasted coffee beans, sensory evaluation of the fragrance composition, and the burden on the aroma collection device were examined.

(1) Aroma recovery First, an outline of the aroma recovery device A used in the present embodiment is shown.
The aroma recovery device A of the present invention has the configuration shown in FIGS. Specifically, the fragrance recovery device A of the present invention includes a pulverizer 11, a fine powder flake preliminary removal device 12, a first flow channel 1, an airflow generator 13, a fine powder flake removal device 14, a second flow channel 2, An aroma compound adsorption device K is provided. In FIG. 2, the fragrance compound adsorbing device K is described so as to be parallel to the installation surface of the fragrance collection device A (parallel to the ground contact surface, that is, horizontal). On the other hand, it was arranged substantially perpendicularly, and the gas ventilation direction of the adsorbent part was substantially the same as the gravity direction.
The aroma collection device A includes a roller mill as the crushing device 11. The pulverizing apparatus 11 communicates with the fine powder preliminarily removing apparatus 12, and the other parts can be pulverized in a sealed state.
The fine powder preliminary removing device 12 communicates with the crushing device 11. As the fine powder flake preliminary removal device 12, a vibration classifier equipped with a sieve (aperture 0.8 mm) is used, and the first flow path 1 communicates with the fine powder flake preliminary removal device 12 and the airflow generation device 13. The airflow generation device 13 communicates with the first flow path 1 and the second flow path 2.
The aroma recovery device A includes a suction blower as the airflow generation device 13. With this suction blower, continuous air flow can be generated in the pulverizer 11, the fine powder preliminary removing device 12, the first flow path 1, the fine powder thin piece removing device 14, the second flow path 2, and the fragrance compound adsorbing device K. It is. Further, a suction pump is provided as a linear velocity adjusting device 4 downstream of the air flow of the fragrance compound adsorbing device K, and an air flow is generated together with the air flow generating device 13.
The aroma recovery device A includes a cyclone type separation device as the fine powder flake removal device 14.
The inner diameters of the first channel 1 and the second channel 2 were 200 mm.
The aroma recovery device A includes an aroma compound adsorption device K in the introduction path 3 branched from the second flow path 2 having an inner diameter of 200 mm. The introduction path 3 was designed so that half of the gas flowing in the second flow path before the inlet 3A of the introduction path flows into the introduction path 3. The total amount of gas that has flowed into the introduction path 3 flows into the aroma compound adsorption device K.

  Further, as Comparative Example 1, an odor collection device a1 that is the same as the fragrance collection device A except that the fragrance compound adsorption device k1 branched from the upper part of the crushing device 11 is provided instead of the fragrance compound adsorption device K. The aromatic compound adsorbing device k1 has an introduction path that branches from the upper part of the pulverizing apparatus 11 and introduces an airflow into the adsorbent, and a discharge path that discharges the airflow coming out of the adsorbent. The amount of gas flowing in the introduction path branched from the upper part of the pulverizer 11 was designed to be the same amount as the gas flowing in the introduction path 3 of the fragrance recovery apparatus A.

  Further, as Comparative Example 2, instead of the fragrance compound adsorption device K, an odor collection device a2 that is the same as the fragrance collection device A except that the fragrance compound adsorption device k2 branched from the middle of the first flow path 1 is prepared. did. The fragrance compound adsorbing device k2 has an introduction path that branches from the first flow path 1 having an inner diameter of 200 mm and introduces an air flow into the adsorbent, and a discharge path that discharges the air flow emitted from the adsorbent. The amount of gas flowing in the introduction path was designed so that half of the gas flowing in the first flow path 1 (that is, the same amount of gas flowing in the introduction path 3 of the fragrance recovery device A) flows before the inlet.

The aroma compound adsorbing device K, the aroma compound adsorbing device k1, and the aroma compound adsorbing device k2 were all filled with the same type and amount of adsorbent.
And the aromatic compound at the time of roasted coffee bean grinding | pulverization was collect | recovered using the aromatic recovery apparatus A of this invention, the aromatic recovery apparatus a1 of the comparative example 1, and the aromatic recovery apparatus a2 of the comparative example 2.

Specifically, the aromatic compound was recovered by the following method.
In a state where the airflow is generated by the airflow generation device 13, the roasted coffee beans (L value: 24) are pulverized to a pulverization size of about 1 mm at 100 kg / h with a roller mill (pulverization device 11). A roasted coffee bean coarsely pulverized product containing fine powder and flakes was obtained.
Using each fragrance recovery device (A, a1 or a2), in the classification device (fine powder flake preliminary removal device 12), a part of the fine powder and flakes 22 was removed from the roasted coffee bean coarsely pulverized product 23 and discarded. Further, the fine powder and flakes 22 (including fine powder and flakes mainly derived from chaff) that have not been removed by the fine flake preliminary removing device 12 are used to remove the gas (aroma compound 21 from the crushing device 11 during the pulverization of roasted coffee beans). Gas), the first flow path 1 communicated from the fine powder preliminarily removing device 12 was passed by the air flow. The removal of fine powder and flakes 22 from the roasted coffee bean coarsely pulverized product 23 yields a roasted coffee bean refined pulverized product that has been pulverized to a desired size. It can be stored outside the collection device A until it is used for producing coffee products.
The fine powder and flakes 22 were removed from the gas containing the aroma compound 21 generated from the roasted coffee beans and the fine powder and flakes 22 when the roasted coffee beans were pulverized by the fine powder flake removing device 14.
The fine powder and flakes 22 removed from the gas were accommodated in a disposal unit (not shown) communicating with the fine powder flake removal device 14 and discarded.
On the other hand, the gas from which the fine powder and the thin piece 22 were removed was passed through the second flow path 2 communicating with the fine powder thin piece removing device 14. The linear velocity of the gas passing through the second flow path was 4.1 m / s. Half of the gas flowing into the second flow path 2 as described above flowed into the introduction path 3.
During the crushing of roasted coffee beans, the gas flowing into the introduction path 3 was accommodated (coarsely filled) in the adsorbent accommodating part Kb of the aroma compound adsorbing device (K, k1, or k2). The adsorbent was aerated to adsorb the aromatic compound 21 contained in the gas.

The adsorbent and aeration of each fragrance compound adsorbing apparatus were set under the following conditions in common. As the adsorbent accommodating portion, a cylindrical side wall type basket having no holes in the side surface portion was used. Moreover, in order to suppress cracking, the adsorbent was filled in the aromatic compound adsorbing device after absorbing pure water and before completely drying.
Aroma compound adsorbent: SP-207 (styrene divinylbenzene copolymer synthetic adsorbent, manufactured by Mitsubishi Chemical Corporation)
Cross-sectional diameter of adsorbent part: 100mm
Linear velocity of inflow gas to adsorbent: 2.0 m / s
Length of adsorbent part (length in the gas aeration direction): 8.0 cm
Adsorbent usage: 2500ml
Gas type: Air Crushing and gas aeration time to adsorbent part: 5 hours In this example, the cross-sectional diameter of the adsorbent part is the same as the cross-sectional diameter (inner diameter) in the gas aeration direction of the basket described above. .

After aeration for 5 hours using each fragrance recovery device, 25 kg of propylene glycol (PG) was passed through the adsorbent of each fragrance compound adsorption device at SV = 10 to desorb the fragrance compound 21 from the adsorbent. SV (Space velocity) is a unit representing how many times the volume of the resin is passed per hour. In this way, roasted coffee bean flavor (fragrance composition as a PG solution) containing each of the aroma compounds collected by the aroma compound adsorption devices K, k1, and k2 was obtained. These fragrance compositions were obtained as Invention product 1, Comparative product 1 and Comparative product 2, respectively.
Here, half of the gas containing the aromatic compound generated from 500 kg of roasted coffee beans subjected to crushing (crushing at 100 kg per hour for 5 hours) was passed through the adsorbent (as described above, the second flow path 2 Half of the gas that flows to the inlet 3 and the adsorbent), so that the adsorbent was adsorbed with gas containing 250 kg of roasted coffee beans, and the aromatic compound was desorbed by PG. Thus, 25 kg of PG solution (fragrance composition) was obtained, and the weight of the fragrance composition was 10% with respect to the weight of the roasted coffee beans in which the fragrance compound was generated. 1 and 2 were prepared.
On the other hand, the aromatic compound of the roasted coffee beans coarsely pulverized product was recovered by steam distillation to prepare Comparative Product 1. Specifically, 2000 g of crushed roasted coffee beans are stored in a 3 L column, steam is fed from the bottom of the column under atmospheric pressure, steam distillation is performed for 2 hours, and steam containing an aromatic compound obtained from the top of the column is stored. It condensed with the cooling pipe | tube, and 2000g of aqueous solution containing an aromatic compound was obtained. Next, after passing the aqueous solution obtained in 50 ml of the adsorbent (SP-207), 200 g of PG solution was passed through the adsorbent, and the adsorbed aromatic compound was desorbed to obtain 200 g of a PG solution as a steam distillation flavor. This steam distilled flavor was designated as Comparative product 3. Here, similarly to the inventive product 1 and the comparative products 1 and 2, the fragrance can be directly compared so that it becomes 10% by mass in the same manner as the inventive product 1 and the comparative products 1 and 2.

(2) Burden of fragrance collection device After collection of the fragrance compound, it was confirmed whether or not the adsorbent after desorption of the fragrance compound was reusable.
The reusability can be confirmed by checking the adsorbents (hereinafter referred to as adsorbent q1, adsorbent q2, and adsorbent Q, respectively) contained in the aromatic compound adsorbing devices (k1, k2, and K) before desorption by PG. This was confirmed by comparing the pressure of the liquid flow after desorption. Specifically, after desorption and after desorption, the pressure when the ultrapure water was flowed at SV = 10 after the replacement with ultrapure water was measured, and then the pressure after desorption relative to the pressure before desorption Was calculated.
As a result, the adsorbent q1 and the adsorbent q2 were 10 times and 5 times the pressure, respectively, and it was recognized that clogging occurred. In such a case, the adsorbent needs to be washed or discarded several times. On the other hand, in the adsorbent Q, the pressure difference was the same, clogging did not occur, and it was confirmed that several washings and disposals are unnecessary.
From the above, it was confirmed that both the labor and cost of regeneration of the adsorbent are reduced by the fragrance recovery device of the present invention. Moreover, in the apparatus of the comparative example, it was confirmed that it is industrially unsuitable to collect the aroma generated from the roasted coffee beans when the roasted coffee beans are pulverized.
(3) Sensory evaluation of the fragrance composition The fragrance composition of the present invention product 1 and comparative products 1 to 3 are added in the addition amounts shown in Table 2 below with respect to the base material (commercial sugar-free black coffee). Then, a fragrance product having a Bx of 1.0 ° and a pH of 6.5 before retort sterilization was prepared.
Retort sterilization conditions were set at 121 ° C. for 10 minutes, and retort sterilization was performed on each flavored product. The obtained flavored product after retort sterilization had a pH of 5.8.
Among the fragrant products after retort sterilization, sensory evaluation was performed by ten well-trained panelists on the present product 1 and comparative products 1 to 3. The average sensory evaluation results of 10 panelists are shown in Table 2 below.

  As shown in Table 2 above, the fragrance composition of the product 1 of the present invention, unlike the comparative product, gives a scent when the roasted coffee beans are ground, that is, the aroma generated when the roasted coffee beans are crushed. It was an excellent flavor. This is because, as confirmed in (2), the adsorbent is clogged with fine powder and flakes, and therefore the adsorption efficiency of the aroma compound is poor, and it seems that the characteristics of the aroma and the intensity of the aroma differed.

[Example 3]
About each fragrance | flavor composition of this invention product 1 prepared by carrying out similarly to Example 1, and the comparative product 3, it analyzed using GC / MS. In addition, this invention product 1 and the comparative product 3 were prepared 3 each, and used for the analysis.

SBSE (Stir Bar Sorative Extraction) method was used as a fragrance collection method. Twister (registered trademark) manufactured by GUSTER Co., Ltd. was placed in a vial containing the fragrance composition of Invention Product 1 or Comparative Product 3, and stirred. Twister (registered trademark) is a coating of PDMS (polydimethyl siloxane) on a 1.5-cm long Stir Bar (star bar), which is stirred in a vial containing a liquid sample. Thus, components in the liquid sample can be extracted.
After extracting the aroma compound contained in each fragrance composition, it was introduced into GC / MS (gas chromatograph / mass spectrometer) by an automatic heating desorption system.

The GC / MS measurement conditions are shown below.
GC / MS; 7890A GC / 5975C inert XL MSD (quadrupole mass spectrometer) (manufactured by Agilent Technologies)
Column: InertCap-WAX, 60 m x 0.25 mm x inner diameter (ID) 0.25 µm (manufactured by GL Sciences Inc.)
Carrier gas: He
Mode: Constant flow Column flow rate: 1.4 mL / min MS: Electron impact ionization method (EI mode), 70 eV
Injection method: Gerstel TDU
Initial temperature: 20 ° C
Rate: 720 ° C / min Final temperature: 260 ° C
Hold time: 2 minutes Initial oven temperature: 40 ° C
Hold time: 5 minutes Rate: 5 ° C / min Final temperature: 230 ° C
Hold time: 20 minutes

The total ion chromatogram obtained by analyzing the aroma collected by the SBSE method by GC / MS as described above is shown in FIGS. FIG. 5 is a total ion chromatogram of the product 1 of the present invention, and FIG. 5 and 6, the peak that is shaken off at RT = about 23 minutes is a peak attributed to PG used for desorption.
5 and 6, the horizontal axis represents the retention time (RT), and the vertical axis represents the peak intensity.

The area ratio of each component contained in each fragrance composition was classified by a retention index (RI).
Specifically, it was classified into a component (top) with RI of acetoin or lower and a component with RI greater than acetoin. The acetoin RI was 1294, and the acetoin RT was about 15 min.
Based on the obtained total ion chromatograms, the component (top) having RI of acetoin or less relative to the total area value of the total ion chromatograms of the perfume compositions of the present invention product 1 and comparative product 3 and the total ion chromatogram The area% of the component having an RI greater than acetoin relative to the total area value was determined. The results of the three inventive products 1 were 89:11, 100: 0, and 93: 7, respectively, and the results of the three comparative products 3 were 27:73, 29:71, and 30:70 . In addition, for the base material (commercial unsweetened black coffee) before retort sterilization, the aroma collected by the SBSE method is analyzed by GC / MS in the same manner as the above method, and the area% of each component is similarly obtained. It was. The obtained results are shown in Table 3 below. The numerical values shown in Table 3 are three average values of each product.
Further, based on the obtained total ion chromatograms, the area percentages of 2-methylfuran, 2-methylbutyldehyde, and isovaleraldehyde with respect to the component (top) in which the fragrance compositions of the inventive product 1 and the comparative product 3 are acetoin or lower (top) (Vs. top area value) was determined. In addition, for the base material (commercial unsweetened black coffee) before retort sterilization, the aroma collected by the SBSE method is analyzed by GC / MS in the same manner as the above method, and the area% of each component is similarly obtained. It was. The obtained results are shown in Table 4 below.

From Table 3 above, it was found that the fragrance composition of the product 1 of the present invention has a fragrance balance in which the content of the component (top) with RI of acetoin or less is large and the specific gravity of the top is high. Here, components having an RI of acetoin or less have high volatility, and the content of the base material (commercial sugar-free black coffee) is small, and the content of the fragrance composition of Comparative Product 3 obtained by steam distillation is also small. It was found that the product 1 of the present invention has a strong scent at the top due to a large content of components having an RI of acetoin or less, and thus makes it possible to feel the aroma generated when the roasted coffee beans are crushed.
In addition, from Table 4 above, it was found that the fragrance composition of the product 1 of the present invention had a higher content ratio of 2-methylfuran, 2-methylbutyraldehyde, and isovaleraldehyde, compared to the comparative product 3 and the base material. .

[Example 4]
For flavoring products (before and after retort sterilization) and base materials (commercial sugar-free black coffee) using the fragrance compositions of the present invention product 1 and comparative product 3 prepared in the same manner as in Example 2, Analyzed using GC / MS. In addition, this invention product 1 and the comparative product 3 were prepared 3 each, and used for the analysis.

  From each of the obtained total ion chromatograms, in the same manner as in Example 3, the component (top) where RI is acetoin or less and the area% of the component where RI is larger than acetoin (each area% of the substrate) were determined. . The obtained results are shown in Table 5 below.

  Further, from each of the obtained total ion chromatograms, in the same manner as in Example 3, the area percentages of 2-methylfuran, 2-methylbutylaldehyde and isovaleraldehydride (each area percentage of the base material) were obtained. The obtained results are shown in Table 6 below.

From Table 5 above, in the fragranced product (before retort sterilization) using the fragrance composition of the product 1 of the present invention, the effect of adding the top fragrance could be confirmed. In particular, it was found that the contents of 2-methylfuran, 2-methylbutyldehyde, and isovaleraldehyde were higher than those of the fragrance product using the base material (commercially available sugar-free black coffee) and comparative product 3.
Moreover, the addition effect of the top fragrance | flavor was able to be confirmed in the fragrance | flavor goods (after retort sterilization) using the fragrance | flavor composition of this invention product 1. In particular, it was found that the contents of 2-methylfuran, 2-methylbutyldehyde, and isovaleraldehyde were higher than those of the fragrance product using the base material (commercially available sugar-free black coffee) and comparative product 3. Therefore, it was found that the top fragrance remained even after retort sterilization.
Therefore, from Table 5 above, the flavored product using the fragrance composition of the product 1 of the present invention has the highest content of components having RI of acetoin or less before and after retort sterilization. It was found that the fragrance was greatly enhanced, which caused the aroma generated when the roasted coffee beans were crushed.

  From Table 6 above, the flavored product using the fragrance composition of the product 1 of the present invention has a content of 2-methylfuran, 2-methylbutyldehyde, and isovalardehyde of interest from the base material before and after retort sterilization. Was found to be enhanced by about 20%.

DESCRIPTION OF SYMBOLS 1 1st flow path 2 2nd flow path 3 Introducing path 3A Inlet path entrance 3B Inlet path exit 4 Linear velocity adjusting device 11 Crushing device 12 Fine powder flake preliminary removal device 13 Airflow generating device 14 Fine powder flake removal device 21 Aroma Compound 22 Fine powder and flakes 23 Coarse pulverized product of roasted coffee beans 24 Exhaust gas K Aroma compound adsorbing device Ka1, Ka2 Reticulated lid Kb Adsorbent accommodating part k1 Aroma compound adsorbing device k2 used in Comparative Example 1 Aroma used in Comparative Example 2 Compound adsorption equipment

Claims (22)

Crushing roasted coffee beans to obtain a roasted coffee bean coarsely pulverized product containing fine powder and flakes,
Removing the fine powder and flakes from the gas containing the aromatic compound and fine powder and flakes generated from the roasted coffee beans when the roasted coffee beans are crushed;
An adsorbing step in which the gas from which the fine powder and flakes have been removed is passed through an adsorbent to adsorb the aromatic compound to the adsorbent;
A recovery step of recovering the fragrance compound from the adsorbent and preparing a fragrance composition containing the fragrance compound;
Including
The adsorbent is accommodated in an adsorbent accommodating portion in an aromatic compound adsorbing device, and the adsorbent accommodating portion has net-like lids at both ends in the gas ventilation direction.
A method for producing a fragrance composition from roasted coffee beans.   The fragrance composition from roasted coffee beans according to claim 1, wherein the step of removing the fine powder and flakes from the coarsely pulverized product of roasted coffee beans is performed before the step of removing the fine powder and flakes from the gas. Manufacturing method.   The manufacturing method of the fragrance | flavor composition from the roasted coffee beans of Claim 1 or 2 which performs the process of removing the said fine powder and flakes with a fine powder flake removal apparatus.   The manufacturing method of the fragrance | flavor composition from the roasted coffee beans as described in any one of Claims 1-3 which generate | occur | produces the flow of the said gas using an airflow generator. In the gas flow path from which the fine powder and flakes have been removed, an introduction path that branches from the flow path and communicates with the aromatic compound adsorption device is provided.
From the roasted coffee beans according to any one of claims 1 to 4, wherein only a part of the gas from which the fine powder and flakes have been removed is passed through the introduction path and the adsorbent to recover the aroma compound. A method for producing a perfume composition.   The adsorbent includes a styrene divinylbenzene copolymer, a copolymer of ethylvinylbenzene and divinylbenzene, a polymer of 2,6-diphenyl-9-phenyl oxide, a polycondensation polymer of methacrylic acid and a diol, and a modified silica gel. The manufacturing method of the fragrance | flavor composition from the roasted coffee beans as described in any one of Claims 1-5 which is 1 or more selected.   The method for producing a fragrance composition from roasted coffee beans according to any one of claims 1 to 6, wherein the aromatic compound is desorbed from the adsorbent using an organic solvent in the recovery step.   The method for producing a fragrance composition from roasted coffee beans according to claim 7, wherein the organic solvent is ethanol or propylene glycol.   Manufacture of the fragrance | flavor composition from the roasted coffee beans as described in any one of Claims 1-8 whose linear velocity of the gas which flows in into the said adsorption agent exists in the range of 0.1-35.0 m / s. Method. Method for producing a ventilation direction of the gas is the direction of gravity and the opposition direction, the perfume composition from roasted coffee beans according to any one of claims 1-9.   The manufacturing method of the fragrance | flavor composition from the roasted coffee beans as described in any one of Claims 1-10 whose said aroma compound adsorption | suction apparatus is a fluidized bed column in which the said adsorption agent was accommodated.   The manufacturing method of the fragrance | flavor composition from the roasted coffee beans as described in any one of Claims 1-11 including the process of adjusting the linear velocity of the gas which flows in into the said adsorption agent.   The method for producing a fragrance composition from roasted coffee beans according to claim 12, wherein the linear velocity of the gas flowing into the adsorbent is adjusted using a blower or a suction pump. Roasted coffee beans crusher,
A first flow path that communicates with the pulverizing device and through which a gas containing aroma compounds and fine powder and flakes generated when the roasted coffee beans are crushed;
A fine powder flake removal device communicating with the first flow path to remove the fine powder and flakes;
A second flow path that communicates with the fine powder flake removal device and through which the gas from which the fine powder and flakes have been removed can pass;
An aroma compound adsorbing device in communication with the second flow path;
An airflow generator for generating a continuous airflow from the pulverizer to the aromatic compound adsorbing device;
With
The aroma compound adsorbing device has an adsorbent accommodating portion in which an adsorbent is accommodated, and the adsorbent accommodating portion has net lids at both ends in the gas flow direction, and an aroma recovery device from roasted coffee beans . The fragrance recovery device from roasted coffee beans according to claim 14 , further comprising an introduction path branched from the second flow path, the introduction path communicating with the fragrance compound adsorption device. The fragrance recovery device from roasted coffee beans according to claim 14 or 15 , further comprising a fine powder flake preliminary removal device between the pulverization device and the first flow path. It said vent direction of the gas adsorbent, the gravitational direction and the opposition direction, aroma recovery system from roasted coffee beans according to any one of claims 14-16. The aroma recovery device for roasted coffee beans according to any one of claims 14 to 17 , wherein the aroma compound adsorption device is a fluidized bed column in which the adsorbent is accommodated. The fragrance recovery device from roasted coffee beans according to any one of claims 14 to 18 , further comprising a linear velocity adjusting device that adjusts a linear velocity of the gas from which the fine powder and flakes have been removed. The fragrance recovery device from roasted coffee beans according to any one of claims 14 to 19 , wherein the linear velocity adjusting device is a blower or a suction pump. The fragrance recovery device from roasted coffee beans according to any one of claims 14 to 20 , wherein a cross-sectional diameter of an adsorbent portion accommodated in the adsorbent accommodating portion is 10 mm or more. The fragrance recovery device from roasted coffee beans according to any one of claims 14 to 21 , wherein the length of the adsorbent portion accommodated in the adsorbent accommodating portion in the gas aeration direction is 1000 mm or less.

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