WO2023188340A1

WO2023188340A1 - Tobacco extract composition and production method therefor

Info

Publication number: WO2023188340A1
Application number: PCT/JP2022/016716
Authority: WO
Inventors: 拓也岩本; 大史藤倉
Original assignee: 日本たばこ産業株式会社
Priority date: 2022-03-31
Filing date: 2022-03-31
Publication date: 2023-10-05

Abstract

A production method for a tobacco extract composition, comprising: a heating step for heating a tobacco starting material under oxygen-containing gas bubbling; and a recovery step for recovering volatile components generated in the heating step.

Description

Tobacco extract composition and method for producing the same

The present invention relates to a tobacco extract composition and a method for producing the same.

In recent years, non-combustible flavor suction products have been developed. In the article, an aerosol is generated by heating an aerosol-generating base material. Patent Document 1 relates to a method for manufacturing a pre-vapor preparation used in such an electronic vaping device, and discloses a manufacturing method comprising a step of heating a tobacco material, recovering volatile components, and combining the volatile components with a pre-vapor preparation. .

Special table 2019-507592 publication

The inventors conducted a preliminary study on the method described in Patent Document 1, but found that there was room for improvement, particularly in terms of collection efficiency. In view of such circumstances, an object of the present invention is to provide a method for producing a tobacco extract composition with excellent collection efficiency.

The inventors have discovered that the above problem can be solved by setting the flow rate of oxygen in a specific range in the heating step. That is, the above-mentioned problem is solved by the present invention described below.
Aspect 1
a heating step of heating tobacco raw materials under gas aeration containing oxygen; and a recovery step of recovering volatile components generated in the heating step;
A method for producing a tobacco extract composition, comprising:
Aspect 2
The manufacturing method according to aspect 1, wherein the flow rate of the gas is 2 to 10 L/min.
Aspect 3
The manufacturing method according to aspect 1 or 2, wherein the heating step is performed in a container, and the volume of the tobacco raw material or the raw material mixture containing the raw material in the container is 10 to 40% by volume.
Aspect 4
The manufacturing method according to any one of aspects 1 to 3, wherein the tobacco raw material has a particle size of 0.5 to 2 mm as measured according to ASTM E11-95.
Aspect 5
The manufacturing method according to any one of aspects 1 to 4, wherein the tobacco raw material is selected from burley varieties, yellow varieties, or a combination thereof.
Aspect 6
When the diameter of the tube through which the volatile matter is discharged in the heating step is D1, and the diameter of the tube into which the volatile matter is introduced in the recovery step is D2,
D2/D1≦0.17
The manufacturing method according to any one of aspects 1 to 5.
Aspect 7
A tobacco extract composition produced by the production method according to any one of aspects 1 to 6.
Aspect 8
The tobacco extract composition according to aspect 7, wherein the turbidity (OD660) measured using a spectrophotometer is 0.90 to 1.80 when the concentration of the polyol component is 15 to 35% by weight.

According to the present invention, a tobacco extract composition can be produced with excellent collection efficiency.

Conceptual diagram of tobacco extract composition manufacturing equipment Schematic cross-sectional diagram showing an example of a non-combustion indirect heating smoking article Appearance of tobacco extract composition

Hereinafter, the present invention will be explained in detail. In the present invention, "X to Y" includes the end values of X and Y.

1. Manufacturing method The method for manufacturing the tobacco extract composition according to the present embodiment includes a heating step of heating tobacco raw materials under gas aeration containing oxygen, and a recovery step of recovering volatile components generated in the heating step. A tobacco extract composition is a composition that exhibits a flavor extracted from tobacco raw materials. FIG. 1 shows one aspect of the manufacturing method according to this embodiment. In the figure, 100 is a tobacco raw material, 110 is a container, 102 is an air introduction pipe, 104 is an exhaust pipe, 200 is a tobacco extract composition, 120 is a collection container, 122 is an ice water bath, and 130 is a pipe.

(1) Heating process 1) Tobacco raw material Various materials can be used as the tobacco raw material 100, for example, yellow variety, burley variety, orient variety, native variety, and other Nicotiana tabacum or Nicotiana rustica. species, and mixtures thereof can be used. As a mixture, a blend of the above-mentioned varieties as appropriate can be used so as to provide the desired aroma and flavor. Further, raw materials from any production area can be selected so that the tobacco extract composition according to this embodiment has desired aroma and taste characteristics. For example, when the tobacco extract composition according to the present embodiment is used in a product with a high nicotine content, it is preferable to prepare the tobacco extract composition from a high nicotine-rich variety with a nicotine content of 6% by weight or more. Examples of such varieties and production areas include Burley variety from Japan and sun-dried variety from the Philippines. Details of the tobacco varieties are disclosed in "Tobacco Encyclopedia, Tobacco Research Center, March 31, 2009." Additionally, as described in WO2021/070932, leaves with high nicotine content obtained through specific fertilization and harvesting can also be used. Specifically, in the cultivation of Burley species, the leaves are treated with fertilizer with a nitrogen content of 6 to 15 kg/10a between one week before and one week after pruning; Harvesting and removing unnecessary leaves at an early stage; Harvesting the leaves after extending the period from the point of plucking to harvesting by one to two weeks longer than usual; Obtaining the leaves through air drying. Alternatively, the tobacco raw material may be subjected to a known alkali treatment.

The tobacco raw material 100 may be shredded or powdered tobacco raw material (hereinafter also referred to as "raw material pieces"). In such a case, if the particle size is too large, the stirring efficiency may decrease in this step. On the other hand, if the particle size is too small, it may be difficult to process it into a molded article or the like. From this point of view, it is preferable that the particle size of the raw material pieces is 0.5 to 2 mm as measured according to ASTM-E11-95. Having the particle size means that the raw material pieces do not pass through a sieve with an opening of 0.5 mm (>0.5 mm), but pass through a sieve with an opening of 2.36 mm (<2.5 mm). means. Preferably, this measurement is carried out using a dry piece of raw material by a mechanical shaking method.

The particle size of the raw material pieces can be adjusted to a desired range by classification. For example, particle size can be adjusted as follows. i) Prepare a sieve mesh L having a mesh size near the minimum particle size of the raw material piece, a sieve mesh M having a mesh size near the maximum particle size of the raw material piece, and several sieve meshes between L and M. do. ii) Using these sieve meshes, raw material pieces are sieved and classified by a dry and mechanical shaking method. iii) The classified fractions are appropriately collected to obtain raw material pieces of desired particle size. Specifically, when obtaining raw material pieces with a particle size of 0.5 to 2 mm, the opening size is 2.36 mm, 2 mm, 1.7 mm, 1.4 mm, 1.18 mm, 1 mm, 0.85 mm, 0.71 mm, 0.6 mm. , 0.5 mm, and 0.425 mm sieves and the fractions obtained by classification may be mixed.

The average particle size can be determined by performing classification according to i) to iii) above, measuring the amount of the fraction remaining in each sieve, and dividing it by weight. For example, classification using sieves with openings of 2.36 mm, 2 mm, 1.7 mm, 1.4 mm, 1.18 mm, 1 mm, 0.85 mm, 0.71 mm, 0.6 mm, 0.5 mm, and 0.425 mm. The average particle size can be determined by measuring the weight of the fraction obtained and dividing the fraction by weight.

2) Temperature It is preferable that the container 110 is equipped with a stirring device, and the tobacco raw material 100 is stirred. In this step, the tobacco raw material 100 is preferably heated to a temperature of 100 to 270°C. The temperature of the tobacco raw material 100 can be measured by arranging a temperature sensor in the container 110 so as to be in contact with the tobacco raw material 100. The temperature sensor may be a thermocouple. The temperature is preferably 200 to 250°C. By heating the tobacco raw material 100, volatile components are generated. It is also possible to provide a branch in the pipe 130 via a valve so that the volatile matter generated before the lower limit of the temperature is reached and the volatile matter generated when the upper limit of the temperature is exceeded are not introduced into the collection container 120. .

3) Flow rate This step is carried out under oxygen-containing gas ventilation. Gas ventilation can promote the discharge of volatile matter generated within the container to the outside of the container. The gas is not limited, but may include, for example, air or a mixed gas of an inert gas and oxygen. Among these, from the viewpoint of availability or workability, compressed gas is preferred, and compressed air is more preferred. Although the pressure of the compressed gas is not limited, compressed gas at a desired pressure can be supplied to the container 110 using, for example, a mass flow control unit. A mass flow control unit is a device that measures and controls the mass flow rate of a fluid, and includes a control flow sensor, a bypass, a valve, and an electrical circuit. For example, mass flow controller/meter (model number: SEC/SEF-B40) and mass flow control unit (model number: PAC-D2) manufactured by Horiba Estec Co., Ltd. can be mentioned.

The flow rate of the gas is 2 to 10 L/min. When the flow rate is within this range, the efficiency of capturing volatile matter can be improved. From this viewpoint, the lower limit of the flow rate is preferably 2.5 L/min or more, more preferably 3 L/min or more, and the upper limit thereof is preferably 10 L/min or less, more preferably 8 L/min or less.

The volume of the contents in the container is preferably 10 to 40% by volume, more preferably 15 to 20% by volume. The content is a tobacco raw material or a raw material mixture containing the raw material. If the volume exceeds the upper limit, stirring efficiency may decrease. Moreover, if the volume is less than the lower limit, it is difficult to generate a sufficient amount of volatilized flavor components.

The gas vented in this step contains oxygen. By including oxygen in the gas, a tobacco extract composition with improved aroma and taste can be produced while improving the efficiency of trapping volatile matter. Although the reason for this is not limited, it is presumed that the combustion-supporting gas comes into contact with the raw material to promote the reaction of the components contained in the raw material.

4) Atmosphere The tobacco raw material 100 can be heated in a bulk state without using a solvent, but it can also be heated in a state immersed in a solvent. As the solvent, polyols such as glycerin and propylene glycol are preferred. If the tobacco raw material and the solvent are mixed in advance or the tobacco raw material is pre-immersed in the solvent before heat treatment, the solvent and the raw material are heated in a sufficiently mixed state, so that it is possible to improve the collection efficiency. For example, tobacco raw material 100 and a solvent can be mixed and left under harmonized conditions (relative humidity 60%, 23° C.) for about 12 to 24 hours. Furthermore, in this step, a solvent supply port may be provided in the container 110, and the solvent may be supplied into the container from the supply port.

(2) Collection process The collection container 120 is connected to the container 110 via a pipe 130. Volatile components exhausted from container 110 are introduced into collection container 120. The collection container 120 may be filled with a collection solvent. Moreover, it is preferable that the collection container 120 constitutes a closed space. In order to obtain an extract processed at a predetermined temperature, a device for fractionating the extract depending on the temperature may be used in combination.

The collection solvent is not limited as long as it can dissolve the flavor component, but preferably water or an aqueous organic solvent such as glycerin or ethanol can be used. The ambient temperature or the temperature of the collection solvent during collection is not limited, but from the viewpoint of increasing collection efficiency, it is preferably about -20 to 10°C. For this purpose, the collection container 20 may be immersed in an ice water bath.

When the diameter of the pipe from which volatile matter is discharged in the heating process (also referred to as "exhaust pipe") is D1, and the diameter of the pipe through which volatile matter is introduced in the recovery process (also referred to as "introduction pipe") is D2. , these preferably satisfy the following relationship. When this relationship is satisfied, the volatile components are liquefied by inertial collision, so that the recovery efficiency of the volatile components is improved. The diameter of the introduction tube may be constant or variable throughout the tube. When the diameter of the inlet pipe varies, the diameter of the portion connected to the discharge pipe is set as D2.
D2/D1≦0.17
When this relationship is satisfied, volatile components can be collected without the need for additional processes or equipment such as bubbling or cooling, thereby simplifying the process.

2. Tobacco Extract Composition Tobacco extract composition 200 is manufactured as described above. The tobacco extract composition contains at least a nicotine component, which is an indicator of flavor components. The tobacco extract composition 200 further includes components that can impart tobacco-like astringency, aroma, and sweetness that cannot be achieved with conventional flavoring agents. It is presumed that this component is caused by the generation of volatile components at the above temperature.

The tobacco extract composition has a turbidity (OD660) of about 0.90 to about 1 when the concentration of the polyol component contained in the tobacco extract composition is 15 to 35% by weight. It has the characteristic that it is .80. A tobacco extract composition with low turbidity is less likely to generate burnt components when used in smoking articles. Turbidity is measured with reference to JIS K0101.

3. Smoking Article The tobacco extract composition according to this embodiment is suitable for smoking articles. For example, it is useful as an aerosol source for a non-combustion, indirect heating type flavor suction article as shown in FIG. It is also useful as a flavor source for combustion type smoking articles or non-combustion direct heating type smoking articles, or as a flavoring agent for filters and the like. In particular, since the tobacco extract composition is useful as an aerosol source for a non-combustion, indirect heating type flavor suction article as shown in FIG. 2, this article will be described below as an example.

Figures 2(1) and (2) illustrate preferred embodiments of non-combustible flavor aspirate articles and non-combustible flavor aspirate systems. In the figure, 10 is a non-combustible flavor suction article, 1c is a capsule which is a flavor generation segment, 2 is an atomization section, 4 is an aerosol source, 40 is an aerosol generation segment, 5 is a mouthpiece, 6 is a housing, and 8 is a power source It is. Since the non-combustion flavor suction article of this embodiment indirectly heats the capsule, it is also referred to as a "non-combustion indirect heating type flavor suction article." The article is an article that generates an aerosol from an aerosol generation source disposed upstream of a flavor-generating segment, and causes the aerosol to carry a flavor component from the flavor-generating segment to produce a flavor.

1) Capsule The capsule 1c is sealed so that gas can communicate between the outside and the inside. The aerosol generated from the aerosol source 4 is introduced into the container and is sealed so that it can pass from the container toward the mouth end. For this reason, openings are preferably provided at both longitudinal ends of the container. The container is filled with a flavor source. Flavor sources include known tobacco materials. Although the shape of the tobacco material is not limited, it is preferably granular.

2) Aerosol Source The aerosol source 4 can be constructed by supporting the above-described aerosol-generating base material on a porous body such as a fiber filler. Although the length of the aerosol source 4 is not limited, it is preferably 10 to 25 mm. The tobacco extract composition according to this embodiment can be supported on the porous body and used as an aerosol source.

3) Atomization section The atomization section 2 is preferably capable of electrically heating the aerosol source 4 to about 200 to 300°C. The heating generates an aerosol, which is introduced into the capsule 1c, passes through the filling while creating an atmosphere of 30 to 80°C, carries flavor components, and is inhaled by the user. The combination of a non-combustible flavor suction article and a power source is also referred to as a non-combustible flavor suction system. The atomizer 4 may be a coil, for example, and can generate an aerosol using electricity supplied from a power source 8, as shown in FIG. 2(2). Such a system 10 is disclosed in International Publication No. 2016/075749, for example.

4) Mouthpiece The mouthpiece 5 may be equipped with a filter.

5) Housing The housing 6 may be made of a known material, but is preferably made of polymer, for example.

[Example 1]
Burley leaf shreds from Brazil and yellow leaf shreds from Brazil were mixed at a weight ratio of 1:1. The particle size of each piece was 0.5 to 1.18 mm as measured according to ASTM E11-95. Glycerin was added in an amount of 16.0% by weight based on the total weight of the mixed minced meat to prepare a mixture. 50 g of the mixture was taken out and charged into a 1000 mL separable flask equipped with a stirring device. An air introduction tube and an air introduction tube for discharging volatile components from inside the flask were connected to the flask. A thermocouple was placed in contact with the groove inside the flask.

The flask was heated with a mantle heater (set temperature: 250°C), and air was introduced into the flask at a flow rate of 3 L/min. At this time, a mass flow controller/meter (model number: SEC/SEF-B40) and a mass flow control unit (model number: PAC-D2) manufactured by Horiba Estec were used. Volatile components generated during a period of 10 minutes and 30 seconds from the start of heating were introduced into a collection container filled with a collection liquid. The collection vessel was immersed in an ice water bath at 0°C. The temperature of the raw material during collection was 100 to 200°C. The amount collected was 10.1 g.

Using a solvent obtained by mixing glycerin/propylene glycol at a ratio of 7/3 (weight ratio), the collected liquid obtained as described above was diluted 2 times. The tobacco extract composition thus obtained was filled into a cartridge of a non-combustion, indirect heating type smoking article shown in FIG. The product was subjected to a smoking test by well-trained panelists. As a result, it was revealed that the product had a fragrant taste that could not be achieved with conventional fragrances. Specific evaluation comments were as follows.
Example 1: Although the sucking response such as a slightly burnt feeling and aroma was weakened, a sufficient tobacco-like aroma and taste was felt.

[Example 2]
A tobacco extract composition was produced and evaluated in the same manner as in Example 1, except that the air flow rate was 5.1 L/min. The amount collected was 14.2 g. When smoking was carried out in the same manner as in Example 1, evaluation results equivalent to those in Example 1 were obtained. Specific evaluation comments were as follows.
Example 2: The tobacco-like aroma and sweetness were reproduced, and the tobacco-like aroma and smoking sensation were felt.

[Comparative example 1]
A tobacco extract composition was produced and evaluated in the same manner as in Example 1, except that the air flow rate was 1 L/min. The amount collected was 7.3 g. When smoking was carried out in the same manner as in Example 1, evaluations were obtained that it tasted raw, had a strong raw material odor, and had a weak burning sensation. As shown in FIG. 3, there was also a difference in appearance between the tobacco extract compositions obtained in Example 1 and Comparative Example 1.

1c capsule (flavor generating segment)
2 Atomization section 4 Aerosol source 40 Aerosol generation segment 5 Mouthpiece 6 Housing 8 Power source 10 Non-combustible flavor suction article 30 Heating device 31 Body 32 Heater 33 Metal tube 34 Battery unit 35 Control unit 36 Recess 37 Ventilation hole
100 Tobacco raw material 110 Container 102 Air introduction pipe 104 Exhaust pipe 200 Tobacco extract composition 120 Collection container 122 Ice water bath 130 Pipe

Claims

a heating step of heating tobacco raw materials under gas aeration containing oxygen; and a recovery step of recovering volatile components generated in the heating step;
A method for producing a tobacco extract composition, comprising:
The manufacturing method according to claim 1, wherein the flow rate of the gas is 2 to 10 L/min.
The manufacturing method according to claim 1 or 2, wherein the heating step is performed in a container, and the volume of the tobacco raw material or the raw material mixture containing the raw material in the container is 10 to 40% by volume.
The manufacturing method according to any one of claims 1 to 3, wherein the tobacco raw material has a particle size of 0.5 to 2 mm as measured according to ASTM E11-95.
The manufacturing method according to any one of claims 1 to 4, wherein the tobacco raw material is selected from burley varieties, yellow varieties, or a combination thereof.
When the diameter of the tube through which the volatile matter is discharged in the heating step is D1, and the diameter of the tube into which the volatile matter is introduced in the recovery step is D2,
D2/D1≦0.17
The manufacturing method according to any one of claims 1 to 5.
A tobacco extract composition produced by the production method according to any one of claims 1 to 6.
The tobacco extract composition according to claim 7, wherein the turbidity (OD660) measured using a spectrophotometer is 0.90 to 1.80 when the concentration of the polyol component is 15 to 35% by weight.