RU2676074C1 - Wax encapsulated zeolite flavour delivery system for tobacco - Google Patents

Abstract

FIELD: tobacco industry.SUBSTANCE: invention relates to a tobacco flavour delivery system comprising a flavour material entrained in a zeolite material and forming a core; and a wax material encapsulating the core and forming an encapsulated flavour particle.EFFECT: ensuring the uniformity of taste of the smoking article and storage stability of flavours added to the tobacco substrate.16 cl, 13 dwg, 4 tbl

Description

The present invention relates to flavor delivery systems for smoking articles in which the flavor is incorporated into zeolite and encapsulated in wax. This flavor delivery system can be combined with tobacco for smoking products.

Flammable smoking articles, such as cigarettes, typically contain a tobacco substrate, which is cut tobacco (usually in the form of a cut filler) surrounded by a paper wrapper forming a tobacco rod. To use a cigarette, the smoker sets fire to one end of the cigarette, and the shredded tobacco rod begins to burn. The smoker then takes inhaled smoke into his mouth, puffing at the opposite end or end of the cigarette to the mouth, which usually contains a filter. In these traditional cigarettes, tobacco burns and temperatures form, releasing volatile compounds into the smoke inhaled by the smoker. It is known that to modify the aroma of smoke inhaled by a smoker, cigarettes are equipped with single-segment and multi-segment mouthpiece filters containing flavors such as menthol.

Several smoking articles are known in which an aerosol generating substrate, such as a tobacco substrate, is heated rather than burned. Such products may be referred to by the term “aerosol generating products”. Examples of systems using aerosol generating products include systems that heat a tobacco-containing substrate above 200 degrees Celsius to form a nicotine-containing aerosol. Typically, in such heated aerosol generating articles, the inhaled aerosol is typically generated by transferring heat from a heat source to a substrate or aerosol forming material that can be located inside, around, or downstream of the heat source. During use of the aerosol generating article, volatile compounds are released from the aerosol forming substrate by transferring heat from the heat source and into the air drawn through the article. When the released compounds are cooled, they condense to form an aerosol inhaled by the consumer.

For example, in the manufacture of these smoking articles, the tobacco substrate is heated or dried to remove water. During this heating or drying step, volatile compounds, such as flavors, are removed from the tobacco substrate, changing the taste of the finished smoking article. Currently, aromatics are sprayed onto the dried tobacco substrate and this process is referred to as “top fill”. This procedure is complex because the dosage and final concentration of aromatic substance on the tobacco substrate may depend on environmental conditions and the design of the spray device. In addition, the aromatic substance can be moved in such a way as to stand out from the tobacco substrate during storage. All of these factors can lead to undesirable variability in the taste of the product.

It is desirable to improve the uniformity of the taste of the smoking article and the storage stability of flavorings added to the tobacco substrate (tobacco rod or aerosol generating substrate).

The flavor delivery systems of the invention described herein can be used in traditional combustible smoking articles or in an aerosol generating substrate of aerosol generating smoking articles. Aroma delivery systems can provide smokers with a predictable and stable release of aroma. This is especially useful when combined with aerosol generating substrates that are heated during the production of an aerosol generating substrate.

As described herein, a flavor delivery system for tobacco includes a flavor included in zeolite and encapsulated in wax. Preferably, the wax material has a melting point of about 100 degrees Celsius or higher. The aromatic substance may be a hydrophobic liquid. The zeolite material may be hydrophobic. Compositions for smoking include a flavor delivery system and tobacco. Preferably, the tobacco is homogenized tobacco or molded tobacco sheet.

Various aspects of the flavor delivery system described herein may have one or more advantages over standard tobacco compositions. For example, aroma delivery systems provide an improved aroma sensation compared to tobacco compositions not containing an aroma delivery system. Wax material and zeolite material do not contribute or alter the aromatic notes of the tobacco composition. Wax materials encapsulate a zeolite core with an aromatic substance incorporated to protect the aromatic substance during manufacture and storage of the smoking article including these tobacco compositions, and also release the aromatic substance in the predicted manner during the use of the smoking article. Combining the flavor delivery system with the tobacco material to form the tobacco composition also provides a uniform distribution of the flavor in the tobacco composition. Aroma delivery systems can replace or improve the notes of tobacco aromatic substances that have been modified during the manufacture of the aerosol generating substrate. In addition, the wax coating or shell surrounding or encapsulating the zeolite core comprising the aromatic substance can be a sacrificial layer that can act as a heat exchanger, further protecting the core from the release of the aromatic substance during the manufacture or storage of the tobacco composition. Further advantages of one or more aspects of the flavor delivery system described herein will become apparent to those skilled in the art after reading and understanding the present invention.

The term “wax material” refers to products of natural or synthetic wax that are hydrophobic and can transform into a molten-liquid state (dropping temperature) at temperatures below 200 degrees Celsius and practically do not contain ash-forming compounds.

The term "flavoring" or "aromatic substance" refers to organoleptic compounds, compositions or materials that alter the taste or aromatic characteristics of a tobacco substrate when consumed.

The term “zeolite material” refers to a silica-based material having a microporous structure. Typically, zeolites are microporous aluminosilicate materials.

The term “smoking article” includes cigarettes, cigars, cigarillos and other articles in which smoking material, such as tobacco, is ignited and burned to produce smoke. The term “smoking article” also includes articles in which the smoking composition does not burn, such as, but not limited to, smoking articles that directly or indirectly heat the smoking composition without igniting or burning the smoking composition, or smoking articles in which the smoking composition does not burn or heat, and an air stream or chemical reaction is used to deliver nicotine, an aromatic compound, or other materials from the tobacco substrate.

As used herein, the term “smoke” or “smoke inhaled by a smoker” is used to describe the aerosol generated by heating or burning a tobacco substrate of a smoking article. The aerosol generated by the smoking article may, for example, be smoke generated by combustible smoking articles, such as cigarettes, or aerosols generated by non-combustible smoking articles, such as heated smoking articles or unheated smoking articles.

As used herein, the term “spraying” refers to a process in which a liquid, which may contain molten material, a solution, an emulsion, or a combination thereof, is forced to flow through one or more openings in the atomizer and is separated into droplets or particles.

The present invention provides flavor delivery systems for smoking articles. The aroma delivery system includes an aromatic substance included in the core forming zeolite material. Wax material surrounds the core and forms an encapsulated core or double encapsulated flavor.

The flavor delivery system described herein provides an improved method for incorporating flavorings into a smoking article. The types of flavors used in smoking articles are generally relatively volatile and it is difficult to maintain acceptable levels of flavors in smoking articles during manufacture and storage. Volatile flavors can also move to other parts of the smoking article and can adversely affect the characteristics of other components of the smoking article, such as any sorbents located inside the filter.

The aroma delivery system can in a controlled manner release the aromatic substance or flavor into the environment by increasing the ambient temperature. The wax material forms a shell around the core. Preferably, the wax material has a melting point (drop formation) in excess of about 100 degrees Celsius. The melting point (dropping) can be determined using a standard research method for determining the dropping temperature of waxes, known from ASTM D3954-94 (2010).

The aromatic substance or flavor may be distributed in the zeolite material. In many embodiments, the aromatic substance or flavor is incorporated into the zeolite material with supercritical carbon dioxide. The core particle can then be encapsulated with a wax material to form an encapsulated core.

The core particle may be dispersed in the wax material during the formation of the encapsulated core. Preferably, the core particle is dispersed in the wax material when the wax material is in molten form. The encapsulated core particle may be formed in any suitable manner. Preferably, the encapsulated core particle is formed by any suitable method, such as atomization by spray cooling of a mixture of molten wax and core particle.

Spray cooling provides a more uniform particle size than, for example, conventional spray drying. In addition, spray cooling reduces the amount of heat applied to the aromatic substance, thereby reducing evaporation losses or undesirable changes in the aromatic substance. Preferably, the spray cooling is carried out with an inert gas, such as carbon dioxide or nitrogen, to further reduce the conversion or undesirable changes in the aromatic substance.

Any suitable zeolite material capable of absorbing flavor may be used to form a core particle. Many zeolites have been synthesized and many zeolites found in nature are known. Zeolites have been classified as “hydrophobic” or “dealuminated” zeolites. The degree of hydrophobicity is due to the ratio Si / Al. Zeolites with a high Si / Al ratio carry less lattice charge and are commonly referred to as “hydrophobic” or “dealuminated”; the opposite is true for zeolites with a high content of alumina, which are called "hydrophilic". Some examples of hydrophobic zeolites include silicalite, mordenite and zeolite Y. One of the differences between these zeolites is the size and accessibility of pores present in zeolite crystals. For example, silicalite and zeolite Y have three-dimensional pore systems that are readily available, while the pore system of mordenite is two-dimensional and therefore not readily available. Regarding pore size, both zeolite Y and mordenite belong to the largest known zeolite groups with pore sizes of approximately 7 and 7.5 A, respectively; on the other hand, silicalite has a pore size of approximately 5.5 A (see D.W. Breck, Zeolite Molecular Sieves, Wiley, New York, 1974.). However, there is a size limit for selective molecular absorption by hydrophobic dealuminated zeolites, and in many cases hydrophobic zeolites cannot absorb molecules that are too large and do not fit into their microporous structure. Preferably, the zeolite material is hydrophobic to include an aromatic substance.

Examples of hydrophobic zeolite materials are commercially available under the trade names UK8 and UZ8 from Chemiewerk, Germany. Examples of hydrophilic zeolite materials are commercially available under the trade names 13X8 and 4A from Silkem, Slovenia.

In many embodiments, the zeolite material has a particle size of approximately less than 100 micrometers, or approximately less than 50 micrometers, or approximately less than 20 micrometers. In many embodiments, the zeolite material has a particle size greater than about 1 micrometer, or greater than about 5 micrometers, or greater than about 10 micrometers. Preferably, the zeolite material has a particle size in the range of from about 1 micrometer to about 50 micrometers, or from about 1 micrometer to about 20 micrometers.

The microporous structure of the zeolite can be saturated with flavorings in any suitable way. Preferably, the microporous zeolite structure is saturated with a flavor by saturation with carbon dioxide in a supercritical state. As shown in the examples below, the flavor is dispersed in carbon dioxide at a temperature and pressure suitable for the formation of a single phase. This single phase saturates the microporous structure of the zeolite to incorporate the flavor into the zeolite material.

Flavoring agents or aromatic substances can be liquid or solid aromatic substances (at room temperature of approximately 22 degrees Celsius and a pressure of one atmosphere) and can include aromatic compositions, materials containing aromatic substances, and precursors of aromatic substances. The flavor may include one or more natural flavors, one or more synthetic flavors, or a combination of natural and synthetic flavors. Preferably, the aromatic substance is a liquid. Preferably, the aromatic substance is a hydrophobic liquid.

A hydrophobic liquid aromatic substance is usually able to dissolve in organic solvents, but slightly soluble in water. Preferably, this hydrophobic liquid aromatic substance is characterized by a Hildebrand solubility parameter of less than 30 MPa ^1/2 . Incompatibility with water of most oily liquids can actually be expressed using the Hildebrand solubility parameter δ, which is usually below 25 MPa ^1/2 , while for water it is 48 MPa ^1/2 , and 15–16 MPa ^1/2 for alkanes . This parameter provides an applicable polarity scale correlated with the energy density of the cohesive bond of the molecules. For the occurrence of natural mixing, it is necessary to maintain a minimum difference in the parameters δ of the mixed molecules. The solubility parameters reference book (published by AFM Barton, CRC Press, Bocca Raton, 1991) provides a list of δ values for many chemicals, as well as methods for calculating recommended group fractions that allow calculating δ values for complex chemical structures.

Flavors or aromas refer to a variety of aromatic materials of natural or synthetic origin. They include single compounds and mixtures. Preferably, the flavoring or aromatic substance has aromatic properties that improve the sensation of a non-combustible smoking article to provide, for example, a sensation similar to that of smoking a combustible smoking article. For example, a flavoring or aromatic substance can improve aromatic properties, such as the degree of filling of the oral cavity and versatility. Versatility in the general sense is known as the general balance of aroma, being more “rich” without the dominance of individual sensory attributes. The degree of filling of the oral cavity is described as the perception of density and volume in the oral cavity and throat of the consumer.

Suitable aromatic substances and aromas contain, but are not limited to, any natural or synthetic aromatic substance or aroma, such as tobacco, smoky, menthol, peppermint (such as peppermint and curly mint), chocolate, licorice, citrus and other fruit flavors, gamma octalactone, vanillin, ethyl vanillin, aromas for fresh breath, spicy aromas such as cinnamon, methyl salicylate, linalool, bergamot oil, geranium oil, lemon oil, ginger oil and the like.

Other suitable aromatic substances and aromas may include aromatic compounds selected from the group consisting of acid, alcohol, ester, aldehyde, ketone, pyrazine, combinations or mixtures thereof, and the like. Suitable aromatic compounds may be selected, for example, from the group consisting of phenylacetic acid, solanone, megastigmatienone, 2-heptanone, benzyl alcohol, cis-3-hexenyl acetate, valerianic acid, valerianic aldehyde, ester, terpene, sesquiterpene, nutcatone, maltol, damascenone, pyrazine, lactone, anethole, iso-s valerianic acid, combinations thereof, etc.

Further specific examples of aromatic substances can be found in modern literature, for example, in the book Perfume and Flavor Chemicals, 1969, authors S. Arctander, Montclair N.J. (USA); Fenaroli's Handbook of Flavor Ingredients, CRC Press or Synthetic Food Adjuncts by M.B. Jacobs, van Nostrand Co., Inc .. They are well known to those skilled in the art of flavoring, that is, giving a product a smell or taste.

In some embodiments, the flavoring agent is a highly effective flavoring agent and is typically used in concentrations that result in less than 200 ppm in an aerosol or smoke inhaled by a smoker. Examples of such flavors are key tobacco flavors such as beta-damascenone, 2-ethyl-3,5-dimethylpyrazine, phenylacetaldehyde, guaiacol and furaneol. A person can feel other flavors only at higher levels of concentration. These flavors, which are referred to herein as low-performance flavors, are typically used in concentrations that result in an order of magnitude greater amount of flavor released into the aerosol or smoke inhaled by the smoker. Suitable low-performance flavors include, but are not limited to, natural or synthetic menthol, peppermint, spearmint, coffee, tea, spices (such as cinnamon, cloves and ginger), cocoa, vanilla, fruit flavors, chocolate, eucalyptus, geranium, eugenol and linalool .

Some flavors suitable in the invention described herein are capable of saturating the zeolite material, preferably by combining the flavor with supercritical carbon dioxide and the zeolite material. These flavors include, for example, 3-methylbutanal, furfurylthiol, dimethyl trisulfide, 2-ethyl-3,5 (6) -dimethylpyrazine, guaiacol, 3-ethylphenol, or 4-isopropylphenol.

The aromatic substance may be present in the core in any suitable amount. In many embodiments, the aromatic substance is present in the core in an amount of at least about 1 wt.%. In many embodiments, the aromatic substance is present in the core in an amount of less than about 50 wt.%. In many embodiments, the aroma is present in the core in an amount of from about 1 to about 50 wt.%, Or from about 1 to about 25 wt.%, Or from about 1 to about 10 wt.%.

The core may have any suitable particle size or largest transverse size. In many embodiments, the core has a particle size of less than about 30 micrometers, or about less than 20 micrometers. In many embodiments, the core has a particle size of greater than about 1 micrometer, or greater than about 5 micrometers. In many embodiments, the core has a particle size in the range of from about 1 to about 30 micrometers, or from about 1 to about 25 micrometers, or from about 1 to about 20 micrometers.

Wax materials suitable for encapsulating core particles are selected from the group consisting of natural and synthetic waxes and mixtures thereof. Natural waxes are obtained from animals, plants, minerals and oil. Waxes of animal origin include, for example, beeswax, Chinese wax, lanolin, shellac and spermaceti wax and the like. Vegetable waxes include, for example, carnauba wax, candelilla wax, Mirica wax, sugarcane wax, castor wax, esparto wax, Japanese wax, jojoba wax, whipworm wax, rice bran wax, soy wax and the like . Waxes of mineral origin include, for example, ceresin wax, montan wax, ozocerite wax, peat wax and the like. Waxes of petroleum origin include, for example, paraffin wax, petroleum jelly, microcrystalline wax and the like. Synthetic waxes include, for example, polyethylene waxes, Fischer-Tropsch waxes, chemically modified waxes, substituted amide waxes, polymerized alpha olefins, and the like.

Particularly suitable wax materials do not alter the aromatic substance of the tobacco substrate, have a suitable melting or dropping point, flash point, flash point, polarity and are safe to use. The flash point and ignition temperature of wax materials is especially important when the flavor delivery system described herein is combined with tobacco and heated to produce a tobacco substrate. It is preferable to use wax materials having a flash point and a flash point that are higher than the temperatures affecting the wax materials during the manufacturing process. The flash point is the lowest temperature at which the flame ignites the vapor of the heated filler, while the ignition temperature is the lowest temperature at which the vapor ignites and burns for at least 2 seconds.

In many embodiments, the wax material has a melting point of about 50 degrees or higher, or about 75 degrees or higher, or about 90 degrees or higher. The aromatic substance may be released from the aroma delivery system when the wax material is heated above its melting point. In preferred embodiments, the wax material of the aroma delivery system has a melting point of about 100 degrees Celsius or higher, or about 120 degrees Celsius or higher, or about 140 degrees Celsius or higher, or about 150 degrees Celsius or higher. In many embodiments, the wax material has a melting point in the range of from about 100 degrees Celsius to 150 degrees Celsius or from about 110 degrees Celsius to about 140 degrees Celsius. In many embodiments, the wax material has a melting point of up to about 200 degrees Celsius.

Examples of suitable waxes include polyethylene waxes, polyethylene glycol waxes or vegetable waxes. Typical examples of polyethylene waxes are marketed under the trade name CERIDUST by Clariant International Ltd., Switzerland. Typical examples of polyethylene glycol waxes are marketed under the trade name CARBOWAX by Dow Chemical Co., USA. Typical examples of vegetable waxes are marketed under the trade name REVEL by Loders Croklaan, The Netherlands.

Using the flavor delivery system described herein to provide a flavor within a smoking article advantageously reduces the loss of flavor during storage in order to maintain a large proportion of the flavor in the smoking article. Therefore, the aroma delivery system can deliver a more saturated aromatic substance to the smoke inhaled by the smoker. Since the loss of flavor is reduced, it is possible to incorporate a smaller amount of flavor in each smoking article while providing the same effect on the flavor as provided in modern smoking articles.

The encapsulated core may have any suitable particle size or largest transverse size. In many embodiments, the encapsulated core has a particle size of approximately less than 200 micrometers or approximately less than 100 micrometers. In many embodiments, the encapsulated core has a particle size of greater than about 5 micrometers, or greater than about 10 micrometers. In many embodiments, the encapsulated core has a particle size in the range of from about 5 to about 200 micrometers, or from about 5 to about 100 micrometers, or from about 5 to about 80 micrometers.

The core may be combined with the wax material in any suitable amount to form an encapsulated core or flavor delivery system. In many embodiments, the core represents at least about 1% by weight of the total weight of the encapsulated core particle. In many embodiments, the core represents at least about 5% by weight of the total weight of the encapsulated core particle. In many embodiments, the core represents less than about 50 weight percent of the total weight of the encapsulated core particle. In many embodiments, the core represents a range of from about 1 to about 50 wt.% Of the total weight of the encapsulated core particle, or from about 5 to about 50 wt.% Of the total weight of the encapsulated core particle, or from about 5 to about 25 wt.% of the total weight of the encapsulated core particle.

The aroma delivery system can be combined with tobacco material to form a tobacco or smoking composition that provides a stable and predictable release of the aromatic substance as the tobacco or smoking composition is heated to a temperature at which the wax material melts and releases the aromatic substance into the smoke inhaled by the smoker , or aerosol for use. The aroma delivery system may be combined with shredded tobacco to form a tobacco composition or a smoking composition for use with traditional combustible smoking articles. Preferably, the aroma delivery system may be combined with reconstituted or homogenized tobacco to form a tobacco or smoking composition for use with aerosol generating articles. Preferably, the homogenized tobacco is a molded leaf tobacco.

Smoking articles that include aerosol generating devices typically comprise an aerosol forming substrate that is assembled, often with other components, in the form of a rod. Typically, the shape and size of such a rod is designed to be inserted into an aerosol generating device comprising a heating element for heating the aerosol forming substrate.

An “aerosol forming substrate”, as used herein, is a type of smoking composition that can be used to produce aerosol in an aerosol generating device. The aerosol forming substrate may release an aromatic compound when burned or heated. The aerosol forming substrate may contain both solid and liquid components. The aerosol forming substrate may contain tobacco and an aroma delivery system where the aromatic substance is released from the substrate by heating. The aerosol forming substrate may further comprise an aerosol forming substance. Examples of suitable substances for aerosol formation are glycerin and propylene glycol. Optionally, the aerosol forming substrate may be provided on or incorporated into the carrier, the carrier may take the form of powder, granules, beads, grains, thin tubes, strips or sheets. The aerosol forming substrate may be applied to the surface of the carrier in the form of, for example, a sheet, foam, gel or suspension. The aerosol forming substrate may be applied over the entire surface of the carrier or alternatively may be applied in a pattern to provide a non-uniform flavor delivery during use.

Homogenized tobacco can be used to make an aerosol generating substrate for use in smoking articles that are heated in an aerosol generating device. As used herein, the term “homogenized tobacco” means material formed by agglomeration of tobacco particles. Tobacco dust formed during grinding of tobacco during transportation and manufacture, leaf blade, stems and other tobacco waste, which are ultimately finely ground, can be mixed with a particle agglomeration binder. Homogenized tobacco may contain other additives in addition to the aroma or flavor delivery composition, including, but not limited to, aerosol forming agents, plasticizers, moisturizers, and non-tobacco fibers, fillers, aqueous and non-aqueous solvents, and combinations thereof. Homogenized tobacco may be molded, extruded or rolled. Several reduction methods are known in the art for the manufacture of homogenized tobacco materials. These include, but are not limited to, papermaking processes of the type described, for example, in US Pat. No. 5,724,998; molding processes (sheet forming) related to the type described, for example, in US 5724998; processes for the restoration of pasty mass related to the type described, for example, in US 3894544; and extrusion processes of the type described, for example, in GB 983928.

An aroma delivery system can be integrated into a molded leaf tobacco substrate formed during leaf formation. This type of method is known as the leaf forming method and is widely used in the tobacco industry to produce reconstituted or homogenized tobacco for use in a conventional cigarette. Molded leaf tobacco substrates can be formed by combining homogenized tobacco powder with water, glycerin and other optional additives to form a slurry and combining the aroma delivery system in the slurry. The suspension can then be molded and dried (heated) to remove water and form a substrate of molded leaf tobacco.

The leaf forming process may include applying temperatures up to about 140 ° C, such as, for example, from about 90 ° C to 140 ° C. Accordingly, the wax material of the aroma delivery system is preferably stable at such temperatures. Preferably, the wax material is stable at such temperatures, so that the aromatic substance is not released during the heating step during sheet forming. In many embodiments, the wax material has a melting point substantially equal to the drying temperature in the drying step during sheet forming. In some embodiments, the wax material has a melting point that is less than the drying temperature in the drying step during sheet forming. In these embodiments, at least a portion of the shell or wax material is melted away from the core during melting and distributed within the homogenized tobacco material. Preferably, the wax material has a melting point in excess of the temperature used to form the substrate of the molded tobacco sheet.

All scientific and technical terms used in this document have the meanings commonly used in this field, unless otherwise indicated. The following definitions are intended to facilitate understanding of some of the terms often used in this document.

The singular forms used in this application include embodiments having references to the plural, unless the content clearly indicates otherwise.

Used in this application, the union “or” is usually used in a meaning including “and / or”, unless the content clearly indicates otherwise. The term “and / or” means one or all of the listed elements or a combination of any two or more of the listed elements.

Used in this application, the expressions “have”, “having”, “include”, “including”, “contain”, “containing” or the like are used in their broad sense, and generally mean “including without limitation”. It should be understood that the expressions "consisting essentially of," "consisting of," etc. belong to the category of “comprising”, etc.

The words “preferred” and “preferably” refer to embodiments of the invention that may provide certain advantages in certain circumstances. However, other embodiments may also be preferred under the same or other circumstances. In addition, listing one or more preferred embodiments does not imply that other embodiments are not suitable, and is not intended to exclude other embodiments from the scope of the invention, including the claims.

1 is a schematic illustration of an exemplary aroma or encapsulated aroma core delivery system 10. The schematic is not necessarily drawn to scale and presented for purposes of illustration and not limitation. The graphic materials show various aspects described in this invention. However, it should be understood that other aspects not shown in the graphic materials fall within the scope and essence of the present invention.

As shown in FIG. 1, the aroma delivery system 10 includes an aromatic substance 12 included in the zeolite material 14 forming the core 11, and a wax material 16 encapsulating the core 11.

The core 11 has a particle size or largest transverse dimension D ₁ . The aroma delivery system 10 has a particle size or largest transverse dimension D ₂ .

Non-limiting examples depicting an aroma delivery system as described above, and tobacco substrates and smoking articles containing such aroma delivery systems are described below.

Examples

Various wax materials have been evaluated as described below with respect to their applicability in the aroma delivery system as described above.

Flash point and flash point for selected wax fillers were determined according to ISO 2592 (Cleveland's open method). The flash point is the lowest temperature at which the flame ignites the vapor of the heated filler, while the ignition temperature is the lowest temperature at which the vapor ignites and burns for at least 2 seconds. It should be understood that in practice the melting point of the wax material will depend, for example, on any impurities or other components in the wax, as well as pressure. The results of this study (at atmospheric pressure) are shown in table 1.

Table 1 Type of wax Temperature
ignition
(° C) Flash point
(° C) Provider Melting temperature
(° C) Rice Bran (Kahlwax 2811) Natural wax 299 333 Kahlwax / kahlwax 79–85 Sunflower Wax (Kahlwax 6607) Natural wax 305 335 Kahlwax / kahlwax 74–80 Carnauba Wax (Kahlwax 2442L) Natural wax 315 345 Kahlwax / kahlwax 82–86 Candelilla Wax (Kahlwax 2039) Natural wax 269 299 Kahlwax / kahlwax 68–73 Wax brand Cutina Solid fat 325 341 CareChemicals 83–88 Licowax 521 PED Polyethylene wax 249 > 309 Clariant / Parka d.o.o. 101-106 Ceridust 2051 Polyolefin wax 297 329 Clariant / Parka d.o.o. 108–116 Ceridust 3610 Polyethylene wax 263 > 303 Clariant / Parka d.o.o. 125-130 Deurex MX 9820 Polypropylene wax 277 329 Deurex / deurex 110–118 Deurex ME 1620 Polyethylene wax 261 > 321 Deurex / deurex 122–130 Deurex MT 9120 Fischer-Tropsch Wax 295 339 Deurex / deurex 112–120 Sasolwax h1 Fischer-Tropsch Wax 287 327 Sasolwax / HDS Chemie 112 Sasolwax h105 Fischer-Tropsch Wax there is no data there is no data Sasolwax / HDS Chemie 117 Vestowax EH100 Fischer-Tropsch Wax 267 295 Evonik / Evonik 102-110 Vestowax SH105 Fischer-Tropsch Wax 310 333 Evonik / Evonik 108–114 PEG 6000 Polymer 233 > 259 Merck 55-60 PEG 35000 Polymer 259 > 319 Merck 60–65 Ceridust 6050M Polypropylene wax 271 319 Clariant / Parka d.o.o. 142–148 Revel a Solid fat 319 347 Loders croklaan -

Organoleptic analysis of wax materials is carried out using the descriptive criterion of "general organoleptic neutrality" to indicate differences in saturation. Since organoleptic and psychological fatigue occurs after 7–8 samples, a balanced incomplete block plan (BiB) (ISO 29842) was chosen for the evaluation study (ISO 8587). Evaluation experts receive five samples per session at random and must evaluate the samples according to the criterion. To achieve a sufficient level of accuracy, four sessions are conducted. The results of this BiB assessment are presented in table 2.

table 2 BiB score score Total score Total score LSD = 13LSD = 13 0 Tixosil 45 A I Deurex MT 9120 37 A B Sasolwax h1 35 A B C Ceridust 3610 33 A B C Ceridust 2051 33 A B C Cutina hr 33 A B C Vestowax EH 100 32 B C II Vestowax SH 105 28 B C D Sasolwax h105 27 B C D E Kahlwax 2811 (Rice bran) 27 B C D E III Kahlwax 2442L (Karnaubsky) 25 B C D E F Kahlwax 2039 (Candelilla) 23 C D E F IV Deurex ME 1620 eighteen D E F Deurex MX 9820 17 D E F Licowax PED 521 GR fifteen E F Kahlwax 6607 (Sunflower) fourteen F

Several flavor delivery systems are formed by incorporating an aromatic substance into a zeolite material by incorporating carbon dioxide in a supercritical state. Thus, the solubility of various flavorings in carbon dioxide in a supercritical state is determined.

The phase equilibrium of aromatic substances in CO ₂

Observation of the phase behavior is carried out in a cell with a viewing window with a volume of 62 ml, which is under high pressure. The maximum working pressure and temperature are 700 bar and 200 ° C. This cell with a viewing window is equipped with a propeller stirrer for vortex mixing. The cell with the viewing window is heated by means of an electric heating element connected to a thermostat (Eurotherm 2216e). The temperature inside the cell is measured with a Ni-Cr thermocouple (GTH 1150 Greisinger electronic, accuracy ± 1.0 ° C). Pressure is measured with a digital pressure gauge (Wika, accuracy 0.1 bar). Liquid CO _{2 was} charged into the cell with a viewing window by means of a high pressure pump (max. Pressure 600 bar).

Observations of phase equilibria are carried out for guaiacol flavor in carbon dioxide in the pressure range from 50 to 600 bar at temperatures of 40 ° C, 60 ° C and 80 ° C. The cell with a viewing window with a volume of 62 ml, which was under high pressure, was filled with 20 ml of guaiacol under room conditions. The operating conditions used to monitor the phase behavior are shown in FIG. 2 and are represented as circles.

Observations of phase equilibria are carried out for 3-methylbutanal in carbon dioxide. A mixture of 3-methylbutanal and CO _{2 is} initially brought to a heterogeneous state (biphasic region). The temperature is kept constant and the pressure is slowly changed by changing the volume of the cell until the second phase disappears. Phase transitions are determined visually. The phase transition line is plotted for two different volume ratios of CO ₂ - 3-methylbutanal relative to the total maximum cell volume: 5 and 2 (volume / volume) and is shown in FIG. 3 . In FIG. Figure 3 shows that the solubility of CO ₂ in the liquid phase is relatively high, even at moderate pressures, as indicated by an increase in the liquid level in the two-component system. There is complete miscibility between CO ₂ and 3-methylbutanal over the phase transition line — the single-phase region. Phase transition lines for a two-component system with a high ratio of CO _2: 3-methylbutanal (R = 5) is slightly higher than the ratio of 2.

Observation of phase equilibria was carried out for the aromatic mixture of PMI Key flavoring in carbon dioxide. The PMI Key flavor blend is shown in the following table 3.

Table 3 Compound Odor quality Molar mass in g / mol guaiacol smelling of smoke 124.14 3-ethylphenol phenolic, smelling like skin 122.16 dimethyl trisulfide cabbage, sulfur 126.26 2-ethyl-3,6-dimethylpyrazine earthen 136.20 4-isopropylphenol phenolic, plastic 136.19 2-furfurylthiol coffee 114.17

Monitors the phase behavior of the system consisting of a mixture of aromatic substance PMI Key / CO ₂ in the pressure range from 50 to 250 bar in the temperature range from 40 ° C to 130 ° C. A mixture of the PMI key and CO ₂ aroma is first brought to a heterogeneous state (biphasic region). The temperature is kept constant and the pressure is slowly increased by changing the cell volume until the second phase disappears. Phase transitions are determined visually. The phase transition line is plotted for the ratio of CO ₂ : a mixture of aromatic substances key = 5 (volume / volume) relative to the total maximum volume of the cell. It can be seen that the phase transition line follows a linear trend. The results are shown in FIG. 4 .

Sieving zeolite

Two different zeolite materials are used to cover a range of polarities of commercially available zeolites. The following materials were analyzed as typical examples of hydrophilic zeolites: 13X & 4A (SILKEM, Slovenia). The following materials were analyzed as typical examples of hydrophobic zeolites: UK8 & UZ8 (Chemiewerk, Bad Kestritz, Germany). The incorporation of zeolites 13X and UZ8 into the leaf forming process in a volume of 3% by weight and the formation of a tobacco substrate are analyzed using silicon as an example in an aerosol formed by a tobacco substrate. The results show that silicon dioxide was not detected in the aerosol.

Aromatic release from zeolite core

To assess the ability of a material based on silicon dioxide (zeolites) to hold and release aromatic ingredients, thermogravimetric analyzes were performed to evaluate the loss of aromatic substance in zeolite materials loaded with aromatic substance. In FIG. 5 shows the results of the release of aromatic substances by different zeolites that can be used as core material. The retention of aromatic substances by hydrophilic zeolites is in the range from 7.7 to 8.2%, while hydrophobic zeolites exhibit retention of aromatic ingredients up to 23%. Release temperatures indicate that the core material should protect the ingredients of the aroma from unintentional release of the aroma during sheet formation.

Assessment of core shell materials

The following table 4 shows the placement of the zeolite material (UZ8) loaded with flavor and encapsulated in a wax material (Ceridust 3610). An aroma delivery system was formed by incorporating the aroma into the zeolite to form a core and then cooling it by spraying the core with a wax material (Ceridust 3610) to form an encapsulated core or aroma delivery system. The core comprised approximately 10% by weight of the total weight of the first seven delivery systems. The last sample contained 20 wt.% Of the core loaded into the shell material.

Table 4 Sheath material Core material Core loading Ceridust 3610 UZ8 loaded with 3-methylbutanal 10% Ceridust 3610 UZ8 loaded with furfurylthiol 10% Ceridust 3610 UZ8 loaded with dimethyl trisulfide 10% Ceridust 3610 UZ8 loaded with 2-ethyl-3,5 (6) -dimethylpyrazine 10% Ceridust 3610 UZ8 loaded with guaiacol, 3-ethylphenol,
4-isopropylphenol 10% Ceridust 3610 UZ8 loaded with Key standard flavor 10% Ceridust 3610 UZ8 loaded with Key optimized fragrance 10% Ceridust 3610 UZ8 loaded with Key optimized fragrance twenty%

These samples were then analyzed for particle size distribution, bulk density, and morphology.

Particle size distribution is measured by laser diffraction using a Malvern Mastersizer 2000. The Hydro MU liquid distribution device is used to measure particles distributed in ethanol. After distributing the samples in ethanol, the ultrasonic bath is turned on for 3 minutes to crush the agglomerates. After 1 minute, the measurement begins. All samples are measured twice and indicate average values. The interpretation of the data is carried out according to the Fraunhofer theory.

Mastersizer crushes agglomerates using an ultrasonic bath before measuring particle size; The particle size measured by laser diffraction differs from the expected particle size of the sieved fractions. Sifting of the samples does not destroy the agglomerates and the sieved fractions actually consist of agglomerates, and not of fractions of single particles.

In FIG. 6 and FIG. 7 shows particle size distributions of core-shell samples from the examples shown in Table 2 formed by the spray cooling process described above. Two particle size ranges (63–125 μm and 125–250 μm) are collected and analyzed for bulk density and aromatic release, as presented below.

The bulk density of core-shell samples from the examples shown in Table 2 is measured according to DIN ISO 697. FIG. 8 and FIG. 9 shows bulk densities.

In FIG. 10 shows images obtained by scanning electron microscope (SEM) of pure Ceridust C3610 spray-cooled. In FIG. 11 is an image obtained by scanning electron microscope (SEM) of pure unloaded zeolite UZ8. In FIG. 12 shows an image obtained by a scanning electron microscope (SEM), the flavor delivery system consisting of Ceridust C3610 + 10% of the unloaded zeolite.

As shown in FIG. 10–12 , the particle shape of pure atomized Ceridust 3610 and the particle shape of the encapsulated zeolites is spherical and the surface is almost smooth. In contrast, particles of pure unloaded zeolites have an angular shape. In the volume of particles of the sprayed suspension of Ceridust 3610 and unloaded zeolites, almost no angular particles were detected, which indicates that most of the zeolites are encapsulated in Ceridust 3610.

Aromatic Release

The release of aroma from the aroma delivery system was then evaluated. The aroma delivery system described herein was formed by saturation of zeolites and subsequent spray cooling. An aroma delivery system was added to the suspension of the molded sheet before the formation of the substrate of the molded sheet tobacco at a concentration of 3% (v / v). The molded sheet was formed according to a standard leaf forming procedure, including a drying step at a temperature of about 100 ° C. During the manufacture of the molded sheet, nothing unusual was observed, indicating no loss or low loss of aroma. Using the formed molded sheet, consumables (tobacco sticks) were made for use in an aerosol generating substrate.

The release of aromatic substance was analyzed in accordance with the reference regimen of intensive smoking according to the Ministry of Health of Canada. The results are shown in FIG. 13 .

Claims (20)

1. A flavor delivery system for tobacco, comprising: an aromatic substance incorporated into the zeolite material and forming a core; and a waxy material surrounding the core and forming an encapsulated aromatic particle. 2. The flavor delivery system of claim 1, wherein the wax material has a melting point of about 100 degrees Celsius or higher. 3. The aroma delivery system according to claim 1 or 2, characterized in that the zeolite material is hydrophobic. 4. The aroma delivery system according to claim 1 or 2, characterized in that the aromatic substance is a hydrophobic liquid. 5. The aroma delivery system according to claim 1 or 2, characterized in that the zeolite material has a particle size in the range from about 1 micrometer to about 20 micrometers. 6. The aroma delivery system according to claim 1 or 2, characterized in that the encapsulated aromatic particle has a particle size in the range from about 5 micrometers to about 80 micrometers. 7. A composition for smoking containing tobacco material and a flavor delivery system according to any one of claims 1 to 6. 8. The composition for smoking according to claim 7, characterized in that the tobacco material contains homogenized tobacco. 9. The composition for smoking according to claim 7, characterized in that the tobacco material contains a molded sheet of tobacco. 10. Composition for smoking according to any one of paragraphs. 7-9, characterized in that at least part of the wax material during melting is separated from the core and distributed inside the tobacco material. 11. A smoking article containing an aerosol forming substrate that contains a smoking composition according to any one of claims. 7-10. 12. A method of forming a composition for smoking, including: the combination of tobacco material with a flavor delivery system according to any one of paragraphs. 1-6 for the formation of the tobacco mixture; and heating the tobacco mixture to form a composition for smoking. 13. The method of forming a composition for smoking according to claim 12, characterized in that the tobacco material contains homogenized tobacco and water, and at least one part of the water is removed from the tobacco mixture during the heating step to form a composition for smoking. 14. The method of forming a composition for smoking according to claim 12 or 13, characterized in that at least part of the wax material is melted at the heating stage. 15. The method of forming a composition for smoking according to claim 12 or 13, characterized in that the wax material is not melted at the heating stage. 16. The use of aroma delivery system according to any one of paragraphs. 1-6 in the composition for smoking according to any one of paragraphs. 7-10 to replace or improve notes of tobacco flavoring.

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