UA118860C2 - Wax encapsulated zeolite flavour delivery system for tobacco - Google Patents

Abstract

A flavour delivery system for tobacco includes a flavour material entrained in a zeolite material and forming a core and a wax material encapsulating the core.

Description

The present invention relates to flavoring delivery systems for smoking products, where the flavoring material is included in zeolite and encapsulated in wax. This flavoring delivery system can be combined with tobacco for smoking products.

Combustible smoking products, such as cigarettes, typically contain a tobacco substrate, which is cut tobacco (usually in the form of cut filler) surrounded by a paper wrapper that forms a tobacco rod. To use a cigarette, the smoker lights one end of the cigarette and the rod of cut tobacco begins to burn. The smoker then inhales the smoke by taking a puff on the opposite end or end of the cigarette that is brought to the mouth, which usually contains a filter. In these traditional cigarettes, tobacco is burned and temperatures are generated that help release volatile compounds into the inhaled smoke. Cigarettes are known to be equipped with single-segment and multi-segment mouthpiece filters containing flavors such as menthol to modify the flavor of inhaled smoke.

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 marked with the term "aerosol generating product". Examples of systems that use products that generate an aerosol include systems that heat a substrate that contains tobacco above 200 degrees Celsius to form an aerosol that contains nicotine. Typically, in such aerosol-generating heating products, the respirable aerosol is generated by the transfer of heat from the heat source to the substrate or aerosol-forming material, which may be located within, around, or downstream of the heat source. During use of an aerosol-generating product, volatile compounds are released from the aerosol-generating substrate by heat transfer from the heat source and into the air drawn through the product.

As the released compounds cool, they condense to form an aerosol that is inhaled by the consumer.

For example, in the manufacture of these smoking products, the tobacco substrate is heated or dried to remove water. During this heating or drying step, volatile compounds such as flavorings are removed from the tobacco substrate, altering the flavor of the finished smoking product. At this time, flavoring agents are sprayed onto the dried tobacco substrate and this one

The process is denoted by the term "top filling". This procedure is complex because the dosage and final concentration of the flavoring substance on the tobacco substrate can depend on environmental conditions and the design of the spray device. In addition, the flavoring substance can migrate in such a way that it is released from the tobacco substrate during storage. All these factors can lead to undesirable variability in the taste of the product.

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

The flavoring delivery systems of the present invention described herein may be used in conventional combustible smoking products or in the aerosol generating substrate of aerosol generating smoking products. Flavoring delivery systems can provide smoking products with a predictable and consistent release of flavoring. This is particularly useful in combination with aerosol generating substrates that are heated during the production of the aerosol generating substrate.

As described herein, a tobacco flavoring delivery system comprises a flavoring material incorporated into a zeolite and encapsulated in a wax.

Preferably, the waxy material has a melting point of approximately 100 degrees Celsius or higher. The flavoring material can be a hydrophobic liquid.

The zeolite material can be hydrophobic. Smoking compositions contain a flavoring delivery system and tobacco. Preferably, the tobacco is homogenized tobacco or formed leaf tobacco.

Various aspects of the flavoring delivery system described herein may have one or more advantages over standard tobacco compositions. For example, flavoring delivery systems provide an improved flavoring experience compared to tobacco compositions that do not contain a flavoring delivery system. The wax material and the zeolite material do not affect or change the notes of the flavoring substance of the tobacco composition. The wax materials encapsulate a zeolite core with an incorporated flavoring agent to protect the flavoring material during manufacture and storage of a smoking product 60 comprising these tobacco compositions and also predictably release the flavoring material during use of the smoking product. Combining the flavoring delivery system with the tobacco material to form the tobacco composition also ensures uniform distribution of the flavoring material in the tobacco composition. Flavoring delivery systems can replace or enhance tobacco flavoring notes that have been modified during the manufacture of the aerosol generating substrate. In addition, the wax coating or shell that surrounds or encapsulates the zeolite core that includes the flavoring agent can be a sacrificial layer that can perform a heat dissipation function, further protecting the core from releasing the flavoring material during the manufacture or storage of the tobacco composition. Additional advantages of one or more aspects of the flavoring delivery system described herein will become apparent to those skilled in the art after reading and understanding the present invention.

The term "waxy material" refers to natural or synthetic wax products that are hydrophobic and can enter the molten-liquid state (dropping point) at temperatures below 200 degrees Celsius and are virtually free of ash-forming compounds.

The term "flavoring" or "flavoring substance" refers to organoleptic compounds, compositions or materials that change the taste or aroma characteristics of the tobacco substrate when it is consumed.

The term "zeolite material" refers to a silicon dioxide-based material having a microporous structure. Usually, zeolites are microporous aluminosilicate materials.

The term "smoking product" includes cigarettes, cigars, cigarillos and other products 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 smoking does not burn or heat, but uses airflow or a chemical reaction to deliver nicotine, flavoring compounds, or other materials from the tobacco substrate.

As used herein, the term "smoke" or "inhaled smoke" is used to describe the aerosol produced by heating or burning the tobacco substrate of a smoking product. Aerosol produced by a smoking product can be, for example, smoke produced by combustible smoking products such as cigarettes or aerosols produced by non-combustible smoking products such as heated smoking products or non-heated smoking products.

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

The present invention provides flavoring delivery systems for smoking products.

The flavoring delivery system contains the flavoring material incorporated into the zeolite material forming the central portion. The waxy material surrounds the core and forms an encapsulated core or double-encapsulated flavoring material.

The flavoring delivery system described herein provides an improved way to incorporate flavors into a smoking product. The types of flavoring used in smoking products are usually relatively volatile, and it is difficult to maintain acceptable levels of flavoring in smoking products during manufacture and storage. Volatile flavors can also migrate to other parts of the smoking product and can adversely affect the performance of other components of the smoking product, such as any sorbents located within the filter.

The flavoring delivery system can controllably release the flavoring agent or flavoring into the environment by increasing the temperature of the environment. The waxy material forms a shell around the central part. Preferably, the waxy material has a melting (dropping) temperature greater than approximately 100 degrees Celsius. The melting (dropping) temperature can be determined using the standard test method for determining the dropping temperature of waxes known from the ABTM 03954-94(2010) standard.

The flavoring agent or flavoring may be dispersed in the zeolite material. In many embodiments, the flavoring agent or flavoring agent is incorporated into the zeolite material with carbon dioxide in a supercritical state. The core particle can then be encapsulated with the wax material to form the encapsulated core.

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

Spray cooling provides a more uniform particle size than, for example, traditional spray drying. In addition, spray cooling reduces the amount of heat that is supplied to the flavoring material, thereby reducing losses due to evaporation or undesirable changes in the flavoring material. Spray cooling is preferably carried out with an inert gas, such as carbon dioxide or nitrogen, to further reduce conversion or undesirable changes in the flavoring material.

Any applicable zeolite material capable of absorbing flavoring can be used to form the core particle. Many zeolites have been synthesized and many naturally occurring zeolites are known. Zeolites have been classified as "hydrophobic" or "dealuminated" zeolites. The degree of hydrophobicity is determined by the ratio

ZI/AI. Zeolites with a high 5Zi/AI ratio carry less lattice charge and are usually called "hydrophobic" or "dealuminated"; the opposite is true for zeolites with a high aluminum oxide content, which are called "hydrophilic". Some examples of hydrophobic zeolites include silicalite, mordenite, and zeolite U. One of the differences between these zeolites is the size and accessibility of the pores that are present in the zeolite crystals. For example, silicalite and zeolite U have three-dimensional pore systems that are readily accessible, while mordenite's pore system is two-dimensional and therefore not as readily accessible. In terms of pore size, both zeolite B and mordenite belong to the largest known groups of zeolites with pore sizes of approximately 7 and 7.5 Å, respectively; on the other hand, silicalite has a pore size of about 5.5 Å (see R.M.VheskK, 2eoiye MoiIesshiag Zieme5, UMiIeu, Mem HogKk, 1974.). However, there is a size limit for

From selective molecular absorption by hydrophobic dealuminated zeolites, and in many cases hydrophobic zeolites cannot absorb molecules that are too large to pass into their microporous structure. Preferably, the zeolite material is hydrophobic to incorporate the flavoring agent.

Examples of hydrophobic zeolite materials are available commercially under the tradename SHOK8 and 0028 from SpPetieuzhetgk, Germany. Examples of hydrophilic zeolite materials are commercially available under the trade names 13X8 and 4A from

ZiIKet, Slovenia.

In many embodiments, the zeolite material has a particle size of less than about 100 micrometers, or less than about 50 micrometers, or less than about 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 zeolite can be saturated with flavors in any applicable way. Predominantly, the microporous structure of the zeolite is saturated with flavoring by means of saturation with carbon dioxide in a supercritical state. As shown in the examples presented below, the flavoring 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 flavoring into the zeolite material.

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

A hydrophobic liquid flavoring substance is usually able to dissolve in organic solvents, but is poorly soluble in water. Preferably, this hydrophobic liquid flavoring substance is characterized by a Hildebrand solubility parameter of less than 30

MPa", The water incompatibility of most oily liquids can actually be expressed by the Hildebrand solubility parameter b, which is usually below 25 MPa", while for water it is 48 MPa", and 15-16 MPa!? for alkanes. This parameter provides an applicable scale of polarity, which correlates with the energy density of the cohesive bond of molecules. For spontaneous mixing to occur, it is necessary to maintain a minimum difference in the parameters b of the mixing molecules. In the Handbook of Solubility Parameters (ed. A.E.M. Vapop, SKS Rgezv5,

Vossa Kapp, 1991) provides a list of b values for many chemicals, as well as methods for calculating recommended group fractions that allow calculation of b values for complex chemical structures.

Flavorings or flavoring substances refer to a variety of flavoring materials of natural or synthetic origin. They include single compounds and mixtures. Preferably, the flavoring or flavoring substance has flavoring properties that enhance the sensation of a non-combustible smoking product to provide, for example, a sensation similar to that of smoking a combustible smoking product. For example, a flavoring or flavoring agent can improve flavoring properties such as mouthfeel and balance. Balance in the general sense is known as the overall harmony of the flavoring substance, which is more "rich" without the dominance of individual sensory features. The degree of mouth filling is described as the perception of saturation and volume in the mouth and throat of the consumer.

Suitable flavoring agents and flavors include, but are not limited to, any natural or synthetic flavoring agent or flavor such as tobacco, smoke, menthol, mint (such as peppermint and spearmint), chocolate, licorice, citrus and other fruit aromas, gamma-octalactone, vanillin, ethyl vanillin, breath fresheners, spicy aromas such as cinnamon, methyl salicylate, linalool, bergamot oil, geranium oil, lemon oil, ginger oil, etc.

Other suitable flavoring agents and flavors may include flavoring compounds selected from the group consisting of an acid, an alcohol, an ester, an aldehyde, a ketone, a pyrazine, combinations or mixtures thereof, and the like. Suitable flavoring compounds may be selected from, e.g.

Zo from the group consisting of phenylacetic acid, solanone, megastigmatrienone, 2-heptanone, benzyl alcohol, cis-3-hexenyl acetate, valeric acid, valeric aldehyde, ester, terpene, sesquiterpene, nutkatone, maltol, damascenone, pyrazine, lactone, anethole, iso-5 valeric acid, their combinations, etc.

Further specific examples of flavoring substances can be found in modern literature, for example, in the book Repite apa BRiamoig SPpetisa!5, 1969, author 5. Agsiapaeg, Mopisiaig M.9U. (USA);

Eepagoi"5 Napabook oi Riamoshg Ipdgediepiz SES Rgev5, or Zupipeyys Rooy Adiypsi5 author M.V.

Uasore, map Movzigapa So., Ips. They are well known to experts in the field of aromatization, i.e. adding a smell or taste to a product.

In some embodiments, the flavoring agent is a highly effective flavoring agent and is typically used in concentrations that result in less than 200 parts per million in aerosol or inhaled smoke. Examples of such flavoring agents are key tobacco flavoring compounds such as beta-damascenone, 2-ethyl-3,5-dimethylpyrazine, phenylacetaldehyde, guaiacol and furaneol. Humans can perceive other aromas only at higher concentration levels. These flavorants, referred to herein as low-efficiency flavorants, are typically used in concentrations that result in an order of magnitude greater amount of flavorant being released into the aerosol or inhaled smoke. Suitable low-impact flavorings include, but are not limited to, natural or synthetic menthol, peppermint, spearmint, coffee, tea, spices (such as cinnamon, cloves, and ginger), cocoa, vanilla, fruit flavorings, chocolate, eucalyptus, geranium, eugenol and linalool.

Certain flavors useful in the invention described herein are capable of permeating into the zeolite material, preferably by combining the flavoring with supercritical carbon dioxide and the zeolitic material. These flavors include, for example, 3-methylbutanal, furfurylthiol, dimethyltrisulfide, 2-ethyl-3,5(6)-dimethylpyrazine, guaiacol, 3-ethylphenol, or 4-isopropylphenol.

The flavoring material may be present in the central portion in any applicable amount. In many embodiments, the flavoring agent is present in the central portion in an amount of at least about 1 wt.95. In many embodiments, the flavoring agent is present in the central portion in an amount less than about 50 wt. 95. In many embodiments, the flavoring agent is present in the central portion in an amount of from about 1 to about 50 wt. 95, or from about 1 to about 25 wt. 95, or from about 1 to about 10 wt. 95.

The central portion may have any applicable particle size or largest transverse dimension. In many embodiments, the central portion has a particle size of about less than 30 micrometers or about less than 20 micrometers. In many embodiments, the central portion has a particle size greater than about 1 micrometer or greater than about 5 micrometers. In many embodiments, the central portion 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 useful for encapsulating the 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. Animal waxes include, for example, beeswax, china wax, lanolin, shellac, spermaceti wax, and the like.

Vegetable waxes include, for example, carnauba wax, candelilla wax, mirica wax, sugarcane wax, castor wax, esparto wax, japonica wax, jojoba wax, ourikuri wax, rice bran wax, soy wax, and the like. Mineral waxes include, for example, ceresine wax, montan wax, mountain wax, peat wax, and the like.

Petroleum waxes 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 applicable wax materials do not alter the flavoring of the tobacco substrate, have a suitable melting or dropping point, flash point, ignition point, polarity, and are safe to use. The flash point and ignition of wax materials is particularly important when the flavoring delivery system described herein is combined with tobacco and heated in the manufacture of the tobacco substrate. It is preferable to use wax materials having a flash point and ignition temperature that exceed the temperatures affecting the wax materials in the manufacturing process. The flash point is the lowest temperature at which a flame will ignite the vapors of the heated filler, while the ignition temperature is the lowest temperature at which the vapors ignite and burn 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. Flavoring may be released from the flavoring delivery system when the wax material is heated above its melting point. In preferred embodiments, the wax material of the flavoring delivery system has a melting point of approximately 100 degrees

Celsius or above or about 120 degrees Celsius or above 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 about 100 degrees Celsius to about 150 degrees Celsius, or about 110 degrees Celsius to about 140 degrees Celsius. In many embodiments, the waxy material has a melting point of up to about 200 degrees Celsius.

Examples of applicable waxes include polyethylene waxes, polyethylene glycol waxes or vegetable waxes. Typical examples of polyethylene waxes are sold under the trade name SEKISO5T by Siagiapi Ipieeeegpayopa! (4., Switzerland. Typical examples of polyethylene glycol waxes are sold under the trade name SAKVOUMAH by the company Juom/ Spetisai! Co., USA. Typical examples of vegetable waxes are sold under the trade name KEME/!. by the company I ode5 StoKiIaap, the Netherlands.

Use of the flavoring delivery system described herein to provide flavoring within a smoking product advantageously reduces the loss of flavoring during storage in order to retain a greater proportion of flavoring in the smoking product. Therefore, the flavoring delivery system can deliver a more saturated flavoring to the inhaled smoke. Because the loss of flavoring is reduced, less flavoring can be included in each smoking product, while providing the same flavoring effect as is provided in modern smoking products.

The encapsulated central portion may have any applicable particle size or maximum transverse dimension. In many embodiments, the encapsulated central portion has a particle size of about less than 200 micrometers or about less than 100 micrometers. In many embodiments, the encapsulated core has a particle size greater than about 5 micrometers or greater than about 10 micrometers. In many embodiments, the encapsulated central portion has a particle size ranging 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 can be combined with the wax material in any applicable amount to form an encapsulated core or flavoring delivery system. In many embodiments, the central portion represents at least about 1 wt. 95 of the total weight of the encapsulated particle of the central part. In many embodiments, the central portion is at least about 5 wt. 90 of the total weight of the encapsulated particle of the central part. In many embodiments, the central portion is less than about 50 wt. 95 of the total weight of the encapsulated particle of the central part. In many embodiments, the core portion ranges from about 1 to about 50 wt. 95 of the total weight of the encapsulated core particle, or from about 5 to about 50 wt. 95 of the total weight of the encapsulated core particle, or from about 5 to about 25 wt. 95 of the total weight of the encapsulated particle of the central part.

The flavoring delivery system can be combined with a tobacco material to form a tobacco or smoking composition that provides a consistent and predictable release of the flavoring as the tobacco or smoking composition is heated to a temperature at which the waxy material melts and releases the flavoring into inhaled smoke. or in an aerosol for use. The flavoring delivery system can be combined with cut tobacco to form a tobacco composition or smoking composition for use with traditional combustible smoking products. Preferably, the flavoring delivery system can be combined with reconstituted or homogenized tobacco to form a tobacco composition or smoking composition for use with aerosol generating products. Preferably, homogenized tobacco is formed leaf tobacco.

Smoking products that include aerosol generating devices typically contain an aerosol generating substrate that is assembled, often with other components, in the form of a rod.

Typically, such a rod is shaped and sized to allow insertion into an aerosol generating device containing a heating element for heating the aerosol generating substrate. "Aerosol-forming substrate", in the context of this document, is a type of smoking composition that can be used to produce an aerosol in an aerosol-generating device. The aerosol-forming substrate may release the aroma compound when burned or heated. The substrate can contain both solid and liquid components. The aerosol-forming substrate may contain tobacco and a flavoring delivery system where the flavoring is released from the substrate upon heating. The aerosol-forming substrate may additionally contain an aerosol-forming substance. Examples of suitable substances for aerosol formation are glycerin and propylene glycol. Optionally, the substrate that forms the aerosol can be provided on the carrier or included in the carrier, which can take the form of powder, granules, pellets, pieces, bundles of spaghetti, strips or layers. The substrate that forms the aerosol can be applied to the surface of the carrier in the form of, for example, a layer, a foam, a gel or a suspension. The aerosol-forming substrate can be applied to the entire surface of the carrier or, alternatively, can be applied in a pattern to provide non-uniform delivery of the flavoring agent during use.

Homogenized tobacco can be used to make an aerosol generating substrate for use in smoking products that are heated in an aerosol generating device. As used herein, the term "homogenized tobacco" means the material formed by the agglomeration of tobacco in particulate form. Tobacco dust generated by grinding tobacco during transportation and manufacturing, leaf lamina, stalks and other tobacco waste that is very finely ground can be mixed with a binder to agglomerate the tobacco in the form of particles. Homogenized tobacco may contain other additives in addition to the flavoring composition or flavoring delivery composition, including, but not limited to, aerosolizing agents, plasticizers, wetting agents and non-tobacco fibers, fillers, aqueous and non-aqueous solvents, and combinations thereof. Homogenized tobacco can be molded, extruded or 60 rolled. Several recovery methods are known from the prior art for the production of homogenized tobacco materials. They include, among other things, paper production processes of the type described, for example, in document 05 5724998; forming processes (formation of sheets) related to the type described, for example, in document 05 5724998; dough recovery processes of the type described, for example, in document 5 3894544; and extrusion processes of the type described, for example, in document SV 983928.

The flavoring delivery system can be incorporated into the substrate of formed sheet tobacco formed in the sheet forming process. This type of method is known as a sheet 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 suspension and combining a flavoring delivery system in the suspension.

The slurry can then be formed and dried (heated) to remove the water and form the formed sheet tobacco substrate.

The process of forming the sheets may include the application of temperatures up to about 140 "C, such as 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, whereby the flavoring agent is not released during the heating step of the sheet forming process. In many embodiments, the waxy material has a melting point that is substantially equal to the drying temperature of the drying step of the sheeting process. In some embodiments, the waxy material has a melting point that is less than the drying temperature in the drying step of the sheet forming process. In these embodiments, at least a portion of the shell or waxy material melts away from the core and is dispersed within the homogenized tobacco material. Preferably, the waxy material has a melting temperature greater than emperature used to form the substrate of molded leaf tobacco.

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

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

The conjunction "or" used in this application is generally used in a sense that includes "and/or" unless the context clearly indicates otherwise. The term "and/or" means one or all of the listed items or a combination of any two or more of the listed items.

As used in this application, the terms "have", "which has", "include", "which includes", "contain", "containing" or the like are used in their broadest sense, and generally mean "including without limitation". It should be understood that the terms "consisting essentially of 3", "which consists of", etc. refer to the category "which contains", etc.

The words "preferred" and "predominantly" refer to embodiments of the invention that may provide certain advantages under certain circumstances. However, other embodiments may also be preferred under the same or different circumstances. In addition, the listing of 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.

In fig. 1 shows a schematic representation of a typical flavoring delivery system 10 or an encapsulated flavoring core. The schematic representation is not necessarily to scale and is presented for purposes of illustration and not limitation. The graphic materials depict various aspects described in the present invention.

However, it should be understood that other aspects not depicted in the graphic materials fall within the scope and spirit of this invention.

As shown in the figure, the flavoring delivery system 10 includes a flavoring material 12 incorporated into a zeolite material 14 forming a central portion 11 and a waxy material 16 encapsulating the central portion 11.

The central part 11 has the particle size or the largest transverse dimension of 0Och.

Flavoring delivery system 10 has a particle size or largest cross-sectional dimension of O''.

Non-limiting examples illustrating a flavoring delivery system as described above and tobacco substrates and smoking products containing such flavoring delivery systems are described below.

Examples

Various wax materials were evaluated as described below for their applicability in a flavoring delivery system as described above.

Flash and ignition temperatures for selected wax fillers were determined according to

IBO 2592 (method using the Cleveland apparatus with an open crucible). The flash point is the lowest temperature at which a flame will ignite the vapors of the heated filler, while the ignition temperature is the lowest temperature at which the vapors ignite and burn 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 on the pressure. The results of this test (at atmospheric pressure) are shown in Table 1.

Table 1

Temperature Temperature Temperature

Type of ignition wax 2 Supplier | melting about flash SS) o

So) So)

Rice bran 5.

Sunflower wax Natural wax 305 335 Kapizakh/Capizakh 74-80

Kapizakh 6607

Carnauba wax (Kapimah Natural wax 315 345 Kapizakh/Kapizhakh 82-86 24421

Candelilla wax (Kapimah Natural wax 269 2993 Kapizakh/Kapizhakh 68-73 2039

Psomzhakh 521 Polyethylene 249 5309 SiapapuRagka 101-106

REO wax 9.0.0. wax 9.0.0. wax 9.0.0.

Smaller

Fischer's wax - from Zazoimakh/nО5

Fischer's wax - from Zazoimakh/nО5

Smaller

Smaller

RE b00o 55-50

RES 35000 60-65 wax 9.0.0.

Hodeg Stockwap | -:- (

The organoleptic analysis of wax materials is carried out using the descriptive criterion "general organoleptic neutrality" to indicate differences in saturation.

Since organoleptic and psychological fatigue occurs after 7-8 samples, a balanced incomplete block plan (Viv) (ISO 29842) was chosen for the evaluation test (I5O 8587).

Evaluation experts receive five samples per session in random order and must evaluate the samples according to the criterion. To achieve a sufficient level of accuracy, four sessions are conducted.

The results of this VIV assessment are shown in Table 2.

Table 2 0 art pvbdu----- 0 |thovyi 77777777 Y1117171717145.. 1 A | HER HER 1

Oesehmt920 -////////// Ї777771737

ZagomahNni 77777 | 35 | And Vs

Sepdyvi 3610. ss 17717117 33 (AND AXLES | HER

Sepdyvi205i.i 7/7 |. 33 A AXLES | HER

Sshpanv 77777777 HER 33 |A | AXLES | HER

MevyuzhakhENTO0 - | with | /vi'isI

MevyumakhZNIO5 g | 28 | vi'is1/o

ZavomahNio5i -: | 27 | / v/s o0|1ЕЙ /

Kapmakh2811 (Rysovyvysivk)i | 27 | / В|сСс/| 011 ЕИ / ovo svi 0СЗ58-------ЕН-

Kapmakh2039 (Kandelilskyi) | 23 | / |Сс/ 0 EE

OeshehMEIi6b20 C |Ї7777717718 | 77177717 1 101 EE mm o Yueshekhmhevgo7777777/ |77771771717 177177 1 1011 EE

Shisomach REO BALLON | 77/15... | | | | | EE (Kapmahbb0o7(Sonyashniyum.d | 14 (| | | | | | g

Several flavoring delivery systems are formed by incorporating the flavoring into the molded material using supercritical carbon dioxide. In this way, the solubility of various flavors in carbon dioxide in the supercritical state is determined.

Phase equilibria of the flavoring substance in CO"

Observations of the behavior of the phases are 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 200C. This cell with a viewing window is equipped with a propeller stirrer that provides vortex mixing. The viewing window cell is heated using an electric heating element connected to a thermostat (Eigoipegt 22166).

The temperature inside the cell is measured using a Mi-St thermocouple (ETN 1150 Steiivipdeg eIesigopis, error -1.0 "С). The pressure is measured using a digital manometer (UmMiKa, error 0.1 bar). Liquid CO" was loaded into the cell with a viewing window using a high-pressure pump (max. pressure 600 bar).

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

З Observations of phase equilibrium are carried out for the flavoring agent 3-methylbutanal in carbon dioxide. The mixture of 3-methylbutanal and CO is initially brought into a heterogeneous state (two-phase region). The temperature is kept constant and the pressure is slowly varied by changing the cell volume until the second phase disappears. Phase transitions are determined visually.

The phase transition line is constructed for two different ratios of the volume of CO2 - C3 - methylbutanal relative to the total maximum volume of the cell: 5 and 2 (volume/volume) and is shown in Fig. 3. In fig. It can be seen that the solubility of CO2 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" and 3-methylbutanal above the phase transition line - a single-phase region. The phase transition line for the two-component system with a higher ratio of CO::3-methylbutanal (K-5) is slightly higher compared to a ratio of 2.

Observation of the phase balance is carried out for the flavoring mixture of the flavoring agent "RMI Keu" in carbon dioxide. The mixture of flavoring substance PMI Keu is presented in the following table 3.

Table C

Observe the behavior of the phases in the system consisting of a mixture of the flavoring substance PMI Keu/CoO" in the pressure range from 50 to 250 bar in the temperature range from 40 "C to 130 "C. The mixture of flavoring substance PMI Keu and CO2 is initially brought into a heterogeneous state (two-phase 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 constructed for the ratio

CO::Keu-5 flavoring mixture (v/v) relative to total maximum cell volume. It can be seen that the phase transition line follows a linear trend. The results are presented in fig. 4.

Analysis of zeolite

Two different zeolite materials are used to cover the range of polarities of commercially available zeolites. The following materials were analyzed as typical examples of hydrophilic zeolites: 13X and 4A (5II KEM, Slovenia). The following materials were analyzed as typical examples of hydrophobic zeolites: KV and 28 (SpetieuegK, Bad

Köstryts, Germany). The inclusion of zeolites 13X and Ш28 in the process of forming sheets in the volume of 3 kg. the use and formation of the tobacco substrate are analyzed for the presence of silicon in the aerosol formed by the tobacco substrate. The results show that silicon dioxide was not detected in the aerosol.

Release of flavoring substance from the zeolite core

In order to evaluate the ability of a material based on silicon dioxide (zeolites) to retain and release flavoring ingredients, thermogravimetric analyzes were conducted, during which the loss of flavoring substance in zeolite materials loaded with

With a flavoring agent. In fig. 5 shows the results of the release of the flavoring substance by various zeolites, which can be used as the material of the central part. The flavor retention of hydrophilic zeolites ranges from 7.7 to 8.2 95, while hydrophobic zeolites exhibit flavor ingredient retention of up to 23 95. The release temperatures indicate that the core material must protect the flavor ingredients from inadvertent flavor release. substances in the process of sheet formation.

Evaluation of the materials of the shell of the central part

The following Table 4 shows the placement of the zeolite material (0278) loaded with flavoring and encapsulated in the wax material (Segidivi 3610). The flavoring delivery system was formed by incorporating the flavoring agent into the zeolite to form the core and subsequently cooling the core by spraying with a wax material (Segidiby 3610) to form the encapsulated core or flavoring delivery system. The central part was about 10 weights. 95 of the total weight of the first seven delivery systems. The last sample contained 20 weights. 95 of the central part loaded into the shell material.

Table 4

Loading

Shell material material of the central part of the central part 4-isopropylphenol Keu substance Keu substance Keu substance

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

The particle size distribution is measured by the laser diffraction method using the device

Maimegt Mabwiegwigeg 2000. The device for studying liquid dispersion "Nuygo MI" is used to measure particles that are dispersed in ethanol. After dispersing the samples in ethanol, the ultrasonic bath is turned on for three minutes to grind agglomerates.

Measurements begin after 1 minute. All samples are measured twice and average values are reported. Data interpretation is carried out according to the Fraunhofer theory.

Maevhieghieg grinds the agglomerates using an ultrasonic bath before measuring the particle size; the particle size measured by the laser diffraction method differs from the expected particle size of the sieved fractions. Sieving of samples does not destroy agglomerates and the sieved fractions actually consist of agglomerates and not single particle fractions.

In fig. 6th fig. 7 shows the particle size distributions of the central shell samples from the examples listed in Table 2, formed as a result of the spray cooling process described above. Two ranges of particle sizes (63-125 µm and 125-250 µm) are collected and analyzed for bulk density and flavor release, presented below.

The volume density of the samples of the central part-shell from the examples specified in Table 2 is measured according to IM I5O 697. Fig. 8 and fig. 9 shows volume densities.

In fig. 10 shows images obtained using a scanning electron microscope (SEM) of pure spray-cooled Segidivy C3610. In fig. 11 shows a scanning electron microscope (SEM) image of pure unloaded zeolite 028. Fig. 12 presents a scanning electron microscope (SEM) image of a flavoring delivery system consisting of Segidib5i C3610--10 95 unloaded zeolite.

As shown in fig. 10-42, the shape of the particles of the pure atomized Segidibia 3610 and the shape

Z particles with encapsulated zeolites are spherical, and the surface is almost smooth. In contrast, the particles of pure unloaded zeolites have an angular shape. In the volume of particles of the sprayed suspension of Segidivy 3610 and unloaded zeolites, almost no angular particles were detected, which indicates that most of the zeolites are encapsulated in Segidivy 3610.

Release of flavoring substance

Flavor release from the flavor delivery system was then assessed. The aroma delivery system described in this document was formed by saturating zeolites and subsequent cooling by spraying. The flavoring delivery system was added to the molded sheet suspension prior to forming the molded sheet tobacco substrate at a concentration of C 95 (w/w). The molded sheet was formed according to a standard sheet forming procedure, which includes a drying step at a temperature of approximately 100 C. Nothing unusual was observed during the manufacture of the molded sheet, indicating no or low loss of flavoring agent. Using the formed molded sheet, consumables (tobacco sticks) were produced for use in the aerosol generating substrate.

The release of the flavoring substance was analyzed according to the reference regime of intensive smoking according to the Ministry of Health Canada. The results are shown in fig. 13.

Claims (16)

FORMULA OF THE INVENTION 1. A flavoring delivery system for smoking products, which contains: flavoring material, which is included in the zeolite material and forms the central part; and a waxy material that surrounds the central portion and forms the encapsulated flavoring substance particle. 2. The flavoring delivery system of claim 1, wherein the waxy material has a melting point of about 100 degrees Celsius or higher. 3. The aroma delivery system according to claim 1 or claim 2, characterized in that the zeolite material is hydrophobic. 4. A flavoring delivery system according to any of the preceding items, characterized in that the flavoring material is a hydrophobic liquid. 5. The flavoring delivery system of any of the preceding claims, wherein the zeolite material has a particle size in the range of about 1 micrometer to about 20 micrometers. b. A flavoring delivery system according to any one of the preceding claims, wherein the encapsulated flavoring agent particle has a particle size in the range of about 5 micrometers to about 80 micrometers. 7. A smoking composition comprising a tobacco material and a flavoring delivery system according to any of the preceding items. 8. The composition for smoking according to claim 7, which is 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 formed leaf tobacco. 10. The composition for smoking according to any one of claims 7-9, which is characterized in that at least part of the waxy material is separated from the central part during melting and is dispersed inside the tobacco material. 11. A smoking product comprising an aerosol-forming substrate comprising a smoking composition according to any one of claims 7-10. 12. A method of forming a composition for smoking, which includes: combining tobacco material with a flavoring substance delivery system according to any of claims 1-6 to form a tobacco mixture; and heating the tobacco mixture to form the smoking composition. 13. The method of forming a composition for smoking according to claim 12, which is characterized by the fact that the tobacco material contains homogenized tobacco and water, and at the stage of heating, at least part of the water is removed from the tobacco mixture to form the composition for smoking. 14. The method of forming a composition for smoking according to claim 12 or claim 13, which is characterized by the fact that at the heating stage at least part of the wax material is melted. 15. The method of forming a composition for smoking according to claim 12 or claim 13, which is characterized by the fact that the wax material is not melted during the heating stage. 16. 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M. Hrushevskyi, 12/2, Kyiv, 01008, Ukraine SE "Ukrainian Institute of Intellectual Property", 1 Glazunova St., Kyiv - 42, 01601