ES2666365T3 - Low fragrance carrier adsorption particle, cigarette filter, filter cigarette, and method for preparing low fragrance carrier adsorption particles - Google Patents

Abstract

A method of preparing a flavor-bearing low-adsorption particle, comprising: spraying a liquid flavor-emitting composition containing a flavoring and a flavor-containing material onto a low adsorption core particle with a lower BET surface area at 700 m2 / g, while stirring the low adsorption core particle under reduced pressure.

Description

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DESCRIPTION

Low fragrance carrier adsorption particle, cigarette filter, filter cigarette, and method for preparing low fragrance carrier adsorption particles

Technical field

The present invention relates to a method for preparing the low adsorption particle carrying flavoring.

Prior art

The flavoring carrier particles are included in a cigarette filter, the aroma of the flavoring is emitted in the mainstream of a cigarette, and the smoker enjoys the aroma. For example, patent document 1 describes an aroma microsphere in which the surface of a particulate vehicle, such as calcium carbonate, is covered with a glucan film containing a flavoring agent. This aroma microsphere is prepared according to the following procedure. A particulate vehicle is placed inside a fluidized bed granulation dryer, and an aqueous solution or dispersion of glucan containing a flavoring is continuously or intermittently sprayed onto the surface of the particulate vehicle, while hot air is blown at, for example, 80 ° C or less, inside the dryer, followed by drying.

However, in the method of patent document 1, it takes a relatively long time when a large amount of a flavoring is subjected to the treatment. As a result, it is difficult to increase the amount of a transported flavoring. Patent document 2 describes a method for preparing a low-adsorption particle carrying flavoring, which comprises mixing a liquid composition that emits an aroma containing a flavoring (menthol), a solvent and materials that can be perceived as materials containing flavoring ( additives such as glucans, carbohydrates, polysaccharides, gelatin suitable as film-forming materials, etc.) with a low adsorption core particle (porous silica) with a specific surface area bEt of 600-1200 m2 / g, while stirring, and Dry (for example, in a spray dryer) the low adsorption core particle to remove the solvent.

Prior art documents

Patent documents

Patent document 1: WO 2008/072627

Patent document 2: JP 2006248832

Compendium of the invention

Problem to solve by the invention

Therefore, a main object of the present invention is to provide a method for preparing a low-adsorption particle carrying flavoring that carries a relatively large amount of a flavoring, by treatment in a relatively short time.

Means to solve the problem

To solve the above problem, a method is provided for preparing a low-adsorption particle carrying flavoring, which comprises spraying a liquid composition that emits aroma, containing a flavoring and a material containing a flavoring, onto a low-core particle. adsorption with a specific BET surface area less than 700 m2 / g, while stirring the low adsorption core particle under reduced pressure.

Effects of the invention

In accordance with the present invention, a low-adsorption particle bearing flavoring is provided that conveys a relatively large amount of a flavoring, by treatment in a relatively short time.

A cigarette filter comprising a filter section comprising the low adsorption particle carrying prepared flavoring, and a filter cigarette comprising a cigarette cylinder and said filter can be prepared.

Brief description of the drawings

Figure 1 is a schematic view of a cross-section illustrating an example of an apparatus for preparing a particle of low flavoring carrier adsorption.

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Figure 2 is a schematic view of a cross section illustrating a filter cigarette, comprising a particle of low adsorption of flavoring carrier.

Figure 3 is a schematic view of a cross section illustrating a filter cigarette.

Figure 4 is a schematic view of a cross section illustrating a filter cigarette.

Figure 5 is a schematic view of a cross section illustrating a filter cigarette.

Figure 6 is a graph illustrating a measurement result of the amounts of a transported flavoring and

a material that contains a flavoring.

Figure 7 is a fractured partial schematic view illustrating an apparatus for trapping components contained in the smoke of the mainstream of a cigarette.

Mode for carrying out the invention

Hereinafter, the embodiments of the present invention will be described in detail.

A low-adsorption particle bearing aromatizer comprises a low adsorption core particle and an aroma generating medium transported on the surface of the low adsorption core particle, and which includes a flavoring and a material containing a flavoring containing the flavoring The material containing the flavoring agent is present in an amount of 5 to 20% with respect to the total weight of the low adsorption particle carrying flavoring, and the flavoring is present in an amount of 10 to 50% with respect to the weight of the material It contains a flavoring.

The low adsorption core particle has a specific BET surface area less than 700 m2 / g. In the present specification, the BET specific surface refers to a specific surface obtained according to the public knowledge BET method. The core particle with a specific BET surface area less than 700 m2 / g shows a relatively low adsorption of the components contained in the smoke of the mainstream of a cigarette, and thus, shows little effect on the aroma and taste of the smoke .

Examples of such a low adsorption core particle include calcium silicate, activated carbon with a low degree of activation, silica, ceramics, crystalline cellulose, wood, plant technical product, a styrene-divinylbenzene copolymer, an ethylene copolymer. vinyl acetate, and a water absorbent polymer such as polyvinyl alcohol and sodium polyacrylate.

It is preferable that the low adsorption core particle has an average particle size of 75 to 2000 | im, and for example, a low adsorption core particle with an average particle size of 75 to 1000 | im can be suitably used. In addition, the low adsorption core particle preferably has a water retention capacity of 10% or greater, and more preferably, has a water retention capacity of 20 to 40%. In this document, water retention capacity means the proportion of water retention amount in the case where a core particle is soaked in water, with respect to the dry weight of the core particle, any of the particles of The core of the previous examples shows the water retention capacity mentioned above.

The aroma generating medium that covers the surface of the low adsorption core particle includes a flavoring and a material containing a flavoring containing the flavoring.

Examples of the flavoring include a hydrophilic flavoring and a hydrophobic flavoring. Examples of the hydrophilic flavoring include tobacco leaf extract, natural vegetable flavoring (for example, licorice, carob, plum extract, peach extract, and the like), acids (for example, malic acid, tartaric acid, citric acid, acid butyric acid, and the like), saccharides (glucose, fructose, isomerized sugar, and the like). Examples of the hydrophobic flavoring include menthol, cocoa (powder, extract, and the like), esters (e.g., isoamyl acetate, linalyl acetate, isoamyl propionate, linalyl butyrate, and the like), natural essential oils (such as oils vegetable essentials, for example, vanilla extract, peppermint, peppermint, cassia, jasmine, and the like; as animal essential oils, for example, musk, gray amber, algalia, chastity, and the like), and individual aromas (e.g. anethole , limonene, linalool, eugenol, vanillin, and the like).

The carrier material containing the flavoring contains a film-forming material and an emulsifying agent if needed. Representative examples of the film-forming material used in the present invention include glucan, and examples of glucan include pululane, maltodextrin and hydroxypropyl cellulose. Glucan is water soluble. A film forming material such as glucan is capable of containing a flavoring including the flavoring in the film formed of the film forming material. The film-forming material can be used for any of a hydrophilic flavoring and a hydrophobic flavoring.

Examples of the emulsifying agent include glycerol fatty acid ester, sucrose fatty acid ester (sugar ester), sorbitan fatty acid ester, propylene glycol fatty acid ester, and lecithin.

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The emulsifying agent molecules contain a hydrophobic flavoring in an aqueous medium causing the hydrophobic group of the molecule to adsorb around the oil droplet of the hydrophobic flavoring, and contain the hydrophobic flavoring also after drying.

In the low flavor adsorption particle of the present invention, the material containing a flavor is present in an amount of 5 to 20%, and preferably 5 to 10%, with respect to the total weight of the low adsorption particle carrier of flavoring. In addition, the flavoring is present in an amount of 10 to 50% with respect to the weight of the material containing a flavoring.

The low adsorption particle carrier of flavoring can be prepared by spraying a liquid composition that emits aroma containing the flavoring and the material containing a flavoring, on the low adsorption core particle, while stirring the low pressure adsorption core particle reduced

The flavoring contained in the liquid composition that emits aroma is the same as those described above, and the material containing a flavoring is also the same as those described above.

When the liquid composition emitting aroma contains only one hydrophilic flavoring as flavoring, it is preferable that the liquid composition emitting aroma contains glucan as a film-forming material and a hydrophilic flavoring, and which also contains water as a solvent to dissolve the glucan and the flavoring hydrophilic

When the liquid composition emitting aroma contains a hydrophobic flavoring as flavoring agent (for example, when the liquid composition emitting aroma contains only a hydrophobic flavoring as flavoring, or when the liquid composition emitting aroma contains a hydrophobic flavoring as well as a hydrophilic flavoring such as flavoring agent), it is preferable that the liquid composition emitting aroma contains glucan as a film-forming material, water as a glucan solvent, a hydrophobic flavoring (and a hydrophilic flavoring), an oily solvent for dissolving the hydrophobic flavoring (for example, an oil vegetable or a saturated fatty acid triglyceride, preferably a medium chain saturated fatty acid triglyceride), and an emulsifying agent. When this composition contains a hydrophilic flavoring in addition to the hydrophobic flavoring, the hydrophilic flavoring dissolves in water.

In the preparation of the low adsorption particle carrying flavoring, it is preferable that the particle of the low adsorption core is at a reduced pressure of 12.3 kPa or less, for example, at a reduced pressure of 7.4 to 12.3 kPa , during the spraying of the liquid composition that emits aroma. Furthermore, at that time, it is preferable that the adsorbent core particle is at a temperature of 60 ° C or less, for example, at a temperature of 40 to 60 ° C. By spraying the liquid composition that emits aroma and the material that contains a flavoring under reduced pressure, there are benefits that a large amount of the flavoring can be transported on the core particle of low adsorption, and also that a composition that emits aroma with a high viscosity (for example, a viscosity of about 2 Pa.s) can be sprayed through a spray nozzle.

To prepare the particle of low aroma carrier adsorption, a tapered mixer tape dryer can be used. The tapered tapered mixer dryer is described, for example, in Japanese Unexamined Patent Application Publication (Kokai) No. 2003-71263, Japanese Unexamined Patent Application Publication (Kokai) No. 2003-290641, and publication of Japanese Unexamined Patent Application (Kokai) No. 2007229633. In addition, a conical mixer dryer manufactured by Okawara Mfg is commercially available. Co., Ltd.

The basic structure of such a tapered tapered mixer dryer will be described with reference to Figure 1. Figure 1 illustrates a schematic view of a cross section illustrating an example of a tapered tapered mixer dryer 10. The tapered tapered mixer dryer 10 it comprises a treatment tank 12 for carrying out the mixing and drying treatment, which is constituted by an inverted conical part 121 and a cylindrical part 122 joined on the inverted conical part 121. The tapered tapered mixer dryer 10 comprises a double helix belt rotor blade 14, provided on the inside of the treatment tank 12. The double helix belt rotor blade 14 is attached to multiple support bars (support bars 18a to 18e in Figure 1 ) which are spaced from each other and fixed to a rotating shaft 16, which extends longitudinally along the central axis of the treatment tank 12. To the wall i Inside the cylindrical part 122 of the treatment tank 12, a pair of vortex flow breakers 20a and 20b (for example, with a plate-like structure) are fixed above the rotor blade 14. A treated product ( low adsorption particles in the present invention) rises along the inner wall of the treatment tank 12 by the action of the belt rotor blade 14, and therefore the vortex flow breakers 20a and 20b causes the product treated move near the center of the treatment tank 12 and fall towards the bottom of the treatment tank 12.

The outer limit of the treatment tank 12 is surrounded with a jacket 22. To heat the contents of the tank, steam is introduced through a steam inlet 22a into this jacket 22 by means of a line L1, and the steam is discharged through a steam outlet 22b towards the outside of the system by means of a line L2.

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The upper opening of the tank is closed by an upper board 24. On this upper board 24, a motor 26 and a speed reducer 28 are installed, and the output shaft of the speed reducer 28 is connected to the rotary axis 16 provided in the inner part of the treatment tank 12. Furthermore, in the upper board 24, an inlet 24a is provided for an object to be treated (low adsorption core particles in the present invention), and in the lower part of the storage tank. treatment 12, an outlet 12a is provided for the treated product (low adsorption particles carrying flavoring in the present invention).

In addition, a sleeve filter 30 is attached to the top board 24. Of the contents of the treatment tank 12, this sleeve filter traps particulate material (low adsorption particles in the present invention) and lets the volatile material (water contained in the composition that emits aroma in the present invention). The volatile material that has passed is conducted to a capacitor 32 by means of a line L3. The condenser 32 is configured by, for example, a water-cooled cooler, and the volatile material passes through the inside of an inner tube 321. The volatile material is cooled by cooling water introduced into an outer tube 322 through a line L5, and is discharged through a line L6 as a condensate (water). Water introduced into outer tube 322 is discharged through line L5. The inner tube 321 is connected to a pressure reducing pump P1 by means of a line L7, and the inside of the treatment tank 12 is decompressed by actuating the pressure reducing pump P1.

The basic structure of the tapered mixer tape dryer is as described above. In addition, to prepare the low-adsorption particle carrying the flavoring of the present invention, a spray nozzle 34 is provided to introduce the liquid composition that emits aroma into the treatment tank 12, so that it penetrates through the upper board 24. The spray nozzle 34 sprays the liquid composition that emits LFC aroma into the treatment tank 12 from a container 36, which contains the liquid composition that emits aroma via a line 8 equipped with a liquid feed pump P2. In addition, to measure the temperature of the low adsorption particles in the treatment tank 12, a temperature sensor (for example, thermocouple) 38 is provided at the bottom of the treatment tank 12.

In order to prepare the low adsorption particles carrying aromatizers using the tapered tapered mixer dryer 10 illustrated in Figure 1, the low adsorption core particles LAP contained in a container 40 are introduced into the treatment tank 12 by means of a line L9. The liquid composition that emits aroma contained in the container 36 is sprayed into the treatment tank 12 from the spray nozzle 34 via the line L8, in accordance with the operation of the liquid feed pump P2, while the interior of the treatment tank 12 by introducing steam with a temperature of 80 ° C or higher, preferably from 100 to 120 ° C, inside the jacket 22, and while the low adsorption particles are stirred by rotating the rotor of blade rotor double helix 14 according to the motor 26 drive. During this spraying, it is preferable that the temperature of the low adsorption particles is maintained at 70 ° C or lower, and preferably 60 ° C or lower. This temperature of the low adsorption particles can be maintained by the heat of evaporation taken by the water of the low adsorption particles, when the water of the liquid composition emitting aroma introduced into the treatment tank 12 is heated and evaporated by steam of 80 ° C or higher, inserted into the jacket 22.

In the low adsorption particles carrying flavoring prepared in this way, only water is removed by volatilization during preparation, but almost all other components other than water contained in the liquid composition that emits aroma applied to the low adsorption core particles during preparation, they are transported on the low adsorption core particles. Accordingly, the liquid composition that emits aroma applied to the low adsorption core particles contains the material containing a flavoring in an amount of 5 to 20%, preferably 5 to 10%, with respect to the weight of the particles of Low adsorption core used, and the flavoring in an amount of 10 to 50% with respect to the weight of the material containing a flavoring contained in the liquid composition that emits aroma. The material containing a flavoring contained in the liquid composition that emits aroma, particularly, a part of an aqueous solution or aqueous dispersion of the film-forming material can be applied to the low adsorption core particles in advance. The application in advance of a part of the aqueous solution or aqueous dispersion of the film-forming material makes it possible to contain that the temperature of the low adsorption core particles rises to the initial stage of preparation of the low adsorption particle carrying flavoring, and also suppresses the generation of fine dust from the low adsorption core particles.

In the low-adsorption particle carrier of flavoring, the surface of the low-adsorption core particle is covered with a solid aroma generating medium, formed from the liquid aroma-emitting composition. In this solid aroma-generating medium, the flavoring is contained by the material containing a flavoring, and therefore it is not produced that the flavoring is volatilized or adsorbed on carbon during the usual storage. When the material containing the flavoring is contacted with a hydrophilic component such as water, contained in the smoke of the mainstream generated by smoking, a part of the material containing a flavoring is dissolved there and thus aroma is emitted. As a result, it is possible to enjoy the aroma and flavor of the flavoring smoke.

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A cigarette filter comprises a filter section that includes the low adsorption particles carrying flavoring of the present invention. In addition, a filter cigarette in accordance with the third aspect of the present invention provides a filter cigarette comprising a cigarette cylinder and the filter of the present invention, which is connected to one end of the cigarette cylinder.

The cigarette filter may comprise a filter section in which the low adsorption particles carrying flavoring are dispersed in a general raw material for filter, for example, a bast of cellulose acetate fiber (bound by a plasticizer such as triacetin ). The so-called carbon filter section (a filter section comprising a filter raw material formed by dispersing activated carbon in a cellulose acetate fiber tow linked by a plasticizer such as triacetin) can be connected to one end of the section of previous filter Alternatively, the cigarette filter may comprise a carbon filter section and a single filter section disposed apart from each other, and the low adsorption particles carrying flavoring of the present invention charged in the space between these two filter sections.

Hereinafter, a cigarette with the filter will be described with reference to figures 2 to 5. In figures 2 to 5, the same elements are indicated by the same reference signs.

Figure 2 is a schematic view of a cross-section of a cigarette (cigarette with filter) 50 equipped with the cigarette filter.

A filter cigarette 50 comprises a cigarette cylinder 52 in which a load of tobacco 521, such as tobacco sting, is wrapped with a smoking paper 522. The cigarette cylinder 52 is the same as that of a general cigarette.

A filter 54 is attached to one end of the cigarette cylinder 52. The filter 54 comprises a carbon filter section 541, which is provided to be connected directly to an end of the cigarette cylinder 52, a filter section containing particles of low adsorption of flavoring carriers 542, which is provided at the end of the side that is downstream of the carbon filter section 541 with respect to the direction of smoke flow from the mainstream, and a simple filter section 543 that is it provides at the end of the side that is downstream of the filter section containing low adsorption particles carrying flavoring 542 with respect to the direction of smoke flow of the main stream.

The carbon filter section 541 is, for example, a filter obtained by wrapping a cellulose acetate fiber 541a, in which the carbon particles 541b are dispersed, with a wrapping paper 541c, and can be the same as a filter of general coal.

The filter section containing low adsorption particles carrying flavoring 542 is, for example, a filter obtained by wrapping a cellulose acetate fiber 542a, in which the low adsorption particles carrying FLAP flavoring of the present invention are dispersed, with a wrapping paper filter 542b.

The simple filter section 543 is, for example, a filter obtained by wrapping a bast of a cellulose acetate fiber 543a with a filter wrapping paper 543b.

The filter 54 consisting of the filter sections 541, 542 and 543, is attached to one end of the cigarette cylinder 52 by a nozzle paper 56.

Figure 3 is a schematic view of a cross-section of a cigarette (cigarette with filter) 60 equipped with the cigarette filter.

In this cigarette with filter 60, a filter 62 attached to a cigarette cylinder 52 by a nozzle paper 56 comprises a carbon filter section 541, directly attached to an end of the cigarette cylinder 52, and a simple filter section 622 provided so that it is separated from the carbon filter section 541, and the assembly is wrapped with a filter wrapping paper 66. The simple filter section 622 is formed of, for example, a bast of a cellulose acetate fiber 622a, as the simple filter section 543 illustrated in Figure 2. The space (cavity) 64 between the carbon filter section 541 and the simple filter section 622 is loaded with the low adsorption particles carrying FLAP flavoring of the present invention .

Figure 4 shows a configuration in which the carbon filter section 541 is suppressed in the filter cigarette with the configuration illustrated in Figure 2, and the filter section containing low adsorption particles carrying flavoring 542 is directly connected to one end of the cigarette cylinder 52.

Figure 5 shows a configuration in which a simple filter section 543 (see Figure 2) is used instead of the filter section 541 in the filter cigarette with the figuration illustrated in Figure 3.

Examples

Hereinafter, the present invention will be described using specific examples, but is not limited to the specific examples.

Preparation of liquid composition that emits aroma

A mixture containing the components shown in Table 1 in the proportions shown in Table 1, was emulsified using an emulsifier (ROBOMICS MARK II, manufactured by PRIMIX Corporation) at 7500 rpm for 15 minutes. At this time, the environment of the emulsifier was cooled with water so that the temperature of the mixture did not exceed 45 ° C. In this way, the liquid compositions emitting aroma from A to D were obtained.

COCONARD MT manufactured by Kao Corporation was used as a medium chain saturated fatty acid triglyceride, LP-20E manufactured by The Nisshin OilliO, Ltd. was used as lecithin, and P-1570 manufactured by Mitsubishkagaku Foods Corporation was used as the ester of sugar.

Table 1

 Components

 Mixing ratio (% by weight)

 Liquid composition that emits aroma A

 Liquid composition that emits aroma B Liquid composition that emits aroma C Liquid composition that emits aroma D

 Pululane

 10 10 10 9.5

 Water

 79 76 80 72.3

 Triglyceride of medium chain saturated fatty acids

 5 5 3 4.8

 Lecithin

 2 2 2 1.9

 Sugar ester

 2 2 2 1.9

 1-Menthol

 2 - - 4.8

 Vanillin

 - 5 - -

 Cocoa powder

 - - 3 -

 Butyric acid

 - - - 4.8

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Preparation of low adsorption particles bearing flavoring Example 1

Here, RIBOCONE RM-50-VD, manufactured by Okawara Mfg, was used. Co., Ltd. As a tapered tapered mixer dryer (see Figure 1). 10 kg of calcium silicate (Sanwa Marume, manufactured by Sanwa Insecticide Co., 15 Ltd; average particle size: 1mm; BET specific surface area: less than 700 m2 / g) and 6 kg of an aqueous solution containing 5% by weight of pululane inside the mixer dryer, and steam was circulated at 120 ° C, at a pressure of 200 kPa, in the jacket. The pressure inside the mixer dryer was set at 12.3 kPa and the calcium silicate particles were stirred. After stirring for 5 minutes, 5 kg of the liquid composition emitting aroma A was sprayed through the spray nozzle into the mixer dryer for 40 minutes, and then stirred and further dried for 20 minutes. Calcium silicate particles carrying flavoring were removed from the mixer dryer, immediately placed in a continuous fluidized bed granulation dryer (MIX GRADE 0.5 TYPE, manufactured by Okawara Mfg. Co., Ltd.), and subjected to exchange of Sensitive heat and dehumidification of calcium silicate particles for 3 minutes, thereby obtaining a product of calcium silicate particles carrying flavoring.

25 Example 2

A product of calcium silicate particles carrying flavoring was obtained according to the same procedure as in Example 1, except that a liquid composition emitting aroma B was used instead of liquid composition emitting aroma A.

Example 3

A product of calcium silicate particles carrying flavoring was obtained according to the same procedure as in Example 1, except that a liquid composition emitting aroma C was used instead of liquid composition emitting aroma A.

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Example 4

A product of calcium silicate particles carrying flavoring was obtained according to the same procedure as in Example 1, except that a liquid composition emitting aroma D was used instead of liquid composition emitting aroma A.

Manufacture of cigarette with filter

A filter cigarette was manufactured with a configuration illustrated in Figure 3. More specifically, the filter cigarette with a configuration illustrated in Figure 3 was manufactured according to the following procedure. From a commercially available filter cigarette product, "Winston Ligths", which is equipped with a filter with a cellulose acetate fiber tow as the filter raw material, the cellulose acetate fiber tow was removed using a pair of tweezers Then, the empty space portion was loaded with a cellulose acetate fiber tow (length: 12 mm; 8Y / 29000 (that is, filament fineness: 8 denier; filament cross section: type Y; total fineness: 29000 denier)) which included 85 mg of activated carbon (KURARAY COAL GGS-H28 / 70 manufactured by Kuraray Chemical Co., Ltd), loaded with 42 mg of the calcium silicate particles carrying flavoring obtained in examples 1 to 4 (at 47 mm in length of space 64 in the longitudinal direction of the cigarette cylinder), and finally loaded with a cellulose acetate fiber tow (length: 11 mm; 2.5Y / 35000). In addition, a cigarette with a reference filter was manufactured in the same manner as before, except that space 64 was not loaded with anything.

These four kinds of filter cigarettes underwent smoking experiments. As a result, it was confirmed that the aroma of the flavoring was emitted in the mainstream smoke, and the aroma and flavor were stronger compared to the reference filter cigarette. This result indicates that a large amount of a flavoring was transported on a low adsorption core particle by a short time treatment according to the method of the present invention.

Measurement of amounts of flavoring transported and material containing a flavoring

In relation to the flavoring carrier particles obtained in examples 1 to 4, the amount of the flavoring transported and the amount of the material containing a flavoring were measured.

The flavoring carrier particles of the comparative examples were prepared according to examples 1 to 3 of the prior art document (WO 2008/072627). In relation to the flavoring carrier particles prepared in this way, the amount of the flavoring transported and the amount of the material containing a flavoring were measured in the same manner as those in examples 1 to 4.

The flavoring carrier particles according to the comparative examples were prepared as follows.

Comparative example 1 (example 1 of the prior art document)

2% by weight of coffee oil was added to a previously prepared aqueous dispersion of pululane containing 10% by weight of pululane. The mixture was vigorously stirred in an emulsifier (emulsifier rotation speed of 2500 rpm), thereby preparing a dispersion of flavoring. On the other hand, 100 g of calcium carbonate particles with an average particle size of 250 µm were loaded into a fluidized bed granulation dryer, and immediately the flavoring dispersion was sprayed intermittently on the particles (in cycles repeated spraying for 1 minute, and then without spraying for 30 minutes), while hot air was blown at 75 ° C with a flow rate of 0.6 m / s. In this way, a total of 10 g of dispersion of flavoring was sprayed on the surface of the calcium carbonate particles, followed by drying. After that, the inside of the fluidized bed was immediately cooled to room temperature, thereby obtaining the desired aroma microspheres.

Comparative example 2 (example 2 of the prior art document)

100 g of calcium carbonate particles with an average particle size of 250 µm were loaded into a fluidized bed granulation dryer, and an aqueous flavoring mixture solution containing 1% by weight of a tobacco flavoring, a which vanillin was added, and 9% by weight of pululane, was continuously sprayed on the particles, while tempered air was blown at 30 ° C with a flow rate of 1.0 m / s. In this way, a total of 5 g of the aqueous mixture solution was sprayed on the surface of the calcium carbonate particles, followed by drying. After that, the temperature of the tempered air was immediately reduced to room temperature, and the particles were cooled with a flow rate of 0.4 m / s, thereby obtaining the desired aroma microspheres.

Comparative example 3 (example 3 of the prior art document)

1% by weight of coffee oil and 0.5% by weight of lecithin was added to a previously prepared aqueous dispersion of pululane containing 10% by weight of pululane. The mixture was vigorously stirred in an emulsifier (emulsifier rotation speed of 7500 rpm, 15 minutes), thereby preparing a dispersion of

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flavoring On the other hand, 300 g of ground coffee bean particles with an average particle size of 250 µm to 1.4 mm were loaded into a rotary fluidized bed granulation dryer (SFC-Mini, manufactured by Freund Corporation) , and the rotary disk drilled in the bottom and the blades of the mixer to prevent lumps were rotated at approximately 500 rpm and approximately 400 rpm, respectively, while hot air was blown at 75 ° C with a flow rate of 0.6 m / s, thereby forming a fluidized bed of the ground coffee bean particles. The flavoring dispersion, maintained at 40 ° C, was continuously sprayed onto the fluidized bed, thereby spraying a total of 90 g of the flavoring dispersion onto the surface of the ground coffee bean particles, followed by drying. After that, the temperature of the hot air was immediately reduced to room temperature, and the particles were cooled with a flow rate of 0.4 m / s, thereby obtaining the desired aroma microspheres.

The amount of flavoring and the amount of material containing a flavoring were determined as follows. Flavoring Measurement

The flavoring carrier particles were subjected to stirring extraction, using a mixture of purified water and methanol. The extract obtained was subjected to a gas chromatography (GC / MS) spectrometer to measure the flavoring.

Measurement of the material that contains a flavoring

The flavoring carrier particles were weighed (weight A), and heated and dried in order to remove water from the particles (weight B after drying). Purified water was added to the particles after drying, and the extraction was carried out with stirring, thereby eluting the material from the flavoring carrier material. The particles were heated and dried further (weight C after drying). The difference between weight C and weight A was considered as the amount of the material containing flavoring.

The result of the measurement is illustrated in Figure 6. Figure 6 illustrates the amount of flavoring transported and the amount of the material containing flavoring in a proportion (% by weight) with respect to the total weight of the particles of the carrier particles of flavoring Figure 6 indicates that the flavoring carrier particles prepared by the claimed method transport a greater amount of a flavoring agent than the flavoring carrier particles according to the comparative examples.

Furthermore, it was possible to prepare the flavoring carrier particles by a treatment in a shorter time than the flavoring carrier particles according to the comparative examples.

Relationship between the BET specific surface of the core particle and the adsorption capacity of the flavoring carrier particle

An aromatizing carrier activated carbon particle was prepared according to the same procedure as the process for preparing the aromatic carrier calcium silicate particle of Example 1, using activated carbon (KURARAY COAL GGS-H28 / 70, manufactured by Kuraray Chemical Co ., Ltd .; average particle size: 0.4 mm; BET specific surface: 1700 m2 / g) instead of calcium silicate as a core particle, and using the aroma-emitting composition of Table 1 as a composition that emits aroma

Specifically, the aromatizing carrier activated carbon particle was prepared as follows:

For the preparation, the RIBOCONE RM-50-SR, manufactured by Okawara Mfg, was used. Co., Ltd. as a tapered tapered mixer dryer (see Figure 1). 15 kg of activated carbon (KURARAY COAL GGS-H28 / 70, manufactured by Kuraray Chemical Co., Ltd .; average particle size: 0.4 mm; BET specific surface: 1700 m2 / g) was placed inside the mixer dryer 6 kg of an aqueous solution containing 5% by weight of pululane, and steam was circulated at 120 ° C at a pressure of 200 kPa in the jacket. The pressure inside the mixer dryer was set at 12.3 kPa, and the activated carbon was stirred. After stirring for 5 minutes, 7.5 kg of liquid composition emitting aroma D was sprayed through the spray nozzle into the mixer dryer for 60 minutes, and then stirred and dried further for 5 minutes. Activated carbon particles carrying flavoring were removed from the mixer dryer, immediately placed in a MIX GRADO 0.5 TYPE continuous fluidized bed granulation dryer, manufactured by Okawara Mfg. Co., Ltd.), and underwent sensible heat exchange and dehumidification of the activated carbon particles for 3 minutes, thereby obtaining a product of activated carbon particles carrying flavoring.

Using 30 mg of the activated carbon particles carrying flavoring prepared in this way, a filter cigarette was manufactured with a configuration illustrated in Figure 3 as follows. Specifically, the filter cigarette with a configuration illustrated in Figure 3 was manufactured according to the following procedure. From a commercially available filter cigarette product, "Winston Ligths", which is equipped with a filter with a cellulose acetate fiber tow as the filter raw material, the cellulose acetate fiber tow was removed using a pair of tweezers Then, the empty space portion was loaded with a cellulose acetate fiber tow (length: 10 mm; 2.5Y / 35000 (that is, filament fineness: 2.5 denier; filament cross section: type Y; total fineness: 35000 denier)), loaded with 30 mg of the activated carbon particles carrying the flavoring

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previously prepared (in 2 mm of length of space 64 in the longitudinal direction of the cigarette cylinder), and finally loaded with a cellulose acetate fiber tow (length: 10 mm; 2.5Y / 35000). In addition, a filter cigarette was manufactured (hereafter referred to as a reference cigarette) in the same manner as above, except that 30 mg of activated carbon was used as it was that did not carry flavoring (KURARAY cOaL GGS-H28 / 70 manufactured by Kuraray Chemical Co., Ltd), instead of the activated carbon particles carrying flavoring.

The filter cigarette manufactured in this way was subjected to a smoking experiment, and the adsorption capacity of the filter with respect to acetone in the mainstream smoke was investigated.

In this experiment, an apparatus 70 illustrated in Figure 7 was used to trap components contained in the smoke from the mainstream of a cigarette. This apparatus 70 has a capture device for trapping the particulate material 71, which comprises a Cambridge filter 711 (a diameter of 47 mm), a smoke flow inlet port of the mainstream of tobacco 71a, which holds a cigarette CIG, and a smoke flow outlet port of tobacco mainstream 71b. In addition, the apparatus 70 comprises a bubbler 72. In the bubbler 72, a solution of capture agent TA is contained to trap gaseous components in the smoke of the mainstream of tobacco. In the present experiment, 10 ml of methanol, containing 200 ppm of anethole, which was an internal standard substance, was put there as the TA capture agent solution. The bubbler 72 was housed in a Dewar 73 vessel containing an RM refrigerant to keep the TA capture agent solution at a low temperature. In the present experiment, a mixture of dry ice and isopropanol was used as the RM refrigerant, and the temperature of the TA capture agent solution was maintained at -70 ° C or lower during the experiment. The flow outlet port 71b of the capture device 71 for trapping particulate material was connected with a pipe 74 that extends into the capture agent solution TA in the bubbler 72. In addition, a suction port 76a was connected of an automatic smoking machine with a pipe 75 extending to the upper space of the capture agent solution TA in the bubbler 72. When a cigarette was lit and the automatic smoking machine 76 was operated, the pressure inside was reduced of the bubbler 72 by suction by means of the pipe 75. According to the pressure reduction, the smoke from the mainstream of the tobacco passed through the Cambridge filter 711 in the capture device 71. At that time, the material in smoke particles from the mainstream of tobacco were trapped in the Cambridge 711 filter, and smoke from the mainstream deprived of particulate material was introduced into the d Capture agent isolution TA in the bubbler 72, via the pipe 74. Bubbling occurred in the capture agent solution TA, and the gaseous material of the mainstream smoke is trapped in the capture agent solution TA .

In the present experiment, the cigarette was fitted in the capture device 71, and underwent a smoking experiment using the automatic smoking machine 76 under the standard smoking conditions defined by the International Organization for Standardization (1 draft: draft 35 ml for 2 seconds, draft interval: 58 seconds). After completing the smoking experiment, the bubbler agent solution 72 was transferred to a serum vial, and the Cambridge filter 711, in which the particulate material was trapped, was also placed inside the serum vial. It was subjected to an extraction by stirring at 250 times / min for 30 minutes. 1 ml of the extract obtained was placed in a vial, for determination with a mass chromatography (GC / MS) spectrometer, and the mainstream smoke components were analyzed under the following conditions.

Analytical conditions of the components in the mainstream smoke:

• CG / EM: HP 7890/5975 manufactured by Hewlett-Packard development Company, D. P.

• Column: DB-1701

• Column flow rate: 1.2 ml / min

• Temperature rise condition: the temperature was maintained at 60 ° C for 5 minutes, and then rose to 160 ° C at 5 ° C / min and 250 ° C at 10 ° C / min, and then maintained at 250 ° C for 30 minutes.

• Injection ratio: 10: 1 division; input: 220 ° C; flow rate: 12 ml / min; total flow rate: 16.2 ml / min

• MS condition: scan parameter: from 33.0 to 200.0; threshold: 50; EM ion source: 230 ° C; MS quadrupole: 150 ° C.

The same analysis was also carried out on a cigarette with a simple filter (that is, the cigarette with a cigarette cylinder of a commercially available filter product, "Winston Lights", and a simple filter consisting of a fiber tow of cellulose acetate (length: 20 mm; 2.5Y / 70000) connected to one end thereof, hereafter referred to as "standard cigarette") and the previous reference cigarette.

From the results of the analysis of the filter cigarette that includes activated carbon particles carrying flavoring, the reference cigarette, and the standard cigarette, the value of the acetone peak area for each of the cigarettes was calculated. Each of the acetone peak area values for the filter cigarette that

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fifteen

twenty

25

30

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It included activated carbon particles carrying flavoring and the reference cigarette was divided by the value of the acetone peak area for the standard cigarette. The value obtained was multiplied by 100, to obtain the decrease in acetone (%) for each of the filtered cigarettes that included activated carbon particles carrying flavoring and the reference cigarette. The decrease in acetone (%) was subtracted from 100% to obtain the percentage of acetone adsorption.

As a result, the percentage of acetone adsorption with respect to the reference cigarette was 48%, and the percentage of acetone adsorption with respect to the filter cigarette that included activated carbon particles carrying flavoring was 45%. This result indicates that when an aromatizing carrier active carbon particle is prepared using activated carbon with a BET specific surface area of 1700 m2 / g as the core particle, the aromatizer carrier activated carbon particle has an adsorption capacity corresponding to approximately 94% with respect to the intrinsic adsorption capacity of the core particle.

Two kinds of filter cigarettes were manufactured in the same manner as the previous reference cigarette, except that activated carbon (30 mg) with a specific surface area of 1700 m2 / g was replaced with activated carbon (30 mg) with a specific surface area. 700 m2 / g and 1000 m2 / g, respectively. The percent adsorption of acetone with respect to these cigarettes was investigated in the same manner as before. As a result, the percentage of acetone adsorption with respect to the first cigarette was 23%, and the percentage of acetone adsorption with respect to the last cigarette was 34%.

From the previous results, it was found that a core particle with a specific surface area of 700 m2 / g or higher, shows a high adsorption capacity with respect to the components contained in the smoke of the mainstream of a cigarette, and a particle of core with a specific surface area less than 700 m2 / g shows a low adsorption capacity with respect to the components contained in the smoke of the mainstream of a cigarette.

List of reference signs

10: tapered tapered mixer dryer, 12: treatment tank, 12a: outlet for treated product, 121: inverted conical part of the treatment tank, 122: cylindrical part of the treatment tank, 14: double helix tape rotor blade , 16: rotary axis, 18a to 18e: grab bars, 20a and 20b: vortex flow breakers, 22: jacket, 22a: steam inlet, 22b: steam outlet, 24: top board, 26: engine, 28 : speed reducer, 24a: input for the object to be treated, 30: sleeve filter, 32: condenser, 321: internal condenser tube, 322: external condenser tube, P1: pressure reducing pump, 34: nozzle spray, 36: container for the liquid composition that emits aroma (LFC), P2: liquid feed pump, 38: temperature sensor, 40: container for low adsorption core particles (LAP), 50 and 60: cigarette with filter, 52: cigarette cylinder, 521: tobacco load, 522: cigarette paper, 54 and 62: filter, 541: filter section containing activated carbon, 542: filter section containing low adsorption particles carrying flavoring, 543: simple filter section, FLAP: low adsorption particles carrying flavoring, 541a, 542a, 543a and 622a: cellulose acetate fiber, 541b: carbon particles, 542b, 543b and 66: filter wrapping paper, 56: nozzle paper, 622: single filter section, 64: cavity, 70: device for trapping contained components in the smoke of the mainstream of a cigarette, 711: Cambridge filter, IGC: cigarette, 71: capture device for trapping particulate material, 71a: smoke flow inlet port of the mainstream of tobacco, 71b: port smoke flow outlet of mainstream tobacco, 72: bubbler, TA: capture agent solution to trap gaseous components in the smoke of mainstream tobacco, 73: Dewar vessel, RM: refrigerant, 74 and 75 : tuber A, 76: automatic smoking machine, 76a: suction port.

Claims (4)

10 fifteen 1. A method for preparing a particle of low adsorption of flavoring carrier, comprising: spray a liquid composition that emits aroma, which contains a flavoring and a material containing a flavoring, onto a low adsorption core particle with a BET specific surface area less than 700 m2 / g, while stirring the low adsorption core particle under reduced pressure. 2. The method for preparing a low-adsorption particle carrying flavoring according to claim 1, wherein the liquid composition emitting aroma contains the material containing a flavoring in an amount of 5 to 20% with respect to a total weight of the low adsorption particles carrying flavoring, and the flavoring in an amount of 10 to 50% with respect to a weight of the material containing a flavoring. 3. The method for preparing a low-adsorption particle carrying flavoring according to claim 1, wherein the reduced pressure is a pressure of 12.3 kPa or less. 4. The method for preparing a low-adsorption particle carrying flavoring according to any one of claims 1 to 3, wherein the low adsorption core particle is maintained at a temperature of 60 ° C or lower during spraying.