JPWO2013011899A1 - Perfume-carrying low adsorptive particles, cigarette filter, cigarette with filter, and method for producing perfume-carrying low adsorbent particles - Google Patents

Abstract

A fragrance carrier comprising: a low adsorptive core particle having a BET specific surface area of less than 700 m ² / g; and a fragrance generating medium that is supported on the surface of the low adsorbent core particle and includes a fragrance and a fragrance holding material that holds the fragrance. Low adsorbent particles, wherein the perfume holding material is present in an amount of 5-20% of the total weight of the perfume-carrying low adsorbent particles, and the perfume is in an amount of 10-50% of the weight of the holding material. A perfume-carrying low adsorptive particle characterized by being present in

Description

  The present invention relates to a perfume-carrying low adsorptive particle, a cigarette filter, a cigarette with a filter, and a method for producing a perfume-carrying low adsorbent particle.

  It has been practiced that particles carrying a fragrance are incorporated into a cigarette filter to release the fragrance from the fragrance and taste it in the cigarette mainstream smoke. For example, Patent Document 1 discloses a fragrance bead in which the surface of a particulate carrier such as calcium carbonate is covered with a glucan film containing a fragrance. In this perfume bead, the particulate carrier is put into a fluidized granulation dryer, and a glucan aqueous solution or aqueous dispersion containing the perfume is continuously or intermittently added while blowing warm air at 80 ° C. or lower. Manufactured by spraying on the surface and drying.

  However, in the method of Patent Document 1, it takes a relatively long time to process a large amount of fragrance, and as a result, it is difficult to increase the amount of fragrance carried.

WO2008 / 072627

  Accordingly, a first object of the present invention is to provide perfume-carrying low adsorptive particles carrying a relatively large amount of perfume in a relatively short time.

  Moreover, an object of this invention is to provide the filter for cigarettes containing such a fragrance | flavor carrying | support low adsorption particle, and a cigarette with a filter.

  Furthermore, this invention aims at providing the manufacturing method of a fragrance | flavor carrying | support low adsorption particle.

In order to solve the above problems, according to the first aspect of the present invention, a low adsorptive core particle having a BET specific surface area of less than 700 m ² / g, and a perfume carried on the surface of the low adsorbent core particle And a fragrance-carrying low-adsorbent particle comprising a fragrance-generating medium containing a fragrance-holding material for holding the fragrance, wherein the fragrance-holding material is in an amount of 5 to 20% of the total weight of the fragrance-carrying low-adsorbent particles. A perfume-carrying low adsorptive particle is provided, wherein the perfume is present in an amount of 10 to 50% of the weight of the retaining material.

  Moreover, according to the 2nd side surface of this invention, a cigarette filter provided with the filter section containing the fragrance | flavor carrying | support low adsorption particle of this invention is provided. Furthermore, according to the 3rd side surface of this invention, the cigarette with a filter provided with the cigarette rod and the cigarette filter of this invention connected to the end of the said cigarette rod is provided.

Further, according to the fourth aspect of the present invention, there is provided a liquid fragrance-releasing composition containing a fragrance and a fragrance holding material while stirring low adsorbent core particles having a BET specific surface area of less than 700 m ² / g under reduced pressure. There is provided a method for producing a perfume-carrying low-adsorption particle, characterized by spraying the low-adsorption core particle.

  According to the present invention, perfume-carrying low adsorptive particles carrying a relatively large amount of a perfume are provided in a relatively short time treatment.

It is a schematic sectional drawing which shows an example of the apparatus for manufacturing the fragrance | flavor carrying | support low adsorption particle of this invention. It is a schematic sectional drawing which shows the cigarette with a filter by one Embodiment of this invention. It is a schematic sectional drawing which shows the cigarette with a filter by other embodiment of this invention. It is a schematic sectional drawing which shows the cigarette with a filter by other embodiment of this invention. It is a schematic sectional drawing which shows the cigarette with a filter by other embodiment of this invention. It is a graph which shows the measurement result of the quantity of the fragrance | flavor carried | supported and the fragrance | flavor holding material. It is a schematic diagram showing a cigarette mainstream smoke component capturing device partially broken.

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

  The perfume-carrying low adsorptive particles of the present invention comprise low adsorbent core particles and an aroma generating medium that is supported on the surface of the low adsorptive core particles and includes a perfume and a perfume holding material that holds the perfume. The perfume holding material is present in an amount of 5-20% of the total weight of the perfume-carrying low adsorbent particles, and the perfume is present in an amount of 10-50% of the weight of the holding material.

The low adsorptive core particles used in the present invention have a BET specific surface area of less than 700 m ² / g. In this specification, the BET specific surface area refers to a specific surface area determined according to a known BET method. Core particles having a BET specific surface area of less than 700 m ² / g have relatively little adsorption of components in cigarette mainstream smoke, and have little influence on the taste of cigarettes.

  Such low adsorptive core particles include calcium silicate, low activated carbon, silica, ceramics, crystalline cellulose, wood, plant raw material, styrene-divinylbenzene copolymer, ethylene-vinyl acetate copolymer, Can be formed from a water-absorbing polymer such as polyvinyl alcohol or sodium polyacrylate.

  The low adsorptive particles preferably have an average particle size of 75 μm to 2000 μm. For example, particles having an average particle size of 75 μm to 1000 μm can be suitably used. The low adsorptive core particles preferably have a water retention rate of 10% or more, more preferably 20 to 40%. Here, the water retention rate refers to the ratio of the water retention amount when the core particles are immersed in water with respect to the dry matter weight of the core particles. All of the core particles exemplified above exhibit such a water retention rate.

  The aroma generating medium that covers the surface of the low adsorptive core particles includes a fragrance and a fragrance holding material that holds the fragrance.

  Examples of the fragrances include hydrophilic fragrances and hydrophobic fragrances. Examples of hydrophilic flavors include leaf tobacco extract, natural plant flavors (eg, licorice, St. John's bread, plum extract, peach extract, etc.), acids (eg, malic acid, tartaric acid, citric acid, butyric acid, etc.), sugars ( For example, glucose, fructose, isomerized sugar, etc.). Examples of hydrophobic flavors include menthol, cocoa (powder, extract, etc.), esters (eg, isoamyl acetate, linalyl acetate, isoamyl propionate, linalyl butyrate), natural essential oils (vegetable essential oils such as vanilla, for example) Extracts, spearmint, peppermint, cassia, jasmine, etc .; animal essential oils include, for example, musk, ambergris, civet, castrium, etc., simple flavors (eg, anethole, limonene, linalool, eugenol, vanillin, etc.).

  The holding material for holding the fragrance contains a film forming material and, if necessary, an emulsifier. A typical example of the film forming material used in the present invention is glucan, and examples of glucan include pullulan, maltodextrin, and hydroxypropylcellulose. Glucan is water soluble. A film-forming material such as glucan can retain a fragrance by incorporating the fragrance into a film formed therefrom. The film-forming material can be used for both hydrophilic fragrances and hydrophobic fragrances.

  Examples of the emulsifier include glycerin fatty acid ester, sucrose fatty acid ester (sugar ester), sorbitan fatty acid ester, propylene glycol fatty acid ester, and lecithin. The emulsifier molecules retain the hydrophobic flavor by adsorbing their hydrophobic groups around the oil droplets of the hydrophobic flavor in an aqueous medium and retain the hydrophobic flavor even after drying.

  In the perfume-carrying low adsorptive particles of the present invention, the perfume-holding material is present in an amount of 5 to 20%, preferably 5 to 10% of the total weight of the perfume-carrying low adsorbent particles. And a fragrance | flavor exists in the quantity of 10 to 50% of the weight of a fragrance | flavor holding material.

  The perfume-carrying low adsorbent particles of the present invention are prepared by spraying a liquid aroma release composition containing a perfume and a perfume holding material onto the low adsorbent core particles while stirring the low adsorbent core particles under reduced pressure. be able to.

  The fragrance contained in the liquid fragrance releasing composition is as described above, and the fragrance holding material is also as described above.

  When the liquid fragrance-releasing composition contains only a hydrophilic fragrance as a fragrance, the composition usually contains glucan as a film forming material and a hydrophilic fragrance, and further dissolves the glucan and the hydrophilic fragrance. It is preferable to include water as a solvent.

  When the liquid fragrance-releasing composition contains a hydrophobic fragrance as the fragrance (for example, when the liquid fragrance-generating composition contains only the hydrophobic fragrance as the fragrance, or contains the hydrophobic fragrance together with the hydrophilic fragrance as the fragrance) The aroma release composition includes glucan as a film forming material, water as a glucan solvent, a hydrophobic fragrance (and a hydrophilic fragrance), and an oily solvent (for example, vegetable oil or fat or the like) that dissolves the hydrophobic fragrance. A saturated fatty acid triglyceride, preferably a medium-chain saturated fatty acid triglyceride) and an emulsifier. When the composition contains a hydrophilic fragrance in addition to the hydrophobic fragrance, the hydrophilic fragrance dissolves in water.

  In producing the perfume-carrying low-adsorbing particles, the low-adsorbing core particles are used under a reduced pressure of 12.3 kPa or less, for example, a reduced pressure of 7.4 to 12.3 kPa, while spraying the liquid aroma release composition. It is preferable to put in. At that time, the adsorbent core particles are preferably at a temperature of 60 ° C. or lower, for example, 40 to 60 ° C. By spraying a liquid fragrance-releasing composition containing a fragrance and a fragrance-holding material under reduced pressure, a large amount of the fragrance can be supported on the low adsorptive core particles, and a high-viscosity fragrance-releasing composition (for example, 2 Pa) (Viscosity of about s) can be sprayed from the spray nozzle.

  A conical ribbon mixer / dryer can be utilized to produce the perfume-carrying low adsorptive particles of the present invention. The conical ribbon mixer / dryer is described in, for example, Japanese Patent Application Laid-Open Nos. 2003-71263, 2003-290641, and 2007-229633, and is commercially available from Okawara Seisakusho.

  The basic structure of such a conical ribbon mixer / dryer will be described with reference to FIG. FIG. 1 schematically shows an example of a conical ribbon mixer / dryer 10 in cross section. The conical ribbon mixing / drying machine 10 includes a processing tank 12 including an inverted conical portion 121 and a cylindrical portion 122 provided on the conical portion 121 in which mixing / drying processing is performed. A double spiral ribbon rotor blade 14 is provided in the treatment tank 12. The spiral ribbon rotary blade 14 is attached to a rotary shaft 16 extending vertically in the center of the processing tank 12 and a plurality of support bars (support bars 18a to 18e in FIG. 1) fixed to the rotary shaft 16 at a distance from each other. It has been. On the inner wall of the cylindrical portion 122 of the treatment tank 12 above the rotor blades 14, for example, vortex breakers 20a and 20b made of a pair of plate-like bodies are fixed. The vortex breakers 20a and 20b move the treatment product (low adsorbent particles in the present invention) that has risen along the inner wall of the treatment tank 12 by the ribbon rotor blade 14 to the vicinity of the center of the treatment tank 12 and the treatment tank. 12 is dropped at the bottom.

  A jacket 22 surrounds the outer periphery of the treatment tank 12, and steam is introduced into the jacket 22 from the steam inlet 22a via the line L1 in order to heat the container contents, and the steam is discharged from the steam. It is discharged out of the system from the outlet 22b via the line L2.

  The upper opening of the container is closed by the top plate 24. A motor 26 and a speed reducer 28 are installed on the top plate 24, and an output shaft of the speed reducer 28 is connected to a rotary shaft 16 installed in the processing tank 12. In addition, the top plate 24 is provided with an inlet 24a for an object to be processed (in the case of the present invention, low adsorptive core particles). A suction port 12a for adsorbent particles) is provided.

  Further, a bag filter 30 is attached to the top plate 24. This bag filter captures particulate matter (low adsorbent particles in the case of the present invention) in the contents of the treatment tank 12 and passes volatiles (in the case of the present invention, water in the fragrance-releasing composition), This is led to the condenser 32 via the line L3. The condenser 32 is constituted by, for example, a water-cooled cooler, and volatile substances pass through the inner cylinder 321. The volatile substances are cooled by cooling water introduced from the line L5 into the outer cylinder 322, and condensed from the line L6. It is discharged as a liquid (water). The water introduced into the outer cylinder 322 is discharged from the line L5. It is connected to the decompression pump P1 via the inner cylinder line L7, and the inside of the processing tank 12 is decompressed by driving the decompression pump P1.

  The basic structure of the conical ribbon mixer / dryer is as described above. In order to introduce the perfume-carrying low adsorptive particles of the present invention, the liquid aroma release composition is introduced into the treatment tank 12. The spray nozzle 34 is provided through the top plate 24, and the liquid fragrance releasing composition is supplied from the container 36 containing the liquid fragrance releasing composition LFC through the line L8 provided with the liquid feeding pump P2 into the processing tank 12. Spray on. Further, a temperature sensor (for example, a thermocouple) 38 for measuring the temperature of the low adsorptive particles in the processing tank 12 is provided at the lower part of the processing tank 12.

  In order to produce the perfume-carrying low adsorptive particles of the present invention using the conical ribbon mixer / dryer 10 shown in FIG. 1, the low adsorbent core particles LAP accommodated in the container 40 are lined in the treatment tank 12. It introduce | transduces in the processing tank 12 through L9. By introducing steam at a temperature of 80 ° C. or higher, preferably 100 to 120 ° C. into the jacket 22, the inside of the treatment tank 12 is heated and the double spiral ribbon rotor blade 14 is rotated by driving the motor 26 to reduce the temperature. While stirring the adsorbent particles, the liquid fragrance releasing composition accommodated in the container 36 is sprayed into the treatment tank 12 from the spray nozzle 34 via the line L8 by driving the liquid feeding pump P2. During this spraying, it is preferable to maintain the temperature of the low adsorptive particles at 70 ° C. or lower, preferably 60 ° C. or lower. The temperature of such low adsorptive particles is such that when the water in the liquid fragrance releasing composition introduced into the treatment tank 12 is heated by the steam of 80 ° C. or more introduced into the jacket 22 and evaporated. It can be maintained by the heat of evaporation taken away by water from the low adsorptive particles.

  The perfume-carrying low adsorptive particles produced in this way are only volatilized and removed during production, and other than the water in the liquid aroma release composition applied to the low adsorbent core particles during production. Almost all of the components are supported on the low-adsorption core particles. Therefore, the liquid fragrance-releasing composition applied to the low adsorptive core particles has a fragrance retaining material in an amount corresponding to 5 to 20%, preferably 5 to 10%, of the weight of the low adsorptive core particles used. And a fragrance in an amount corresponding to 10 to 50% of the weight of the fragrance retaining material contained in the liquid fragrance releasing composition. In addition, the fragrance | flavor holding | maintenance material contained in a liquid fragrance | flavor releasing composition, especially the one part aqueous solution or aqueous dispersion of a film formation material can be previously applied to a low adsorptive nucleus particle. Prior application of an aqueous solution or aqueous dispersion of a part of the film-forming material suppresses the temperature increase of the low-adsorption core particles in the initial stage of production of the perfume-carrying low-adsorption particles, and the fine powder from the low-adsorption core particles Occurrence can be suppressed.

  In the perfume-carrying low adsorptive particles of the present invention, a solid aroma generating medium formed from a liquid aroma releasing composition covers the surface of the low adsorptive core particles. In this solid aroma generating medium, since the fragrance is held by the fragrance holding material, the fragrance is not volatilized or adsorbed by charcoal during normal storage. And if it contacts with hydrophilic components, such as the water | moisture content in the mainstream smoke which generate | occur | produces by smoking a cigarette, a fragrance | flavor holding material will partly melt | dissolve, a fragrance will be discharge | released and the flavor taste of a fragrance | flavor can be tasted.

  The cigarette filter by the 2nd side surface of this invention is equipped with the filter section containing the fragrance | flavor carrying | support low adsorption particle of this invention. And the cigarette with a filter by the 3rd side surface of this invention is connected to the cigarette rod and the end of the said cigarette rod, and the cigarette with a filter provided with the filter of this invention is provided.

  The cigarette filter according to the present invention may include a filter section in which the perfume-carrying non-absorbable particles of the present invention are dispersed in an ordinary filter material such as cellulose acetate fiber tow (bound by a plasticizer such as triacetin). it can. A so-called charcoal filter section (a filter section including a filter material in which activated carbon is dispersed in cellulose acetate tow bound by a plasticizer such as triacetin) can be connected to one end of the filter section. Alternatively, a cigarette filter according to the present invention may comprise charcoal filter sections and plain filter sections spaced apart and include the perfume-carrying low adsorptive particles of the present invention filled in a space between the two filter sections. .

  Hereinafter, with reference to FIGS. 2-5, the cigarette which has the filter of this invention is demonstrated. 2 to 5, like elements are denoted by the same reference numerals.

  FIG. 2 is a schematic cross-sectional view of a cigarette (filtered cigarette) 50 including a cigarette filter according to one embodiment of the present invention. The cigarette 50 with a filter includes a cigarette rod 52 in which a tobacco filler 521 such as a tobacco cut is wound with a cigarette wrapping paper 522. The cigarette rod 52 is the same as a normal cigarette.

  A filter 54 is attached to one end of the cigarette rod 52. The filter 54 is a charcoal filter section 541 provided in direct contact with one end of the cigarette rod 52, and a perfume-carrying low adsorptive particle-containing filter section provided on an end face on the downstream side of the charcoal filter section 541 with respect to the flow direction of mainstream smoke. 542 and a plain filter section 543 provided on the downstream end face of the filter section 542 containing the fragrance-carrying low-adsorbing particles with respect to the flow direction of the mainstream smoke.

  The charcoal filter section 541 is formed by winding, for example, cellulose acetate fiber 541a in which charcoal particles 541b are dispersed with a filter web 541c, and is the same as a normal charcoal filter.

  The filter section 542 containing the perfume-carrying low-adsorbing particles is obtained by winding, for example, cellulose acetate fiber 542a in which the perfume-carrying low-adsorptive particles FLAP of the present invention are dispersed with a filter web 542b.

  The plain filter section 543 is formed, for example, by winding a tow of cellulose acetate fiber 543a with a filter web 543b.

  A filter 54 composed of filter sections 541, 542 and 543 is attached to one end of the cigarette rod 52 by a tip paper 56.

  FIG. 3 is a schematic cross-sectional view of a cigarette (cigarette with filter) 60 including a cigarette filter according to another aspect of the present invention. In this cigarette 60 with a filter, the filter 62 attached to the cigarette rod 52 by the tip paper 56 is provided with a charcoal filter section 541 attached directly to one end of the cigarette rod 52, and spaced apart from the charcoal filter section 541. A plain filter section 622, which is entirely wound by a filter web 66. The plain filter section 622 is made of, for example, a tow of cellulose acetate fiber 622a, similarly to the plane filter section 543 in FIG. A cavity 64 between the charcoal filter section 541 and the plain filter section 622 is filled with the perfume-carrying low adsorptive particles FLAP of the present invention.

  4 is a structure in which the charcoal filter section 541 is omitted in the cigarette with filter of the structure of FIG. 2, and a filter section 542 containing perfume-carrying low-adsorbing particles is provided in direct contact with one end of the cigarette rod 52.

  FIG. 5 shows a structure in which a plain filter section 543 (see FIG. 2) is used instead of the charcoal filter section 541 in the filter cigarette having the structure shown in FIG.

  EXAMPLES Hereinafter, although this invention is demonstrated by a specific example, this invention is not limited by those specific examples.

<Preparation of Liquid Aroma Release Composition>
A mixture containing the components shown in Table 1 in the proportions shown in Table 1 was emulsified at 7500 rpm for 15 minutes with an emulsifier (ROBOMICS MARK II manufactured by PRIMIX Corporation). At this time, the periphery of the emulsifier was cooled with water so that the temperature of the mixture did not exceed 45 ° C. Thus, liquid fragrance release compositions A to D were obtained.

In addition, as a medium-chain fatty acid triglyceride, Cocoon MT manufactured by Kao Corporation was used, LP-20E manufactured by Nisshin Oillio Co., Ltd. was used as lecithin, and P-1570 manufactured by Mitsubishi Chemical Foods Co., Ltd. was used as a sugar ester.

<Preparation of perfume-carrying low adsorptive particles>
Example 1
Here, a conical ribbon mixing / drying machine ribocorn RM-50-VD manufactured by Okawara Seisakusho was used (see FIG. 1). 10 kg of calcium silicate particles (Sanwa Malmo, Sanwa Insectiside; average particle size: 1 mm, BET specific surface area less than 700 m ² / g) and 6 kg of 5% by weight pullulan aqueous solution are put into the above mixer / dryer and put in the jacket. Steam at a temperature of 120 ° C. under a pressure of 200 kPa was circulated, the pressure in the mixer / dryer was set to 12.3 kPa, and the calcium silicate particles were stirred. After stirring for 5 minutes, 5 kg of the liquid fragrance-releasing composition A was sprayed from the spray nozzle into the mixer / dryer over 40 minutes, and further stirred and dried for 20 minutes. Remove perfume-carrying calcium silicate particles from the mixer / dryer and immediately place them in a continuous flow granulation dryer (Mixgrad 0.5 type, manufactured by Okawara Seisakusho) for 3 minutes for sensible heat exchange and dehumidification in the calcium silicate particles To obtain a perfume-carrying calcium silicate particle product.

Example 2
A perfume-carrying calcium silicate particle product was obtained in the same procedure as in Example 1 except that the liquid aroma release composition B was used instead of the liquid aroma release composition A.

Example 3
A perfume-carrying calcium silicate particle product was obtained by the same procedure as in Example 1 except that the liquid aroma release composition C was used instead of the liquid aroma release composition A.

Example 4
A perfume-carrying calcium silicate particle product was obtained by the same procedure as in Example 1 except that the liquid aroma release composition D was used instead of the liquid aroma release composition A.

<Preparation of cigarette with filter>
A cigarette with a filter having the structure shown in FIG. 3 was produced. More specifically, after removing cellulose acetate fiber tow with tweezers from a commercially available cigarette product with a filter having a filter having cellulose acetate fiber tow as a filter material, the activated carbon (manufactured by Kuraray Chemical Co., Ltd.) Cellulose acetate fiber tow (length 12 mm; 8Y / 29000 (that is, single fineness 8 denier; filament cross section Y type; total fineness 29,000 denier), added with 85 mg of Kuraray Coal GGS-H28 / 70), manufactured in Examples 1-4 The fragrance-supported calcium silicate particle product 42 mg (47 mm length of the axial cavity portion 64 of the cigarette rod) was filled, and finally cellulose acetate fiber tow (length 11 mm; 2.5Y / 35000) was filled, A filter with the structure shown in FIG. To prepare a cmdlet. Further, except that nothing is filled in the cavity 64, as above, to produce a cigarette with a control filter.

  When these four kinds of cigarettes with a filter of the present invention were smoked, it was confirmed that the aroma from the fragrance was released in the mainstream smoke, and that the flavor was reinforced compared to the cigarette with a filter of the control. confirmed. These results show that a large amount of perfume can be supported on the low adsorptive core particles in a short time by the method of the present invention.

<Measurement of amount of fragrance and fragrance retaining material supported>
About the fragrance | flavor carrying | support particle | grains obtained in Examples 1-4, the quantity of the carried | supported fragrance | flavor and the quantity of the fragrance | flavor holding material were measured.

  The perfume-carrying particles of the comparative example were prepared according to Examples 1 to 3 in the prior art document (WO2008 / 072627), and the amount of the perfume carried and the amount of the perfume-holding material were similarly measured for the prepared perfume-carrying particles. .

  The perfume-carrying particles of the comparative example were prepared as follows.

Comparative Example 1 (Example 1 of the prior art document)
2% by weight of coffee oil was added to a 10% by weight pullulan aqueous dispersion prepared beforehand. This mixed solution was vigorously stirred in an emulsifier (emulsifier rotation speed: 2500 rpm) to prepare a fragrance dispersion. On the other hand, 100 g of calcium carbonate particles having an average particle diameter of 250 μm are put into a fluidized granulator and the above fragrance dispersion is rapidly sprayed intermittently (spraying for 1 minute while blowing warm air at 75 ° C. at a flow rate of 0.6 m / second. After 30 minutes, the spray stop cycle was repeated, and a total of 10 g of the fragrance dispersion was sprayed onto the surface of the calcium carbonate particles and dried. Thereafter, the inside of the fluidized bed was quickly cooled to room temperature to obtain desired fragrance beads.

Comparative Example 2 (Example 2 of the prior art document)
100 g of calcium carbonate particles having an average particle size of 250 μm are placed in a fluidized granulation dryer, and 1% by weight of a flavoring for tobacco added with vanillin and 9% by weight of pullulan while blowing warm air at 30 ° C. at a flow rate of 1.0 m / second. A total of 5 g of the mixed aqueous solution was sprayed onto the surface of the calcium carbonate particles and dried. Thereafter, the temperature of the warm air was quickly lowered to room temperature and cooled at a flow rate of 0.4 m / sec to obtain desired fragrance beads.

Comparative Example 3 (Example 3 of the prior art document)
1% by weight of coffee oil and 0.5% by weight of lecithin were added to a 10% by weight pullulan aqueous dispersion prepared in advance. This liquid mixture was vigorously stirred in an emulsifier (emulsifier rotation speed: 7500 rpm, 15 minutes) to prepare a perfume dispersion. On the other hand, 300 g of ground coffee bean particles having an average particle size of 250 μm to 1.4 mm are placed in a tumbling fluidized granulator (Freund Sangyo Co., Ltd., SFC-MINI), and the bottom rotating plate is about 500 rpm, preventing granulation. The stirrer blade was rotated at about 400 rpm, and 75 ° C. warm air was blown at a flow rate of 0.6 m / sec to form a fluidized bed of ground coffee bean particles. A 90 g total of the fragrance dispersion was sprayed onto the surface of the coffee bean particles and dried by continuously spraying the fragrance dispersion on the fluidized bed while maintaining the temperature at 40 ° C. Thereafter, the temperature of the warm air was quickly lowered to room temperature and cooled at a speed of 0.4 m / sec to obtain desired fragrance beads.

  The amount of the fragrance and the amount of the fragrance retaining material were measured as follows.

Perfume measurement:
The perfume-carrying particles were extracted by shaking with purified water / methanol mixture. The extract was subjected to a gas chromatograph mass spectrometer (GC / MS), and the fragrance was measured.

Perfume retention material measurement:
The perfume-carrying particles were weighed (weight A) and dried by heating for the purpose of removing moisture in the particles (weight B after drying). Purified water was added to the dried particles, and extraction was performed by shaking to elute the fragrance retaining material. The extracted particles were further dried by heating (weight C after drying). The difference between the weight C and the weight A was defined as the amount of the fragrance retaining material.

  The measurement results are shown in FIG. FIG. 6 shows the amount of the perfume carried and the amount of the perfume holding material as a ratio (% by weight) to the total weight of the perfume-carrying particles. FIG. 6 shows that the perfume-carrying particles of the present invention carry a larger amount of perfume than the perfume-carrying particles of the comparative example.

  Further, the fragrance-carrying particles of the present invention could be prepared in a shorter time than the fragrance-carrying particles of the comparative example.

<Relationship between BET specific surface area of core particles and adsorption capacity of fragrance-supporting particles>
An activated carbon (Kuraray Chemical Co., Ltd., KGS-H28 / 70; average particle size: 0.4 mm; BET specific surface area: 1700 m ² / g) is used as the core particle instead of calcium silicate. Using the fragrance-releasing composition D of 1, fragrance-supported activated carbon particles were prepared according to the same method as the method for preparing the fragrance-supported calcium silicate particles of Example 1.

  Specifically, perfume-supporting activated carbon particles were prepared as follows.

For the preparation, a conical ribbon mixer / dryer ribocorn RM-50-SR manufactured by Okawara Seisakusho was used (see FIG. 7). 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 area: 1700 m ² / g) and 6 kg of 5% by weight pullulan aqueous solution were put into the mixer / dryer, and the jacket Steam at a temperature of 120 ° C. under a pressure of 200 kPa was circulated therein, the pressure in the mixer / dryer was set to 12.3 kPa, and the activated carbon was stirred. After stirring for 5 minutes, 7.5 kg of the liquid fragrance releasing composition D was sprayed from the spray nozzle into the mixer / dryer for 60 minutes, followed by further stirring and drying for 5 minutes. Remove the perfume-supporting activated carbon particles from the mixing / mixing / dryer and immediately put them in a continuous fluidized granulation dryer (Mixgrad 0.5 type manufactured by Okawara Seisakusho) to exchange sensible heat and dehumidify the activated carbon particles for 3 minutes. A fragrance-supported activated carbon particle product was obtained.

  Using the prepared perfume-carrying activated carbon particles 30 mg, a cigarette with a filter having the structure shown in FIG. 3 was prepared as follows. Specifically, after removing the cellulose acetate fiber tow which is a filter material with tweezers from a commercially available cigarette product with a filter having a filter having a cellulose acetate fiber tow as a filter material `` Winston Light '', Cellulose acetate fiber tow (length 10 mm; 2.5 Y / 35000 (ie, single fineness 2.5 denier; filament cross section Y type; total fineness 35000 denier)) prepared, 30 mg of fragrance-supported activated carbon particles (cigarette rod) 3 (length 2 mm of the space 64 in the axial direction) and finally filled with cellulose acetate fiber tow (length 10 mm; 2.5Y / 35000) to produce a cigarette with a filter having the structure shown in FIG. . In addition, a cigarette with a filter (hereinafter referred to as a control) was used in the same manner as described above except that 30 mg of activated carbon (Kuraray Chemical Co., Ltd., Kuraray Coal GGS-H28 / 70) not carrying a fragrance was used as it was instead of the fragrance-carrying activated carbon particles. Cigarette).

  The produced cigarette with filter was smoked, and the acetone adsorption ability in the mainstream smoke was examined.

  In this experiment, the apparatus 70 shown in FIG. 7 was used in order to capture components in the cigarette mainstream smoke. The apparatus 70 includes a Cambridge filter 711 (diameter 47 mm) and a particulate matter trap 71 including a cigarette mainstream smoke inflow port 71a and a cigarette mainstream smoke outflow port 71b for holding a cigarette CIG. In addition, the device 70 includes an impinger 72. In the impinger 72, a chemical TA that captures gas phase components in the mainstream smoke of tobacco is accommodated. In this experiment, 10 mL of methanol containing 200 ppm of anethole as an internal standard substance was added as a chemical solution TA. The impinger 72 is accommodated in a dewar bottle 73 that contains a refrigerant RM for maintaining the captured chemical solution TA at a low temperature. In this experiment, a mixture of dry ice and isopropanol was used as the refrigerant RM, and the capture chemical solution TA was maintained at a temperature of −70 ° C. or lower during the experiment. A conduit 74 extending into the chemical TA in the impinger 72 is connected to the outflow port 71 b of the particulate matter trap 71. A conduit 75 extending into the space above the captured drug solution TA in the impinger 71 is connected to the suction port 76a of the automatic smoker 76. When the cigarette is ignited and the automatic smoker 76 is driven, the pressure in the impinger 72 is reduced by suction through the conduit 75, and the cigarette mainstream smoke passes through the Cambridge filter 711 in the trap 71. At that time, the particulate matter in the tobacco mainstream smoke is captured by the Cambridge filter 711, the mainstream smoke from which the particulate matter has been removed is introduced into the captured chemical TA within the impinger 72 via the conduit 74, and bubbling occurs. The gas phase component in the mainstream smoke is captured by the captured chemical TA.

  In this experiment, the cigarette was set in the trap 71 and smoked under the standard smoking conditions of ISO (1 puff: 35 mL smoke in 2 seconds, puff interval: 58 seconds) by the automatic smoker 76. After the end of smoking, the drug solution in the impinger 72 was transferred to a serum bottle, and a Cambridge filter 711 that trapped particulate matter was placed therein, and extracted by shaking at 250 times / minute for 30 minutes. 1 mL of this extract was placed in a GC / MS analysis vial, and components in mainstream smoke were analyzed under the following conditions.

Analysis conditions for mainstream smoke components:
GC / MS: HP 7890/5975 manufactured by Hewlett-Packard
Column: DB-1701
-Column flow rate: 1.2 mL / min-Temperature rising condition: held at 60 ° C for 5 minutes, then raised to 160 ° C at 5 ° C / minute, raised to 250 ° C at 10 ° C / minute, held for 30 minutes did.

Injection: split ratio 10: 1; inlet 220 ° C .; flow rate 12 mL / min; total flow rate 16.2 mL / min MS conditions: scan parameters 33.0-200.0; threshold 50; MS ion source 230 ° C .; MS Quadrupole 150 ° C.

  The same analysis was conducted using a cigarette with a plain filter (a cigarette rod of a commercially available cigarette product with a filter “Winston Light”), and a plain filter made of cellulose acetate fiber tow (length 20 mm; 2.5 Y / 70,000) at one end. The control cigarette was connected to the above-mentioned reference cigarette).

  Acetone peak area values for filtered cigarettes and control cigarettes containing fragrance-supported activated carbon particles were calculated by calculating the peak area values of acetone from the analysis results of cigarettes with filters, control cigarettes and reference cigarettes containing fragrance-supported activated carbon particles, respectively. Was divided by the acetone peak area value for the reference cigarette, and the value was multiplied by 100 to obtain the acetone reduction rate (%). The acetone reduction rate (%) was subtracted from 100% to calculate the acetone adsorption rate.

As a result, the acetone adsorption rate for the control cigarette was 48%, and the acetone adsorption rate for the filter cigarette containing the fragrance-supported activated carbon particles was 45%. As a result, when activated carbon particles having a BET specific surface area of 1700 m ² / g were used as core particles to produce fragrance-supported activated carbon particles, the fragrance-supported activated carbon particles corresponded to about 94% of the intrinsic adsorption capacity of the core particles. It shows that the adsorption capacity is maintained.

Two kinds of cigarettes with filters similar to the above-mentioned control cigarette were prepared except that the activated carbon (30 mg) with a specific surface area of 1700 m ² / g was replaced with activated carbon (30 mg) with a specific surface area of 700 m ² / g and 1000 m ² / g. did. When the acetone adsorption rate of these cigarettes was examined in the same manner as above, the former cigarette was 23% and the latter cigarette was 34%.

From the above results, the core particles having a specific surface area of 700 m ² / g or more show a high adsorbability for the components in the cigarette mainstream smoke, but the core particles having a specific surface area of less than 700 m ² / g are the cigarette mainstream smoke. It turns out that it shows a low adsorption capacity for the components in it.

DESCRIPTION OF SYMBOLS 10 ... Conical ribbon mixing / drying machine, 12 ... Processing tank, 12a ... Discharge port of processed material, 121 ... Reverse cone part of processing tank, 122 ... Cylindrical part of processing tank, 14 ... Double spiral ribbon rotor blade, 16 Rotating shaft, 18a to 18e ... Support bar, 20a to 20b ... Eddy current breaker, 22 ... Jacket, 22a ... Steam inlet, 22b ... Steam outlet, 24 ... Top plate, 26 ... Motor, 28 ... Reducer, 24a ... Input port for workpiece, 30 ... bag filter, 32 ... condenser, 321 ... condenser inner cylinder, 322 ... condenser outer cylinder, P1 ... vacuum pump, 34 ... spray nozzle, 36 ... liquid fragrance release composition (LFC) container, P2 ... liquid pump, 38 ... temperature sensor, 40 ... low adsorbent nuclear particle (LAP) container 50, 60 ... filter cigarette, 52 ... cigarette rod, 521 ... cigarette filling Filler 522 ... Cigarette paper, 54, 62 ... Filter, 541 ... Filter section with activated carbon, 542 ... Filter section with perfume-carrying low adsorbent particles, 543 ... Plain filter section, FLAP ... Fragrance-carrying low adsorbent particles, 541a, 542a, 543a, 622a ... cellulose acetate fiber, 541b ... charcoal particles, 542b, 543b, 66 ... filter web, 56 ... chip paper, 622 ... plain filter section, 64 ... cavity 70 ... cigarette mainstream smoke component supplementing device, 711 ... Cambridge filter, CIG ... cigarette, 71 ... particulate matter trap, 71a ... tobacco mainstream smoke inflow port, 71b ... tobacco mainstream smoke outflow port, 72 ... impinger, TA ... chemical solution for capturing gas phase components in tobacco mainstream smoke 73 ... Dewar bottle, RM ... refrigerant, 74, 75 ... conduit, 76 ... automatic smoker, 76a ... suction port

Claims (8)

A fragrance carrier comprising: a low adsorptive core particle having a BET specific surface area of less than 700 m ² / g; and a fragrance generating medium that is supported on the surface of the low adsorbent core particle and includes a fragrance and a fragrance holding material that holds the fragrance. Low adsorbent particles, wherein the perfume holding material is present in an amount of 5-20% of the total weight of the perfume-carrying low adsorbent particles, and the perfume is in an amount of 10-50% of the weight of the holding material. A perfume-carrying low adsorptive particle characterized by being present in The fragrance-carrying low-adsorbent particles according to claim 1, wherein the low-adsorbent core particles having a BET specific surface area of less than 700 m ² / g are stirred under reduced pressure while containing a fragrance and a fragrance-holding material. A perfume-carrying low adsorptive particle produced by spraying a release composition onto the low adsorbent core particle.   A cigarette filter comprising a filter section containing the perfume-carrying low adsorptive particles according to claim 1 or 2.   A cigarette rod with a filter comprising the cigarette rod and one end of the cigarette rod and comprising the filter according to claim 3. While the low adsorbent core particles having a BET specific surface area of less than 700 m ² / g are stirred under reduced pressure, a liquid aroma release composition containing a fragrance and a fragrance holding material is sprayed onto the low adsorbent core particles. A method for producing perfume-carrying low adsorptive particles.   The liquid fragrance-releasing composition contains the fragrance retaining material in an amount of 5 to 20% of the total weight of the fragrance-carrying low adsorbent particles, and the fragrance is 10 to 50% of the weight of the fragrance retaining material. The method for producing perfume-carrying low adsorptive particles according to claim 5, wherein the perfume-carrying low-adsorbent particles according to claim 5.   The method for producing perfume-carrying low adsorptive particles according to claim 5 or 6, wherein the reduced pressure is a pressure of 12.3 kPa or less.   The method for producing perfume-carrying low adsorptive particles according to any one of claims 5 to 7, wherein the low adsorptive core particles are maintained at a temperature of 60 ° C or lower during the spraying.

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