TWI481705B - Flavoring agent-carrying low adsorbent particle, cigarret filter, cigarret with filter, and method for making a flavoring agent-carrying low adsordent particle - Google Patents

Description

Method for producing low-absorbability particles by using a low-absorbability particle, a filter for cigarettes, a cigarette with a filter, and a fragrance

The present invention relates to a method for producing a low-absorbability particle, a filter for a cigarette, a cigarette with a filter, and a fragrance-supporting low-absorbency particle.

The particles for holding the fragrance are set in the filter for cigarettes, and the fragrance derived from the fragrance is released in the mainstream cigarette of the cigarette to taste. For example, Patent Document 1 discloses a fragrance particle in which a surface of a particulate carrier such as calcium carbonate is coated with a glucan film containing a fragrance. In the fragrance granules, the particulate carrier is placed in a flow granulation dryer, and the aqueous solution of the polydextrose containing the fragrance or the aqueous dispersion is continuously or intermittently sprayed on the particles while being blown into a warm air of 80 ° C or lower. The surface of the carrier is dried and manufactured.

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

[Previous Technical Literature] (Patent Literature)

Patent Document 1: WO 2008/072627

Accordingly, a first object of the present invention is to provide a low-absorbency particle carrying a relatively large amount of flavoring agent in a relatively short period of time.

Further, an object of the present invention is to provide a cigarette filter and a filter-attached cigarette comprising such a fragrance-supporting low-absorbency particle.

Further, it is an object of the present invention to provide a method for producing a low-absorbability particle.

In order to solve the above problems, according to a first aspect of the present invention, a low-absorbability particle having a BET specific surface area of less than 700 m ² /g and a supported low-absorbing particle are provided. a perfume holding medium having a fragrance and a fragrance-maintaining material for holding the fragrance-maintaining material of the surface of the low-adsorption core particle, wherein the fragrance-maintaining material is low-suction by the fragrance The total amount of the particles is 5 to 20% by weight, and the fragrance is present in an amount of 10 to 50% by weight of the above-mentioned holding material.

According to a second aspect of the present invention, there is provided a filter for cigarettes comprising a filter segment comprising a fragrance-supporting low-absorbency particle of the present invention. Further, according to a third aspect of the present invention, there is provided a cigarette with a filter comprising a cigarette rod and a filter for cigarettes according to the present invention which is connected to one end of the cigarette rod.

According to a fourth aspect of the present invention, there is provided a method for producing a low-absorbability particle containing a fragrance, which is characterized in that a low-adsorption core particle having a BET specific surface area of less than 700 m ² /g is decompressed under reduced pressure The liquid aroma-releasing composition containing the fragrance and the fragrance-maintaining material was sprayed on the low-absorbance core particles while stirring.

According to the present invention, the treatment of a relatively large amount of the fragrance can be carried out for a relatively short period of time to carry the low sorption particles.

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

The fragrance-supporting low-absorption particle system of the present invention comprises: a low-absorption core particle, and a fragrance generating medium which is supported on the surface of the low-adsorption core particle and contains a fragrance and a fragrance-maintaining material which retains the fragrance. . The perfume retaining material is present in an amount of from 5 to 20% by weight based on the total weight of the perfume-supporting low-absorbency particles, and the perfume is present in an amount of from 10 to 50% by weight based on the weight of the retaining material.

The low sorption core particles used in the present invention have a BET specific surface area of less than 700 m ² /g. In the present specification, the BET specific surface area means a specific surface area determined by a known BET method. The core particles having a BET specific surface area of less than 700 m ² /g are less absorbed by the components in the mainstream cigarette of cigarettes, and have less influence on the flavor of cigarettes.

Such low sorption nuclear particles can be obtained by calcium citrate, activated carbon with low activation, cerium oxide, ceramics, crystalline cellulose, wood, phytoplasma, styrene-divinylbenzene copolymer, ethylene The vinyl acetate copolymer is further formed by a water-absorptive polymer such as polyvinyl alcohol or sodium polyacrylate.

The low-adsorption core particles preferably have an average particle diameter of from 75 μm to 2000 μm, and for example, those having an average particle diameter of from 75 μm to 1000 μm can be suitably used. Further, the low sorption core particles preferably have a water retention ratio of 10% or more, more preferably 20 to 40%. Here, the water retention ratio refers to the ratio of the water retention amount when the core particles are immersed in water to the dry matter weight of the core particles. Any of the above-exemplified nuclear particle systems indicates such a water retention rate.

The aroma generating medium that coats the surface of the low sorbent core particles contains a fragrance and a fragrance retaining material that retains the fragrance.

Among the perfume examples are hydrophilic perfumes and hydrophobic perfumes. Examples of hydrophilic perfumes include tobacco leaf extracts, natural vegetable flavors (eg, licorice, stalks (St. John's-bread), plum extract, peach extract, etc.), acids (eg, malic acid, tartaric acid, citric acid, Butyric acid, etc.), sugars (such as glucose, fructose, high-fructose corn syrup, etc.). Examples of hydrophobic perfumes include menthol, cocoa (powder, extract, etc.), esters (eg, isoamyl acetate, linalyl acetate, isoamyl propionate, agaric acid ester, etc.), natural Essential oils (plant essential oils such as vanilla extract, spearmint, peppermint, cassia, jasmine, etc.; animal essential oils such as musk, ambergris, civet, sea Castoreum, etc., monomeric perfumes (eg, anethole, limonene, linalool, eugenol, vanillin, etc.).

The film-forming material and the emulsifier as needed are contained in the material for holding the fragrance. A representative example of the film-forming material used in the present invention is polydextrose, and the polydextrose contains pullulan, maltodextrin, and hydroxypropylcellulose. Polydextrose is water soluble. A film-forming material such as polydextrose is a composition in which a fragrance is incorporated from a film formed thereby to retain a fragrance. The film forming material can be used for any of a hydrophilic fragrance and a hydrophobic fragrance.

Examples of the emulsifier include glycerin fatty acid ester, sucrose fatty acid ester (sucrose ester), sorbitan fatty acid ester, propylene glycol fatty acid ester, and lecithin. milk The agent molecules are in an aqueous medium which retains the hydrophobic perfume by sorbing the hydrophobic groups around the oil droplets of the hydrophobic perfume and retaining the hydrophobic perfume after drying.

In the perfume-supporting low-absorbency particles of the present invention, the perfume-retaining material is present in an amount of from 5 to 20%, preferably from 5 to 10%, based on the total weight of the low-absorbent particles. The perfume is then present in an amount from 10 to 50% by weight of the perfume retaining material.

While stirring the low-adsorption core particles under reduced pressure, the liquid aroma-releasing composition containing the fragrance and the flavor-maintaining material is sprayed on the low-adsorption core particles, thereby preparing the fragrance of the present invention to be low. Soluble particles.

The fragrance contained in the liquid aroma release composition is as previously described, and the perfume retaining material is as previously described.

When the liquid aroma release composition contains only a hydrophilic fragrance as a fragrance, the composition generally contains polydextrose as a film-forming material and a hydrophilic fragrance, and further preferably contains a solvent as a dissolved polydextrose and a hydrophilic fragrance. Water.

When the liquid aroma release composition contains a hydrophobic fragrance as a fragrance (for example, when the liquid aroma release composition contains only a hydrophobic fragrance as a fragrance, or a hydrophilic fragrance and a hydrophobic fragrance as a fragrance), the fragrance release The composition is preferably a polydextrose as a film-forming material, water as a solvent for polydextrose, a hydrophobic fragrance (and a hydrophilic fragrance), an oily solvent in which a hydrophobic fragrance is dissolved (for example, vegetable oil or saturated fatty acid triglycerin). An ester, preferably a medium chain fatty acid triglyceride, and an emulsifier. The composition is a hydrophilic fragrance when it is added to a hydrophobic fragrance and contains a hydrophilic fragrance. Dissolved in water.

When the fragrance is used to hold the low-absorbency particles, when the liquid-like aroma release composition is sprayed, the low-adsorption core particles are preferably placed under a reduced pressure of 12.3 kPa or less, for example, under a reduced pressure of 7.4 to 12.3 kPa. . Further, at this time, the sorbent core particles are preferably at a temperature of 60 ° C or lower, for example, a temperature of 40 to 60 ° C. By spraying the liquid aroma-releasing composition containing the fragrance and the fragrance-maintaining material under reduced pressure, a large amount of the fragrance can be supported on the low-adsorption core particles, and at the same time, the high-viscosity aroma can be released. The advantage of the spray (from a viscosity of around 2 Pa.s) from the nozzle.

To produce the low sorbent particles for the perfume of the present invention, a conical ribbon mixing/drying machine can be utilized. The conical ribbon mixing/drying machine is described in, for example, JP-A-2003-71263, JP-A-2003-290641, JP-A-2007-229633, and commercially available from Okawara.

The basic structure of such a conical ribbon mixing/drying machine will be described with reference to Fig. 1. Fig. 1 is a schematic view showing an example of a conical ribbon mixing/drying machine 10 in a cross section. The conical ribbon mixing/drying machine 10 is internally mixed/dried. The treatment tank 12 including the reverse conical portion 121 and the cylindrical portion 122 connected thereto is provided. A double spiral ribbon rotating blade 14 disposed in the processing tank 12 is provided. A rotating shaft 16 extending in the longitudinal direction of the center of the processing tank 12, the spiral ribbon rotating blade 14 is attached to a plurality of supporting rods (the supporting rods 18a to 18e in the first drawing) which are spaced apart from each other and fixed to the rotating shaft 16 on. Above the rotary wing 14, the inner wall of the cylindrical portion 122 of the treatment tank 12 is fixed to, for example, a vortex breaker 20a composed of a pair of plate-like bodies, 20b. The eddy current interrupters 20a and 20b move the processed material (lowly absorbing particles in the present invention) which is raised along the inner wall of the processing tank 12 by the ribbon rotating blade 14 toward the vicinity of the center of the processing tank 12. At the same time, it falls on the lower portion of the treatment tank 12.

The outer periphery of the processing tank 12 surrounds the jacket 22, and in the jacket 22, steam is introduced from the steam introduction port 22a via the line L1 in order to heat the contents of the container, and the vapor is discharged from the steam discharge port 22b via the line L2 to Out of line.

The upper opening portion of the container is blocked by the top plate 24. The top plate 24 is provided with a motor 26 and a speed reducer 28, and the output shaft of the speed reducer 28 is coupled to a rotating shaft 16 provided in the processing tank 12. Further, the top plate 24 is provided with an input port 24a of the object to be treated (in the case of the present invention, a low-absorbability core particle), and a treatment material is provided at the bottom of the treatment tank 12 (in the case of the present invention, the fragrance is low-suction) The outlet of the sexual particle) 12a.

Further, the bag filter 30 is attached to the top plate 24. The bag filter captures the granules in the contents of the treatment tank 12 (in the case of the present invention, low sorbing particles), and allows the volatile matter (in the case of the present invention, the water in the scent release composition) to pass. It is introduced into the condenser 32 via the line L3. The condenser 32 is constituted by, for example, a water-cooled cooler, and contains volatile matter in the inner cylinder 321, and the volatile matter is cooled by the cooling water introduced into the outer cylinder 322 from the line L5, and becomes a condensate (water). Line L6 is discharged. 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 treatment tank 12 is depressurized by driving the decompression pump P1.

The basic structure of the conical ribbon mixing/drying machine is as above, but In order to prepare the low-absorbability particles in the fragrance of the present invention, the nozzles 34 introduced into the treatment tank 12 by introducing the liquid aroma release composition are passed through the top plate 24, and the composition LFC is released from the liquid aroma. The container 36 sprays the liquid aroma release composition into the treatment tank 12 via a line L8 having a liquid supply pump P2. Further, a temperature sensor (for example, a thermocouple) 38 for measuring the temperature of the low-adsorption particles in the treatment tank 12 is provided below the treatment tank 12.

In order to use the conical ribbon mixing/drying machine 10 shown in Fig. 1 to produce the fragrance-supporting low-absorption particles of the present invention, the low-adsorption core particles LAP contained in the container 40 are passed through the treatment tank 12 via The line L9 is introduced into the treatment tank 12. The inside of the jacket 22 is heated by introducing steam having a temperature of 80 ° C or higher, preferably 100 ° C to 120 ° C, and the double spiral ribbon rotor 14 is rotated by the driving of the motor 26 to stir the low sorption. The particles are sprayed from the nozzle 34 into the treatment tank 12 via the line L8 while driving the liquid aroma release agent liquid storage pump P2 accommodated in the container 36. The temperature of the low absorbing particles in the spray is maintained at 70 ° C or lower, preferably 60 ° C or lower. When the water in the liquid aroma release composition introduced into the treatment tank 12 is heated and evaporated by the vapor introduced into the jacket 22 at 80 ° C or higher, the evaporation of water can be taken away from the low sorption particles. Heat maintains the temperature of such low sorbent particles.

The fragrance-supporting low-absorbency particles produced in this manner are only volatilized and removed during production, and the components other than the moisture in the liquid aroma release composition suitable for the low-adsorption core particles during production are almost all Low sorption of nuclear particles. Therefore, it is suitable for liquid scent of low sorption nuclear particles. The gas release composition contains a perfume retaining material in an amount of 5 to 20% by weight, preferably 5 to 10% by weight, based on the weight of the low-absorbing core particles used, and contains a liquid fragrance-releasing composition. A fragrance in an amount of from 10 to 50% by weight of the perfume retaining material contained in the article. Further, the fragrance-retaining material contained in the liquid aroma release composition can be applied to a low-adsorption core particle in advance, in particular, an aqueous solution or an aqueous dispersion of a part of the film-forming material. When an aqueous solution or an aqueous dispersion of a part of the film forming material is applied in advance, it is possible to suppress an increase in the temperature of the low-absorbing nuclear particles in the initial stage of production of the low-wicking particles, and to suppress the low sorption. The nuclear particles produce a fine powder.

The fragrance of the present invention carries low-absorbency particles, and coats the surface of the low-adsorption core particles with a solid aroma generating medium formed by releasing the composition from the liquid aroma. In the solid aroma generating medium, the fragrance is held by the fragrance retaining material, so that the fragrance is not volatilized or adsorbed by charcoal during general storage. Then, when it comes into contact with a hydrophilic component such as moisture in the mainstream smoke generated by smoking a cigarette, the flavor retaining material is partially dissolved to release the aroma and taste the flavor of the flavor.

A filter for cigarettes according to a second aspect of the present invention includes a filter segment containing the fragrance-supporting low-absorption particles of the present invention. Further, a filter cigarette according to a third aspect of the present invention includes a cigarette rod and a cigarette attached to the one end of the cigarette rod and having the filter of the present invention.

The filter for cigarettes of the present invention may comprise a filter for dispersing the fragrance of the present invention to impart low sorption particles in a general filter material such as a cellulose acetate tow (bonded with a plasticizer such as triacetin). Section. can At one end of the filter section, a so-called charcoal filter section (for example, a filter section having a filter material in which activated carbon is dispersed in a cellulose acetate tow bonded by a plasticizer such as triacetin) is attached. Alternatively, the filter for cigarettes according to the present invention has a charcoal filter section and a common filter section which are disposed apart from each other, and can be filled with the fragrance of the present invention between the two filter sections to maintain low sorption. Sex particles.

Hereinafter, a cigarette having the filter of the present invention will be described with reference to Figs. 2 to 5 . In the second to fifth figures, the same elements are denoted by the same reference symbols.

Fig. 2 is a schematic cross-sectional view showing a cigarette (a cigarette with a filter) 50 including a filter for cigarettes according to an aspect of the present invention. The cigarette 50 with a filter is provided with a cigarette rod 52 which is wrapped in a cigarette paper 522 by a tobacco filler 521 such as a tobacco cut. The cigarette rod 52 is the same as a general cigarette.

A filter 54 is attached to one end of the cigarette rod 52. The filter 54 is provided with a charcoal filter section 541 which is provided in direct contact with one end of the cigarette rod 52; the fragrance contained in the flow side end surface of the charcoal filter section 541 is low with respect to the flow direction of the mainstream smoke. The filter section 542 of the absorbing particles; and the ordinary filter section 543 provided on the flow side end surface of the filter section 542 in which the fragrance-supporting low sorbent particles are loaded with respect to the flow direction of the mainstream smoke.

The activated carbon filter section 541 is obtained by winding, for example, a cellulose acetate fiber 541a in which the activated carbon particles 541b are dispersed in a filter take-up paper 541c, which is the same as a general charcoal filter.

The filter section 542 filled with the fragrance to hold the low sorbent particles is The filter take-up paper 542b is wrapped in a dispersion in which the fragrance of the present invention is carried, for example, a cellulose acetate fiber 542a in which the low-adsorption particles FLAP are dispersed.

The normal filter section 543 is a bundle of, for example, cellulose acetate fibers 543a wrapped in a filter take-up paper 543b.

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

Fig. 3 is a schematic cross-sectional view showing a cigarette (a cigarette with filter) 60 having a filter for cigarettes according to another aspect of the present invention. In the cigarette 60 with the filter, the sheet 56 is attached to the filter 62 of the cigarette rod 52, and has a charcoal filter section 541 directly attached to one end of the cigarette rod 52, and a charcoal filter section therewith. The ordinary filter segments 622, which are disposed at intervals of 541, are all wrapped by the filter take-up paper 66. The ordinary filter section 622 is composed of, for example, a tow of cellulose acetate fibers 622a, similarly to the ordinary filter section 543 of Fig. 2 . A cavity 64 between the charcoal filter section 541 and the normal filter section 622 is filled with the fragrance-carrying low-absorbance particle FLAP of the present invention.

Fig. 4 is a view in which the structure of the charcoal filter section 541 is omitted in the filter-attached cigarette of the structure of Fig. 2, and the filter section 542 containing the fragrance-carrying low-absorbing particles is directly attached to the cigarette rod 52. Set at one end.

Fig. 5 is a view showing a configuration in which the filter unit 543 (see Fig. 2) is used in place of the charcoal filter section 541 in the filter-attached cigarette constructed in Fig. 3.

(Example)

The present invention will be described below by way of specific examples, but the present invention is not limited to such The system is limited.

<Modulation of liquid aroma release composition>

The components shown in the following Table 1 were mixed at a ratio shown in Table 1 and emulsified by an emulsifier (ROBOMICS Mark II manufactured by Primix Co., Ltd.) at 7500 rpm for 15 minutes. At this time, the periphery of the emulsifier was cooled with water in order to prevent the temperature of the mixture from exceeding 45 °C. Thus, liquid aroma is released to release compositions A to D.

Further, the medium chain fatty acid triglyceride was Coconard MT manufactured by Kao Corporation, the egg phospholipid was LP-20E manufactured by Nisshin Olympus Co., Ltd., and the sucrose ester was P-1570 manufactured by Mitsubishi Chemical Food Co., Ltd.

<Flour is responsible for the modulation of low sorption particles> (Example 1)

Here, a conical ribbon mixing/drying machine Ribocone RM-50-VD manufactured by Okawara Seisakusho Co., Ltd. (refer to Fig. 1) is used. 10 kg of calcium citrate particles (Sanwa Marume, Inc., an average particle diameter of 1 mm, a BET specific surface area of less than 700 m ² /g) and 6 kg of a 5 wt% aqueous pullulan solution were placed in the above mixing/drying machine. The steam at a temperature of 120 ° C was circulated in a jacket under a pressure of 200 kPa, the pressure in the mixer/dryer was set to 12.3 kPa, and calcium silicate particles were stirred. After stirring for 5 minutes, the liquid aroma release composition A5 kg was sprayed into the mixing/drying machine from the nozzle for 40 minutes, and further stirred and dried for 20 minutes. The calcium citrate particles were taken out from the mixing/drying machine and rapidly placed in a continuous flow granulation drying apparatus (Mix grade 0.5 manufactured by Okawara Seisakusho Co., Ltd.) to carry out sensible heat exchange in the calcium citrate particles for 3 minutes. Dehumidification, the fragrance is supported by calcium citrate particles.

(Example 2)

A perfume-supported calcium citrate particle product was obtained in the same manner 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-supported calcium citrate particle product was obtained in the same manner 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-supported calcium citrate particle product was obtained in the same manner as in Example 1 except that the liquid aroma release composition D was used instead of the liquid aroma release composition A.

<Production of cigarettes with filter>

A filter-attached cigarette of the configuration shown in Fig. 3 was produced. Specifically, a commercially available filter-attached cigarette product "Winston light" having a cellulose acetate fiber tow as a filter material is used, and the cellulose acetate fiber tow of the filter material is removed by a clip, and then refilled with Activated carbon (Kuraray coal GGS-H28/70, manufactured by Kuraray Chemical Co., Ltd.) 85 mg of cellulose acetate fiber tow (length 12 mm; 8Y/29000 (ie, single denier 8 denier; filament cross section Y type, total) The fineness of 29000 Danny)), the perfume produced in Examples 1 to 4 was loaded with 42 mg of calcium citrate particle product (the length of the cavity portion 64 in the axial direction of the cigarette rod was 47 mm), and finally filled with cellulose acetate fiber tow (length 11 mm) ; 2.5Y/35000), a filter-attached cigarette of the structure shown in Fig. 3 was produced. Further, except for the fact that none of them was filled in the cavity portion 64, the filter-attached cigarette was produced in the same manner as described above.

It was confirmed that the fragrance-derived aroma was released from the mainstream smoke when the four kinds of filter cigarettes of the present invention were pumped, and it was confirmed that the flavor was enhanced as compared with the control filter-attached cigarette. The results show that, according to the method of the present invention, a large amount of the perfume can be supported on the low-adsorption core particles in a short period of time.

<Measurement of the amount of spices and perfume retaining materials to be held>

The amount of the perfume to be carried by the perfume retaining material obtained in Examples 1 to 4 and the amount of the perfume retaining material were measured.

The perfume-supporting particles of the comparative example were prepared in accordance with Examples 1 to 3 of the prior art document (WO 2008/072627), and the amount of the perfume and the amount of the perfume-retaining material supported by the prepared perfume-supporting particles were measured in the same manner.

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

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

Coffee oil was added in an amount of 2% by weight to 10% by weight of the pullulan aqueous dispersion of the pre-modulated pullulan. The mixture was vigorously stirred in an emulsifier (emulsifier rotation number: 2,500 rpm) to prepare a fragrance dispersion. In addition, 100 g of calcium carbonate particles having an average particle diameter of 250 μm were placed in a flow granulation dryer, and the fragrance dispersion was rapidly sprayed intermittently while blowing a warm air of 75 ° C at a flow rate of 0.6 m/sec (spray for 1 minute). After the spraying was stopped for 30 minutes, the cycle was repeated, and a total of 10 g of the fragrance dispersion was sprayed on the surface of the calcium carbonate particles and dried. Thereafter, the inside of the fluidized bed was rapidly cooled to room temperature to obtain the desired flavor granules.

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

100 g of calcium carbonate particles having an average particle diameter of 250 μm were placed in a flow granulation dryer, and while blowing a temperature of 30° C. at a flow rate of 1.0 m/sec, 1% by weight of the tobacco flavor containing vanillin was added. A 9 wt% perfume aqueous solution of pullulan was continuously sprayed, and a total of 5 g of the mixed aqueous solution was sprayed onto the surface of the calcium carbonate particles and dried. Thereafter, the warm air temperature was rapidly lowered to room temperature, and cooled at a flow rate of 0.4 m/sec to obtain the desired perfume particles.

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

Coffee oil 1% by weight and lecithin 0.5% by weight were added to 10% by weight of the pullulan aqueous dispersion of pre-modulated pullulan. The mixture was vigorously stirred in an emulsifier (emulsifier rotation number: 7,500 rpm, 15 minutes) to prepare a fragrance dispersion. Further, 300 g of pulverized coffee bean particles having an average particle diameter of 250 μm to 1.4 mm were placed in a rotary flow granulation dryer (SFC-MINI manufactured by FREUND Industries Co., Ltd.), the bottom rotating drain hole cover was rotated at about 500 rpm, the granulation preventing stirring blade was rotated at about 400 rpm, and the 75 ° C warm air was blown at a flow rate of 0.6 m/sec. Crush the flow layer of the coffee bean particles. In the flow layer, a total of 90 g of the fragrance dispersion was sprayed onto the surface of the coffee bean particles by continuous spraying while maintaining the above-mentioned fragrance dispersion at 40 ° C and dried. Thereafter, the warm air temperature was rapidly lowered to room temperature, and cooled at a flow rate of 0.4 m/sec to obtain the desired perfume particles.

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

Determination of spices:

Vibrating extraction was carried out in a blend of purified water/methanol in the perfume-supporting particles. The extract was supplied to a gas chromatography chromatography mass spectrometer (GC/MS) and the fragrance was measured.

Determination of perfume retention materials:

The particles were weighed and held (particles A), and dried by heating (weight B after drying) for the purpose of removing moisture in the particles. The dried particles are added with purified water and subjected to vibration extraction to dissolve the perfume retaining material, and the extracted particles (weight C after drying) are further dried by heating. The difference between the weight C and the weight A was made the amount of the fragrance holding material.

The measurement results are shown in Fig. 6. Fig. 6 is a graph showing the amount of the perfume to be supported and the amount of the perfume retaining material in terms of the ratio (% by weight) of the perfume-supporting particles to the total weight. Fig. 6 is a view showing that the perfume-supporting particles of the present invention hold more perfume than the perfume-carrying particles of the comparative example.

Further, the perfume-supporting particles of the present invention can be prepared by treating the particles in the comparative example for a shorter period of time.

<Relationship between BET specific surface area of nuclear particles and sorption energy of perfume-supporting particles>

The activated carbon (Kuraray coal GGS-H28/70, Kuraray Co., Ltd., average particle diameter: 0.4 mm, BET specific surface area: 700 m ² /g) was used instead of calcium citrate to serve as a core particle, and the aroma release composition D of Table 1 was used. As the aroma release composition, the activated carbon particles were prepared by the same method as the method of preparing the calcium citrate particles in the perfume of Example 1.

Specifically, the fragrance-supporting activated carbon particles are prepared as follows.

For the preparation, Riconcon RM-50-SR (see Fig. 7) of a conical ribbon mixing/drying machine manufactured by Okawara Seisakusho Co., Ltd. was used. 15 kg of activated carbon (Kuraray coal GGS-H28/70, Kuraray coal GGS-H28/70, average particle diameter: 0.4 mm, BET specific surface area: 700 m ² /g) and 6 kg of a 5 wt% pullulan aqueous solution were placed in the above-mentioned mixing/drying machine. The steam at a temperature of 120 ° C was circulated in a jacket under a pressure of 200 kPa, and the pressure in the mixer/dryer was set to 12.3 kPa, and the activated carbon was stirred. After stirring for 5 minutes, the liquid aroma release composition D7.5 kg was sprayed into the mixing/drying machine from the nozzle for 60 minutes, and further stirred and dried for 5 minutes. The activated carbon particles were taken out from the mixing/mixing/drying machine and rapidly placed in a continuous flow granulation drying apparatus (Mix grade 0.5 manufactured by Okawara Seisakusho Co., Ltd.) to carry out sensible heat exchange in the activated carbon particles for 3 minutes. Dehumidification is carried out to obtain a perfume-supporting activated carbon particle product.

Using the prepared fragrance, 300 mg of activated carbon particles were used, and a filter-attached cigarette having the structure shown in Fig. 3 was produced as follows. Specifically, a commercially available filter-attached cigarette product "Winston light" having a cellulose acetate fiber tow as a filter material is used, and the filter material is removed by a clip. After the cellulose acetate fiber tow, the cellulose acetate fiber tow is filled in the cavity (length 10 mm, 2.5 Y/35000 (that is, single denier 2.5 denier, fiber cross section Y type, total fineness 35,000 denier)) 30 ml of activated carbon particles (the length of the cavity portion 64 in the axial direction of the cigarette rod 2 mm) was filled with the prepared fragrance, and finally filled with cellulose acetate fiber tow (length 10 mm, 2.5Y/35000), and the third figure was produced. A cigarette with a filter constructed as shown. In addition, a cigarette with a filter was prepared in the same manner as described above except that 30 g of the activated carbon (Kuraray coal GGS-H28/70, manufactured by Kuraray Chemical Co., Ltd.) was used as the substitute activated carbon. Hereinafter referred to as a control cigarette).

A cigarette with a filter made by smoking, studying the acetone sorption energy in mainstream smoke.

In this experiment, in order to capture the components of mainstream cigarette smoke, the apparatus 70 shown in Fig. 7 was used. This device 70 is a trap 71 having a granular substance, and the trap 71 of the granular material is provided with a Cambridge filter 711 (diameter: 47 mm), a tobacco mainstream smoke inlet 71a for holding the cigarette CIG, and tobacco mainstream smoke. The outflow port 71b. Further, the device 70 is provided with an impeller 72. The sampler 72 houses a chemical solution TA that traps a gas phase component in the tobacco mainstream smoke. In the present experiment, 10 ml of methanol containing 200 ppm of anethole as an internal standard substance was placed as a drug solution TA. The sampler 72 is housed in a Dewar flask 73 that accommodates a refrigerant RM that is used to maintain the chemical solution TA at a cold temperature. In this experiment, a mixture of dry ice and isopropanol was used as the refrigerant RM, and the trapping solution TA was maintained at a temperature below -70 ° C in the experiment. Capturing in granular matter The outlet 71b of the catcher 71 is connected to a conduit 74 extending into the liquid chemical TA in the sampler 72. Then, the suction port 76a of the automatic smoker 76 is connected to the duct 75 in the sampler 71 extending in the space in which the upper portion of the liquid chemical TA is captured. If the cigarette is ignited and the automatic smoker 76 is driven, the sampler 72 is depressurized by attraction through the conduit 75, and the tobacco mainstream smoke is then passed through the Cambridge filter 711 in the trap 71. At this time, the granular material in the tobacco mainstream smoke is captured by the Cambridge filter 711, and the mainstream smoke from which the particulate matter has been removed is introduced into the trapping liquid TA in the sampler 72 via the conduit 74 to generate foam and cause mainstream smoke. The gas phase component is captured by the capture solution TA.

In the present experiment, the cigarette was attached to the trap 71, and the automatic smoking device 76 was used to smoke under the standard smoking conditions of ISO (1 puff: 35 ml for 2 seconds, and the interval of the smoke: 58 seconds). After the end of the smoking, the drug solution in the sampler 72 was transferred to a serum bottle, and a Cambridge filter 711 in which the particulate matter was caught was placed therein, and extracted by shaking at 250 times/min. for 30 minutes. 1 ml of this extract was placed in a micro vial for GC/MS analysis, and the components in the mainstream smoke were analyzed under the following conditions.

Analysis conditions for components in mainstream smoke:

. GC/MS: HP 7890/5975

. Column: DB-1701

. Column flow: 1.2ml/min

. The temperature rising condition was maintained at 60 ° C for 5 minutes, and then the temperature was raised to 160 ° C at 5 ° C / minute, and the temperature was raised to 250 ° C at 10 ° C / minute and held for 30 minutes.

. Injection: split ratio 10:1; injection port 220 ° C; flow rate 12 ml / min; total flow rate 16.2 ml / min

. MS conditions: scan parameters 33.0 to 200.0; threshold 50; MS ion source 230 ° C; MS quadrupole 150 ° C.

For cigarettes with a common filter (a cigarette rod with a commercially available cigarette product "Winston light", and connected at one end to a cellulose acetate tow (length 20 mm, 2.5Y/70000) The same analysis was also performed for a conventional filter; hereinafter referred to as a reference cigarette) and the aforementioned control cigarette.

From the analysis results of the cigarette, the control cigarette, and the reference cigarette containing the filter carrying the activated carbon particles, the peak area value of the acetone was calculated, and the filter-containing cigarette and the control cigarette containing the activated carbon particles were added. The acetone peak area value is divided by the acetone peak area value of the reference cigarette, and the value is multiplied by 100 times to determine the acetone reduction rate (%), and the acetone reduction rate (%) is subtracted from 100% to calculate the acetone adsorption rate. .

As a result, the acetone sorption rate of the control cigarette was 48%, and the acetone sorption rate of the filter cigarette containing the scent-bearing activated carbon particles was 45%. This result shows that when the activated carbon-supporting activated carbon particles are produced using activated carbon having a BET specific surface area of 700 m ² /g as the core particles, the perfume-carrying activated carbon particles maintain about 94% of the intrinsic sorption energy of the core particles. It sucks.

Two kinds of filter-containing cigarettes similar to the above-mentioned control cigarettes were prepared except that activated carbon (30 mg) having a specific surface area of 700 m ² /g and 1000 m ² /g was used instead of activated carbon (30 mg) having a specific surface area of 700 m ² /g. . When the cigarettes were investigated for the same rate as the above, the cigarettes of the former were 23%, and the cigarettes of the latter were 34%.

From the above results, it is understood that the nuclear particles having a specific surface area of 700 m ² /g or more represent high sorption energy for components in mainstream cigarette smoke, but the nuclear particles having a specific surface area of less than 700 m ² /g indicate that they are mainly for cigarettes. The absorbing energy of the ingredients in the smoke is low.

10‧‧‧Conical ribbon mixing/drying machine

12‧‧‧Processing tank

12a‧‧‧ Discharge of treatment tank

14‧‧‧Double spiral ribbon rotor

16‧‧‧Rotary axis

18a to 18e‧‧‧ support rods

20a to 20b‧‧‧ eddy current interrupter

22‧‧‧ Jacket

22a‧‧‧Vapor inlet

22b‧‧‧Vapor discharge

24‧‧‧ top board

24a‧‧‧Input of the treated object

26‧‧‧Motor

28‧‧‧Reducer

30‧‧‧ bag filter

32‧‧‧Condenser

34‧‧‧Nozzles

36‧‧‧Liquid aroma release composition (LFC) containment container

38‧‧‧temperature sensor

40‧‧‧Low-absorbable nuclear particle (LAP) containment container

50, 60‧‧‧With filter cigarette

52‧‧‧ cigarette rod

54, 62‧‧‧ filter

56‧‧‧Sheet paper

64‧‧‧empty department

66, 542b, 543b‧‧‧ filter take-up paper

70‧‧‧Communication components in cigarette mainstream smoke

71‧‧‧Capture of granular matter

71a‧‧‧Tobacco mainstream smoke inlet

71b‧‧‧Tobacco mainstream smoke outlet

72‧‧‧sampler

73‧‧‧Dova

74, 75‧‧‧ catheter

76‧‧‧Automatic smoker

76a‧‧‧ attracting mouth

121‧‧‧The reverse cone of the treatment tank

122‧‧‧The cylindrical part of the treatment tank

321‧‧‧ inner tube of the condenser

322‧‧‧Condenser

521‧‧‧Tobacco filler

522‧‧‧ cigarette paper

541‧‧‧ Filter section loaded with activated carbon

541a, 542a, 543a, 622a‧‧‧ cellulose acetate fiber

541b‧‧‧ charcoal particles

541c‧‧‧Filter take-up paper

542‧‧‧ Filter section containing perfume to hold low sorbent particles

543‧‧‧Ordinary filter section

622‧‧‧Ordinary filter section

711‧‧‧Cambridge filter

CIG‧‧‧ Cigarettes

FLAP‧‧ ‧ Spices hold low sorbent particles

P1‧‧‧ decompression pump

P2‧‧‧ liquid pump

RM‧‧‧Refrigerant

TA‧‧‧Drug to capture the gas phase components of tobacco mainstream smoke

Fig. 1 is a schematic cross-sectional view showing an example of an apparatus for producing a low-absorbability particle by the fragrance of the present invention.

Fig. 2 is a schematic cross-sectional view showing a cigarette with a filter according to an embodiment of the present invention.

Fig. 3 is a schematic cross-sectional view showing a cigarette with a filter according to another embodiment of the present invention.

Fig. 4 is a schematic cross-sectional view showing a cigarette with a filter according to still another embodiment of the present invention.

Fig. 5 is a schematic cross-sectional view showing a cigarette with a filter according to still another embodiment of the present invention.

Fig. 6 is a graph showing the measurement results of the amount of the fragrance and the fragrance retaining material carried.

Fig. 7 is a schematic view showing a part of a trapping device for a component in a cigarette mainstream smoke.

Since the attached drawings are merely illustrations and cannot represent all the technical features of this paper, there is no designated representative figure in this case.

Claims (5)

A method for producing a low-adsorption particle of a fragrance, characterized in that a low-adsorption core particle having a BET specific surface area of less than 700 m ² /g is stirred under reduced pressure, and a fragrance and a polydextrose are contained. The liquid aroma release composition is sprayed on the aforementioned low absorbing core particles to produce. The method for producing a low-absorbability particle according to the invention of claim 1, wherein the liquid aroma release composition is 5 to 20% by weight of the total weight of the low-absorbency particles. The amount contains the aforementioned polydextrose, and the aforementioned fragrance is contained in an amount of 10 to 50% by weight based on the weight of the aforementioned polydextrose. The method for producing a low-absorbability particle according to the first or second aspect of the invention, wherein the pressure reduction is a pressure of 12.3 kPa or less. The method for producing a low-absorbability particle according to the first aspect or the second aspect of the invention, wherein the low-adsorption core particle is maintained at a temperature of 60 ° C or lower in the spraying. The method for producing a low-absorbability particle according to the first or second aspect of the invention, wherein the polydextrose is pullulan.