CN107034015B - Method for producing perfume-carrying low-adsorption particles - Google Patents
Method for producing perfume-carrying low-adsorption particles Download PDFInfo
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- CN107034015B CN107034015B CN201710059867.8A CN201710059867A CN107034015B CN 107034015 B CN107034015 B CN 107034015B CN 201710059867 A CN201710059867 A CN 201710059867A CN 107034015 B CN107034015 B CN 107034015B
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/06—Use of materials for tobacco smoke filters
- A24D3/14—Use of materials for tobacco smoke filters of organic materials as additive
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/04—Tobacco smoke filters characterised by their shape or structure
- A24D3/048—Tobacco smoke filters characterised by their shape or structure containing additives
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/06—Use of materials for tobacco smoke filters
- A24D3/08—Use of materials for tobacco smoke filters of organic materials as carrier or major constituent
- A24D3/10—Use of materials for tobacco smoke filters of organic materials as carrier or major constituent of cellulose or cellulose derivatives
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/06—Use of materials for tobacco smoke filters
- A24D3/16—Use of materials for tobacco smoke filters of inorganic materials
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/06—Use of materials for tobacco smoke filters
- A24D3/16—Use of materials for tobacco smoke filters of inorganic materials
- A24D3/163—Carbon
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/06—Use of materials for tobacco smoke filters
- A24D3/16—Use of materials for tobacco smoke filters of inorganic materials
- A24D3/166—Silicic acid or silicates
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Cigarettes, Filters, And Manufacturing Of Filters (AREA)
- Fats And Perfumes (AREA)
- Seasonings (AREA)
Abstract
The present invention provides a perfume-carrying low-adsorption particle, which comprises: having a thickness of less than 700m2A low adsorption core particle having a BET specific surface area of per gram, and a flavor-generating agent supported on the surface of the low adsorption core particle and containing a flavorant and a flavorant-holding material for holding the flavorant, wherein the flavorant-holding material is present in an amount of 5 to 20% by weight of the total weight of the low adsorption core particle supported by the flavorant, and the flavorant is present in an amount of 10 to 50% by weight of the holding material.
Description
The present application is a divisional application of the chinese invention application "low adsorbent particles with perfume carrier, filter for cigarette, filter cigarette, and method for producing low adsorbent particles with perfume carrier" filed on 7/11/2012 and application No. 201280035198.6.
Technical Field
The present invention relates to a flavor-carrying low-adsorption particle, a filter for a cigarette, a filter-equipped cigarette, and a method for producing a flavor-carrying low-adsorption particle.
Background
Flavor-carrying particles are incorporated into a cigarette filter, and flavor derived from the flavor is released into cigarette mainstream smoke to taste the cigarette mainstream smoke. For example, patent document 1 discloses a flavor bead in which a dextran film containing a flavor is coated on the surface of a particulate carrier such as calcium carbonate. The flavor bead is manufactured by the following method: the particulate carrier is put into a fluidized granulation dryer, and an aqueous solution or aqueous dispersion of glucan containing a perfume is continuously or intermittently sprayed onto the surface of the particulate carrier while blowing warm air at, for example, 80 ℃ or lower, and dried.
However, the method of patent document 1 takes a long time to treat a large amount of perfume, and as a result, it is difficult to increase the amount of perfume to be carried.
Documents of the prior art
Patent document
Patent document 1: WO2008/072627
Disclosure of Invention
Problems to be solved by the invention
Accordingly, a first object of the present invention is to provide a perfume-carrying low-adsorption particle carrying a relatively large amount of perfume by a short treatment.
Another object of the present invention is to provide a filter for a cigarette containing the low adsorptive particles having the flavorant supported thereon, and a cigarette with the filter.
Further, an object of the present invention is to provide a method for producing a low-adsorptive particle having a fragrance carried thereon.
Means for solving the problems
In order to solve the above-described problems, according to a first aspect of the present invention, there is provided a fragrance-carrying low-adsorption particle comprising: having a thickness of less than 700m2A low adsorption core particle having a BET specific surface area of per gram, and a fragrance generating medium which is supported on the surface of the low adsorption core particle and contains a fragrance and a fragrance retaining material retaining the fragrance, wherein the fragrance retaining material is present in an amount of 5 to 20% by weight of the total weight of the low adsorption core particle supported by the fragrance, and the fragrance is present in an amount of 10 to 50% by weight of the retaining material.
Further, according to a second aspect of the present invention, there is provided a cigarette filter comprising a filter portion containing the low-adsorptive flavor-carrying 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 cigarette filter of the present invention attached to one end of the cigarette rod.
Further, according to a fourth aspect of the present invention, there is provided a method for producing a fragrance-supporting low-adsorption particle, comprising: one side of the mixture is treated under the reduced pressure condition to have the thickness of less than 700m2Stirring of low-adsorptive core particles having BET specific surface area/gSpraying a liquid flavor-releasing composition comprising a flavorant and a flavorant-holding material onto the low-adsorbability core particles while stirring.
ADVANTAGEOUS EFFECTS OF INVENTION
According to the present invention, a perfume-carrying low-adsorption particle carrying a relatively large amount of perfume can be provided by a short treatment.
Drawings
FIG. 1 is a schematic sectional view showing an example of an apparatus for producing a fragrance-carrying low-adsorptive particle 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 of a cigarette with a filter according to another embodiment of the present invention;
FIG. 4 is a schematic sectional view showing a filter cigarette according to still another embodiment of the present invention;
FIG. 5 is a schematic sectional view showing a filter cigarette according to still another embodiment of the present invention;
FIG. 6 is a graph showing the measurement results of the amounts of the flavorant and the flavorant-holding material carried;
fig. 7 is a partial cross-sectional schematic view showing a device for trapping components in cigarette mainstream smoke.
Symbol
10 … conical ribbon mixer/dryer, 12 … treatment tank, 12a … treatment substance discharge port, 121 … treatment tank inverted conical part, 122 … treatment tank cylindrical part, 14 … double helical ribbon paddle, 16 … rotary shaft, 18a 18e … support rod, 20a 20b … vortex eliminator, 22 … jacket, 22a … steam inlet, 22b … steam outlet, 24 … top plate, 26 … motor, 28 … speed reducer, 24a … treatment substance inlet, 30 … bag filter, 32 … condenser, 321 … condenser inner cylinder, 322 … condenser outer cylinder, P1 … pump, 34 … nozzle, 36 … liquid flavor release composition (LFC) storage container, P2 … liquid feed pump, 38 … temperature sensor, 40 … low adsorption nuclear particle (LAP) storage container
50,60 … filter cigarettes, 52 … cigarette rod, 521 … tobacco filler, 522 … cigarette paper, 54,62 … filter, 541 … activated carbon-loaded filter section, 542 … flavor-loaded low-adsorbability particle filter section, 543 … normal filter section, FLAP … flavor-loaded low-adsorbability particle, tobacco smoke filter section, tobacco,
541a,542a,543a, 622a … cellulose acetate fiber, 541b … carbon particle, 542b,543b,66 … filter wrapping paper, 56 … tipping paper, 622 … normal filter portion, 64 … cavity
70 … catching device of main stream smoke of cigarette, 711 … Cambridge filter, CIG … cigarette, catching device of 71 … granular substance, 71a … tobacco main stream smoke inlet, 71b … tobacco main stream smoke outlet, 72 … sampler, TA … liquid medicine for catching gas phase component in tobacco main stream smoke, 73 … Dewar flask, RM … refrigerant, 74,75 … conduit, 76 … automatic smoking device, 76a … suction port
Detailed Description
Embodiments of the present invention will be described in detail below.
The low-adsorptive perfume-carrying particles of the present invention comprise: a low-adsorption 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 retaining material for retaining the fragrance. The perfume-holding material is present in an amount of 5 to 20% by weight of the total weight of the perfume-carrying low-adsorption particles, and the perfume is present in an amount of 10 to 50% by weight of the holding material.
The low-adsorptivity core particles used in the present invention have a size of less than 700m2BET specific surface area in g. In the present specification, the BET specific surface area refers to a specific surface area determined by a known BET method. BET specific surface area of less than 700m2The/g core particles have less adsorption to components in cigarette mainstream smoke and have little influence on the flavor of the cigarette.
Such low-adsorptive core particles can be formed from calcium silicate, activated carbon having a low degree of activation, silica, ceramics, crystalline cellulose, wood, plant itself (phytoplasma), styrene-divinylbenzene copolymer, ethylene-vinyl acetate copolymer, and water-absorbing polymers such as polyvinyl alcohol and sodium polyacrylate.
The low-adsorbability particles preferably have an average particle diameter of 75 to 2000 μm, and for example, particles having an average particle diameter of 75 to 1000 μm can be preferably used. The low-adsorptive core particles are preferably particles having a water retention of 10% or more, more preferably 20 to 40%. Here, the water retention rate refers to a ratio of a water retention amount when the core particles are immersed in water to a dry weight of the core particles. The above-exemplified core particles all show such a water retention rate.
A fragrance-generating medium for coating the surface of a low-adsorbability core particle contains a fragrance and a fragrance-retaining material for retaining the fragrance.
Examples of perfumes include hydrophilic perfumes and hydrophobic perfumes. Examples of the hydrophilic flavor include tobacco leaf extract, natural plant flavors (e.g., licorice, carob bean, plum extract, peach extract, etc.), acids (e.g., malic acid, tartaric acid, citric acid, butyric acid, etc.), sugars (e.g., glucose, fructose, high fructose syrup, etc.). Examples of the hydrophobic flavors include menthol, cacao (powder, extract, etc.), esters (e.g., isoamyl acetate, linalyl acetate, isoamyl propionate, linalyl butyrate, etc.), natural essential oils (e.g., vanilla extract, spearmint, peppermint, cassia seed, jasmine, etc., as plant essential oils; e.g., musk, ambergris, civet, castoreum, etc., as animal essential oils), monomeric flavors (e.g., anethole, limonene, linalool, eugenol, vanillin, etc.).
The holding material for holding the perfume includes a film-forming material and an emulsifier as required. Representative examples of the film-forming material used in the present invention are dextrans, and dextrans include pullulan, maltodextrin, and hydroxypropyl cellulose, for example. Dextran is water soluble. The film-forming material such as dextran can retain the perfume by adding the perfume to the film formed therefrom. The film-forming material may be used for both hydrophilic and hydrophobic flavors.
Examples of the emulsifier include glycerin fatty acid ester, sucrose fatty acid ester (sugar ester), sorbitan fatty acid ester, propylene glycol fatty acid ester, lecithin. In an aqueous medium, the emulsifier molecules retain the hydrophobic perfume by adsorbing these hydrophobic groups around the oil droplets of the hydrophobic perfume, and also retain the hydrophobic perfume after drying.
In the perfume-carrying low-adsorption particle of the present invention, the perfume-retaining material is present in an amount of 5 to 20%, preferably 5 to 10%, of the total weight of the perfume-carrying low-adsorption particle. The perfume is present in an amount of 10 to 50% by weight of the perfume holding material.
The low adsorptive particle having a fragrance carrier of the present invention can be produced by the following method: while stirring the low-adsorption core particles under reduced pressure, a liquid flavor-releasing composition containing a flavor and a flavor-retaining material is sprayed onto the low-adsorption core particles.
The perfume contained in the liquid fragrance-releasing composition is as described above, and the perfume-retaining material is also as described above.
In the case where the liquid fragrance-releasing composition contains only a hydrophilic fragrance as the fragrance, the composition usually contains dextran as the film-forming material and a hydrophilic fragrance, and preferably further contains water as a solvent for dissolving dextran and a hydrophilic fragrance.
In the case where the liquid fragrance-releasing composition contains only the hydrophobic fragrance as the fragrance (for example, in the case where the liquid fragrance-generating composition contains only the hydrophobic fragrance as the fragrance, or in the case where the liquid fragrance-generating composition contains the hydrophilic fragrance together with the hydrophobic fragrance as the fragrance), the fragrance-releasing composition preferably contains dextran as the film-forming material, water as the solvent for dextran, the hydrophobic fragrance (and the hydrophilic fragrance), an oily solvent (for example, vegetable oil or a composition containing fatty acid triglyceride, preferably medium-chain saturated fatty acid triglyceride) in which the hydrophobic fragrance is dissolved, and an emulsifier. When the composition contains a hydrophilic perfume in addition to the hydrophobic perfume, the hydrophilic perfume is dissolved in water.
In the production of the flavor-carrying low-adsorptive particles, the low-adsorptive core particles are preferably placed under a reduced pressure of 12.3kPa or less, for example, a reduced pressure of 7.4 to 12.3kPa, during spraying of the liquid flavor releasing composition. In this case, the adsorbent core particles are preferably at a temperature of 60 ℃ or lower, for example, 40 to 60 ℃. By spraying a liquid flavor-releasing composition containing a flavor and a flavor-retaining material under reduced pressure, a large amount of flavor can be supported on the low-adsorbable core particles, and a high-viscosity flavor-releasing composition (for example, a viscosity of about 2Pa · s) can be sprayed from a nozzle.
For producing the low adsorptive particles having a flavorant supported thereon of the present invention, a conical ribbon mixer/dryer can be used. The conical helical 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 Dachuan.
The basic structure of such a conical ribbon mixer/dryer will be described with reference to fig. 1. Fig. 1 schematically shows an example of a conical ribbon mixer/dryer 10 in cross section. The conical ribbon mixer/dryer 10 performs mixing/drying processing inside, and includes a processing tank 12 including an inverted conical portion 121 and a cylindrical portion 122 connected thereto. A double-spiral ribbon stirring paddle 14 is provided in the treatment tank 12. A plurality of support bars (support bars 18a to 18e in fig. 1) for fixing the rotation shaft 16 are attached to a rotation shaft 16 extending in the longitudinal direction at the center in the treatment tank 12, with the ribbon-like stirring paddles 14 being attached. Above the propeller 14, vortex eliminators 20a, 20b, for example, formed of a pair of plate-like bodies, are fixed to the inner wall of the cylindrical portion 122 of the treatment tank 12. The vortex eliminators 20a, 20b move the treatment object (low adsorption particles in the present invention) that has risen along the inner wall of the treatment tank 12 by the action of the ribbon-shaped stirring paddle 14 toward the vicinity of the center of the treatment tank 12, and drop down to the lower part of the treatment tank 12.
The jacket 22 is surrounded on the outer periphery of the treatment tank 12, and in order to heat the vessel contents, steam is introduced from the steam inlet 22a through the line L1 in the jacket 22, and the steam is discharged from the steam outlet 22b to the outside of the system through the line L2.
The upper opening of the container is closed by a top plate 24. The top plate 24 is provided with a motor 26 and a speed reducer 28, and an output shaft of the speed reducer 28 is connected to the rotating shaft 16 provided in the treatment tank 12. The top plate 24 is provided with an inlet 24a for the object to be treated (low-adsorptive nuclear particles in the case of the present invention), and the bottom of the treatment tank 12 is provided with an outlet 12a for the object to be treated (low-adsorptive particles carried by the flavorant in the case of the present invention).
Further, a bag filter 30 is attached to the top plate 24. The baghouse filter captures particulates (low adsorptive particles in the case of the present invention) in the contents of the treatment tank 12, passes the volatile substances (water in the flavor-releasing composition in the case of the present invention), and guides the volatile substances to the condenser 32 through a line L3. The condenser 32 is constituted by, for example, a water-cooled cooler, and the volatile passes through the inner cylinder 321, and the volatile is cooled by cooling water introduced from the line L5 into the outer cylinder 322 to become a condensate (water), and discharged from the line L6. The water introduced into the outer tube 322 is discharged through a line L5. The inside of the treatment tank 12 is depressurized by driving a depressurization pump P1 connected to a depressurization pump P1 through an inner line L7.
The basic configuration of the conical ribbon mixer/dryer is as described above, but in order to produce the flavor-supporting adsorbent particles of the present invention, a nozzle 34 for introducing a liquid flavor releasing composition into the treatment tank 12 is provided so as to penetrate the top plate 24, and the liquid flavor releasing composition is sprayed into the treatment tank 12 from a container 36 containing the liquid flavor releasing composition LFC through a line L8 provided with a liquid feed pump P2. A temperature sensor (e.g., thermocouple) 38 for measuring the temperature of the adsorbent particles in the treatment tank 12 is provided at the lower portion of the treatment tank 12.
In order to produce the flavor-carrying low-adsorption particles of the present invention using the conical ribbon mixer/dryer 10 shown in fig. 1, low-adsorption core particles LAP stored in the container 40 are introduced into the treatment tank 12 through the line L9 in the treatment tank 12. The inside of the treatment tank 12 is heated by introducing steam having a temperature of 80 ℃ or higher, preferably 100 to 120 ℃ into the jacket 22, and the liquid flavor releasing composition contained in the container 36 is sprayed from the nozzle 34 into the treatment tank 12 through the line L8 by the driving of the liquid feed pump P2 while the low-adsorbability particles are stirred by the rotation of the double helical ribbon-shaped stirring paddle 14 by the driving of the motor 26. In the spraying, the temperature of the low-adsorbability particles is preferably maintained at 70 ℃ or lower, preferably 60 ℃ or lower. When the water in the liquid flavor releasing composition introduced into the treatment tank 12 is heated and evaporated by the steam of 80 ℃ or higher introduced into the jacket 22, the temperature of the low-adsorption particles can be maintained by depriving the evaporation heat of the water from the low-adsorption particles.
The perfume-carrying low-adsorption particles produced as described above volatilize and remove moisture only during production, and components other than moisture in the liquid perfume releasing composition applied to the low-adsorption core particles during production are substantially carried by the low-adsorption core particles. Therefore, the liquid flavor release composition applied to the low-adsorbability core particle contains 5 to 20%, preferably 5 to 10%, of the flavor retaining material relative to the weight of the low-adsorbability core particle used, and contains 10 to 50% of the flavor relative to the weight of the flavor retaining material contained in the liquid flavor release composition. In addition, a partial aqueous solution or an aqueous dispersion of the flavor-retaining material, particularly the film-forming material, contained in the liquid flavor-releasing composition may be applied in advance to the low-adsorptive core particles. The preliminary application of the partial aqueous solution or aqueous dispersion of the film-forming material can suppress the temperature rise of the low-adsorbability core particles in the initial stage of production of the fragrance-carrying low-adsorbability particles, and can suppress the generation of fine powder from the low-adsorbability core particles.
In the flavor-carrying low-adsorptive particles of the present invention, a solid flavor-generating medium formed of a liquid flavor-releasing composition coats the surface of the low-adsorptive core particles. In this solid flavor-generating medium, the flavor is held by the flavor-holding material, and therefore, the flavor does not volatilize or is not adsorbed by carbon during normal storage. When the cigarette is contacted with a hydrophilic component such as water in mainstream smoke generated by smoking, part of the flavor retaining material dissolves to release the flavor, thereby enabling the flavor of the flavor to be tasted.
The cigarette filter according to the second aspect of the present invention includes a filter portion containing the low adsorptive particles having the flavorant of the present invention carried thereon. A filter-tipped cigarette according to a third aspect of the present invention provides a filter-tipped cigarette including a cigarette rod and the filter of the present invention connected to one end of the cigarette rod.
The cigarette filter of the present invention may comprise a filter part in which the low adsorptive flavor-carrying particles of the present invention are dispersed in a common filter material such as cellulose acetate tow (bonded by a plasticizer such as triacetin). A so-called charcoal filter unit (a filter unit including a filter material in which activated carbon is dispersed in cellulose acetate tow bonded with a plasticizer such as triacetin) may be connected to one end of the filter unit. Alternatively, the cigarette filter of the present invention may comprise a carbon filter part and a normal filter part which are separately arranged, and may contain the low adsorptive particles having the flavorant of the present invention filled in the space between the 2 filter parts.
Hereinafter, a cigarette having a filter according to the present invention will be described with reference to fig. 2 to 5. In fig. 2 to 5, the same elements are denoted by the same reference numerals.
Fig. 2 is a schematic cross-sectional view of a cigarette (filter cigarette) 50 provided with a filter for a cigarette according to an embodiment of the present invention. The filter-tipped cigarette 50 includes a cigarette rod 52 in which a tobacco filler 521 such as cut tobacco is wrapped with a cigarette wrapper 522. The cigarette rod 52 is the same as a conventional cigarette.
A filter 54 is attached to one end of the cigarette rod 52. The filter 54 includes a carbon filter 541 provided in direct contact with one end of the cigarette rod 52, a filter 542 containing the low adsorptive particles with flavorant on the downstream side of the carbon filter 541 with respect to the flow direction of mainstream smoke, and a normal filter 543 provided on the downstream side of the filter 542 containing the low adsorptive particles with flavorant on the downstream side with respect to the flow direction of mainstream smoke.
The carbon filter unit 541 is similar to a normal carbon filter in that, for example, cellulose acetate fibers 541a in which carbon particles 541b are dispersed are wound around filter-wrapping paper 541 c.
In the filter section 542 containing the flavor-supporting low-adsorptive particles, for example, cellulose acetate fibers 542a in which the flavor-supporting low-adsorptive particles FLAP of the present invention are dispersed are wrapped and wrapped with filter wrapping paper 542 b.
The normal filter section 543 is wound with a tow of, for example, cellulose acetate fibers 543a with filter-wrapping paper 543 b.
The filter 54 including the filter portions 541, 542, and 543 is attached to one end of the cigarette rod 52 with tipping paper 56.
Fig. 3 is a schematic cross-sectional view of a cigarette (filter cigarette) 60 provided with a filter for a cigarette according to another embodiment of the present invention. In the filter cigarette 60, the filter 62 attached to the cigarette rod 52 with the tipping paper 56 includes a charcoal filter 541 directly attached to one end of the cigarette rod 52 and a normal filter 622 provided at a distance from the charcoal filter 541, and the whole is wrapped with the filter wrapping paper 66. The normal filter portion 622 is composed of a tow of, for example, cellulose acetate fibers 622a, as in the normal filter portion 543 in fig. 2. A cavity (cavity)64 between the carbon filter 541 and the normal filter 622 is filled with the fragrance-carrying low adsorptive particle FLAP of the present invention.
Fig. 4 shows a filter-tipped cigarette having the structure of fig. 2, in which the carbon filter 541 is omitted, and a filter 542 containing low adsorptive particles carried with a flavorant is provided in direct contact with one end of the cigarette rod 52.
Fig. 5 shows a filter-tipped cigarette having the structure of fig. 3, in which a general filter unit 543 (see fig. 2) is used instead of the charcoal filter unit 541.
Examples
The present invention will be described below with reference to specific examples, but the present invention is not limited to these specific examples.
< preparation of liquid fragrance releasing composition >
A mixture containing the components shown in Table 1 below at the ratios shown in Table 1 was emulsified for 15 minutes at 7500rpm by an emulsifier (ROBOMICS MARK II manufactured by Primix Co.). At this time, the periphery of the emulsifier was cooled with water in such a manner that the temperature of the mixture did not exceed 45 ℃. Liquid fragrance-releasing compositions a to D were obtained as described above.
Coconard MT manufactured by Kao corporation was used as medium-chain triglyceride, LP-20E manufactured by Nisshin Oillio corporation was used as lecithin, and P-1570 manufactured by Mitsubishi chemical food was used as sugar ester.
[ Table 1]
< preparation of fragrance-supporting Low-adsorptive particles >
Example 1
Here, a conical ribbon mixer/dryer Ribocone RM-50-VD (see FIG. 1) manufactured by Dachuan original method was used. Calcium silicate particles (Sanwa Marume manufactured by Sanwa Islands Co., Ltd.; average particle diameter: 1mm, BET specific surface area less than 700 m)2/g)10kg and 6kg of a 5 wt% aqueous solution of pullulan were charged into the above mixing/drying machine, and steam at a temperature of 120 ℃ was circulated in a jacket under a pressure of 200kPa, the pressure in the mixing/drying machine was set to 12.3kPa, and the calcium silicate particles were stirred. After 5 minutes of stirring, 5kg of the flavor releasing composition a in a liquid state was sprayed from the nozzle into the mixer/dryer for 40 minutes, and then further stirred and dried for 20 minutes. The flavor-supported calcium silicate particles were taken out from the mixer/dryer, and rapidly put into a continuous flow granulation dryer (Mix grade0.5, manufactured by dakawa, inc.) to perform sensible heat exchange and dehumidification in the calcium silicate particles for 3 minutes, thereby obtaining a flavor-supported calcium silicate particle product.
Example 2
A calcium silicate-supported perfume particle product was obtained by the same procedure as in example 1, except that a liquid flavor releasing composition B was used instead of the liquid flavor releasing composition a.
Example 3
A calcium silicate-on-fragrance particulate product was obtained by the same procedure as in example 1, except that a liquid fragrance releasing composition C was used instead of the liquid fragrance releasing composition a.
Example 4
A calcium silicate-supported perfume particle product was obtained by the same procedure as in example 1, except that a liquid flavor releasing composition D was used instead of the liquid flavor releasing composition a.
Production of Filter cigarettes
A cigarette with a filter having the structure shown in fig. 3 was produced. Specifically, after removing cellulose acetate tow from a commercially available filter-equipped cigarette product "Winston Light" having a filter containing cellulose acetate tow as a filter material with tweezers, the cellulose acetate tow (length 12 mm; 8Y/29000 (i.e., 8 denier per filament; the section of a single fiber is Y-shaped; total fineness 29000 denier), 42mg (length of the axial cavity 64 of the cigarette rod 47mm) of the flavor-supporting calcium silicate particle product produced in examples 1 to 4, and finally, cellulose acetate tow (length 11 mm; 2.5Y/35000), a filter cigarette having the structure shown in fig. 3 was produced, and further, a control filter cigarette was produced in the same manner as described above except that none of the substances was filled in the cavity 64.
When the 4 kinds of the filter cigarettes of the present invention were smoked, it was confirmed that the flavor derived from the flavorant was released in the mainstream smoke and that the flavor was enhanced as compared with the control filter cigarette. These results show that according to the method of the present invention, a large amount of perfume can be loaded on the low-adsorptive core particles by a short treatment.
< measurement of amount of fragrance carried and fragrance-retaining Material >
The amount of the flavorant carried and the amount of the flavorant-holding material were measured for the flavorant-carrying particles obtained in examples 1 to 4.
The flavor-carrying particles of comparative examples were prepared according to examples 1 to 3 of the prior art document (WO2008/072627), and the amount of the flavor carried and the amount of the flavor-retaining material were measured in the same manner for the prepared flavor-carrying particles.
The flavor-supporting particles of the comparative examples were prepared as follows.
Comparative example 1 (example 1 of Prior Art document)
To a previously prepared aqueous amylopectin dispersion containing 10 wt% of amylopectin was added 2 wt% of coffee oil. The mixture was strongly stirred in an emulsifier (rotation speed of the emulsifier was 2500rpm), to prepare a perfume dispersion. On the other hand, 100g of calcium carbonate particles having an average particle size of 250 μm were placed in a fluidized granulation dryer, and hot air at 75 ℃ was blown at a flow rate of 0.6 m/sec to rapidly and intermittently spray the above-mentioned flavor dispersion (spraying was stopped for 30 minutes after spraying for 1 minute, and this cycle was repeated), and a total of 10g of the flavor dispersion was sprayed onto the surfaces of the calcium carbonate particles and dried. The fluidized bed was then rapidly cooled to room temperature to obtain the desired flavor beads.
Comparative example 2 (example 2 of Prior Art document)
100g of calcium carbonate particles having an average particle size of 250 μm were placed in a fluidized granulation dryer, and while blowing warm air at 30 ℃ at a flow rate of 1.0 m/sec, a flavor-mixed aqueous solution containing 1 wt% of a flavor for tobacco to which vanillin was added and 9 wt% of pullulan was continuously sprayed, and a total of 5g of the mixed aqueous solution was sprayed onto the surfaces of the calcium carbonate particles and dried. Then, 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 flavor beads.
Comparative example 3 (example 3 of Prior Art document)
To a previously prepared aqueous amylopectin dispersion containing 10 wt% of amylopectin, 1 wt% of coffee oil and 0.5 wt% of lecithin were added. The mixture was strongly stirred in an emulsifier (emulsifier rotation speed 7500rpm, 15 minutes) to prepare a perfume dispersion. On the other hand, 300g of ground coffee bean particles having an average particle size of 250 μm to 1.4mm were put into a rotary fluidizing granulation dryer (SFC-MINI, manufactured by Preund industries, Ltd.), a bottom rotary perforated plate was rotated at about 500rpm and a stirring paddle for preventing granulation was rotated at about 400rpm, and hot air at 75 ℃ was blown at a flow rate of 0.6 m/sec to form a fluidized bed of ground coffee bean particles. The flavor dispersion was continuously sprayed onto the fluidized bed while keeping the temperature of the flavor dispersion at 40 ℃ to thereby spray 90g in total of the flavor dispersion onto the surface of coffee bean particles, followed by drying. Then, the warm air temperature was rapidly lowered to room temperature, and cooled at a second rate of 0.4 m/sec, to obtain the desired flavor beads.
The amount of perfume and the amount of perfume-holding material were measured as follows.
Measurement of perfume:
the flavor carrying particles are extracted by shaking with a mixture of purified water and methanol. The extract was supplied to a gas chromatography mass spectrometer (GC/MS) and the aroma was measured.
Measurement of perfume holding Material:
the flavor-carrying particles were weighed (weight a), and dried by heating for the purpose of removing water in the particles (weight B after drying). Adding refined water into the dried particles, and performing oscillation extraction to dissolve out the perfume holding material. The extracted particles were further dried by heating (weight after drying C). The difference between weight C and weight a was taken as the amount of perfume holding material.
The measurement results are shown in fig. 6. Fig. 6 shows the amount of the perfume supported and the amount of the perfume holding material in the ratio (wt%) of the perfume supporting particle to the total weight. Fig. 6 shows that the flavor carrying particle of the present invention carries a larger amount of flavor than the flavor carrying particle of the comparative example.
Further, the flavor carrying particle of the present invention can be prepared by a shorter treatment time than the flavor carrying particles of the comparative examples.
< correlation between BET specific surface area of core particle and adsorption energy of fragrance-supporting particle >
Activated carbon (Kuraray Coal GGS-H28/70, manufactured by Kuraray Chemical Co., Ltd.; average particle diameter: 0.4 mm; BET specific surface area: 1700 m)2/g) flavor-releasing composition D in table 1 was used as a flavor-releasing composition instead of calcium silicate as the core particle, and flavor-supported activated carbon particles were produced in the same manner as the production method of flavor-supported calcium silicate particles in example 1.
Specifically, the flavor-supporting activated carbon particles were prepared as follows.
A conical ribbon mixer/dryer Ribocone RM-50-SR (see FIG. 7) manufactured by Dachuan original method was used. Activated carbon (Kuraray Coal GGS-H28/70, manufactured by Kuraray Chemical Co., Ltd.; average particle diameter: 0.4 mm; BET specific surface area: 1700 m)2/g)15kg and 6kg of a 5 wt% aqueous solution of amylopectin were charged into the above mixing/drying machine, and steam at a temperature of 120 ℃ was circulated in a jacket under a pressure of 200kPa, and the pressure in the mixing/drying machine was set to 12.3kPa, and the activated carbon was stirred. Stirring was carried out for 5 minutes, and 7.5kg of the flavor releasing composition D in a liquid state was sprayed from the nozzle into the mixer/dryer for 60 minutes, and then further stirredStirring and drying are carried out for 5 minutes. The flavor-supporting activated carbon particles were taken out from the mixer/dryer, and rapidly put into a continuous flow granulation dryer (Mix Grade0.5, manufactured by dakawa, inc.) to perform sensible heat exchange and dehumidification in the activated carbon particles for 3 minutes, thereby obtaining a flavor-supporting activated carbon particle product.
Using 30mg of the prepared flavor-supporting activated carbon particles, a cigarette with a filter having a structure shown in fig. 3 was prepared as follows. Specifically, after removing cellulose acetate tow as a filter material from a commercially available filter-equipped cigarette product "Winston Light" having a filter having cellulose acetate tow as a filter material, the cavity was filled with 30mg of the prepared flavor-supporting activated carbon particles (length 10 mm; 2.5Y/35000 (i.e., single fiber 2.5 denier; single fiber cross-section Y type; total fineness 35000 denier)), and finally, the cellulose acetate tow (length 10 mm; 2.5Y/35000) was filled to produce a filter-equipped cigarette having the structure shown in FIG. 3. A filter-tipped cigarette (hereinafter referred to as a control cigarette) was produced in the same manner as described above except that 30mg of an activated carbon (Kuraray Coal GGS-H28/70, manufactured by Kuraray Chemical Co.) having no flavorant was used as it is instead of the flavorant-carrying activated carbon particles.
The filter-tipped cigarettes produced were smoked, and the acetone adsorption energy in the mainstream smoke was examined.
In this experiment, the device 70 shown in fig. 7 was used in order to capture components in the mainstream smoke of a cigarette. The device 70 has a granular substance catcher 71, and the granular substance catcher 71 includes a cambridge filter 711 (diameter 47mm), a tobacco mainstream smoke inlet 71a and a tobacco mainstream smoke outlet 71b for holding cigarettes CIG. Further, the device 70 is provided with a sampler 72. The sampler 72 accommodates a chemical liquid TA for trapping gas phase components in tobacco mainstream smoke. In this experiment, 10mL of methanol containing 200ppm of anethole as an internal standard substance was placed as a drug solution TA. The sampler 72 is housed in a dewar 73 in which a refrigerant RM for keeping the trapping chemical solution TA at a low temperature is housed. In this experiment, a mixture of dry ice and isopropyl alcohol was used as the refrigerant RM, and the trapping chemical solution TA was kept at a temperature of-70 ℃ or lower in the experiment. The outlet 71b of the particulate matter trap 71 is connected to a conduit 74 extending into the chemical solution TA in the sampler 72. A duct 75 extending into a space above the chemical liquid TA in the sampler 71 is connected to the suction port 76a of the automatic smoking device 76. When the cigarette is lit and the automatic smoking device 76 is driven, the pressure in the sampler 72 is reduced by suction through the duct 75, and the mainstream tobacco smoke is caused to pass through the cambridge filter 711 in the catcher 71. At this time, particulate matter in the tobacco mainstream smoke is trapped by the cambridge filter 711, and the mainstream smoke from which the particulate matter has been removed is introduced into the trapping chemical TA in the sampler 72 via the duct 74, and is foamed to trap the gas phase component in the mainstream smoke in the trapping chemical TA.
In this experiment, cigarettes were attached to the catcher 71, and smoking was performed by the automatic smoking device 76 under ISO standard smoking conditions (1 puff: 35mL for 2 seconds, puff interval: 58 seconds). After completion of smoking, the liquid medicine in the sampler 72 was transferred to a serum bottle, and a cambridge filter 711 in which particulate matter was trapped was put therein, and extracted for 30 minutes by shaking 250 times/minute. This extract (1 mL) was put into a glass bottle for GC/MS analysis, and the components in the mainstream smoke were analyzed under the following conditions.
Conditions for analysis of constituents in mainstream smoke:
GC/MS: HP7890/5975 manufactured by Hewlett-Packard
Column: DB-1701
Column flow rate: 1.2 mL/min
Temperature rise conditions: after holding at 60 ℃ for 5 minutes, the temperature was raised to 160 ℃ at 5 ℃/minute, to 250 ℃ at 10 ℃/minute, and held for 30 minutes.
Injection: the split ratio is 10: 1; an injection port is 220 ℃; the flow rate is 12 mL/min; total flow 16.2 mL/min
MS conditions: scanning parameters are 33.0-200.0; a threshold value of 50; an MS ion source of 230 ℃; MS quadrupole 150 ℃.
The same analysis was carried out for a cigarette with a normal filter (a cigarette rod having a commercially available filter-tipped cigarette product "Winston Light" and having a normal filter made of cellulose acetate tow (length 20 mm; 2.5Y/70000) attached to one end thereof; hereinafter referred to as a reference cigarette) and the above-mentioned control cigarette.
Acetone peak area values were calculated from the analysis results of the filter-tipped cigarette containing the flavor-supporting activated carbon particles, the control cigarette and the standard cigarette, respectively, the acetone peak area values of the filter-tipped cigarette containing the flavor-supporting activated carbon particles and the control cigarette were divided by the acetone peak area value of the standard cigarette, respectively, and the acetone peak area values were multiplied by 100 times to obtain an acetone reduction rate (%), and the acetone reduction rate (%) was subtracted from 100% to calculate the acetone adsorption rate.
As a result, the acetone adsorption rate of the control cigarette was 48%, and the acetone adsorption rate of the filter-tipped cigarette containing the flavor-supporting activated carbon particles was 45%. The results show that: using a nozzle having a diameter of 1700m2When the flavor-supporting activated carbon particles are produced using activated carbon having a BET specific surface area of/g as core particles, the flavor-supporting activated carbon particles retain an adsorption energy of about 94% of the intrinsic adsorption energy of the core particles.
Using a specific surface area of 700m2G and 1000m2Active carbon (30 mg)/g replacement of specific surface area 1700m22 cigarettes with filters similar to the control cigarette were produced except for the activated carbon (30 mg)/g. In these cigarettes, the acetone adsorption rate was examined in the same manner as described above, and the former cigarette was 23%, and the latter cigarette was 34%.
From the above results, it is understood that the specific surface area is 700m2The core particles having a specific surface area of less than 700m exhibit a high adsorption energy to components in the mainstream smoke of a cigarette2The/g core particles exhibit low adsorption energy relative to the constituents in the mainstream smoke of a cigarette.
Claims (5)
1. A method for producing a fragrance-carrying low-adsorption particle, comprising: under reduced pressure of 12.3kPa or lower at 60 ℃ or lower, has a thickness of less than 700m2(ii) spraying a liquid flavor-releasing composition containing a flavor and dextran onto the low-adsorption core particles having a BET specific surface area of,/g, while stirring.
2. The method for producing a flavor-supporting low-adsorbent particle according to claim 1, wherein the liquid flavor releasing composition contains the glucan in an amount of 5 to 20% by weight of the total weight of the flavor-supporting low-adsorbent particle, and the flavor in an amount of 10 to 50% by weight of the glucan.
3. The method for producing the flavor-supporting low-adsorptive particles according to claim 1 or 2, wherein the reduced-pressure condition is a pressure of 7.4 to 12.3 kPa.
4. The method for producing flavor-supporting low-adsorption particles according to claim 1 or 2, wherein the low-adsorption core particles are kept at a temperature of 40 to 60 ℃ in the spraying.
5. The method for producing flavor-carrying low-adsorptive particles according to claim 3, wherein the low-adsorptive core particles are kept at a temperature of 40 to 60 ℃ in the spraying.
Applications Claiming Priority (3)
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| JP2011-157216 | 2011-07-15 | ||
| JP2011157216 | 2011-07-15 | ||
| CN201280035198.6A CN103649287A (en) | 2011-07-15 | 2012-07-11 | Fragrance-supporting low-adsorption particles, cigarette filter, filter cigarette, and method for manufacturing fragrance-supporting low-adsorption particles |
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| CN201280035198.6A Division CN103649287A (en) | 2011-07-15 | 2012-07-11 | Fragrance-supporting low-adsorption particles, cigarette filter, filter cigarette, and method for manufacturing fragrance-supporting low-adsorption particles |
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| CN201710059867.8A Expired - Fee Related CN107034015B (en) | 2011-07-15 | 2012-07-11 | Method for producing perfume-carrying low-adsorption particles |
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| EP (1) | EP2733193B1 (en) |
| JP (1) | JP5719932B2 (en) |
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| JP6521239B2 (en) * | 2015-04-28 | 2019-05-29 | 戸田工業株式会社 | Hydrophobic magnetic iron oxide particle powder and method for producing the same |
| CN104946394B (en) * | 2015-07-17 | 2018-08-24 | 云南中烟工业有限责任公司 | A kind of preparation facilities of embedded non-burning flavoring material |
| CN107802024B (en) * | 2017-10-25 | 2020-04-28 | 江苏中烟工业有限责任公司 | Preparation method of adsorbent-containing core material for low-temperature cigarettes |
| CN107853751A (en) * | 2017-12-06 | 2018-03-30 | 南通烟滤嘴有限责任公司 | Position cooling and dehumidifying device is molded in filter-stick forming device |
| RU2761271C1 (en) * | 2018-10-18 | 2021-12-06 | Джапан Тобакко Инк. | Smoking product, method for manufacturing the specified smoking product and method for recognizing granular activated carbon |
| CN109938402B (en) * | 2019-03-22 | 2021-12-21 | 内蒙古昆明卷烟有限责任公司 | Aerosol generator |
| US20210100741A1 (en) * | 2019-10-04 | 2021-04-08 | Pure Laboratories, Llc | Flavored bioactive extracts and methods of flavor introduction |
| EP4115747A4 (en) * | 2020-03-04 | 2024-01-17 | Japan Tobacco Inc. | Fragrance-carrying constituent member of tobacco product, tobacco product, and method for producing same |
| CN115702693B (en) * | 2021-08-16 | 2024-04-12 | 湖北中烟工业有限责任公司 | Sweet cigarette containing slow-release and controlled-release sweet essence filter tip and double-barrier transfer paper and preparation method thereof |
| CN113841922B (en) * | 2021-10-09 | 2023-03-10 | 湖北中烟工业有限责任公司 | Preparation method and application of compound-flavor essence spice for cigarettes |
| WO2023187223A1 (en) * | 2022-04-01 | 2023-10-05 | Amplicon Ab | Nicotine formulations |
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| JP2006248832A (en) * | 2005-03-10 | 2006-09-21 | Taiyo Kagaku Co Ltd | Substance-supporting porous silica |
| WO2008072627A1 (en) * | 2006-12-13 | 2008-06-19 | Japan Tobacco Inc. | Perfumed beads and filter for cigarette |
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| JP5719932B2 (en) | 2015-05-20 |
| ES2666365T3 (en) | 2018-05-04 |
| EP2733193A4 (en) | 2015-06-03 |
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| EP2733193A1 (en) | 2014-05-21 |
| EP2733193B1 (en) | 2018-04-11 |
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| RU2570785C2 (en) | 2015-12-10 |
| KR20160035098A (en) | 2016-03-30 |
| TWI481705B (en) | 2015-04-21 |
| KR101874151B1 (en) | 2018-07-03 |
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