WO2012118033A1 - 喫煙物品用香料含有シートの製造方法、該方法により製造される喫煙物品用香料含有シート、およびそれを含む喫煙物品 - Google Patents
喫煙物品用香料含有シートの製造方法、該方法により製造される喫煙物品用香料含有シート、およびそれを含む喫煙物品 Download PDFInfo
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- WO2012118033A1 WO2012118033A1 PCT/JP2012/054827 JP2012054827W WO2012118033A1 WO 2012118033 A1 WO2012118033 A1 WO 2012118033A1 JP 2012054827 W JP2012054827 W JP 2012054827W WO 2012118033 A1 WO2012118033 A1 WO 2012118033A1
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/14—Forming reconstituted tobacco products, e.g. wrapper materials, sheets, imitation leaves, rods, cakes; Forms of such products
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
- A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/10—Chemical features of tobacco products or tobacco substitutes
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/10—Chemical features of tobacco products or tobacco substitutes
- A24B15/12—Chemical features of tobacco products or tobacco substitutes of reconstituted tobacco
- A24B15/14—Chemical features of tobacco products or tobacco substitutes of reconstituted tobacco made of tobacco and a binding agent not derived from tobacco
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
- A24B15/281—Treatment of tobacco products or tobacco substitutes by chemical substances the action of the chemical substances being delayed
- A24B15/282—Treatment of tobacco products or tobacco substitutes by chemical substances the action of the chemical substances being delayed by indirect addition of the chemical substances, e.g. in the wrapper, in the case
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
- A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
- A24B15/301—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances by aromatic compounds
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
- A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
- A24B15/302—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances by natural substances obtained from animals or plants
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
- A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
- A24B15/302—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances by natural substances obtained from animals or plants
- A24B15/303—Plant extracts other than tobacco
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
- A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
- A24B15/34—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances containing a carbocyclic ring other than a six-membered aromatic ring
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/12—Steaming, curing, or flavouring tobacco
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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
- A24D1/00—Cigars; Cigarettes
- A24D1/002—Cigars; Cigarettes with additives, e.g. for flavouring
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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
- A24D1/00—Cigars; Cigarettes
- A24D1/02—Cigars; Cigarettes with special covers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
- B05D3/0254—After-treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/04—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases
- B05D3/0406—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases the gas being air
- B05D3/0426—Cooling with air
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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
Definitions
- the present invention relates to a method for producing a sheet containing a fragrance and used for a smoking article, a fragrance-containing sheet for a smoking article produced by the method, and a smoking article including the same.
- Patent document 1 and patent document 2 suppress the volatilization / dissipation of a fragrance component by disposing the fragrance component with a natural polysaccharide on the filter part of a cigarette, and release the fragrance by pressing and destroying it during smoking.
- Patent Document 3 discloses that a cigarette filter part is coated with a flavor component with a water-soluble matrix such as dextrin to suppress volatilization / dissipation of the flavor component, and a water-soluble matrix is formed by moisture in mainstream smoke during smoking. Dissolving and releasing perfume is disclosed.
- the fragrance component when the fragrance component is arranged in the filter part which is a non-burning part of the cigarette, it is necessary to operate the filter part during smoking, or the fragrance is dissolved by dissolving the water-soluble matrix with moisture in the mainstream smoke. In order to release, there is a time lag before tasting the flavor.
- Patent Documents 4 to 6 are reported as examples in which a fragrance component is arranged on a cigarette chopping which is a burning part or a wrapping paper which encloses it.
- Patent Document 4 discloses that a fragrance material in which a flavor component is incorporated into a three-dimensional network structure of glucan molecules is applied to a wrapping paper that encloses a tobacco filler. Since the cigarette of patent document 4 takes in a flavor component in the inside of the three-dimensional network structure of a glucan molecule, and fixes and hold
- Patent Document 5 a liquid perfume and a carrageenan sol are mixed and dropped into an ionic solution (a solution containing potassium ions) to prepare a granular gel, which is dried in the air, thereby being stable and stable up to 180 ° C.
- ionic solution a solution containing potassium ions
- the preparation of "aromatized fragrance material" is disclosed.
- a metal ion gelation accelerator
- Patent Document 6 a slurry containing a fragrance component such as menthol and a polysaccharide is dried to prepare a sheet containing the fragrance component coated with a polysaccharide gel, and this is cut into tobacco. It is reported that it is added in increments. In this report, it takes 1 week at 40 ° C. to dry the slurry.
- a fragrance component such as menthol and a polysaccharide
- the present invention is a fragrance-containing sheet having a high fragrance content and a high fragrance preparation yield, and is capable of producing a fragrance-containing sheet for smoking articles having a high storage perfume property when blended in a smoking article in a short time. It is an object of the present invention to provide a possible method, and to provide a fragrance-containing sheet for smoking articles that has high storage aroma when blended in a smoking article and can be manufactured in a short time.
- the content of a fragrance containing at least one of carrageenan and gellan gum, a fragrance, an emulsifier, and 70 to 95% by weight of water and based on the polysaccharide is provided.
- a method for producing a fragrance-containing sheet for smoking articles comprising a step and a heat drying step including heating the gelled raw material and drying at a sample temperature of 70 to 100 ° C.
- the emulsifier is 0.5 to 5% by weight of lecithin with respect to the polysaccharide.
- the emulsifier is an ester selected from the group consisting of glycerin fatty acid ester, polyglycerin fatty acid ester, sorbitan fatty acid ester, propylene glycol fatty acid ester and sucrose fatty acid ester.
- the polysaccharide is contained in the raw material slurry at a concentration of 2 to 5% by weight.
- the fragrance is menthol.
- the content of the menthol is in the range of 250 to 500% by weight with respect to the polysaccharide.
- a fragrance-containing sheet for smoking articles characterized by being produced by the above method.
- a smoking article containing tobacco cuts wherein the tobacco cuts are blended with a cut article of the fragrance-containing sheet for smoking articles.
- the fragrance for smoking articles has a high fragrance content, a high fragrance preparation yield, and a high storage perfume property when blended in a smoking article. It is possible to produce the containing sheet in a short time. Moreover, the fragrance
- seat for smoking articles of this invention has high storage incense retention property when mix
- seat (example of this invention).
- concentrations The graph which shows the menthol content after storage of the menthol containing sheet
- seat (when a polysaccharide is a carrageenan).
- seat (when a polysaccharide is gellan gum).
- seat (when a polysaccharide is gellan gum).
- seat (when a polysaccharide is carrageenan).
- seat (when a polysaccharide is gellan gum).
- any fragrance can be used as long as it is a fragrance used for smoking articles.
- Main flavors include menthol, leaf tobacco extract, natural plant flavors (e.g. cinnamon, sage, herbs, chamomile, kuzukusa, sweet tea, clove, lavender, cardamom, clove, nutmeg, bergamot, geranium, honey essence, rose Oil, lemon, orange, cinnamon, caraway, jasmine, ginger, coriander, vanilla extract, spearmint, peppermint, cassia, coffee, celery, cascarilla, sandalwood, cocoa, ylang ylang, fennel, anise, licorice, st john's bread , Plum extract, peach extract, etc.), saccharides (e.g., glucose, fructose, isomerized sugar, caramel, etc.), cocoa (powder, extract, etc.), esters (e.g., isoamyl acetate,
- a menthol-containing sheet for smoking articles is: A polysaccharide containing at least one of carrageenan and gellan gum, menthol, emulsifier, and 70 to 95% by weight of water, the content of menthol based on the polysaccharide is in the range of 100 to 1000% by weight, and is in a sol state Extending the raw material slurry at 60 to 90 ° C. on the substrate, A step of cooling the stretched raw material slurry to a sample temperature of 0 to 40 ° C. to cause gelation, and a heat drying step including heating the gelled raw material and drying at a sample temperature of 70 to 100 ° C. Manufactured by the method.
- sample temperature means the temperature of the surface of the sample (ie, slurry or sheet).
- the raw material slurry comprises (i) a step of preparing a polysaccharide aqueous solution by mixing and heating a polysaccharide containing at least one of carrageenan and gellan gum, and (ii) It can be prepared by a method including a step of adding and kneading and emulsifying menthol and an emulsifier to such an aqueous solution.
- the step (i) can be performed by adding a small amount of polysaccharide to water and dissolving it with stirring.
- the heating temperature here can be 60 to 90 ° C., preferably 75 to 85 ° C.
- the step (ii) can be performed by a known emulsification technique using a homogenizer because the raw material slurry has a viscosity that does not hinder the emulsification of about 10,000 mPas (sol state) at the heating temperature.
- the polysaccharide is preferably contained in the raw material slurry at a concentration of 2 to 5% by weight.
- the raw slurry can contain 200-500 grams of polysaccharide. More preferably, the polysaccharide is contained in the raw slurry at a concentration of 3 to 5% by weight (see Example 10 described later).
- the formulation of the raw material slurry can be, for example, 50 to 500 ml of 500 grams of polysaccharide, 500 to 5000 grams of menthol, and 5% by weight of an emulsifier solution with respect to 10 liters of water.
- the water content of the raw slurry is 70 to 95% by weight, preferably 80 to 90% by weight.
- the ratio (weight ratio) between the polysaccharide and menthol in the raw material slurry can be 1: 1 to 1:10, preferably 1: 2.5 to 1: 5. That is, the blending amount of menthol can be 100 to 1000% by weight based on the polysaccharide, and preferably 250 to 500% by weight based on the polysaccharide (see Example 11 described later).
- the polysaccharide in the raw slurry only needs to contain one of carrageenan and gellan gum, but may contain both.
- the polysaccharide may be composed only of carrageenan and / or gellan gum, or may contain other polysaccharides such as tamarind gum in addition to carrageenan and / or gellan gum.
- other polysaccharides are contained in the slurry at a blending amount of carrageenan and gellan gum or less.
- the carrageenan ⁇ -carrageenan can be used as the carrageenan.
- the polysaccharide has a property of gelling upon cooling once after heating, and fixing and coating menthol micelles.
- carrageenan and gellan gum it has been found in the present invention that these aqueous solutions exhibit particularly good sol-gel transition properties in response to temperature (see Examples 4 and 9 below). That is, the carrageenan aqueous solution and the gellan gum aqueous solution have a characteristic that once cooled and gelled, the gel is not easily returned to the sol even if the temperature is raised, and the gel state can be maintained (see FIGS. 2B and 7B). reference).
- menthol coated with carrageenan or gellan gum can be kept stable even if it is cooled and then exposed to high temperatures in the heat drying process, and the menthol in the film is stable. Yes (see FIGS. 7D and 7F). Such characteristics are referred to as “temperature-responsive sol-gel transition characteristics” in the present invention.
- the temperature-responsive sol-polysaccharide having the gel transition property has an advantage that it can be coated with menthol to achieve a high storage fragrance, and the temperature-responsive sol- If the gel transition property is used, there is an advantage that it is not necessary to add a metal ion (gelation accelerator).
- l-menthol can be used as the menthol.
- a naturally-derived emulsifier such as lecithin, specifically, sun lecithin A-1 (Taiyo Chemical Co., Ltd.) can be used.
- lecithin when lecithin is used as an emulsifier, lecithin can be contained in the slurry in an amount of 0.5 to 5% by weight based on the polysaccharide.
- carrageenan is used as the polysaccharide
- the amount of lecithin added is preferably 0.5 to 2% by weight based on the polysaccharide.
- gellan gum is used as the polysaccharide
- the amount of lecithin added is preferably 0.5 to 5% by weight, more preferably 0.5 to 2% by weight based on the polysaccharide (see Example 12 described later). reference).
- an ester selected from the group consisting of glycerin fatty acid ester, polyglycerin fatty acid ester, sorbitan fatty acid ester, propylene glycol fatty acid ester and sucrose fatty acid ester can be used.
- Glycerin fatty acid esters include, for example, fatty acid monoglycerides such as monostearic monoglyceride and succinic monoglyceride; polyglycerin fatty acid esters include, for example, pentaglyceryl monostearate; sorbitan fatty acid esters include, for example, sorbitan monostearate; Glycol fatty acid esters include, for example, propylene glycol monostearate; sucrose fatty acid esters include, for example, sucrose stearate (see Example 13 below). These emulsifiers can also be contained in the slurry in an amount of 0.5 to 5% by weight based on the polysaccharide.
- the extension of the raw material slurry can be performed by extruding the raw material slurry onto the base material using a casting gate or through a slit die.
- the substrate any substrate from which the menthol-containing sheet produced by dry molding can be peeled can be used.
- PET polyethylene terephthalate
- the raw material slurry can be extended, for example, so that the thickness at the time of drying is about 0.1 mm, which is the same thickness as a normal tobacco cut.
- the expanded raw material slurry is sufficiently gelled (40 ° C. or lower) before drying, and generally the emulsion is frozen. Then, it is once cooled to a temperature at which it is not destroyed (0 ° C. or higher), that is, 0 to 40 ° C., preferably 0 to 30 ° C., more preferably 15 to 25 ° C.
- the raw material slurry before cooling has a temperature of 60 to 90 ° C., preferably 75 to 85 ° C., and is in a sol state.
- Such pre-cooling can be performed by applying cold air (eg, 10 ° C.) generated by a simple air blow or a spot cooler (eg, SWIDEN SS-25DD-1) to the extended raw material slurry for 2 to 3 minutes.
- cold air eg, 10 ° C.
- a spot cooler eg, SWIDEN SS-25DD-1
- the extended raw material slurry is brought into contact with a tube through which a refrigerant (for example, 10 ° C.) generated by a cold / hot water generator (chiller, for example, Apiste PCU-1600R) passes for 1-2 minutes. It may be done by.
- the preliminary cooling may be performed by leaving the extended raw material slurry at room temperature.
- the raw material slurry is extended on the base material and once cooled, it has an advantage that the extended raw material slurry is not easily deformed even if it is exposed to a high temperature in the subsequent drying step.
- Example 6 The effect of such cooling on the scent retention of fragrance-containing sheets (eg, menthol-containing sheets) is demonstrated in Example 6 (FIG. 4B) described below, and lower cooling temperatures may lead to higher menthol content. This is demonstrated in Example 7 (FIG. 5) described later.
- the heated and dried raw material slurry can be dried by any heating and drying means such as hot air drying and infrared heat drying.
- heating and drying means such as hot air drying and infrared heat drying.
- drying of the raw slurry is also simply referred to as “drying”.
- the drying of the raw material slurry includes heating the cooled raw material slurry and drying it at a sample temperature of 70 to 100 ° C., and the sample temperature is preferably 100 ° C. or less over the entire drying time.
- sample temperature means the temperature of the surface of the sample (ie, slurry or sheet).
- total drying time refers to a period during which heating is performed in the heat dryer. The total drying time is generally 20 minutes or less, preferably 7 to 20 minutes, more preferably 10 to 18 minutes.
- the sample temperature may be less than 70 ° C. during the drying step, but in order to shorten the drying time, it is preferable that the period during which the sample temperature is less than 70 ° C. is short.
- the raw material slurry can be dried by drying the cooled raw material slurry at a sample temperature of 70 to 100 ° C. over a period of 1/2 or more of the total drying time. The sample temperature is below 100 ° C. over the entire drying time. More preferably, the raw material slurry can be dried by drying the cooled raw material slurry at a sample temperature of 70 to 100 ° C. over the entire drying time.
- Total drying time when expressed as “at a sample temperature of 70-100 ° C. over time” means the total drying time excluding the opening period when the sample temperature is rising to the desired sample temperature. For example, in Example 5 (FIGS. 3A to 3G) described later, since the sample temperature is rising to the desired sample temperature for a period of about 1 minute from the start of heat drying, this initial period is “total drying time”. Are excluded from “total drying time” when expressed as “at a sample temperature of 70-100 ° C.”.
- the raw slurry can be dried by drying the raw slurry to a sheet form having a moisture content of less than 10% with a total drying time of 20 minutes or less.
- Example 5 it is demonstrated in Example 5 (FIGS. 3D to 3G) described later that when the raw material slurry is dried at the above-described sample temperature, the sheet obtained by drying can achieve high storage aroma retention.
- hot air drying in order to maintain a sample temperature of 70 to 100 ° C., drying with hot air having a temperature of 100 ° C. or higher is preferably performed at the initial drying of the raw slurry, and then the same as the initial hot air temperature.
- the slurry is dried at a temperature or lower than the initial hot air temperature (preferably 70 ° C. or more and less than 100 ° C.).
- a drying operation for example, high-temperature drying with hot air of 100 ° C. or higher
- a drying operation is included in the subsequent drying step so that the prepared raw slurry is once cooled so that the sample temperature becomes 70 to 100 ° C.
- the produced menthol-containing sheet has a high menthol content, a high menthol preparation yield, and can maintain the menthol content at a high value even after storage.
- the hot air temperature may be constant throughout the drying process, or may be changed during the drying process.
- the raw material slurry is preferably dried by initial drying at a high temperature with hot air of 100 ° C. or higher and subsequent drying at a low temperature with hot air of less than 100 ° C.
- “initial drying” means initial drying in a drying process using hot air having a high temperature of 100 ° C. or higher
- “late drying” means initial drying using low-temperature hot air of less than 100 ° C.
- the drying of the raw slurry is Initial drying over a quarter of the total drying time at a hot air temperature of 100 ° C. or higher, then Performed by late drying at a hot air temperature of less than 100 ° C. over a quarter of the total drying time, and the raw slurry is in the form of a sheet having a moisture content of less than 10% with a total drying time of 20 minutes or less This can be done by drying.
- the menthol-containing sheet of the present invention has a high menthol content after production and can maintain the menthol content at a high value even after storage (sample of Example 1 described later) No. 4, see sample number 5 in example 2 and sample number 6 in example 3).
- the initial drying can be performed at a hot air temperature of, for example, 100 ° C. or higher and 130 ° C. or lower for 4 to 6 minutes
- the late drying is performed at a hot air temperature of, for example, 70 ° C. or higher and lower than 100 ° C. It can be performed for 4 to 6 minutes.
- the amount of hot air can be set to 3 to 20 m / second, for example.
- the total drying time is generally 20 minutes or less, preferably 7 to 20 minutes, more preferably 10 to 18 minutes.
- initial drying is performed at a hot air temperature of 100 ° C. or higher and 130 ° C. or lower until moisture on the surface of the raw material slurry evaporates and a sufficient film is formed on the surface of the slurry, and then hot air of 70 ° C. or higher and lower than 100 ° C. is quickly obtained.
- Late drying can be performed by switching to temperature.
- the hot air temperature during the initial drying may be constant, or may be changed so as to decrease sequentially between 100 ° C. and 130 ° C.
- the hot air temperature during late drying may be constant, or may be changed so as to decrease sequentially between 70 ° C. and less than 100 ° C.
- the hot air dryer used in the examples described later has three drying chambers, and the sample is conveyed by the belt conveyor in the order of the first chamber ⁇ the second chamber ⁇ the third chamber.
- the chamber may be used for initial drying (above 100 ° C.) at the same or different temperatures
- the third chamber may be used for late drying (below 100 ° C.)
- the first chamber may be used for initial drying (100 ° C.
- the second and third chambers may be used for late drying (less than 100 ° C.) at the same or different temperatures.
- the drying is a state in which the menthol-containing sheet is sufficiently dried, the menthol-containing sheet can be easily peeled from the substrate, and the menthol-containing sheet can be engraved in a subsequent engraving step. Do until it becomes. Specifically, drying is performed until the water content of the menthol-containing sheet is less than 10% by weight, preferably 3 to 9% by weight, more preferably 3 to 6% by weight (see Example 8 described later).
- the water content here refers to a value measured by the measurement method described in the examples described later.
- the menthol content (immediately after preparation) of the menthol-containing sheet of the present invention is preferably 45% by weight or more, more preferably 55 to 75% by weight.
- the menthol content after storage (50 ° C., 30 days) of the menthol-containing sheet of the present invention is preferably 45% by weight or more, more preferably 48 to 63% by weight.
- the menthol content refers to a value measured by the measurement method described in Examples described later.
- the menthol-containing sheet of the present invention can be blended in a tobacco cut of a smoking article, for example, by cutting into a size equivalent to a normal tobacco cut.
- the cut menthol-containing sheet can be blended in an amount of 2 to 10 g per 100 g of tobacco cut.
- the cut menthol-containing sheet is preferably blended in the tobacco cut.
- the menthol-containing sheet of the present invention can be blended in any smoking article, for example, a burning smoking article in which tobacco leaves are burned to taste the flavor of tobacco, especially cigarette cigarettes.
- the menthol-containing sheet of the present invention can be blended into cigarette cuts of cigarettes comprising a tobacco rod comprising a cigarette cut and a cigarette wrap around the cigarette cut.
- Example 1 (1) Preparation of raw slurry (10 liter scale) 10 liters of water Gellan Gum (Gelcogel / Saneigen FFI) 150 grams Tamarind Gum (Bistop D-2032 / Saneigen FFI) 150 grams Lecithin (Sun Lecithin A-1 / Taiyo Chemical Co., Ltd.) 120ml (5% aqueous solution) Menthol (Takasago Fragrance Industry Co., Ltd.) 1500 g Water (10 L) is kept at 80 ° C and stirred with a mixer (PRIMIX TK AUTO MIXER Model 40 / solution stirring rotor installed / 2000 rpm) while gellan gum (150 g) and Tamarind gum (150 g) was dissolved little by little so as not to become lumpy (required time about 20 minutes), and menthol (1500 g) was added.
- Gellan Gum Gellan Gum
- Tamarind Gum Bastop D-2032 / Saneigen FFI
- Hot-air dryer Hot-air dryer with the following configuration Drying section: 3 rooms (each zone length 2.5 m, total length 7.5 m) Hot air flow rate and type: 1st chamber: punching plate, air flow 5 m / sec: 2nd chamber: punching plate, air flow 10 m / sec: 3rd chamber: floating jet, 20 m / sec air flow 1st chamber 2nd chamber
- the hot air was applied to the menthol-containing sheet conveyed on the belt through a punched plate having a hole functioning as a flow control plate.
- hot air was blown from above and below to the menthol-containing sheet that was floated and conveyed together with the base film.
- the menthol-containing sheets of Sample Nos. 1 to 4 were prepared by changing the hot air drying conditions as described in Table 1 below.
- the temperature described is the hot air temperature.
- the drying time was set so that the menthol-containing sheet was sufficiently dried and could be easily peeled off from the base film, and the menthol-containing sheet could be engraved in a subsequent engraving step.
- the moisture content of the menthol-containing sheet obtained in this example was about 3%.
- the measurement solution was subjected to the following GC-TCD and quantified by a calibration curve method.
- the measurement solution was subjected to the following GC-FID and quantified by a calibration curve method.
- the menthol content (mg) of the prepared menthol-containing sheet and the menthol content (mg) of the menthol-containing sheet stored in an accelerated environment were respectively measured.
- Table 1 shows “initial menthol content (%)” and “ It is shown as “menthol content (%) after storage”.
- a menthol-containing sheet (1 ⁇ 10 mm cut, about 5 mm) was placed in an open container and stored in a thermostat set at 50 ° C. (Yamato Science Co., Ltd. “Drying” Oven “DX600) for a maximum of 30 days.
- the menthol aroma retention rate was calculated by the following formula, and the aroma retention function of the menthol-containing sheet was evaluated.
- Menthol perfume retention rate (%) ⁇ (menthol content after storage) / (initial menthol content) ⁇ ⁇ 100 (5)
- the menthol-containing sheets of sample numbers 1 to 4 were prepared using the hot air drying machine described above using the hot air drying conditions described in Table 1.
- the moisture content and initial menthol content of the menthol-containing sheet were measured according to the above-described method, and the results are shown in Table 1.
- the menthol content after storage for 30 days is shown in Table 1
- the menthol content after storage for 7 days, 14 days, and 30 days is shown in FIG.
- reference numerals 1 to 7 represent sample numbers 1 to 7, respectively.
- Sample number 1 When the raw slurry is stretched and dried into a sheet by using the hot-air drying molding machine described above, it starts drying at a low hot air temperature (about 70 ° C) in order to prevent the formation of a surface film in the first half of drying, and is completely completed in the second half of drying. In order to aim at drying, the technique of drying at high hot air temperature (about 120 degreeC) is often taken. Following this method, a menthol-containing sheet of sample number 1 was prepared, and a fully dried sample (water content 3.1%) could be prepared with a total drying time of 12 minutes.
- the “initial menthol content” after preparation of the sheet was sufficiently high at 81.5%, but the “post-storage menthol content” after storage in the accelerated environment (20 days) was as low as 13.6%.
- the sheet of 1 had a problem with the storage aroma.
- Sample number 2 In Sample No. 2, a high drying temperature was adopted in order to make the drying time shorter than Sample No. 1. For this reason, in Sample No. 2, a fully dried sample (water content 3.2%) could be prepared with a total drying time of 6 minutes.
- the “initial menthol content” after preparation of the sheet was sufficiently high at 62.4%, but the “post-storage menthol content” after storage in the accelerated environment (30 days) was as low as 29.2%.
- the sheet of 2 had a problem with the storage aroma.
- sample number 3 In sample number 3, the hot air temperature was set to 70 ° C. throughout the drying process. Therefore, in sample No. 3, a fully dried sample (water content 3.1%) could be prepared with a total drying time of 60 minutes.
- the “initial menthol content” after preparation of the sheet is sufficiently high at 75.8%
- the “menthol content after storage” after storage in the accelerated environment (30 days) is also high at 59.2%. Both the fragrance retention property and the storage fragrance property were good. However, the time required for drying was as long as 60 minutes.
- Sample number 4 In Sample No. 4, contrary to Sample Nos. 1 and 2, which were shifted from low temperature drying to high temperature drying, initial drying (first chamber and second chamber) was performed with hot air of high temperature (120 ° C.), and later drying (first drying) (3 rooms) was performed with hot air at a low temperature (70 ° C.). In sample No. 4, the total drying time was as short as 7.5 minutes, but a sufficiently dried sample (water content 3.4%) could be prepared. In addition, the “initial menthol content” after preparation of the sheet is sufficiently high at 75.7%, and the “menthol content after storage” after storage in the accelerated environment (30 days) is also high at 62.4%. Both the fragrance retention property and the storage fragrance property were good. As described above, when initial drying at a high temperature and late drying at a low temperature were employed, a sheet having excellent fragrance retention could be prepared in a relatively short drying time.
- Example 2 A menthol-containing sheet of sample number 5 was prepared in the same manner as in Example 1 except that the slurry was dried under the hot air drying conditions described in Table 2 below, and the water content and menthol content were measured. The results are shown in Table 2.
- sample number 5 the amount of hot air was increased as compared to sample numbers 1 to 4.
- the hot air was blown from above and below to the menthol-containing sheet conveyed in a floating state.
- the second chamber and the third chamber hot air was applied to the menthol-containing sheet conveyed on the belt by ventilation.
- sample No. 5 initial drying (first chamber) was performed with hot air of high temperature (120 ° C.) for 4 minutes, and late drying (second chamber and third chamber) was performed with hot air of low temperature (70 ° C.) for 8 minutes.
- a fully dried sample (water content 3.1%) could be prepared with a total drying time of 12 minutes.
- the “initial menthol content” after preparation of the sheet is sufficiently high at 72.7%
- the “menthol content after storage” after storage in the accelerated environment (30 days) is also high at 58.5%. Both the fragrance retention property and the storage fragrance property were good.
- a sheet having excellent fragrance retention could be prepared in a relatively short drying time.
- Example 3 The menthols of sample numbers 6 and 7 were prepared in the same manner as in Example 1 except that the slurry was dried under the hot air drying conditions described in Table 3 below using a hot air dryer having four drying compartments. A containing sheet was prepared and the water content and menthol content were measured. The results are shown in Table 3.
- menthol-containing sheets were prepared using a hot-air drying molding machine having four drying compartments.
- sample No. 6 the initial drying (1st to 3rd chambers) is performed for 6.6 minutes with hot air (110 ° C ⁇ 100 ° C), and the second drying (4th chamber) is performed with hot air of low temperature (80 ° C) for 2.2 minutes. went.
- sample No. 6 a fully dried sample (water content 5%) could be prepared with a total drying time of 8.8 minutes.
- the “initial menthol content” after preparation of the sheet is sufficiently high at 63.5%
- the “menthol content after storage” after storage in the accelerated environment (30 days) is also high at 59.9%. Both the fragrance retention property and the storage fragrance property were good.
- Sample No. 7 was all dried with hot air at 100 ° C. without distinction between initial drying and late drying. Sample No. 7 did not adopt late drying at a low temperature, but in the drying process of the slurry, as in Sample Nos. 4 to 6, it was estimated that the sample temperature did not become too high due to the presence of moisture in the sample. Is done. That is, sample No. 7 was able to prepare a sufficiently dried sample (water content 4.9%) with a total drying time of 8.8 minutes. In addition, the “initial menthol content” after preparation of the sheet is sufficiently high at 61.9%, and the “menthol content after storage” after storage in an accelerated environment (for 30 days) is also high at 60.8%. Both the fragrance retention property and the storage fragrance property were good. As described above, even when the same hot air temperature of 100 ° C. was adopted throughout the entire drying process, a sheet having excellent perfume retention properties could be prepared in a relatively short drying time, similar to Sample Nos. 4 to 6. .
- Example 4 the temperature-responsive sol-gel transition characteristics of an aqueous polysaccharide solution (slurry) were examined.
- Gellan Gum (Gelcogel / San-Eigen EF Eye) 5 g Water (0.1 L) is maintained at 70 ° C., and gellan gum (5 g) is stirred with ATEC Japan High Performance Mixer DMM. It dissolved little by little so that it might not become lumps, and the polysaccharide aqueous solution (slurry) was prepared.
- FIGS. 2A and 2B show how the viscosity (fluidity) of the slurry changes due to such a temperature change.
- Example 5 sheets with sample numbers 1-7 were prepared as described in Examples 1-3, and the temperature of the sample during the drying process was measured. Tables 1 to 3 can be referred to for the hot air drying conditions of the samples Nos. 1 to 7.
- the sample temperature was measured by directly measuring the sample (slurry) during the drying process using a non-contact thermometer (manufactured by Optics, PT-7LD).
- sample numbers 1 to 7 are shown in FIGS. 3A to 3G, respectively.
- “with cooling” refers to a sample that has been cooled to about 20 ° C. by applying cold air (10 ° C.) before the drying process
- “without cooling” refers to casting a slurry without performing such cooling. It refers to a sample that has been quickly dried. From the results in FIGS. 3A-3G, it can be seen that the cooling of the slurry does not affect the temperature of the sample during the drying process.
- Sample No. 1 employed hot air drying conditions of 4 minutes at a hot air temperature of 70 ° C., 4 minutes at a hot air temperature of 80 ° C., and then 4 minutes at a hot air temperature of 120 ° C.
- the sample temperature increased as the hot air temperature increased, and finally exceeded 100 ° C. and reached nearly 120 ° C. (FIG. 3A). It is shown that the “menthol content after storage” of Sample No. 1 sheet is as low as 13.6% (Table 1). It is considered that the internal structure of the sheet was destroyed by the high sample temperature, and the menthol content was lowered after storage.
- Sample No. 2 employed hot air drying conditions of 2 minutes at a hot air temperature of 120 ° C., 2 minutes at a hot air temperature of 130 ° C., and 2 minutes at a hot air temperature of 176 ° C.
- the sample temperature increased with increasing hot air temperature and finally exceeded 100 ° C. and reached nearly 140 ° C. (FIG. 3B). It is shown that the “menthol content after storage” of Sample No. 2 sheet is as low as 29.2% (Table 1). It is considered that the internal structure of the sheet was destroyed by the high sample temperature, and the menthol content was lowered after storage.
- Sample No. 3 employs a hot air temperature of 70 ° C. for 60 minutes as a hot air drying condition.
- FIG. 3C shows the sample temperature from the start of drying to 14 minutes later, but the sample temperature did not exceed 70 ° C. over the entire drying time. It is shown that the “menthol content after storage” of Sample No. 3 sheet is as high as 59.2% (Table 1). Since the sheet of Sample No. 3 did not reach a high temperature over the entire drying time, it is considered that a high menthol content could be maintained after storage in an accelerated environment. However, since the sheet of Sample No. 3 was dried at a sample temperature of less than 70 ° C., a drying time of 60 minutes was required.
- Sample No. 4 employs hot air drying conditions of 120 ° C. for 5 minutes and then 70 ° C. for 2.5 minutes. The sample temperature reached a maximum of 95 ° C. under a hot air temperature of 120 ° C. and decreased to 72 ° C. under a hot air temperature of 70 ° C. (FIG. 3D). It is shown that the “menthol content after storage” of Sample No. 4 sheet is as high as 62.4% (Table 1). The sheet of Sample No. 4 was maintained at a lower sample temperature as compared with Sample Nos. 1 and 2 over the entire drying time, so it is considered that a high menthol content could be maintained after storage in an accelerated environment.
- Sample No. 5 adopted hot air drying conditions of 4 minutes at a hot air temperature of 120 ° C., and then 8 minutes at a hot air temperature of 70 ° C. The sample temperature reached a maximum of 95 ° C. under a hot air temperature of 120 ° C. and decreased to 70 ° C. under a hot air temperature of 70 ° C. (FIG. 3E). It is shown that the “menthol content after storage” of Sample No. 5 is as high as 58.5% (Table 2). The sheet of Sample No. 5 was maintained at a lower sample temperature compared to Sample Nos. 1 and 2 over the entire drying time, so it is considered that a high menthol content could be maintained after storage in an accelerated environment.
- Sample No. 6 employed hot air drying conditions of 2.2 minutes at a hot air temperature of 110 ° C., then 4.4 minutes at a hot air temperature of 100 ° C., and then 2.2 minutes at a hot air temperature of 80 ° C.
- the sample temperature was maintained in the range of about 80-90 ° C. (FIG. 3F). It is shown that the “menthol content after storage” of Sample No. 6 is as high as 59.9% (Table 3).
- the sheet of Sample No. 6 was maintained at a lower sample temperature compared to Sample Nos. 1 and 2 over the entire drying time, so it is considered that a high menthol content could be maintained after storage in an accelerated environment.
- Sample No. 7 adopted 8.8 minutes at a hot air temperature of 100 ° C. as hot air drying conditions.
- the sample temperature was maintained in the range of about 80-90 ° C. (FIG. 3G). It is shown that the “menthol content after storage” of the sheet of sample number 7 is as high as 60.8% (Table 3).
- the sheet of Sample No. 7 was maintained at a lower sample temperature as compared with Sample Nos. 1 and 2 over the entire drying time, and thus it is considered that a high menthol content could be maintained after storage in an accelerated environment.
- the menthol-containing sheet can be formed in a short time when the slurry is dried at a sample temperature of 70 to 100 ° C. over the entire drying time (excluding about 1 minute at the beginning of the drying time).
- Example 6 In this example, the effect of cooling the slurry before the drying step on the “menthol content after storage” of the menthol-containing sheet was demonstrated. Specifically, as described in Examples 1 to 3, the sheets of sample numbers 1 to 7 were prepared, and for each sheet, the “post-storage menthol content” and the slurry of the sheets prepared through cooling of the slurry. The “prepared menthol content” of the sheets prepared without cooling were compared. As described in Example 1, storage was performed by placing the sheet in a thermostat set at 50 ° C. for 7 days, 14 days, and 30 days.
- sample numbers 1 to 3 are shown in FIG. 4A
- sample numbers 4 to 7 are shown in FIG. 4B.
- “with cooling” refers to a sample that has been cooled to about 20 ° C. by applying cold air (10 ° C.) before the drying step
- “without cooling” refers to casting a slurry without performing such cooling. It refers to a sample that has been quickly dried.
- the “no cooling” sample had a slurry temperature below 50 ° C. between slurry casting and drying.
- FIGS. 4A and 4B The data “with cooling” in FIGS. 4A and 4B is the same as the data in FIG.
- the sheets of Sample Nos. 1 and 2 had a low menthol content after 30 days storage without reaching 30%, regardless of the presence or absence of cooling.
- the sample No. 3 sheet had a menthol content of more than 50% after storage for 30 days regardless of whether it was cooled or not, but the preparation of the sample No. 3 sheet required a drying time of 60 minutes. there were.
- the sample No. 7 sheet had a menthol content of 30% after storage for 30 days, while the menthol content after storage for 30 days was 61%. Was maintained until.
- the sheet when the menthol-containing sheet is prepared by cooling the raw slurry once and drying at a sample temperature of 70 to 100 ° C., the sheet can be formed in a short time and the menthol content is high after storage. Can be maintained.
- Example 7 the relationship between the cooling temperature of the slurry and the “initial menthol content” of the menthol-containing sheet was examined. Specifically, regarding the sheet of sample number 6 described in Example 3, various sheets were prepared by changing the cooling temperature of the slurry to 20 ° C., 30 ° C., 40 ° C., 50 ° C., and 60 ° C. The menthol content of the sheet immediately after preparation, that is, “initial menthol content” was measured.
- Example 4 the gelation of the slurry occurs at a cooling temperature of 40 ° C. or less, and the slurry containing the polysaccharide once cooled and gelled returns to the sol even if the temperature is raised thereafter. It has been shown to be difficult. In general, it is known that an emulsion is frozen and broken when the temperature falls below 0 ° C.
- a cooling temperature of 0 to 40 ° C. is preferable, and a cooling temperature of 0 to 30 ° C. is more preferable.
- Example 8 the relationship between the water content of the menthol-containing sheet and the menthol aroma retention rate was examined. Specifically, with respect to the sheet of sample number 6 described in Example 3, the total drying time of the slurry was increased to 8.16 minutes, 7.92 minutes, 7.64 minutes, 7.44 minutes, 7.08 minutes by increasing the belt conveyance speed in the hot air dryer. The sheets having various moisture contents were prepared. The moisture content of the prepared sheet was measured. The sheet preparation conditions and moisture content are shown in Table 4 below.
- the prepared sheet was placed in a thermostat set at 50 ° C. as described in Example 1 for 30 days.
- menthol content was measured and each measurement result is shown in the following Table 5 as "initial menthol content” and "menthol content of the sheet
- Menthol perfume retention rate (%) ⁇ (menthol content after storage) / (initial menthol content) ⁇ ⁇ 100 The result is shown as “accelerated storage immediately after manufacture” in FIG.
- seat which passed 2 months after preparation was set
- FIG. The menthol content was measured for the sheets immediately after preparation and after storage, and the respective measurement results are shown in the following Table 5 as “initial menthol content” and “menthol content of sheets stored 2 months after production”. Further, the menthol aroma retention rate was calculated according to the above formula. The results are shown in FIG. 6 as “accelerated storage after 2 months of manufacture”.
- the menthol content of the sheet immediately after preparation was approximately 50 to 60% in all the sample numbers 8-1 to 8-5.
- a sheet having a moisture content of about 6% was a sheet having a moisture content of 93% and about 9% (Sample No. 8-4).
- Is a sheet having a moisture content of 90% and about 11% is 87% and a sheet having a moisture content of about 15% (Sample No. 8-2) is 63% and about 23%.
- a sheet with a moisture content of% was shown to have a menthol scent retention of 6%.
- a sheet having a water content of about 6% was a sheet having a water content of 95% and about 9% (sample number 8).
- -4) is 87%
- a sheet having a moisture content of about 11% is 32%
- a sheet having a moisture content of about 15% is 8%
- a sheet having a moisture content of about 23% was shown to have a menthol scent retention of 8%.
- the sheet it is desirable to dry the sheet so that the moisture content of the sheet is less than 10%, preferably 9% or less, since the menthol aroma retention rate sharply decreases as the moisture content of the sheet increases.
- a high menthol aroma retention rate can be maintained if the sheet has a moisture content of about 9% or less even when the sheet of 2 months after preparation is further stored in an accelerated environment.
- the moisture content of the sheet is less than 3%, the menthol aroma retention rate is good, but “cracking” or “peeling” occurs in the sheet, so the moisture content after drying the sheet is 3% or more. Is desirable.
- Example 9 the effect of the type of polysaccharide on the menthol content after storage of the menthol-containing sheet was examined.
- Carrageenan, gellan gum, pectin, and konjac glucomannan were used as polysaccharides.
- the polysaccharide aqueous solution was cooled to 25 ° C. over about 900 seconds. Thereafter, the temperature was raised over about 900 seconds. It was measured with a rheometer (Thermo-Haake, RheoStress 1) how the viscosity (fluidity) of the polysaccharide aqueous solution was changed by temperature decrease and temperature increase.
- the results of the carrageenan aqueous solution are shown in FIGS. 7A and 7B
- the results of the gellan gum aqueous solution are shown in FIGS. 2A and 2B
- the results of the pectin aqueous solution are shown in FIGS. 7G and 7H
- the results of the konjac glucomannan aqueous solution are shown in FIGS.
- the carrageenan aqueous solution and the gellan gum aqueous solution were provided with “temperature-responsive sol-gel transition characteristics”.
- the aqueous pectin solution did not have “temperature-responsive sol-gel transition characteristics”.
- the konjac glucomannan aqueous solution did not have “temperature-responsive sol-gel transition characteristics” as shown in FIGS. 7K and 7L.
- the sheet was prepared according to the same method as in Example 1 as follows.
- the dispersed slurry was cast on a substrate (PET film / Futamura Chemical Co., Ltd. FE2001) at a thickness of 1 mm (wet state). Then, it cooled to about 20 degreeC with the cold air of about 10 degreeC generated with the spot cooler (Suiden SS-25DD-1).
- Example 2 a hot air dryer was used to dry-mold the water content to about 6% to prepare a carrageenan-containing sheet.
- the water content was measured by GC-TCD measurement (see Example 1).
- a hot air temperature of 110 ° C. for 3 minutes, a hot air temperature of 100 ° C. for 6 minutes, and then a hot air temperature of 80 ° C. for 3 minutes (total drying time 12 minutes) were adopted.
- the control sheet (without cooling) was prepared by dry-casting the cast slurry without cooling.
- the hot air drying conditions of the control sheet were as follows: hot air temperature of 110 ° C. for 2.5 minutes, then hot air temperature of 100 ° C. for 5 minutes, and then hot air temperature of 80 ° C. for 2.5 minutes (total drying time 10 minutes).
- FIG. 7C shows the change in sample temperature during the drying process.
- “with cooling” refers to a sample that has been cooled to about 20 ° C. by applying cold air (10 ° C.) before the drying process
- “without cooling” means that the slurry is quickly dried after casting the slurry without performing such cooling. It refers to the sample that was allowed to enter. From FIG. 7C, it can be seen that cooling of the slurry does not affect the temperature of the sample during the drying process.
- the dispersed slurry was cast on a substrate (PET film / Futamura Chemical Co., Ltd. FE2001) at a thickness of 1 mm (wet state). Then, it cooled to about 20 degreeC with the cold air of about 10 degreeC generated with the spot cooler (Suiden SS-25DD-1).
- Example 1 a hot air type dryer was used to dry-form the water content to about 6% to prepare a gellan gum-containing sheet.
- the water content was measured by GC-TCD measurement (see Example 1).
- a hot air temperature of 110 ° C. for 2.8 minutes, a hot air temperature of 100 ° C. for 5.5 minutes, and a hot air temperature of 80 ° C. for 2.8 minutes (total drying time of about 11 minutes) were adopted.
- the control sheet (without cooling) was prepared by dry-casting the cast slurry without cooling.
- the hot air drying conditions of the control sheet were 2.3 minutes at a hot air temperature of 110 ° C., 4.5 minutes at a hot air temperature of 100 ° C., and then 2.3 minutes at a hot air temperature of 80 ° C. (total drying time was about 9 minutes).
- FIG. 7E shows the change in sample temperature during the drying process.
- “with cooling” refers to a sample that has been cooled to about 20 ° C. by applying cold air (10 ° C.) before the drying process
- “without cooling” means that the slurry is quickly dried after casting the slurry without performing such cooling. It refers to the sample that was allowed to enter. It can be seen from FIG. 7E that the cooling of the slurry does not affect the temperature of the sample during the drying process.
- the dispersed slurry was cast on a substrate (PET film / Futamura Chemical Co., Ltd. FE2001) at a thickness of 1 mm (wet state). Then, it cooled to about 20 degreeC with the cold air of about 10 degreeC generated with the spot cooler (Suiden SS-25DD-1).
- a pectin-containing sheet was prepared by dry molding to a moisture content of about 6% using a hot air dryer.
- the water content was measured by GC-TCD measurement (see Example 1).
- a hot air temperature of 110 ° C. for 2.8 minutes, a hot air temperature of 100 ° C. for 5.5 minutes, and a hot air temperature of 80 ° C. for 2.8 minutes were adopted.
- the control sheet (without cooling) was prepared by dry-casting the cast slurry without cooling.
- the hot air drying conditions of the control sheet were as follows: hot air temperature of 110 ° C. for 2.5 minutes, then hot air temperature of 100 ° C. for 5 minutes, and then hot air temperature of 80 ° C. for 2.5 minutes (total drying time 10 minutes).
- FIG. 7I shows the change in sample temperature during the drying process.
- “with cooling” refers to a sample that has been cooled to about 20 ° C. by applying cold air (10 ° C.) before the drying process
- “without cooling” means that the slurry is quickly dried after casting the slurry without performing such cooling. It refers to the sample that was allowed to enter. From FIG. 7I it can be seen that cooling of the slurry does not affect the temperature of the sample during the drying process.
- the dispersed slurry was cast on a substrate (PET film / Futamura Chemical Co., Ltd. FE2001) at a thickness of 1 mm (wet state). Then, it cooled to about 20 degreeC with the cold air of about 10 degreeC generated with the spot cooler (Suiden SS-25DD-1).
- Example 1 it dried with the hot air type dryer to about 6% of moisture content, and prepared the konjac glucomannan containing sheet
- the water content was measured by GC-TCD measurement (see Example 1).
- a hot air temperature of 110 ° C. for 3 minutes a hot air temperature of 100 ° C. for 6 minutes, and then a hot air temperature of 80 ° C. for 3 minutes (total drying time 12 minutes) were adopted.
- the control sheet (without cooling) was prepared by dry-casting the cast slurry without cooling.
- the hot air drying conditions of the control sheet were as follows: hot air temperature of 110 ° C. for 2.5 minutes, then hot air temperature of 100 ° C. for 5 minutes, and then hot air temperature of 80 ° C. for 2.5 minutes (total drying time 10 minutes).
- FIG. 7M shows the change in sample temperature during the drying process.
- “with cooling” refers to a sample that has been cooled to about 20 ° C. by applying cold air (10 ° C.) before the drying process
- “without cooling” means that the slurry is quickly dried after casting the slurry without performing such cooling. It refers to the sample that was allowed to enter. From FIG. 7M, it can be seen that cooling of the slurry does not affect the temperature of the sample during the drying process.
- the initial menthol content shows about 70% by weight
- the menthol content after storage for 30 days is about 65% by weight.
- Menthol aroma retention rate 90% or more.
- the initial menthol content showed about 55% by weight
- the initial menthol content shows about 60% by weight
- the menthol content after 30 days storage is About 30% by weight (menthol aroma retention rate: about 55% to about 65%).
- the initial menthol content shows about 30% by weight, regardless of whether the slurry was cooled before the drying step, and contains menthol after storage for 30 days.
- the amount indicated about 15% by weight (menthol aroma retention about 50%).
- carrageenan or gellan gum was used as a polysaccharide, and after cooling before the drying step, drying was performed.
- Example 10 In this example, the effect of the polysaccharide concentration on the menthol content after storage of the menthol-containing sheet was examined.
- a raw material slurry containing carrageenan and a raw material slurry containing gellan gum were prepared.
- menthol was added in an amount (weight ratio) 5 times that of the polysaccharide
- 5% lecithin aqueous solution was added in an amount (weight ratio) 2/5 times that of the polysaccharide.
- the raw material slurry containing each concentration of polysaccharide was brought to 70 ° C. to 25 ° C. over about 900 seconds. Then, it heated up to 70 degreeC over about 900 second. It was measured with a rheometer (Thermo-Haake, RheoStress 1) how the viscosity (fluidity) of the slurry changed due to temperature drop and temperature rise.
- the results for the carrageenan-containing slurry are shown in FIGS. 8A and 8B, and the results for the gellan gum-containing slurry are shown in FIGS. 8D and 8E.
- the carrageenan is preferably contained in the raw material slurry at a concentration of 2 to 5% by weight.
- gellan gum is preferably contained in the raw material slurry at a concentration of 2 to 5% by weight.
- the menthol content (initial menthol content) of the sheet immediately after being prepared and the menthol content (menthol content after storage) of the sheet stored in an accelerated environment were measured.
- the acceleration environment is as described in the first embodiment.
- the menthol content was measured according to the same method as in Example 1.
- the result of the carrageenan-containing sheet is shown in FIG. 8C, and the result of the gellan gum-containing sheet is shown in FIG. 8F.
- the initial menthol content was about 70% by weight in both cases of 3% by weight and 5% by weight, and the menthol content after storage for 30 days was 70%.
- Example 11 In this example, the effect of the menthol blending ratio in the raw slurry on the menthol content and the menthol yield after storage of the menthol-containing sheet was examined.
- menthol for the carrageenan-containing sheet, menthol of 1-fold weight, 2.5-fold weight, 5-fold weight, 10-fold weight, 15-fold weight, and 20-fold weight was blended with respect to 5% by weight (in the raw material slurry). .
- menthol for gellan gum-containing sheets, 0.5 times the weight, 1 times the weight, 2.5 times the weight, 5 times the weight, 10 times the weight, 15 times the weight and 20 times the weight of the gellan gum of 3% by weight (in the raw material slurry) Weight menthol was formulated.
- the menthol content (initial menthol content) of the sheet immediately after being prepared and the menthol content (menthol content after storage) of the sheet stored in an accelerated environment were measured.
- the acceleration environment is as described in the first embodiment.
- the menthol content was measured according to the same method as in Example 1.
- the results of the carrageenan-containing sheet are shown in FIGS. 9A to 9E, and the results of the gellan gum-containing sheet are shown in FIGS. 9F to 9J.
- the notation [1: x] represents the weight ratio between the polysaccharide and the menthol in the raw material slurry.
- [1: 5] indicates that menthol having 5 times the weight of the polysaccharide is contained in the raw material slurry. It is contained in In these figures, “immediately after production” means immediately after sheet preparation, and “50 ° C. and one month later” means after storage at 50 ° C. for 30 days.
- Menthol yield (%) ⁇ (Measured value of menthol content in sheet) / (Menthol content) ⁇ ⁇ 100.
- “Menthol yield” immediately after the sheet was prepared showed a value exceeding 50% in the sample in which the blended amount of menthol is in the range of 1 to 10 times the weight, as shown in FIG. 9C.
- the “menthol yield” after storage was highest for a sheet containing 2.5 times the weight of menthol.
- a sheet containing 5 times or 10 times the weight of menthol has a lower “menthol yield” after storage than a sheet containing 2.5 times the weight of menthol, but the menthol content (absolute amount) in the sheet is Many (see FIG. 9A).
- FIGS. 9D and 9E show the relationship between the menthol blending ratio (%) and the menthol content (%), and the relationship between the menthol blending ratio (%) and the menthol yield (%), respectively.
- the menthol blending ratio (%) represents ⁇ menthol blending amount / (menthol blending amount + carrageenan blending amount) ⁇ ⁇ 100.
- the sheet having a menthol content of 2.5 times to 10 times the weight (that is, a menthol content of 71 to 91%) showed a high menthol content after storage.
- the sheet having a menthol blending amount of 1 to 5 times weight (that is, a menthol blending ratio of 50 to 83%) showed a high menthol yield after storage.
- 9A to 9E show that the blending amount of menthol with respect to carrageenan is preferably in the range of 1 to 10 times weight, more preferably in the range of 2.5 times weight to 5 times weight.
- the “initial menthol content” is highest in the case of a sheet containing 5 times the weight of menthol, and 0.5 times the weight of menthol. In the case of the sheet containing the lowest, the sample having the menthol blending amount in the range of 0.5 times to 5 times the weight depended on the menthol blending amount. “Menthol content after storage” was almost the same as the initial menthol content, but the menthol content was 10 times weight. About the above sample, the menthol content fell with progress of storage days. For this reason, as shown in FIG.
- the menthol aroma retention rate after storage for 30 days was over 90% for samples in which the menthol blending amount was in the range of 0.5 to 5 times the weight, For a sample having a menthol blending amount of 10 times or more, it is about 50%. As described above, the sample having a menthol blending amount in the range of 0.5 times to 5 times the weight has a high menthol perfume retention rate. Especially, the sheet containing 2.5 times the weight of menthol is about A menthol aroma retention rate of 100% was shown.
- “Menthol yield” immediately after the sheet creation showed a value exceeding 50% in the sheet containing 1-fold weight, 2.5-fold weight, and 5-fold weight menthol, as shown in FIG. 9H.
- the “menthol yield” after storage was highest for a sheet containing 2.5 times the weight of menthol.
- the sheet containing 5 times the weight of menthol has a lower “menthol yield” after storage than the sheet containing 2.5 times the weight of menthol, but has a higher menthol content (absolute amount) in the sheet (FIG. 9F). reference).
- FIGS. 9I and 9J show the relationship between the menthol blending ratio (%) and the menthol content (%) and the menthol blending ratio (%) and the menthol yield (%), respectively.
- the menthol blending ratio (%) represents ⁇ menthol blending amount / (menthol blending amount + gellan gum blending amount) ⁇ ⁇ 100.
- the sheet having a menthol content of 2.5 times to 5 times the weight (that is, the menthol content is 71 to 83%) showed a high menthol content after storage.
- a sheet having a menthol blending amount of 1 to 5 times weight (that is, a menthol blending ratio of 50 to 83%) showed a high menthol yield after storage.
- 9F to 9J show that the blending amount of menthol with gellan gum is preferably in the range of 1 to 10 times weight, more preferably in the range of 2.5 times weight to 5 times weight.
- Example 12 In this example, the effect of the amount of lecithin in the raw slurry on the menthol content after storage of the menthol-containing sheet was examined.
- carrageenan-containing sheet 0.001 times weight, 0.005 times weight, 0.01 times weight, 0.02 times weight, 0.05 times weight with respect to 5% by weight (in the raw material slurry) 0.1 times weight, 0.2 times weight, and 0.4 times weight of lecithin were blended. Menthol was blended in an amount 5 times the weight of carrageenan.
- the gellan gum-containing sheet is 0.001 times, 0.005 times, 0.01 times, 0.02 times, 0.05 times, and 3% by weight (in the raw material slurry) of gellan gum. Double weight, 0.1 times weight, 0.2 times weight and 0.4 times weight of lecithin were blended. Menthol was blended in an amount 5 times the weight of gellan gum.
- the menthol content (initial menthol content) of the sheet immediately after being prepared and the menthol content (menthol content after storage) of the sheet stored in an accelerated environment were measured.
- the acceleration environment is as described in the first embodiment.
- the menthol content was measured according to the same method as in Example 1.
- the results for the carrageenan-containing sheet are shown in FIGS. 10A and 10B, and the results for the gellan gum-containing sheet are shown in FIGS. 10C and 10D.
- the numerical values in parentheses represent the weight ratio of lecithin to polysaccharide, for example, [0.01] contains 0.01 times the weight of lecithin in the raw material slurry. Represents that. 10B and 10D, “immediately after production” means immediately after the preparation of the sheet, and “after 50 ° C. and 1 month” means after storage at 50 ° C. for 30 days.
- FIG. 10B shows the relationship between the lecithin content (weight ratio to carrageenan) and menthol content (%). As shown in FIG. 10B, the sheet having a lecithin content of 0.005 to 0.02 times the carrageenan was able to maintain a high menthol content after storage.
- FIG. 10D shows the relationship between the lecithin content (weight ratio with respect to gellan gum) and menthol content (%). As shown in FIG. 10D, the sheet having a lecithin content of 0.005 to 0.05 times the weight of gellan gum was able to maintain a high menthol content after storage.
- the blending amount of lecithin with respect to the polysaccharide is preferably in the range of 0.5 to 5% by weight.
- the amount of lecithin based on the polysaccharide is preferably in the range of 0.5 to 2% by weight.
- the blending amount of lecithin is preferably in the range of 0.5 to 5% by weight, and more preferably in the range of 0.5 to 2% by weight.
- Example 13 In this example, the effect of the type of emulsifier on the menthol content after storage of the menthol-containing sheet was examined.
- the following 8 types of emulsifiers were used as emulsifiers.
- the numbers 1-8 assigned to the emulsifiers correspond to the numbers in FIGS. 11A and 11B.
- Lecithin (Sun Lecithin A-1 manufactured by Taiyo Kagaku Co., Ltd.) 2. Glycerin fatty acid ester (monoglyceride) (Excel S-95 manufactured by Kao Corporation) 2. Compound name: lipophilic glyceryl monostearate Glycerin fatty acid ester (polyglyceride) (Sunsoft A-181E manufactured by Taiyo Chemical Co., Ltd.) Compound name: pentaglycerin monostearate Glycerin fatty acid ester (organic acid monoglyceride) (Step SS manufactured by Kao Corporation) Compound name: Succinic acid monoglyceride5.
- Sorbitan fatty acid ester (Emazole S-10V manufactured by Kao Corporation) Compound name: Sorbitan monostearate6. Sorbitan fatty acid ester (polysorbate) (Emazole S-120V manufactured by Kao Corporation) Compound name: Polyoxyethylene sorbitan monostearate7. Propylene glycol fatty acid ester (Taiyo Chemical Co., Ltd. Sunsoft No. 25CD) Compound name: propylene glycol monostearate8.
- Sucrose fatty acid ester (Ryoto Sugar Ester S-1570 manufactured by Mitsubishi Chemical Foods Corporation) Compound name: Sucrose stearate
- the menthol content (initial menthol content) of the sheet immediately after it was prepared and the menthol content (menthol content after storage) of the sheet stored in an accelerated environment were measured.
- the acceleration environment is as described in the first embodiment.
- the menthol content was measured according to the same method as in Example 1.
- the result of the carrageenan-containing sheet is shown in FIG. 11A, and the result of the gellan gum-containing sheet is shown in FIG. 11B.
- “immediately after production” means immediately after sheet preparation, and “50 ° C. ⁇ one month later” means after storage at 50 ° C. for 30 days.
Abstract
Description
本発明の一態様において、喫煙物品用メンソール含有シート(以下メンソール含有シートという)は、
カラギーナンおよびゲランガムの少なくとも一つを含む多糖類、メンソール、乳化剤、並びに70~95重量%の水を含み、多糖類を基準としたメンソールの含有量が100~1000重量%の範囲にあり、ゾル状態にある60~90℃の原料スラリーを基材上に伸展させる工程、
伸展させた原料スラリーを0~40℃の試料温度に冷却してゲル化させる工程、および
ゲル化した原料を加熱して、70~100℃の試料温度で乾燥させることを含む加熱乾燥工程
を含む方法により製造される。
本発明において原料スラリーは、(i)カラギーナンおよびゲランガムの少なくとも一つを含む多糖類と水とを混合、加熱して多糖類の水溶液を調製する工程と、(ii)かかる水溶液にメンソールと乳化剤とを加えて混練・乳化させる工程とを含む方法により調製することができる。
上述のとおり調製された60~90℃の原料スラリーを、基材上に伸展させる。
本発明のメンソール含有シートの調製において、伸展させた原料スラリーは、乾燥させる前に、スラリーが十分にゲル化し(40℃以下)、かつ一般にエマルジョンが氷結して破壊されない温度(0℃以上)、すなわち0~40℃、好ましくは0~30℃、より好ましくは15~25℃になるように一旦冷却する。ここで冷却前の原料スラリーは、60~90℃、好ましくは75~85℃の温度を有し、ゾルの状態にある。かかる予備冷却は、伸展させた原料スラリーに、単なる送風もしくはスポットクーラー(例えばスイデン SS-25DD-1)により発生させた冷風(例えば10℃)を2~3分間あてることにより行うことができる。あるいは、予備冷却は、伸展させた原料スラリーを、冷温水発生器(チラー、例えば(株)アピステ PCU-1600R)で発生させた冷媒(例えば10℃)を通した管に1~2分間接触させることにより行ってもよい。あるいは、予備冷却は、伸展させた原料スラリーを室温に放置することにより行ってもよい。
伸展され冷却された原料スラリーの加熱乾燥は、熱風乾燥、赤外線加熱乾燥などの任意の加熱乾燥手段により行うことができる。以下、原料スラリーの「加熱乾燥」は、単に「乾燥」ともいう。
100℃以上の熱風温度で全乾燥時間の1/4以上の時間をかけた初期乾燥、その後、
100℃未満の熱風温度で全乾燥時間の1/4以上の時間をかけた後期乾燥
により行い、原料スラリーを、20分以下の全乾燥時間で、10%未満の水分含量を有するシートの形態まで乾燥させることにより行うことができる。
本発明のメンソール含有シートは、たとえば通常のタバコ刻と同等のサイズに裁刻して、喫煙物品のタバコ刻みに配合することができる。メンソール含有シートの裁刻物は、タバコ刻み100gあたり2~10gの量で配合することができる。メンソール含有シートの裁刻物は、好ましくは、タバコ刻み中に分散させて配合される。
(1)原料スラリーの調製(10リットルスケール)
水 10リットル
ゲランガム(ゲルコゲル/三栄源エフ・エフ・アイ) 150グラム
タマリンドガム(ビストップD-2032/三栄源エフ・エフ・アイ) 150グラム
レシチン(サンレシチンA-1/太陽化学(株)) 120ミリリットル
(5%水溶液)
メンソール(高砂香料工業株式会社) 1500グラム
水(10 L)を80℃に保持し、ミキサー(PRIMIX T.K. AUTO MIXER Model 40/溶液攪拌ローター装着/2000 rpm)で攪拌しつつ、ゲランガム(150 g)およびタマリンドガム(150 g)をダマにならないように少量ずつ溶解し(所要時間20分程度)、メンソール(1500 g)を添加した。
得られた原料スラリーを、スリットダイからベースフィルムの上に押し出し、その後、2~3分間、スポットクーラー(スイデン SS-25DD-1)により発生させた冷風(10℃)を当て、原料スラリーが20℃程度になるように冷却し、その後、熱風乾燥機内をベルト搬送することにより熱風乾燥し、フィルム状のメンソール含有シートを得た。実験の詳細を以下に記す。
ベースフィルム:PETフィルム(表面コロナ処理)、厚さ50μm
熱風乾燥機:下記構成を有する熱風型乾燥成形機
乾燥区画:3室(各ゾーン長2.5 m、全長7.5 m)
熱風風量と形式:第1室:パンチング板、風量5 m/秒
:第2室:パンチング板、風量10 m/秒
:第3室:フローティングジェット、風量20 m/秒
第1室および第2室において熱風は、制流板として機能する穴の開いたパンチング板を経由して、べルト上を搬送されるメンソール含有シートに当てられた。第3室において熱風は、ベースフィルムと一緒に浮遊して搬送されるメンソール含有シートに上下方向から通風により当てられた。
メンソール含有シートの水分含量は、以下のとおりGC-TCDで測定した。
Column ;HP Polapack Q (packed column) Constant Flow mode 20.0 mL/min
Injection ;1.0μL
Inlet ;EPC purge packed column inlet Heater;230℃
Gas;He Total flow;21.1 mL/min
Oven ;160℃(hold 4.5 min)→(60℃/min)→220℃(hold 4.0 min)
Detector ;TCD検出器 Reference Gas(He)流量;20 mL/min
make up gas(He)3.0 mL/min
Signal rate ;5 Hz
検量線溶液濃度;0、1、3、5、10、20 [mg-H2O/10 mL] の6点。
メンソール含有シートのメンソール含有量は、以下のとおりGC-FIDで測定した。
Column ;DB-WAX 30m×530μm×1μm
Constant Pressure mode 5.5 psi(velocity;50 cm/sec)
Injection ;1.0μL
Inlet ;Spritless mode 250℃ 5.5 psi
Oven ;80℃→(10℃/min)→170℃(hold 6.0 min)[Max 220℃]
Detector ;FID検出器 250℃ (H2;40 mL/min・air;450 mL/min)
Signal rate ;20 Hz
検量線溶液濃度;0、0.01、0.05、0.1、0.3、0.5、0.7、1.0 [mg-メンソール/mL] の8点。
蔵置後メンソール含有量(%)={メンソール含有量の測定値(mg)/メンソール含有シートの重量(mg)}×100。
(5)結果
試料番号1~4のメンソール含有シートを、上述の熱風型乾燥成形機で、表1に記載される熱風乾燥条件を用いて調製した。メンソール含有シートの水分含量および初期メンソール含有量を、上記手法に従って測定し、その結果を表1に示す。30日蔵置後のメンソール含有量を表1に示し、7日、14日、30日蔵置後のメンソール含有量を図1に示す。図1において符号1~7は、試料番号1~7を表す。
上述の熱風型乾燥成形機で原料スラリーを伸展、乾燥させてシート状に成形する場合、乾燥前半で表面皮膜を生成させないために低い熱風温度(70℃程度)から乾燥をはじめ、乾燥後半では完全乾燥を目指すために高い熱風温度(120℃程度)で乾燥させる手法が取られることが多い。この手法に倣って、試料番号1のメンソール含有シートを調製したところ、全乾燥時間12分で、十分に乾燥した試料(水分含量3.1%)を調製することができた。また、シート調製後の「初期メンソール含有量」は、81.5%と十分に高かったが、加速環境下で(20日間)蔵置後の「蔵置後メンソール含有量」は、13.6%と低く、試料番号1のシートは、蔵置保香性に問題を有していた。
試料番号2では、試料番号1より短い乾燥時間とするために、高温の乾燥温度を採用した。このため、試料番号2では、全乾燥時間6分で、十分に乾燥した試料(水分含量3.2%)を調製することができた。また、シート調製後の「初期メンソール含有量」は、62.4%と十分に高かったが、加速環境下で(30日間)蔵置後の「蔵置後メンソール含有量」は、29.2%と低く、試料番号2のシートは、蔵置保香性に問題を有していた。
試料番号3では、乾燥工程全体において熱風温度を70℃に設定した。このため、試料番号3では、全乾燥時間60分で、十分に乾燥した試料(水分含量3.1%)を調製することができた。また、シート調製後の「初期メンソール含有量」は、75.8%と十分に高く、また、加速環境下で(30日間)蔵置後の「蔵置後メンソール含有量」も59.2%と高く、シート調製後の保香性および蔵置保香性のいずれも良好であった。しかし、乾燥に要した時間が60分と長かった。
試料番号4では、低温乾燥から高温乾燥に移行させた試料番号1および2とは反対に、初期乾燥(第1室および第2室)を高温(120℃)の熱風で行い、後期乾燥(第3室)を低温(70℃)の熱風で行った。試料番号4では、全乾燥時間7.5分と短かったが、十分に乾燥した試料(水分含量3.4%)を調製することができた。また、シート調製後の「初期メンソール含有量」は、75.7%と十分に高く、また、加速環境下で(30日間)蔵置後の「蔵置後メンソール含有量」も62.4%と高く、シート調製後の保香性および蔵置保香性のいずれも良好であった。このように、高温での初期乾燥と低温での後期乾燥を採用すると、優れた保香性を有するシートを、比較的短い乾燥時間で調製することができた。
下記表2に記載される熱風乾燥条件でスラリーを乾燥させた以外は実施例1と同様の手法で、試料番号5のメンソール含有シートを調製し、水分含量およびメンソール含有量を測定した。その結果を表2に示す。
乾燥区画が4室となる熱風型乾燥機を用いて、下記表3に記載される熱風乾燥条件でスラリーを乾燥させた以外は、実施例1と同様の手法で、試料番号6および7のメンソール含有シートを調製し、水分含量およびメンソール含有量を測定した。その結果を表3に示す。
本実施例では、多糖類水溶液(スラリー)の温度応答性ゾル-ゲル転移特性を調べた。
ゲランガム(ゲルコゲル/三栄源エフ・エフ・アイ) 5グラム
水(0.1L)を70℃に保持し、(株)エーテックジャパン 高性能ミキサーDMMで攪拌しつつゲランガム(5g)をダマにならないように少量ずつ溶解し、多糖類水溶液(スラリー)を調製した。
本実施例では、実施例1~3に記載されるとおり試料番号1~7のシートを調製し、乾燥工程の間の試料の温度を測定した。試料番号1~7の試料の熱風乾燥条件は、表1~3を参照することができる。
本実施例では、乾燥工程前のスラリーの冷却が、メンソール含有シートの「蔵置後メンソール含有量」に及ぼす効果を実証した。具体的には、実施例1~3に記載されるとおり試料番号1~7のシートを調製し、それぞれのシートについて、スラリーの冷却を経て調製されたシートの「蔵置後メンソール含有量」とスラリーを冷却することなく調製されたシートの「蔵置後メンソール含有量」を比較した。蔵置は、実施例1に記載されるとおり、シートを、50℃に設定した恒温器に7日間、14日間および30日間置くことにより行った。
本実施例では、スラリーの冷却温度とメンソール含有シートの「初期メンソール含有量」との関係を調べた。具体的には、実施例3に記載される試料番号6のシートについて、スラリーの冷却温度を20℃、30℃、40℃、50℃、60℃と変化させて、種々のシートを調製した。調製直後のシートのメンソール含有量、すなわち「初期メンソール含有量」を測定した。
本実施例では、メンソール含有シートの水分含量とメンソール保香率との関係を調べた。具体的には、実施例3に記載される試料番号6のシートについて、熱風乾燥機内のベルト搬送速度を上げることによりスラリーの総乾燥時間を8.16分、7.92分、7.64分、7.44分、7.08分と変化させて、種々の水分含量を有するシートを調製した。調製されたシートの水分含量を測定した。シートの調製条件および水分含量を以下の表4に示す。
その結果を、図6に「製造直後 加速蔵置」として示す。
本実施例では、多糖類の種類が、メンソール含有シートの蔵置後のメンソール含有量に及ぼす効果を調べた。多糖類として、カラギーナン、ゲランガム、ペクチン、コンニャクグルコマンナンを使用した。
本実験では、各多糖類水溶液の温度応答性ゾル-ゲル転移特性を調べた。
水 0.1リットル
κ-カラギーナン(カラギニンCS-530/三栄源エフ・エフ・アイ) 5グラム
(2)ゲランガム水溶液
実施例4に記載のとおりである。
水 0.1リットル
ペクチン(和光純薬工業株式会社 化学用 かんきつ類由来) 3グラム
(4)コンニャクグルコマンナン水溶液
水 0.1リットル
コンニャクグルコマンナン(群馬県蒟蒻原料商工業協同組合) 1グラム
上記組成の多糖類水溶液を、実施例4の手法に従って調製した。
カラギーナン水溶液は、図7Aに示されるとおり、25℃に降温すると、ゾル-ゲル転移温度である約50℃付近まで粘度は低かったが(約1,000mPas以下)、転移温度より低い温度の下で粘度は急激に上昇し、粘度は10,000,000mPasに達するようになった(ゲル化)。このゲルを昇温すると、図7Bに示されるとおり、転移温度を超えて加熱しても容易にゾルへと戻ることはなく、ゲル状態を維持することができた。
本実験では、各多糖類水溶液を用いてメンソール含有シートを調製し、加熱乾燥工程の間の試料の温度を測定した。
水 10リットル
κ-カラギーナン(カラギニンCS-530/三栄源エフ・エフ・アイ) 500グラム
5%レシチン水溶液(サンレシチンA-1/太陽化学(株)) 200ミリリットル
メンソール(高砂香料工業株式会社) 2500グラム
水(80℃に加熱保温)10リットル(100重量部)をミキサー(PRIMIX T. K. AUTO MIXER Model 40/溶液撹拌ローター装着/2000rpm)で撹拌しつつ、κ-カラギーナン500グラム(5重量部)をダマにならないように少量ずつ溶解した(所要時間 20分程度)。その温度のまま、2500グラム(25重量部)のl-メンソールを添加した。撹拌ミキサーからホモジナイザー(PRIMIX T. K. AUTO MIXER Model 40/ローター-ステーターヘッド装着/4000rpm)に交換して10分間乳化を行い、更に200ミリリットル(2重量部)の5%レシチン水溶液を添加して撹拌した。メンソールは、カラギーナン水溶液に分散した。
水 10リットル
ゲランガム(ゲルコゲル/三栄源エフ・エフ・アイ) 300グラム
5%レシチン水溶液(サンレシチンA-1/太陽化学(株)) 120ミリリットル
メンソール(高砂香料工業株式会社) 1500グラム
水(80℃に加熱保温)10リットル(100重量部)をミキサー(PRIMIX T. K. AUTO MIXER Model 40/溶液撹拌ローター装着/2000rpm)で撹拌しつつ、ゲランガム300グラム(3重量部)をダマにならないように少量ずつ溶解した(所要時間 20分程度)。その温度のまま、1500グラム(15重量部)のl-メンソールを添加した。撹拌ミキサーからホモジナイザー(PRIMIX T. K. Model 40/ローター-ステーターヘッド装着/4000rpm)に交換して10分間乳化を行い、更に120ミリリットル(1.2重量部)の5%レシチン水溶液を添加して撹拌した。メンソールは、ゲランガム水溶液に分散した。
水 10リットル
ペクチン(和光純薬工業株式会社 化学用 かんきつ類由来) 300グラム
5%レシチン水溶液(サンレシチンA-1/太陽化学(株)) 120ミリリットル
メンソール(高砂香料工業株式会社) 1500グラム
水(80℃に加熱保温)10リットル(100重量部)をミキサー(PRIMIX T. K. AUTO MIXER Model 40/溶液撹拌ローター装着/2000rpm)で撹拌しつつ、ペクチン300グラム(3重量部)をダマにならないように少量ずつ溶解した(所要時間 20分程度)。その温度のまま、1500グラム(15重量部)のl-メンソールを添加した。撹拌ミキサーからホモジナイザー(PRIMIX T. K. AUTO MIXER Model 40/ローター-ステーターヘッド装着/4000rpm)に交換して10分間乳化を行い、更に120ミリリットル(1.2重量部)の5%レシチン水溶液を添加して撹拌した。メンソールは、ペクチン水溶液に分散した。
水 10リットル
コンニャクグルコマンナン(群馬県蒟蒻原料商工業協同組合) 100グラム
5%レシチン水溶液(サンレシチンA-1/太陽化学(株)) 40ミリリットル
メンソール(高砂香料工業株式会社) 500グラム
水(80℃に加熱保温)10リットル(100重量部)をミキサー(PRIMIX T. K. AUTO MIXER Model 40/溶液撹拌ローター装着)で撹拌しつつ、コンニャクグルコマンナン100グラム(1重量部)をダマにならないように少量ずつ溶解した(所要時間 20分)。その温度のまま、500グラム(5重量部)のl-メンソールを添加した。撹拌ミキサーからホモジナイザー(PRIMIX T. K. AUTO MIXER Model 40/ローター-ステーターヘッド装着)に交換して10分間乳化を行い、更に、40ミリリットル(0.4重量部)の5%レシチン水溶液を添加して撹拌した。メンソールは、コンニャクグルコマンナン水溶液に分散した。
作成された直後のシートのメンソール含有量(初期メンソール含有量)と、加速環境下で蔵置したシートのメンソール含有量(蔵置後メンソール含有量)とを測定した。加速環境は、実施例1に記載したとおりであり、メンソール含有量の測定は、実施例1と同様の手法で行った。カラギーナン含有シートの結果を図7Dに示し、ゲランガム含有シートの結果を図7Fに示し、ペクチン含有シートの結果を図7Jに示し、コンニャクグルコマンナン含有シートの結果を図7Nに示す。
カラギーナン含有シートについては、図7Dに示されるとおり、乾燥工程前にスラリーを冷却した場合、初期メンソール含有量は、約80重量%を示し、30日蔵置後のメンソール含有量は、60重量%以上を示した(メンソール保香率=約80%)。一方、乾燥工程前にスラリーを冷却しなかった場合、初期メンソール含有量は、約80重量%を示したが、30日蔵置後のメンソール含有量は、約45重量%を示した(メンソール保香率=約60%)。
本実施例では、多糖類の濃度が、メンソール含有シートの蔵置後のメンソール含有量に及ぼす効果を調べた。
本実験では、各濃度の多糖類を含有する原料スラリー(シート調製液)の温度応答性ゾル-ゲル転移特性を調べた。多糖類として、水(100重量部)に対して1重量部(1%)、2重量部(2%)、3重量部(3%)、5重量部(5%)および7重量部(7%)のカラギーナン、並びに水(100重量部)に対して1重量部(1%)、2重量部(2%)、3重量部(3%)、5重量部(5%)および7重量部(7%)のゲランガムを使用した。以下の説明および図8A~8Fにおいて、多糖類の濃度は、水に対する重量百分率(%)で表す。
図8Aおよび8Bに示されるとおり、1重量%のカラギーナンを含有する原料スラリーの場合、25℃まで冷却しても十分にゲル化せず、この原料を昇温した際にゲル状態を維持することは難しかった。また、7重量%のカラギーナンを含有する原料スラリーの場合、降温過程の初期(70~60℃の範囲)において粘度が上昇し、ゾル状態を維持することが難しいため、原料スラリーの調製時にメンソールを分散させることが困難である。
各濃度の多糖類を含有する原料スラリー(10-1の欄を参照)を用いて、カラギーナン含有シートおよびゲランガム含有シートを調製した。シートの調製は、実施例9と同様の手法に従って行った。
カラギーナン含有シートについては、図8Cに示されるとおり、3重量%の場合も5重量%の場合も、初期メンソール含有量は、約80重量%を示し、30日蔵置後のメンソール含有量は、約60重量%を示した(メンソール保香率=約80%)。2重量%の場合、初期メンソール含有量は、74重量%を示し、30日蔵置後のメンソール含有量は、50重量%を超える値を示した(メンソール保香率=68%)。また、6重量%の場合、初期メンソール含有量は、69重量%、30日蔵置後のメンソール含有量は、43重量%を示した(メンソール保香率=62%)。
これら結果より、カラギーナンおよびゲランガムは、原料スラリー中に2~6重量%の濃度で含有されることが好ましく、3~5重量%の濃度で含有されることがより好ましいことがわかる。
本実施例では、原料スラリー中のメンソール配合割合が、メンソール含有シートの蔵置後のメンソール含有量およびメンソール歩留りに及ぼす効果を調べた。
種々のメンソール配合割合を有する原料スラリーを用いて、カラギーナン含有シートおよびゲランガム含有シートを調製した。シートの調製は、実施例9と同様の手法に従って行った。
(1)カラギーナン含有シート
カラギーナン含有シートについては、図9Aに示されるとおり、「初期メンソール含有量」は、10倍重量のメンソールを含有するシートの場合が最も高く、次に、5倍重量のメンソールを含有するシートの場合が高く、次に、2.5倍重量のメンソールを含有するシートの場合が高く、次に1倍重量のメンソールを含有するシートの場合が高く、これらの結果は、メンソール配合量に依存していた。一方、15倍重量および20倍重量のメンソールを含有するシートの場合、「初期メンソール含有量」は20重量%以下であり、とりわけ低かった。「蔵置後メンソール含有量」は、いずれのメンソール配合量の場合も、初期メンソール含有量からほとんど低下しなかった。このため、図9Bに示されるとおり、30日蔵置後のメンソール保香率は、いずれのメンソール配合量の場合も、70%を超えていた。なかでも、2.5倍重量のメンソールを含有するシートは、約100%のメンソール保香率を示した。
メンソール歩留り(%)={(シート中のメンソール含有量の測定値)/(メンソール配合量)}×100。
ゲランガム含有シートについては、図9Fに示されるとおり、「初期メンソール含有量」は、5倍重量のメンソールを含有するシートの場合が最も高く、0.5倍重量のメンソールを含有するシートの場合が最も低く、メンソール配合量が0.5倍重量から5倍重量までの範囲にある試料については、メンソール配合量に依存していた。「蔵置後メンソール含有量」は、メンソール配合量が0.5倍重量から5倍重量までの範囲にある試料については、初期メンソール含有量からほとんど低下しなかったが、メンソール配合量が10倍重量以上の試料に関しては、蔵置日数の経過に伴ってメンソール含有量が低下した。このため、図9Gに示されるとおり、30日蔵置後のメンソール保香率は、メンソール配合量が0.5倍重量から5倍重量までの範囲にある試料に関しては90%を超えていたが、メンソール配合量が10倍重量以上の試料に関しては、50%程度となってしまっている。上述のとおり、メンソール配合量が0.5倍重量から5倍重量までの範囲にある試料は、メンソール保香率が高いが、なかでも、2.5倍重量のメンソールを含有するシートは、約100%のメンソール保香率を示した。
本実施例では、原料スラリー中のレシチン配合量が、メンソール含有シートの蔵置後のメンソール含有量に及ぼす効果を調べた。
種々のレシチン配合量を有する原料スラリーを用いて、カラギーナン含有シートおよびゲランガム含有シートを調製した。シートの調製は、実施例9と同様の手法に従って行った。
(1)カラギーナン含有シート
カラギーナン含有シートについては、図10Aに示されるとおり、レシチン配合量がカラギーナンに対して0.1~0.4倍重量の場合、蔵置後にメンソール含有量は大きく低下した。
ゲランガム含有シートについては、図10Cに示されるとおり、レシチン配合量がゲランガムに対して0.1~0.4倍重量の場合、蔵置後にメンソール含有量は大きく低下した。
本実施例では、乳化剤の種類が、メンソール含有シートの蔵置後のメンソール含有量に及ぼす効果を調べた。
種々のタイプの乳化剤を含有する原料スラリーを用いて、カラギーナン含有シートおよびゲランガム含有シートを調製した。シートの調製は、実施例9と同様の手法に従って行った。メンソールは、多糖類に対して5倍重量の量で配合し、各種の乳化剤は、多糖類に対して0.02倍重量の量で配合した。
(太陽化学株式会社製 サンレシチンA-1)
2.グリセリン脂肪酸エステル(モノグリセリド)
(花王株式会社製 エキセルS-95)
化合物名:親油型モノステアリン酸グリセリン
3.グリセリン脂肪酸エステル(ポリグリセリド)
(太陽化学株式会社製 サンソフトA-181E)
化合物名:モノステアリン酸ペンタグリセリン
4.グリセリン脂肪酸エステル(有機酸モノグリセリド)
(花王株式会社製 ステップSS)
化合物名:コハク酸モノグリセライド
5.ソルビタン脂肪酸エステル
(花王株式会社製 エマゾールS-10V)
化合物名:ソルビタンモノステアレート
6.ソルビタン脂肪酸エステル(ポリソルベート)
(花王株式会社製 エマゾールS-120V)
化合物名:ポリオキシエチレンソルビタンモノステアレート
7.プロピレングリコール脂肪酸エステル
(太陽化学株式会社製 サンソフトNo. 25CD)
化合物名:モノステアリン酸プロピレングリコール
8.ショ糖脂肪酸エステル
(三菱化学フーズ株式会社製 リョート シュガーエステルS-1570)
化合物名:ショ糖ステアリン酸エステル
作成された直後のシートのメンソール含有量(初期メンソール含有量)と、加速環境下で蔵置したシートのメンソール含有量(蔵置後メンソール含有量)とを測定した。加速環境は、実施例1に記載したとおりである。メンソール含有量の測定は、実施例1と同様の手法に従って行った。カラギーナン含有シートの結果を図11Aに示し、ゲランガム含有シートの結果を図11Bに示す。図11Aおよび11Bにおいて、「製造直後」は、シート調製直後を意味し、「50℃・1カ月後」は、50℃で30日蔵置した後を意味する。
図11Aおよび11Bの結果から、レシチンに加えて、各種の乳化剤が使用可能であることがわかる。カラギーナン含有シートについては、乳化剤として、1.レシチン、3.グリセリン脂肪酸エステル(ポリグリセリド)、4.グリセリン脂肪酸エステル(有機酸モノグリセリド)を使用することが特に好ましい。ゲランガム含有シートについては、乳化剤として、1.レシチン、2.グリセリン脂肪酸エステル(モノグリセリド)、3.グリセリン脂肪酸エステル(ポリグリセリド)、4.グリセリン脂肪酸エステル(有機酸モノグリセリド)、5.ソルビタン脂肪酸エステル、7.プロピレングリコール脂肪酸エステル、8.ショ糖脂肪酸エステルを使用することが特に好ましい。
Claims (11)
- カラギーナンおよびゲランガムの少なくとも一つを含む多糖類、香料、乳化剤、並びに70~95重量%の水を含み、多糖類を基準とした香料の含有量が100~1000重量%の範囲にあり、ゾル状態にある60~90℃の原料スラリーを基材上に伸展させる工程、
伸展させた原料スラリーを0~40℃の試料温度に冷却してゲル化させる工程、および
ゲル化した原料を加熱して、70~100℃の試料温度で乾燥させることを含む加熱乾燥工程
を含むことを特徴とする喫煙物品用香料含有シートの製造方法。 - 前記乳化剤が、多糖類に対して0.5~5重量%のレシチンであることを特徴とする、請求項1記載の喫煙物品用香料含有シートの製造方法。
- 前記乳化剤が、グリセリン脂肪酸エステル、ポリグリセリン脂肪酸エステル、ソルビタン脂肪酸エステル、プロピレングリコール脂肪酸エステルおよびショ糖脂肪酸エステルからなる群より選択されるエステルであることを特徴とする、請求項2記載の喫煙物品用香料含有シートの製造方法。
- 前記多糖類が、原料スラリー中に2~6重量%の濃度で含有されることを特徴とする、請求項1~3の何れか1項記載の喫煙物品用香料含有シートの製造方法。
- 前記香料がメンソールであることを特徴とする請求項1~4の何れか1項記載の香料含有シートの製造方法。
- 前記メンソールの含有量が、多糖類に対して250~500重量%の範囲にあることを特徴とする、請求項5記載の喫煙物品用香料含有シートの製造方法。
- 請求項1~4の何れか1項記載の方法により製造されることを特徴とする喫煙物品用香料含有シート。
- 請求項5または6記載の方法により製造されることを特徴とする喫煙物品用香料含有シート。
- 製造後のシートにおけるメンソール含有量が45重量%以上であり、50℃で30日間蔵置した後のシートにおけるメンソール含有量が45重量%以上であることを特徴とする請求項8記載の喫煙物品用香料含有シート。
- タバコ刻みを含む喫煙物品であって、前記タバコ刻みに、請求項7~9の何れか1項記載の喫煙物品用香料含有シートの裁刻物が配合されていることを特徴とする喫煙物品。
- タバコ刻みおよび該タバコ刻みの周囲を巻装するシガレット巻紙を含むタバコロッドを備えたシガレットであって、前記タバコ刻みに、請求項7~9の何れか1項記載の喫煙物品用香料含有シートの裁刻物が配合されていることを特徴とするシガレット。
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EP12751885.0A EP2682007B1 (en) | 2011-03-02 | 2012-02-27 | Method for producing fragrance-containing sheet for smoking article |
KR1020137023165A KR101539158B1 (ko) | 2011-03-02 | 2012-02-27 | 끽연 물품용 향료 함유 시트의 제조방법, 그 방법에 의해 제조되는 끽연 물품용 향료 함유 시트, 및 그것을 포함하는 끽연 물품 |
CA2826425A CA2826425C (en) | 2011-03-02 | 2012-02-27 | Method for preparing flavor-containing sheet for smoking article, flavor-containing sheet for smoking article prepared by the method, and smoking article comprising the same |
RU2013144225/12A RU2565660C2 (ru) | 2011-03-02 | 2012-02-27 | Способ получения содержащего ароматизатор листа для изделия для курения, лист для изделия для курения, содержащий ароматизатор, полученный данным способом, и содержащее его изделие для курения |
ES12751885T ES2705165T3 (es) | 2011-03-02 | 2012-02-27 | Método para producir una hoja que contiene fragancia para artículo para fumar |
CN201280019148.9A CN103561596B (zh) | 2011-03-02 | 2012-02-27 | 用于吸烟物品的含香料片材的制造方法、通过该方法制造的用于吸烟物品的含香料片材及包含该片材的吸烟物品 |
JP2013502344A JP5514952B2 (ja) | 2011-03-02 | 2012-02-27 | 喫煙物品用香料含有シートの製造方法、該方法により製造される喫煙物品用香料含有シート、およびそれを含む喫煙物品 |
UAA201311600A UA106850C2 (uk) | 2011-03-02 | 2012-02-27 | Спосіб одержання листа для виробу для куріння, який містить ароматизатор, лист для виробу для куріння, який містить ароматизатор, одержаний даним способом, і виріб для куріння, який містить його |
US13/963,653 US9526271B2 (en) | 2011-03-02 | 2013-08-09 | Method for preparing flavor-containing sheet for smoking article, flavor-containing sheet for smoking article prepared by the method, and smoking article comprising the same |
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JP2011-045290 | 2011-03-02 | ||
JP2011045290 | 2011-03-02 |
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US13/963,653 Continuation US9526271B2 (en) | 2011-03-02 | 2013-08-09 | Method for preparing flavor-containing sheet for smoking article, flavor-containing sheet for smoking article prepared by the method, and smoking article comprising the same |
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PCT/JP2012/054826 WO2012118032A1 (ja) | 2011-03-02 | 2012-02-27 | 喫煙物品用香料含有シートの製造方法、該方法により製造される喫煙物品用香料含有シート、およびそれを含む喫煙物品 |
PCT/JP2012/054828 WO2012118034A1 (ja) | 2011-03-02 | 2012-02-27 | 喫煙物品用香料含有シートの製造方法、該方法により製造される喫煙物品用香料含有シート、およびそれを含む喫煙物品 |
PCT/JP2012/054827 WO2012118033A1 (ja) | 2011-03-02 | 2012-02-27 | 喫煙物品用香料含有シートの製造方法、該方法により製造される喫煙物品用香料含有シート、およびそれを含む喫煙物品 |
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PCT/JP2012/054828 WO2012118034A1 (ja) | 2011-03-02 | 2012-02-27 | 喫煙物品用香料含有シートの製造方法、該方法により製造される喫煙物品用香料含有シート、およびそれを含む喫煙物品 |
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US (3) | US9622508B2 (ja) |
EP (3) | EP2682007B1 (ja) |
JP (3) | JP5514953B2 (ja) |
KR (3) | KR101539158B1 (ja) |
CN (3) | CN103501641B (ja) |
CA (3) | CA2826382C (ja) |
ES (3) | ES2731724T3 (ja) |
MY (3) | MY156848A (ja) |
RU (3) | RU2553045C2 (ja) |
TW (3) | TWI483687B (ja) |
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