WO2012023178A1 - Filtre de cigarette et son procédé de fabrication - Google Patents

Filtre de cigarette et son procédé de fabrication Download PDF

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Publication number
WO2012023178A1
WO2012023178A1 PCT/JP2010/063877 JP2010063877W WO2012023178A1 WO 2012023178 A1 WO2012023178 A1 WO 2012023178A1 JP 2010063877 W JP2010063877 W JP 2010063877W WO 2012023178 A1 WO2012023178 A1 WO 2012023178A1
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Prior art keywords
menthol
filter
acetate
cigarette filter
amount
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PCT/JP2010/063877
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English (en)
Japanese (ja)
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正人 宮内
綾子 知久
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日本たばこ産業株式会社
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Priority to PCT/JP2010/063877 priority Critical patent/WO2012023178A1/fr
Publication of WO2012023178A1 publication Critical patent/WO2012023178A1/fr

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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
    • A24D3/06—Use of materials for tobacco smoke filters
    • A24D3/062—Use of materials for tobacco smoke filters characterised by structural features
    • A24D3/063—Use of materials for tobacco smoke filters characterised by structural features of the fibers
    • A24D3/064—Use of materials for tobacco smoke filters characterised by structural features of the fibers having non-circular cross-section

Definitions

  • the present invention relates to a cigarette filter added with a fragrance and a method for producing the same.
  • Patent Document 1 discloses a filter in which a perfumed solution in which menthol is dissolved and dispersed in a plasticizer used in a filter plug manufacturing process is added to acetate tow, and a method for manufacturing the filter. In this method, a sucrose higher fatty acid ester is contained in the perfumed liquid. It is described that with such a simple aromatizing operation, there is little volatilization of perfume added during storage, good perfume retention, and the perfume can be continuously released to the smoke passing through the filter during smoking.
  • a fragrance such as menthol remains as a sticky or gelled solid solution on the filter depending on the properties of the higher fatty acid ester of sucrose, and the fragrance is less likely to volatilize from the filter and the fragrance retention is improved.
  • the amount of menthol released from the filter into the smoke decreases over time.
  • storing the product under temperature conditions in a summer vending machine may reduce the amount of release from the filter.
  • the amount of menthol in the smoke of the menthol product decreases and the flavor of the menthol product is impaired.
  • a menthol scented filter was made as a trial as follows.
  • a fragrance solution was prepared by dissolving 27% of menthol in triacetin as a plasticizer.
  • a fragrance liquid heated to about 40 ° C. is added so that the triacetin content is 6 wt%, and the menthol content per filter length of 25 mm is 3 mg.
  • a menthol scented filter was obtained. The obtained menthol-scented filter and a cigarette rod (for 7-star menthol) that had not been scented with menthol were wound up and packaged in a soft pack to prepare a sample product.
  • the obtained sample products were stored under temperature conditions of 22 ° C. (conditioning room) and 55 ° C., collected every predetermined period, smoked under ISO smoking conditions, and the amount of menthol in the smoke was measured.
  • Smoking conditions were such that the puff frequency was once per 60 seconds, the puff was 2 seconds, and the puff volume was 35 mL.
  • Menthol collected by the Cambridge filter was extracted with methanol and quantified using a gas chromatograph GC (HEWLETT PACKARD, 6890 series).
  • the menthol scented filter prepared as described above was put in a sealed pack and stored under temperature conditions of 22 ° C. (conditioning room) and 55 ° C.
  • the menthol scented filter was taken out every predetermined period and replaced with a commercially available mild seven superlite filter part to prepare a cigarette sample.
  • the filter opening was covered with tape, and smoked under ISO smoking conditions as described above, and the amount of menthol in the smoke was measured.
  • Fig. 1 shows the change over time in the amount of menthol cigarette smoke.
  • Triangles indicate the results of cigarettes using a filter stored at 22 ° C.
  • circles indicate the results of cigarettes using a filter stored at 55 ° C. From these results, the amount of menthol in the smoke of the menthol cigarette decreases with time even when the cigarette is stored at 22 ° C., and particularly when the cigarette is stored at a high temperature of 55 ° C.
  • Fig. 2 shows the change over time in the amount of menthol released from the filter.
  • the amount of menthol release from the filter decreased with time, and a significant decrease was observed as the temperature increased. Therefore, it was found that the decrease in the amount of menthol in the smoke of the menthol cigarette was caused by the decrease in the amount of menthol released from the filter.
  • menthol is said to be due to the fact that to penetrate the acetate fiber deep (Wilson, S.A., Theoretical aspects of menthol migration and transfer, 47 th Tobacco Chemist 'Reserch Conference, 1993, Gatlinburg). Recently, it has been found that the menthol distribution in acetate fibers can be measured by utilizing the high spatial resolution and two-dimensional Raman mapping function of the microscope laser Raman system.
  • the filter was stored under various conditions, and the menthol distribution in the acetate fiber was examined.
  • a filter for Mild Seven Impact One Menthol Box was prepared and stored for 2.5 months at 22 ° C. (conditioning room), 8 months at 22 ° C., or 7 days at 55 ° C.
  • a Raman two-dimensional surface analysis was performed using a Nicolet Armager Raman spectrometer (Nicolet TM Almega TM XR, Thermo Fisher Scientific Inc., Waltham, Massachusetts), and menthol in the acetate fiber constituting the filter. Distribution was measured. Data was measured with an exposure time of 1 second, an exposure count of 2 times, and a background exposure count of 512.
  • an optical microscope observation image of the acetate fiber constituting each filter was taken. Based on the 2943 cm ⁇ 1 peak derived from the acetate base of the Raman spectrum, the cross-sectional appearance of the acetate fiber was obtained as a chemical image. Based on the intensity ratio of the peak at 912cm -1 derived peak and acetate substrate 769cm -1 from menthol Raman spectra, to obtain a distribution of menthol in the cross section of the acetate fiber as a chemical image. By using the intensity ratio of the two peaks, the influence of disturbance can be reduced.
  • the distribution of menthol in the acetate fiber was as follows according to the storage conditions. In the filter stored at 22 ° C. for 2.5 months, menthol was unevenly distributed on the acetate fiber surface. In the filter stored at 22 ° C. for 8 months, menthol penetrated deep into the acetate fibers. It was found that the menthol was uniformly distributed in the acetate fiber in the filter stored at 55 ° C. for 7 days (filter that received a thermal history).
  • An object of the present invention is to provide a cigarette filter that can stabilize the release amount of the fragrance from the fragrance added fragrance filter into the smoke when the cigarette is stored, and a method for manufacturing the cigarette filter.
  • a cigarette filter in which acetate tow, which is a bundle of acetate fibers, is formed, and a fragrance is unevenly distributed in the surface region of the acetate fibers.
  • the acetate tow which is a bundle of acetate fibers, is dissolved in a poor solvent for the acetate fibers and brought into contact with an aroma solution, and the acetate tow is formed into a cigarette filter.
  • a method for producing a cigarette filter is provided.
  • FIG. 1 is a graph showing a change with time of the amount of menthol in smoke of a menthol cigarette.
  • FIG. 2 is a diagram showing the change with time of the amount of menthol release from the filter.
  • FIG. 3 is a schematic view of a cross section of an acetate fiber forming a cigarette filter according to the present invention.
  • FIG. 4 is a graph showing the relationship between the menthol release efficiency from the filter and the menthol thermal desorption rate in a low temperature range (up to 40 ° C.).
  • FIG. 5 is a graph showing the change over time in the menthol sorption rate when menthol is sorbed onto an acetate film using various solvents.
  • FIG. 6 is a graph showing menthol thermal desorption rates up to 40 ° C.
  • FIG. 7 is a graph showing menthol release efficiency from an acetate filter in which menthol is sorbed using various solvents.
  • FIG. 8 is a diagram showing the filter inlet temperature when smoking the Mild Seven Superlight.
  • FIG. 9 shows the ratio D 22 / D 40 of the menthol thermal desorption rate D 22 at 22 ° C. to the menthol thermal desorption rate D 40 up to 40 ° C. with respect to acetate fibers sorbed with menthol using various solvents.
  • FIG. FIG. 10 is a configuration diagram of a filter hoist used for trial manufacture of the filter.
  • FIG. 11 is a diagram showing the menthol release efficiency from the filter sample under each storage condition.
  • FIG. 12 shows (a) before start of storage, (b) after storage at 22 ° C. for 12 days, (c) after storage at 40 ° C. for 9 days, (d) after storage at 55 ° C. for 7 days, (e) at 22 ° C.
  • FIG. 13 shows (a) before storage start, (b) after storage at 22 ° C. for 12 days, (c) after storage at 40 ° C. for 9 days, (d) after storage at 55 ° C. for 7 days, (e) at 22 ° C.
  • Patent Document 1 menthol is easily left in an adhesive or gelled solid solution produced by adding a higher fatty acid ester of sucrose.
  • triacetin which is a good solvent for acetate
  • Patent Document 1 does not describe the menthol distribution according to the temperature condition for storing the cigarette or the release amount stabilization from the filter. Further, since the menthol is left in the adhesive body or the gelled solid solution, an increase in the amount of menthol in the smoke of the initial puff cannot be expected.
  • the change with time of menthol in smoke in menthol products is due to the penetration of menthol into the deep part of acetate fiber in the market distribution stage of the product. As described above, the penetration of menthol into the deep part of the acetate fiber is due to equilibrium and proceeds naturally.
  • menthol can be unevenly distributed in the surface region of acetate fiber by aromatizing menthol using a poor solvent of acetate which has low affinity with acetate fiber and does not penetrate inside of acetate fiber. It was. Since the poor solvent for acetate does not penetrate into the deep part of the acetate fiber and is unevenly distributed in the surface region of the acetate fiber, menthol is also unevenly distributed in the surface region of the acetate fiber.
  • menthol can be effectively released from the acetate fibers forming the filter even near room temperature, the change in the amount of menthol released from the filter with time can be reduced, the amount of menthol in the smoke can be stabilized over time, and the smoke of the initial puff An increase in the amount of medium menthol can be achieved simultaneously.
  • FIG. 3 shows a schematic diagram of a cross section of acetate fibers forming the cigarette filter according to the present invention. As shown in FIG. 3, menthol is unevenly distributed along with the poor solvent of acetate on the surface region 2 of the acetate fiber 1.
  • Examples of the menthol scenting method in the acetate filter manufacturing process include a method of adding a plasticizer (triacetin) addition mechanism and a scent solution in which menthol is dissolved in a poor solvent to the acetate filter.
  • a method of adding the fragrance liquid to the acetate filter a method of directly injecting the fragrance liquid into the acetate filter using a nozzle, a method of spraying the fragrance liquid onto the acetate filter, a felt impregnated with the fragrance liquid in the acetate The method of attaching to a filter is mentioned.
  • the thread may be impregnated with a perfume solution in which menthol is dissolved in a poor solvent to produce an acetate filter containing the thread.
  • a suitable acetate poor solvent can be selected based on the solubility parameter (SP).
  • SP solubility parameter
  • the solubility parameter is used as an index of the ease of mutual dissolution of substances. The closer the solubility parameters of the two substances are, the more easily the two substances are soluble in each other. Two substances with similar solubility parameters show similar solubility for substances with different solubility parameters.
  • examples of preferred acetate poor solvents in the present invention include medium chain fatty acid triglycerides (MCT), while polyethylene glycol and liquid paraffin have been found to be undesirable solvents.
  • MCT medium chain fatty acid triglycerides
  • solubility parameters of various solvents will be exemplified.
  • solubility parameter ⁇ t of liquid paraffin is calculated using Molecular Modeling Pro (version 6.0.1, ChemSW, Inc.), it is reported that it is 16.7 (MPa) 1/2 (Hasegawa, T., et al., J. Appl.Polym.Sci., 2010, 116 (3), 1710-1717).
  • the Hansen solubility parameter which is an extension of the Hildebrand solubility parameter ⁇ t, is represented by three terms ( ⁇ d, ⁇ p, ⁇ h): dispersibility, polarity, and hydrogen bonding.
  • ⁇ d, ⁇ p, ⁇ h dispersibility, polarity, and hydrogen bonding.
  • the Hildebrand solubility parameter ⁇ t obtained from the Hansen solubility parameter ( ⁇ d, ⁇ p, ⁇ h) is 19.82 (MPa) 1/2 for PEG400 and 17.27 for MCT, respectively. 36 (MPa) 1/2 .
  • the solubility parameter ⁇ t is 16.7 (MPa) greater than 1/2, are intended to be within the scope of 19.82 (MPa) of less than 1/2.
  • the solubility parameter can be determined by various methods. Specifically, a method for obtaining from the evaporation energy, a method for obtaining the solubility by mixing the substances, the degree of swelling, the shrinkage, the viscosity, the turbidity, and the like, and a method for calculating from the chemical structure (for example, Small's Method, Fedors method). Further, the solubility parameter is described as a physical property value in documents such as Polymer Data Handbook Fundamentals, 1996, Baifukan.
  • the fragrance release efficiency from the filter during smoking can be correlated with the thermal desorption rate of menthol in the low temperature range (up to 40 ° C.) measured by the thermal desorption method.
  • the menthol cigarette was made as a trial as follows. A commercially available menthol cigarette and mild seven superlight were each cut between a filter and a cigarette rod, and a cigarette sample in which the menthol cigarette filter and the mild seven superlight cigarette rod were connected with an adhesive tape was produced.
  • a filter having a triacetin content per weight of cellulose acetate tow of 0, 2, 6, or 9 wt% was trial manufactured.
  • the cellulose acetate used was 2.2Y40000.
  • Menthol was scented in the tobacco used in the Mild Seven One Menthol box.
  • the amount of menthol added to the cigarette was 6 mg / cigarette.
  • a menthol cigarette was manufactured by connecting the above filter to a tobacco rod.
  • Smoking experiments were conducted as follows. A 20-hook linear smoker (manufactured by Filtrona, SM400, ISO standard device) was used. As smoking conditions, the puff frequency was once per 60 seconds, the puff was 2 seconds, the puff volume was 35 mL, and the combustion length was 51 mm from the tip of the cigarette. The filter aperture was covered with tape for the experiment. Smoke was collected on the Cambridge filter, and after the smoking experiment, the Cambridge filter was extracted by shaking with methanol, and the amount of menthol in the mainstream smoke was measured by gas chromatograph GC (manufactured by HEWLETT PACKARD, 6890 series).
  • the filter of the menthol cigarette used for the smoking experiment was extracted with tweezers, extracted by shaking with methanol, and the remaining menthol content was measured by GC.
  • the measured amount of menthol in the smoke was divided by the total content of residual menthol in the filter and the amount of menthol in the smoke to obtain the release efficiency of menthol from the filter.
  • a thermal detachment experiment of menthol was performed as follows.
  • the filter of the menthol cigarette used in the smoking experiment was extracted with tweezers and defibrated, and 16 mg of acetate fiber was collected and filled into a glass tube.
  • the glass tube filled with the acetate fiber was attached to a Thermal Destruction System (manufactured by GERSTEL), and the acetate fiber filled in the tube was heated according to a temperature raising program while flowing a carrier gas (He).
  • He carrier gas
  • the component desorbed from the acetate fiber was collected by a trap kept at a low temperature of ⁇ 50 ° C. through a flow path heated to 200 ° C.
  • the temperature of the tube was finished, the trap was rapidly heated to 270 ° C.
  • the trap component was separated by a separation column and analyzed by gas chromatography mass spectrometry GC / MS (manufactured by Agilent Technologies, GC: 7890A, MS: 5975C).
  • the peak area of menthol in GC corresponds to the thermal desorption amount of menthol.
  • the temperature increase and analysis procedures used in the above thermal desorption experiment were as follows. An operation in which the acetate fiber is held at a predetermined constant temperature for 30 minutes to remove the trap component and then GC analysis is performed is performed at a temperature of 22 ° C, 40 ° C, 60 ° C, 80 ° C, 120 ° C, 160 ° C, or 200 ° C. Repeated to set. The thermal desorption amount of menthol at each temperature was an integrated value of the thermal desorption amount at each temperature up to that temperature.
  • the filter after thermal desorption analysis was extracted by shaking with methanol, and the menthol remaining in the filter was quantified by GC. From the obtained thermal desorption data, the thermal desorption rate of menthol in the low temperature range (up to 40 ° C.) is calculated by the following equation.
  • D 40 is the menthol thermal desorption rate [%] in the low temperature range (up to 40 ° C.)
  • a 40 is the GC peak area integrated value up to 40 ° C. [ ⁇ ]
  • a 200 is the GC peak up to 200 ° C. Area integrated value [ ⁇ ]
  • D 200 is menthol thermal desorption rate up to 200 ° C. [%]
  • R is menthol residual amount [mg] in 16 mg of acetate fiber after thermal desorption
  • T is acetate before thermal desorption
  • the menthol content T [mg] in 16 mg of acetate fiber before heat desorption is calculated using the menthol content calculated from the menthol amount in the filter and the filter weight used when calculating the menthol release efficiency from the filter. Converted.
  • Fig. 4 shows the relationship between the menthol release efficiency from the filter and the menthol thermal desorption rate in the low temperature range (up to 40 ° C).
  • the menthol release efficiency from the filter correlates with the menthol thermal desorption rate in the low temperature range obtained from the thermal desorption experiment. Therefore, it can be seen that the amount of menthol release from the filter can be predicted by the amount of thermal desorption (diffusion) from the filter. In the future, instead of measuring the efficiency of menthol release from the filter, it was found that the thermal desorption rate of menthol in the low temperature range by thermal desorption experiments can be adopted as a simple measurement method.
  • the menthol release rate from the filter that is, the menthol detachment rate in the low temperature range
  • Cellulose acetate flakes (manufactured by Daicel Corporation, L-40) are dissolved in acetone (made by Wako Pure Chemical Industries, reagent special grade) to a concentration of 2 w / v%, and 9.5 wt% triacetin with respect to the acetate there. Was dissolved. 2 mL of the resulting acetone solution was cast into a glass petri dish with an inner diameter of 27 mm, and left in an acetone atmosphere at room temperature for 5 days to slowly evaporate acetone slowly and further dried under reduced pressure at room temperature overnight to produce cellulose. An acetate film was prepared. Acetone was volatilized as follows.
  • a gas displacement desiccator manufactured by ASONE
  • five 100 mL tall beakers containing 30 mL of acetone are arranged, and four glass petri dishes obtained by casting the above cellulose acetate solution are arranged around these tall beakers, and a 1000 mL beaker is arranged.
  • One set was placed on the upside down, and 9 sets were arranged on the plate.
  • the cellulose acetate film was peeled from the glass petri dish, and three films with an inner diameter of 8 mm were punched out to obtain film samples. Among the obtained film samples, those having a weight of 1.7 ⁇ 0.05 mg or 1.9 ⁇ 0.05 mg were subjected to the experiment.
  • the acetate film is taken out from the solution in the screw tube, and the solution adhering to the surface is wiped off, and divided into four parts with a stainless steel double-blade replacement blade, then these are put into a brown crimp vial, extracted with methanol, and a gas chromatograph (made by HEWLETT PACKARD). , 6890 series).
  • the solvents used in the experiment are as follows.
  • Medium chain triglyceride MCT manufactured by Kao Corporation, Coconut MT
  • ethanol manufactured by Wako Pure Chemical Industries, reagent special grade
  • propylene glycol PG manufactured by Wako Pure Chemical Industries, food additive
  • polyethylene glycol PEG200 (Wako Pure Chemical Industries, Ltd.)
  • reagent grade 1 Manufactured, reagent grade 1
  • polyethylene glycol PEG600 manufactured by Wako Pure Chemical Industries, reagent grade 1
  • liquid paraffin manufactured by Wako Pure Chemical Industries, reagent grade 1).
  • Table 1 shows the solvents used in the experiments, the storage period, and the film sample weight.
  • the menthol sorption rate Rm (wt%) per hour was calculated from the following formula using the weight of each acetate film sample weighed in advance after each storage period. .
  • Rm is the menthol sorption rate [wt%]
  • Wm is the menthol content [mg] in the acetate film
  • Wf is the weight [mg] of the acetate film.
  • FIG. 5 shows the change over time in the menthol sorption rate.
  • the sample using MCT as the solvent has a slower menthol sorption rate to the acetate film than the sample using other solvents, and may delay the penetration of menthol into the deep part of the acetate.
  • Tables 2-1 to 2-3 show the composition of the menthol solution used and the amount of the fragrance added.
  • the solvents used for the experiment are as follows.
  • Medium chain fatty acid triglyceride MCT manufactured by Kao Corporation, Coconut MT
  • ethanol manufactured by Wako Pure Chemical Industries, reagent special grade
  • propylene glycol PG manufactured by Wako Pure Chemical Industries, food additive.
  • M in Table 2 represents menthol.
  • the prepared filter sample was put in a sealed container and stored at room temperature for 42 days, or stored in a dryer (ADVANTEC FS-320) at 55 ° C. for 7 days and then stored at room temperature for 35 days.
  • the above filter sample was subjected to Raman two-dimensional surface analysis using a Nicolet Almega Raman spectrometer (Nicolet TM Almega TM XR, Thermo Fisher Scientific Inc., Waltham, Massachusetts), and the menthol distribution within the acetate fiber cross section was analyzed. It was measured. Separately, an optical microscope observation image of the acetate fiber constituting each filter was taken. Details of the measurement are as described above.
  • Results for filter samples stored for 42 days at room temperature are as follows. In the sample using MCT or ethanol as the solvent, menthol was unevenly distributed in the surface region of the acetate fiber. In the sample using PG as the solvent, menthol penetrated deep into the acetate fiber.
  • Results for filter samples stored at 55 ° C. for 7 days and then stored at room temperature for 35 days are as follows.
  • menthol was unevenly distributed in the surface region of the acetate fiber.
  • menthol was uniformly distributed in the acetate fiber.
  • Tables 3-1 to 3-3 show the composition of the menthol solution used and the amount of the fragrance added.
  • the solvents used for the experiment are as follows.
  • Medium chain fatty acid triglyceride MCT manufactured by Kao Corporation, Coconut MT
  • ethanol manufactured by Wako Pure Chemical Industries, reagent special grade
  • propylene glycol PG manufactured by Wako Pure Chemical Industries, food additive.
  • M in Table 3 represents menthol.
  • the method for preparing the filter sample is as follows. A menthol solution using ethanol or PG as a solvent was applied to the end face of the filter with a micropipette. From the result of (2) above, it was found that when menthol solution using MCT as a solvent was applied to the end face of the filter, menthol was unevenly distributed in the surface area of the acetate fiber, but uneven distribution due to uneven application of menthol solution. It is also possible that this occurred.
  • a menthol solution using MCT as a solvent is equipped with a conduit having a cellulose acetate filter inserted at the outlet of the atomizer using an atomizer (Model 9302, manufactured by TSI, Minnesota (USA)) Spraying was continued for 45 seconds at an introduction pressure of 20 psi.
  • a menthol / MCT solution having a weight ratio of 1: 2 viscosity was 18 cp
  • the amount of the fragrance added was 23 ⁇ L per filter (diameter 8 mm, length 25 mm).
  • the prepared filter sample was put in a sealed container and stored at 55 ° C. for 7 days, and subjected to a thermal desorption experiment.
  • the thermal desorption experiment was performed as follows.
  • the filter sample was defibrated, and 16 mg of acetate fiber was collected and filled into a glass tube.
  • a glass tube filled with acetate fibers was attached to TDS (manufactured by GERSTEL), and the acetate fibers filled in the tubes were heated according to a temperature raising program while flowing a carrier gas (He).
  • He carrier gas
  • the component desorbed from the acetate fiber was collected by a trap kept at a low temperature of ⁇ 50 ° C. through a flow path heated to 200 ° C.
  • the temperature of the tube was finished, the trap was rapidly heated to 270 ° C.
  • the trap component was separated by a separation column and analyzed by gas chromatography mass spectrometry GC / MS (manufactured by Agilent Technologies, GC: 7890A, MS: 5975C).
  • the peak area of menthol in GC corresponds to the thermal desorption amount of menthol.
  • the temperature increase and analysis procedures used in the thermal desorption experiment were as follows. The operation of GC analysis after holding the filter acetate fiber at a predetermined constant temperature for 30 minutes to desorb the trap component was repeated by setting the temperature to 22 ° C., 40 ° C., 80 ° C., or 200 ° C. The thermal desorption amount of menthol at each temperature was an integrated value of the thermal desorption amount at each temperature up to that temperature.
  • FIG. 6 shows the menthol thermal desorption rate up to 40 ° C. from the acetate fiber. From FIG. 6, it can be seen that the menthol thermal desorption rate up to 40 ° C. from the acetate fiber is larger when MCT is used as a solvent than when ethanol or PG is used. Therefore, if MCT is used as the solvent, the amount of menthol diffused from the acetate fiber can be stabilized even after a thermal history of 55 days at 55 ° C., that is, the temporal stability of the amount of menthol in smoke can be improved even under summer conditions. Recognize.
  • the prepared filter sample was put in an airtight container and stored for 3 days at 22 ° C. and a relative humidity of 60%, or stored in a dryer at 55 ° C. for 7 days.
  • a cigarette was prepared by attaching a filter sample to a tobacco rod obtained by removing a filter from a cigarette (mild seven super light).
  • Smoking experiments were conducted as follows. A 20-hook linear smoker (manufactured by Filtrona, SM400, ISO standard device) was used. As smoking conditions, the puff frequency was once per 60 seconds, the puff was 2 seconds, the puff volume was 35 mL, and the combustion length was 51 mm from the tip of the cigarette. The filter aperture was covered with tape for the experiment. Smoke was collected on the Cambridge filter, and after the smoking experiment, the Cambridge filter was extracted by shaking with methanol, and the amount of menthol in the mainstream smoke was measured by gas chromatograph GC (manufactured by HEWLETT PACKARD, 6890 series).
  • a filter sample of menthol cigarette subjected to a smoking experiment was extracted with tweezers and extracted by shaking with methanol, and the menthol content remaining in the filter was measured by GC (6890 series, manufactured by HEWLETT PACKARD). The measured amount of menthol in the smoke was divided by the sum of the residual menthol content in the filter sample and the amount of menthol in the smoke to obtain the release efficiency of menthol from the filter sample.
  • Figure 7 shows the menthol release efficiency from the filter sample. From FIG. 7, the sample using MCT as the solvent has a higher menthol release efficiency from the filter sample even after undergoing a thermal history of storage at 55 ° C. for 7 days as compared with the sample using other solvents. This can be interpreted as the stabilization of the diffusion amount of menthol from the acetate fiber into the smoke by suppressing the penetration of menthol into the deep part of the acetate fiber. Therefore, according to the present invention, the amount of menthol delivery can be stabilized.
  • FIG. 8 shows the result of measuring the filter inlet temperature when the filter opening was sealed with tape using Mild Seven Superlite and smoked under the same smoking conditions as in (4) Indicates.
  • FIG. 8 shows that the filter temperature is around room temperature up to the fourth puff.
  • the menthol thermal desorption rate up to 40 ° C. is proportional to the menthol release rate from the filter. For this reason, when the ratio of the menthol thermal desorption rate D 22 at 22 ° C. to the menthol thermal desorption rate D 40 up to 40 ° C. is used as an index, thermal desorption (diffusion) of menthol released from the filter near room temperature. The amount can be compared.
  • the menthol thermal desorption rate D 22 at 22 ° C. is divided by the menthol thermal desorption rate D 40 up to 40 ° C.
  • the value of the obtained ratio D 22 / D 40 is shown in FIG. From FIG. 9, it can be seen that the sample using MCT as the solvent has a higher value of D 22 / D 40 than the sample using other solvents. Therefore, if filter aromatization is performed using MCT as a solvent, an increase in the amount of menthol in the smoke of the initial puff can be expected.
  • FIG. 10 shows the configuration of the filter hoist used for trial production of a filter to be used in the experiment.
  • the acetate tow 10 is opened through a banding jet (BJ) 11, a transport roll 12, a pretension roll (PTR) 13, a groove roll (GR) 14, and a banding jet (BJ) 15, and then passed through a deli berry roll (DR) 16. After being fed and formed into a filter shape by the transport jet 17 and the trumpet guide 18, it is wound up by a hoisting machine 19.
  • BJ banding jet
  • PTR pretension roll
  • GR groove roll
  • BJ banding jet
  • a menthol solution in which menthol is dissolved in a poor solvent of acetate fibers is scented by spraying using a two-fluid nozzle 22.
  • rail paste is applied from the applicator 23 and wrap paste is applied from the applicator 24.
  • the tow spec used was 3.5Y30000, and winding was performed at a winding speed of 500 plugs / piece.
  • Tables 6-1 to 6-3 show the composition of the menthol solution and the menthol content in the filter trial product.
  • a filter of mild seven aqua super light box (commercial product) was also used for the experiment.
  • the menthol content in the filter was quantified using GC (6890 series, manufactured by HEWLETT PACKARD) after cutting the filter into 25 mm lengths, extracting with shaking with methanol.
  • the prototype menthol filter was cut to a length of 25 mm. Also, the menthol cigarette (mild seven aqua menthol super light box) filter was removed to obtain a tobacco rod. A menthol cigarette sample was prepared by attaching the trial menthol filter to a tobacco rod. A menthol cigarette sample was stored in a screw tube.
  • a smoking experiment was conducted as follows.
  • a 20-fold rotary smoker (RM20D, ISO standard) was used.
  • the puff frequency was once per 60 seconds
  • the puff was 2 seconds
  • the puff volume was 35 mL
  • the combustion length was 51 mm from the tip of the cigarette.
  • the filter aperture was covered with tape for the experiment.
  • Smoke was collected on the Cambridge filter, and after the smoking experiment, the Cambridge filter was extracted by shaking with methanol, and the amount of menthol in the mainstream smoke was measured by gas chromatograph GC (manufactured by HEWLETT PACKARD, 6890 series).
  • the menthol release amount for each puff was measured by replacing the Cambridge filter for each puff.
  • the filter was taken out from the sample husk after completion of the smoking experiment, extracted by shaking with methanol, and the menthol content remaining in the filter was measured by GC (HEWLETT PACKARD, 6890 series).
  • the filter sample was defibrated, 16 mg of acetate fiber was collected, filled in a glass tube, and measured using TDS (manufactured by GERSTEL).
  • TDS manufactured by GERSTEL
  • the temperature increase and analysis procedures used in the thermal desorption experiment were as follows. The operation of GC analysis after holding the filter acetate fiber at a predetermined constant temperature for 30 minutes to desorb the trap component was repeated by setting the temperature to 22 ° C., 40 ° C., 80 ° C., or 200 ° C. The thermal desorption amount of menthol at each temperature was an integrated value of the thermal desorption amount at each temperature up to that temperature.
  • (6A) Temporal change in the amount of menthol in smoke Release of menthol from the filter sample by dividing the measured amount of menthol in the smoke by the sum of the residual menthol content in the filter sample after the smoking experiment and the amount of menthol in the smoke The efficiency.
  • Fig. 11 shows the menthol release efficiency from the filter sample under each storage condition.
  • a sample using MCT or a mixed solvent of MCT and ethanol as a solvent has a higher menthol release efficiency from a filter than a commercial product under all storage conditions.
  • a sample using MCT or a mixed solvent of MCT and ethanol as a solvent has a higher menthol release efficiency from the filter than a sample using PG as a solvent under a high storage temperature of 40 ° C. or 55 ° C.
  • the sample using MCT as the solvent had a menthol release efficiency 1.6 times that of the sample using PG as the solvent. Therefore, it can be seen that the use of MCT as a solvent can improve the temporal stability of the amount of menthol in smoke even under summer conditions.
  • FIGS. 12 (a) to 12 (e) show the ratio of the menthol release amount for each puff divided by the amount of menthol in smoke per smoke.
  • FIGS. 13A to 13E show the menthol desorption rate from the filter up to each temperature obtained from the thermal desorption experiment.
  • the sample using MCT as the solvent has a larger amount of menthol release from the filter in the initial puff up to 3 times of puffing than the other samples. I understand that.
  • the sample using MCT as the solvent has a higher menthol desorption rate from the filter at 22 ° C. than the other samples.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Cigarettes, Filters, And Manufacturing Of Filters (AREA)

Abstract

L'invention porte sur un filtre de cigarette qui est fabriqué par moulage de boudins de filasse qui sont des touffes de fibres d'acétate, et qui est caractérisé en ce qu'un agent aromatisant est situé de manière inégale sur les régions de surface des fibres d'acétate.
PCT/JP2010/063877 2010-08-17 2010-08-17 Filtre de cigarette et son procédé de fabrication WO2012023178A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/JP2010/063877 WO2012023178A1 (fr) 2010-08-17 2010-08-17 Filtre de cigarette et son procédé de fabrication

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/JP2010/063877 WO2012023178A1 (fr) 2010-08-17 2010-08-17 Filtre de cigarette et son procédé de fabrication

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WO2012023178A1 true WO2012023178A1 (fr) 2012-02-23

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2015525079A (ja) * 2012-07-25 2015-09-03 セラニーズ アセテート，エルエルシー ３弧孔を含む紡糸口金およびそれから製造された３弧フィラメント

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4826239B1 (fr) * 1970-10-29 1973-08-07
JPH05115274A (ja) * 1990-07-09 1993-05-14 Kimberly Clark Corp タバコの風味がするタバコ用フイルターの製造方法
JP2003530866A (ja) * 2000-04-20 2003-10-21 フィリップ・モーリス・プロダクツ・インコーポレイテッド 香味剤物質で含浸された成形マイクロキャビティ繊維の紙巻たばこフィルター
JP2005160435A (ja) * 2003-12-04 2005-06-23 Ogawa & Co Ltd 糖衣掛け方法並びにそれに用いられる乳化香料及びシロップ
WO2006082748A1 (fr) * 2005-02-02 2006-08-10 Daicel Chemical Industries, Ltd. Materiau pour filtre a cigarette et filtre a cigarette
JP2007070534A (ja) * 2005-09-08 2007-03-22 Daicel Chem Ind Ltd 酢酸セルロース組成物
JP2007217308A (ja) * 2006-02-14 2007-08-30 Kobayashi Pharmaceut Co Ltd 口中清涼化組成物

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4826239B1 (fr) * 1970-10-29 1973-08-07
JPH05115274A (ja) * 1990-07-09 1993-05-14 Kimberly Clark Corp タバコの風味がするタバコ用フイルターの製造方法
JP2003530866A (ja) * 2000-04-20 2003-10-21 フィリップ・モーリス・プロダクツ・インコーポレイテッド 香味剤物質で含浸された成形マイクロキャビティ繊維の紙巻たばこフィルター
JP2005160435A (ja) * 2003-12-04 2005-06-23 Ogawa & Co Ltd 糖衣掛け方法並びにそれに用いられる乳化香料及びシロップ
WO2006082748A1 (fr) * 2005-02-02 2006-08-10 Daicel Chemical Industries, Ltd. Materiau pour filtre a cigarette et filtre a cigarette
JP2007070534A (ja) * 2005-09-08 2007-03-22 Daicel Chem Ind Ltd 酢酸セルロース組成物
JP2007217308A (ja) * 2006-02-14 2007-08-30 Kobayashi Pharmaceut Co Ltd 口中清涼化組成物

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2015525079A (ja) * 2012-07-25 2015-09-03 セラニーズ アセテート，エルエルシー ３弧孔を含む紡糸口金およびそれから製造された３弧フィラメント

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