WO2012004853A1

WO2012004853A1 - Process for production of cigarette filter

Info

Publication number: WO2012004853A1
Application number: PCT/JP2010/061428
Authority: WO
Inventors: 比呂基志方; 正人宮内; 綾子知久
Original assignee: 日本たばこ産業株式会社
Priority date: 2010-07-05
Filing date: 2010-07-05
Publication date: 2012-01-12
Also published as: JP5478727B2; JPWO2012004853A1

Abstract

A process for producing a cigarette filter using an acetate tow or an acetate film, wherein a deep part of an acetate fiber that constitutes the acetate tow or the acetate film is impregnated with a flavoring agent.

Description

Cigarette filter manufacturing method

The present invention relates to a method for producing a cigarette filter in which a fragrance is added.

Conventionally, there has been known a fragrance-scented filter in which a fragrance solution in which a fragrance is dissolved and dispersed in a plasticizer used during a filter plug manufacturing process is added to acetate tow. For example, 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. Furthermore, it is described that fragrances such as menthol remain in the filter as a solid solution such as an adhesive or gel depending on the properties of the higher sucrose fatty acid ester, and the fragrance is less likely to volatilize from the filter, improving the fragrance retention. Yes.

Also, a fragrance added fragrance filter including a thread in which a filter plug is impregnated with a fragrance is known. For example, Patent Documents 2 and 3 disclose a manufacturing apparatus and a manufacturing method for a filter (mainly an acetate filter) including a thread impregnated with a fragrance. In these methods, the threads are aligned in order to efficiently switch fragrances and control the amount of fragrance released into the smoke.

For menthol products, the amount of menthol released from the filter into the smoke decreases over time. In particular, storing the product under temperature conditions in a summer vending machine may reduce the amount of release from the filter. As a result, it is known that the amount of menthol in the smoke of the menthol product decreases and the flavor of the menthol product is impaired.

Here, the experimental results relating to the change over time of the amount of menthol in the smoke are shown. 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. During the manufacturing process of the filter plug using the filter tow (4Y35000), 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. The menthol collected by the Cambridge filter was extracted with a methanol solvent and quantified using a gas chromatograph GC (6890 series manufactured by HEWLETT PACKARD).

In addition, the following experiment was conducted to determine the amount of menthol release from the filter. 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 filter part of a commercially available mild seven superlite to prepare a cigarette sample. The filter opening was covered with tape, and smoked under ISO smoking conditions in the same manner 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., and circles indicate the results of cigarettes using a filter stored at 55 ° C. From these results, the amount of menthol in the smoke of menthol cigarettes decreases with time even when the filter is stored at 22 ° C., and particularly when the filter 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.

Cause of menthol release amount from the filter is lowered, menthol is said to be due to the fact that to penetrate the acetate fiber deep (S.A.Wilson, 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.

Therefore, 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 1 week at 55 ° C. For each filter, a Raman two-dimensional surface analysis was performed using a Nicolet Armager Raman spectrometer (Nicolet ^™ Almega ^™ XR, Thermo Fisher Scientific Inc., Waltham, Massachusetts), and the menthol in the acetate fiber constituting the filter was analyzed. 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. The conditions of the optical system were as follows. Laser wavelength: 532 nm, laser output level: 100% (10 mW), grating: 672 lines / mm, spectrometer aperture: 50 μm pinhole, objective lens: 100 times (NA = 0.9). The map type was an area map, where the X direction step size was 1.0 μm and the Y direction step size was 1.0 μm.

Separately, 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 1 week (the filter subjected to the thermal history).

Therefore, as expected, it was revealed that the decrease in the amount of menthol released from the filter was due to the penetration of menthol into the deep part of the acetate fiber.

The method of dissolving menthol in triacetin of Patent Document 1 and the method of introducing threads impregnated with menthol of Patent Documents 2 and 3 are only for adding menthol to the filter, and within the acetate fiber It is not intended to control the distribution of menthol.

In Patent Document 1, since menthol is easily left as a solid solution such as an adhesive or a gel together with a higher fatty acid ester of sucrose, there is a possibility that a change with time in the distribution of menthol in acetate fibers may be suppressed. . However, the lipophilicity and surface active effects of sucrose fatty acid esters promote the adsorption of moisture-containing components, affecting the tobacco flavor. Further, the penetration of menthol into the deep part of the acetate fiber naturally proceeds toward equilibrium. For this reason, if the menthol is separated from the higher sucrose fatty acid ester and diffuses, it penetrates into the deep part of the filter fiber. Therefore, Patent Document 1 does not suggest stabilizing the amount of menthol released from the filter into the smoke when the cigarette is stored.

Japanese Patent Publication No.43-28077 US Pat. No. 4,281,671 U.S. Pat. No. 7,074,170

An object of the present invention is to provide a method for producing a cigarette filter capable of stabilizing the release amount of the fragrance from the fragrance added fragrance filter into the smoke when the cigarette is stored.

The method for producing a cigarette filter according to the present invention is characterized in that, in the method for producing a cigarette filter using an acetate tow or an acetate film, a perfume is permeated into a deep portion of the acetate fiber or acetate film constituting the acetate tow. A method for producing a cigarette filter.

The present invention includes a step of dissolving cellulose acetate in a solvent, spinning, crimping, dry packaging to produce acetate tow, a step of adding a plasticizer to the acetate tow and winding up to produce a filter plug; In addition, before spinning from the cellulose acetate solution, a perfume may be permeated into the deep part of the produced acetate fiber by adding a perfume to the cellulose acetate.

The present invention includes a step of dissolving cellulose acetate in a solvent, spinning, crimping, dry packaging to produce acetate tow, a step of adding a plasticizer to the acetate tow and winding up to produce a filter plug; The fragrance is added to the cellulose acetate during the period from spinning from the cellulose acetate solution to the production of the acetate tow, and the fragrance is diffused by heat treatment until the manufacturing process of the acetate filter plug is completed. And a method in which a perfume permeates into the deep part of the acetate fiber.

The present invention includes a step of dissolving cellulose acetate in a solvent, spinning, crimping, dry packaging to produce acetate tow, a step of adding a plasticizer to the acetate tow and winding up to produce a filter plug; And adding a fragrance when adding a plasticizer to the acetate tow, applying a heat treatment until the production process of the acetate filter plug is completed, diffusing the fragrance, and allowing the fragrance to penetrate deep into the acetate fiber The method may be used.

In the present invention, a solution is prepared by dissolving acetate flakes, plasticizer and fragrance in a solvent, an acetate film is prepared from the solution, and the fragrance is infiltrated into the deep portion of the acetate film, and a cigarette filter is prepared from the acetate film. It is possible to do it.

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 diagram showing a method for manufacturing 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 changes with time of the menthol distribution rate in the filter for Examples 1 and 2 and Comparative Example 1. FIG. FIG. 6 is a graph showing changes with time in the menthol desorption rate in the low temperature range for Examples 1 and 2 and Comparative Example 1. FIG. FIG. 7 is a graph showing changes in menthol content over time for Examples 3 and 4 and Comparative Example 2.

According to the method of the present invention, the perfume is permeated to the deep part of the acetate fiber in advance in the filter manufacturing stage. For this reason, the concentration gradient of the fragrance | flavor in an acetate fiber is gentle from the storage initial stage, the diffusion rate of the fragrance | flavor in an acetate fiber is slow also during storage, and the diffusion amount of the fragrance | flavor to the deep part of an acetate fiber also decreases. As a result, the temporal change in the amount of fragrance released from the filter into the smoke during storage is reduced. In addition, when fragrance is added to tobacco, the fragrance distributed from the tobacco to the filter during storage stays on the surface of the acetate fiber, so the change in the amount of fragrance released into the smoke is suppressed from the filter. Perfume release efficiency can be improved.

As described in Patent Document 1, for example, perfume fragrance in the filter manufacturing stage is performed simultaneously with the addition of a plasticizer (triacetin), but it is not allowed to permeate the fragrance deep into the acetate fiber. I have not been told. When a fragrance is added simultaneously with the addition of a plasticizer (triacetin), the speed at which the fragrance penetrates into the deep part of the acetate fiber slows down. Therefore, the fragrance is unevenly distributed on the surface of the acetate fiber after manufacturing the filter, Perfume penetrates.

FIG. 3 shows a method for manufacturing a cigarette filter according to the present invention. As shown in FIG. 3, the cigarette filter manufacturing method is divided into a cellulose acetate manufacturing process, a spinning process, and an acetate filter plug manufacturing process. In the cellulose acetate production process, cellulose acetate is produced by pretreatment, acetylation, aging, precipitation, and purification of cotton linter-dissolved pulp. In the spinning process, acetate tow is produced by mixing cellulose acetate flakes, dissolving in a solvent, filtering and defoaming, spinning, crimping, and dry packaging. In the acetate filter plug manufacturing process, an acetate filter plug is manufactured by tow treatment, plasticizer (triacetin) addition, grain addition, winding and winding.

In the present invention, for example, the following method is used to permeate the perfume into the deep part of the acetate fiber.

(1) In the spinning process, a fragrance is added to the cellulose acetate flakes to prepare an acetate raw material mixed with the fragrance. (2) In the spinning step, a fragrance is added to an acetone solvent that dissolves the acetate raw material. In the methods (1) and (2), the perfume can be infiltrated into the deep part of the acetate fiber through the subsequent steps.

(3) In the spinning step, a fragrance is dissolved in an oiling agent for wet spinning / film formation of acetate. (4) In the spinning process, the acetate tow is packed in a pallet together with the fragrance release material. In the methods (3) and (4), heat treatment (for example, storage at 55 ° C.) is applied to diffuse the fragrance until the manufacturing process of the acetate filter plug is completed, and the penetration of the fragrance into the deep portion of the acetate fiber is accelerated. It is preferable to do.

(5) In the acetate filter plug manufacturing process, a plasticizer containing a fragrance is added to acetate tow. Even in the method (5), it is preferable to accelerate the diffusion of the fragrance into the deep part of the acetate fiber by performing a heat treatment (for example, storage at 55 ° C.) until the manufacturing process of the acetate filter plug is completed. .

Next, the evaluation method of the fragrance release efficiency from the filter during smoking will be described. 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.

Commercially available Mild Seven Aqua Menthol One Box, Mild Seven One Menthol Box, Seven Star Light Menthol Box, Seven Star Light Menthol, Salem Light Box, Salem One Box Box, Salem Alaska Menthol, Marlborough Ice Mint Box, Marlborough Ultra Light Menthol Box, Marlborough Black Menthol Box, Marlborough Menthol Box, Marlborough Black Menthol One KS Box, Lark Ultra Menthol KS Box, Kent Ultra 1 KS Box, Kent Citric Menthol 1 Box, Cool purchased from dealer It was.

In addition, 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 and used for the test. Smoke was collected on the Cambridge filter, and after the smoking test, the Cambridge filter was extracted by shaking with a methanol solvent, and the amount of menthol in the mainstream smoke was measured with a gas chromatograph GC (6890 series manufactured by HEWLETT PACKARD).

Further, the filter of menthol cigarette subjected to the smoking test was extracted with tweezers and extracted with shaking with a methanol solvent, 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.

Meanwhile, a thermal detachment test of menthol was performed as follows. The filter of the menthol cigarette used for the smoking test was extracted with tweezers and defibrated, and 16 mg of filter fiber was collected and filled in a glass tube. The glass tube filled with the sample was attached to a Thermal Destruction System (manufactured by GERSTEL), and the sample filled in the tube was heated according to a temperature raising program while flowing a carrier gas (He). The component desorbed from the sample was collected by a trap maintained at a low temperature of −50 ° C. through a channel heated to 200 ° C. The temperature of the tube was finished, the trap was rapidly heated to 270 ° C. at 12 ° C./min, and the unseparated trap components were concentrated and introduced into the separation column. Next, 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 test were as follows. The operation of GC analysis after holding the sample at a predetermined constant temperature for 30 minutes to desorb the trap component is performed at a temperature of 22 ° C, 40 ° C, 60 ° C, 80 ° C, 120 ° C, 160 ° C, or 200 ° C. Set and repeated. The thermal desorption amount of menthol at each temperature is 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 a methanol solvent, 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.

Here, 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. [−], and 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 filter fiber after thermal desorption, T is filter before thermal desorption The menthol content [mg] in 16 mg of fiber. The menthol content T [mg] in 16 mg of the filter fiber before heat desorption is obtained by 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).

Commercial cigarettes were stored after purchase, and trial cigarettes (triacetin content 0-8 wt%) were stored under two conditions after trial production. The first condition was 22 ° C. and relative humidity (RH) 60%. In the second condition, a heat history of one week was given in a dryer (ADVANTEC FS-320) at 55 ° C. while being contained in the package. In FIG. 4, the test result under the first condition is indicated by a black square, and the test result under the second condition is indicated by a white square.

As shown in FIG. 4, the menthol release efficiency from the filter correlates with the menthol thermal desorption rate in the low temperature range obtained from the thermal desorption test. 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 menthol release efficiency from the filter, it was found that the thermal desorption rate of menthol in the low temperature range by a thermal desorption test can be adopted as a simple measurement method.

Further, as can be seen from FIG. 4, when a histol cigarette is given a thermal history for one week at 55 ° C., the menthol release rate from the filter, that is, the menthol detachment rate in a low temperature range is remarkably lowered. This corresponds to a temporal decrease in the amount of menthol in smoke after storage under summer conditions. Therefore, by measuring the thermal detachment rate of menthol in a low temperature region by a thermal desorption test, the effect of suppressing the temporal change in the amount of menthol in the smoke can be verified.

(Examples 1 and 2)
A cellulose acetate filter having a diameter of 8 mm and a length of 25 mm prepared by pre-sorption of menthol was prepared by adding menthol to acetate tow followed by high-temperature treatment. A predetermined amount of menthol was added to the filter by placing the menthol crystals in a beaker, melting by heating, and applying the menthol crystal to the end face of the filter using a micropipette. The amount of menthol added was 2.3 mg (Example 1) or 4.9 mg (Example 2). The obtained filter was placed in a closed glass container and stored in a dryer (ADVANTEC FS-320) at 55 ° C. for 14 days to allow menthol to penetrate into the deep part of the acetate fiber constituting the filter. The obtained filter is called a menthol presorption filter.

The cigarette was produced by connecting the produced menthol presorption filter to a cigarette rod of menthol cigarette (from which the mild seven aqua menthol one box filter was removed).

For comparison, a cigarette was prepared in the same manner as described above using a cellulose acetate filter (Comparative Example 1) to which menthol was not added.

A summary of the prepared samples is shown in Table 1.

The sample was put in a screw tube and stored for 7 days, 29 days, 56 days, or 70 days in a constant temperature and humidity machine (ESPEC Co., Ltd., LHU-113) at 40 ° C. The menthol content in the filter and tobacco and the amount of menthol thermal desorption from the filter were measured.

(1) Results of menthol distribution measurement The menthol in the filter and tobacco was extracted by shaking with a methanol solvent, and quantified using a gas chromatograph GC (6890 series, manufactured by HEWLETT PACKARD).

The M _f menthol amount in the filter, menthol content in cut tobacco of M _t, represents the menthol distribution factor F in the filter by the following equation.

F = _Mf / ( _Mf + _Mt )
FIG. 5 shows the change over time of the menthol distribution rate in the filter. As shown in FIG. 5, when the menthol presorption filters of Examples 1 and 2 were used, the change with time of the menthol distribution rate in the filters was small.

(2) Measurement of menthol thermal desorption amount A thermal detachment test of a menthol presorption filter was performed. The thermal desorption test was performed in the same manner as described above except that the temperature raising and analysis procedures were changed. Here, the operation of GC analysis after holding the sample at a predetermined constant temperature for 30 minutes to desorb the trap component was repeated with the temperature set at 22 ° C., 40 ° C., 80 ° C., or 200 ° C.

FIG. 6 shows the change over time in the menthol desorption rate in the low temperature range. As shown in FIG. 6, when the menthol presorption filters of Examples 1 and 2 were used, the menthol thermal desorption rate in the low temperature region increased with time, and the presorption of Comparative Example 1 was observed. The thermal desorption rate was improved 2 to 3 times compared to the case of using a non-filter.

In Example 1, the menthol in the filter increases with time when the menthol is distributed from the cigarette time (FIG. 5). However, it is possible to suppress the menthol distributed from the tobacco to the filter from penetrating into the deep part of the acetate fiber. For this reason, the menthol thermal desorption rate can be maintained high. In Example 2, the amount of menthol in the filter does not change so much with time even if menthol is distributed from the cigarette time (FIG. 5). Even in Example 2, a sufficient amount of menthol already exists in the deep part of the acetate fiber. For this reason, it is considered that the menthol distributed from the cigarette to the filter inside the menthol cigarette package is unevenly distributed near the surface of the acetate fiber.

The above results indicate that by pre-sorbing menthol on acetate fiber, penetration of menthol into the deep part of acetate fiber during storage of menthol cigarette products can be suppressed, and the change in the amount of menthol in smoke is suppressed over time. This suggests that release efficiency can be improved.

(Examples 3 and 4)
A menthol presorption sample comprising a film prepared by dissolving cellulose acetate flakes with acetone containing menthol Cellulose acetate flakes (manufactured by Daicel, L-40) in acetone (made by Wako Pure Chemicals, reagent grade) at a concentration of 2w A solution in which 9.23 wt% triacetin and 0.53 wt% or 1.39 wt% menthol were dissolved in cellulose acetate was prepared. On the other hand, for comparison, cellulose acetate flakes were dissolved in acetone, triacetin alone was dissolved, and a solution was prepared without dissolving menthol.

2 mL of the resulting acetone solution was cast into a glass petri dish having an inner diameter of 27 mm, and allowed to stand at room temperature for 5 days in an acetone atmosphere to volatilize the acetone slowly and spontaneously, followed by vacuum drying overnight at room temperature. A film was prepared. Acetone was volatilized as follows. In 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. By opening the gas outlet of the gas substitution desiccator to the atmosphere and making the gas substitution desiccator filled with acetone in the vicinity of saturated vapor, the volatilization rate of acetone from the cast cellulose acetate solution can be sufficiently slowed down. . Thus, if the acetone volatilization rate of the cellulose acetate solution is slowed during film production, a film with high transparency and uniform components and structure can be produced.

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 1.9 ± 0.05 mg were used for the test.

Example 3 is a film having a menthol content of 0.53 wt%, Example 4 is a film having a menthol content of 1.39 wt%, and Comparative Example 2 is a film without menthol addition. As in Examples 1 and 2, the thermal desorption rate of menthol in the low temperature range (up to 40 ° C.) was measured. As a result, the thermal desorption rate of menthol was 4.7% in Example 3 and 7.4% in Example 4. These values are the thermal desorption rate in the low temperature range of the filter taken out from the menthol cigarette which was stored at 55 ° C. for 1 week and given a thermal history as shown in FIG. 4, and the thermal desorption rate of Examples 1 and 2 Is at the same level. Therefore, mixing menthol wet with cellulose acetate flakes has the effect of pre-sorbing menthol in the deep part of cellulose acetate fiber, similar to applying high temperature treatment after adding menthol to cellulose acetate fiber Conceivable.

Next, it was confirmed that menthol was uniformly sorbed in the deep part of the cellulose acetate film as follows. Thread (Kanebo Textile Co., Ltd., Katan Yarn 20/200 Black) is passed through the prepared film sample, suspended by fixing with adhesive tape inside the lid of the screw tube, and PEG200 (made by Wako Pure Chemicals, first grade) 10 mL. 5 g of menthol was dissolved and put into a menthol atmosphere. The screw tube was stored for 2 days, 7 days, and 27 days in a constant temperature and humidity machine (ESPEC Co., Ltd., LHU-113) at 40 ° C., and then the menthol content in the film was measured. Menthol content was quantified with a gas chromatograph (HEWLETT PACKARD, 6890 series) after methanol extraction of the film.

FIG. 7 shows the change over time in the menthol content. As shown in FIG. 7, the menthol presorption films of Examples 3 and 4 have less change with time in the menthol content compared to the film of Comparative Example 2 without menthol presorption. That is, it can be seen that in the films of Examples 3 and 4, the menthol vapor dissolved in PEG 200 is difficult to sorb, and the sorption speed after a while after the start of storage is slow. From this, it was found that the menthol could be sufficiently penetrated into the deep part of the film by the method applied to Examples 3 and 4.

From the above results, it is possible to pre-sorb menthol in the deep part of the cellulose acetate film by mixing menthol wet with cellulose acetate flakes, and during the storage of menthol cigarette products having cigarette filters made from this cellulose acetate film It is considered that the penetration of menthol into the deep part of the cellulose acetate filter can be suppressed.

Claims

In the method for producing a cigarette filter using an acetate tow or an acetate film, a fragrance is infiltrated into a deep portion of the acetate fiber or the acetate film constituting the acetate tow.
Dissolving cellulose acetate in a solvent, spinning, crimping, and dry packing to produce acetate tow, adding a plasticizer to the acetate tow, winding up to make a filter plug, The method for producing a cigarette filter according to claim 1, wherein the perfume is permeated into the deep part of the produced acetate fiber by adding a perfume to the cellulose acetate before spinning from the cellulose acetate solution. .
Dissolving cellulose acetate in a solvent, spinning, crimping, and dry packing to produce acetate tow, adding a plasticizer to the acetate tow, winding up to make a filter plug, A perfume is added to the cellulose acetate during the period from spinning from a solution of cellulose acetate to the production of the acetate tow, and the perfume is diffused by heat treatment until the manufacturing process of the acetate filter plug is completed. The method for producing a cigarette filter according to claim 1, wherein a perfume is infiltrated into a deep part of the fiber.
Dissolving cellulose acetate in a solvent, spinning, crimping, and dry packing to produce acetate tow, adding a plasticizer to the acetate tow, winding up to make a filter plug, A fragrance is added when adding a plasticizer to acetate tow, and the fragrance is diffused by applying a heat treatment until the manufacturing process of the acetate filter plug is completed, and the fragrance penetrates deep into the acetate fiber. The manufacturing method of the cigarette filter of Claim 1.
Acetate flakes, plasticizer and fragrance are dissolved in a solvent to prepare a solution, an acetate film is prepared from the solution, and the fragrance is permeated into the deep part of the acetate film, and a cigarette filter is manufactured from the acetate film. The method for producing a cigarette filter according to claim 1.
The method for producing a cigarette filter according to any one of claims 1 to 5, wherein the fragrance is menthol.