MENTHOL-SORBED ACTIVATED CHARCOAL, CIGARETTE FILTER, AND FILTER-TIPPED CIGARETTE
Menthol-sorbed activated charcoal stably holding menthol during storage, and smoothly releasing menthol only during passage of tobacco smoke therethrough is provided. The menthol-sorbed activated charcoal is featured in that to activated charcoal having a specific surface area of 1500 m2/g or more but 1700 m2/g or less as measured by the BET method, menthol is sorbed at a sorption rate of 80% or more but 92% or less with reference to the saturated amount of menthol for the activated charcoal.
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This application is a Continuation Application of PCT Application No. PCT/JP2011/063835, filed Jun. 16, 2011 and based upon and claiming the benefit of priority from prior Japanese Patent Application No. 2010-235577, filed Oct. 20, 2010, the entire contents of all of which are incorporated herein by reference.
BACKGROUND OF THE INVENTION1. Field of the Invention
The present invention relates to menthol-sorbed activated charcoal, a cigarette filter, and a filter-tipped cigarette.
2. Description of the Related Art
In cigarettes, flavorants such as menthol are used to improve the intrinsic aroma and taste of the cigarettes. As menthol flavoring method, the addition to cut tobacco, the addition to inner packing paper of a package, and the addition to a filter are known. Encapsulation of menthol is also a common practice.
It is known that, in the addition of menthol to cut tobacco or inner packing paper, if the amount of menthol is increased, more brown stains occur on the cigarette paper of the tobacco rod during storage of the cigarette. The stains are attributable to the release of dyestuffs from cut tobacco upon the volatilization of menthol.
On the other hand, the use of menthol capsules allows the control of the occurrence of stains on cigarette paper and the deterioration of menthol in smoke. However, the use of menthol capsules requires the processes of the production of the capsules and incorporation of the capsules into the cigarette. As a result, the production cost of cigarette will increase.
On the other hand, U.S. Pat. No. 3,236,244 describes a filter element containing activated charcoal. Menthol is adsorbed to the activated charcoal, to add to a tobacco flavor.
BRIEF SUMMARY OF THE INVENTIONThe present invention is intended to provide menthol-sorbed activated charcoal with stably holds the menthol during storage and smoothly releases the menthol only during passage of tobacco smoke therethrough, as well as a cigarette filter containing the menthol-sorbed activated charcoal.
The present invention is also intended to provide a cigarette which comprises the filter, stably holds the menthol during storage over time in the menthol-sorbed activated charcoal of the filter, smoothly releases menthol only when tobacco smoke passes through the filter during smoking, and reduces the occurrence of stains on the cigarette paper.
A first aspect of the present invention provides menthol-sorbed activated charcoal comprising activated charcoal having a specific surface area of 1500 m2/g or more but 1700 m2/g or less as measured by the BET method, with menthol being sorbed to the activated charcoal at a sorption rate of 80% or more but 92% or less with reference to the saturated amount of menthol for the activated charcoal.
The activated charcoal has a relatively large specific surface area, and has a relatively high degree of activity. Therefore, the activated charcoal is hereinafter referred to as “highly activated charcoal”, thereby differentiating it from general activated charcoal.
A second aspect of the present invention provides a cigarette filter containing the menthol-sorbed activated charcoal of the first aspect.
A third aspect of the present invention provides a filter-tipped cigarette comprising the cigarette filter of the second aspect.
Embodiments of the present invention are described below in detail.
A menthol-sorbed activated charcoal according to an embodiment of the present invention comprises highly activated charcoal having a specific surface area of 1500 m2/g or more but 1700 m2/g or less as measured by the BET method, and to the charcoal, menthol is sorbed at a sorption rate of 80% or more but 92% or less with respect to the saturated amount of menthol for the highly activated charcoal.
The specific surface area by the BET method may be measured as follows:
Apparatus: Autosorb-1-MP (manufactured by Quantachrome)
Pretreatment: 0.010 g of activated charcoal sample for measurement was heated for 15 hours in a vacuum at 0.1 Pa and 573 K,
Measurement method: the specific surface area of the pretreated sample was calculated by the Multipoint BET method at relative pressure P/P0=0.1 to 0.3 using the nitrogen adsorption isotherm data obtained at a temperature of 77 K.
The highly activated charcoal may be any activated charcoal as long as it has a specific surface area of 1500 m2/g or more but 1700 m2/g or less as measured by the BET method. As the highly activated charcoal, for example, coconut shell activated charcoal may be used.
An activated charcoal having a specific surface area of less than 1500 m2/g decreases in the amount of menthol held in the activated charcoal in the filter-tipped cigarette. As a result, it becomes difficult to sufficiently increase the amount of menthol in tobacco smoke during smoking. On the other hand, an activated charcoal having a specific surface area of more than 1700 m2/g may rapidly decrease in the percentage of reduction of menthol during storage.
The highly activated charcoal preferably has an average particle size of 200 to 600 μm.
When used in a filter-tipped cigarette, the sorption rate of menthol for the highly activated charcoal is important for the relationship between the lapsed days of storage and the amount of menthol in tobacco smoke during smoking. If the sorption rate of menthol is less than 80% with reference to the saturated amount of menthol for the highly activated charcoal, the amount of menthol held by the highly activated charcoal decreases when the charcoal is applied to a filter-tipped cigarette. As a result, it becomes difficult to sufficiently increase the amount of menthol in tobacco smoke during smoking. On the other hand, if the sorption rate of menthol is more than 92% with reference to the saturated amount of menthol for the highly activated charcoal, the amount of menthol in tobacco smoke during smoking may decrease with the lapsed days of storage.
The menthol-sorbed activated charcoal according to one embodiment can be produced by, for example, charging desired amounts of menthol and highly activated charcoal, which has a specific surface area of 1500 m2/g or more but 1700 m2/g or less as measured by the BET method, into the chamber of a rotary stirring apparatus, and allowing the menthol to be sorbed to the highly activated charcoal while rotating the highly activated charcoal. The chamber may be heated to an internal temperature of 40 to 80° C.
Next, a cigarette filter according to an embodiment will be described.
The cigarette filter according to an embodiment contains the menthol-sorbed activated charcoal described above.
In one embodiment, the cigarette filter has two or more segments and contains the menthol-sorbed activated charcoal in a part thereof. In another embodiment, the cigarette filter has a structure that many particles of the menthol-sorbed activated charcoal are filled between two columnar filter materials and a plug wrapper wraps the filter materials, including the filled portion.
The filter material is a filter material used in ordinary cigarette filters. For example, tow of cellulose acetate fibers may be used. The bundle of cellulose acetate fibers can be consolidated by the treatment with triacetin.
Next, a filter-tipped cigarette according to an embodiment of the present invention will be described.
The filter-tipped cigarette according to an embodiment includes the above-described cigarette filter.
In one embodiment, the filter-tipped cigarette has the structure shown in
The filter will not be limited to the structure shown in
The above-described menthol-sorbed activated charcoal according to one embodiment has a constitution that to the highly activated charcoal having a specific surface area of 1500 m2/g or more but 1700 m2/g or less as measured by the BET method, menthol is sorbed at a sorption rate of 80% or more but 92% or less with reference to the saturated amount of menthol for the highly activated charcoal. Therefore, menthol is stably held during storage, and menthol is smoothly released only during the passage of tobacco smoke through the charcoal.
By causing the menthol-sorbed activated charcoal to be contained in a filter, and applying this filter into a filter-tipped cigarette, menthol is stably held over time in the menthol-sorbed activated charcoal in the filter during storage, menthol is smoothly released only when tobacco smoke passes through the filter during smoking, and the occurrence of stains on the cigarette paper is reduced. These were confirmed by the following tests.
<Test I>
Coconut shell activated charcoals having specific surface areas of 700, 1000, 1700, and 2000 m2/g as measured by the BET method and an average particle size of 400 μm (four prototypes prepared by changing the specific surface area of Kuraraycoal GGS manufactured by Kuraray Chemical Co., Ltd., through the change of the activation conditions) were provided. A menthol flavorant (manufactured by Fuji Flavor Co., Ltd.) was sorbed to the coconut shell activated charcoal to saturation, thereby preparing four types of menthol-sorbed activated charcoals.
50 mg of the particles of the menthol-sorbed activated charcoal thus obtained was dispersed in one of two cellulose acetate filter materials. These two filter materials were wrapped with a plug wrapper to form a column, thereby making a segmented filter. This filter was butted to the end of a tobacco rod (without menthol flavoring) such that the filter material containing the menthol-sorbed activated charcoal particles was positioned at the tobacco rod side. Subsequently, the whole circumference surface of the filter and the circumference surface of the tobacco rod near the butted portion were wrapped by a tipping paper. Thus, four types of filter-tipped cigarettes were fabricated.
The amount of menthol in tobacco smoke during smoking of the filter-tipped cigarettes thus obtained, in the initial stage (without storage), was measured by the following method, thereby examining the menthol releasability. In addition, the amount of menthol in tobacco smoke during smoking after storage for 0.5, 1.5, and 2.5 months was measured by the following method, and the amount of menthol (relative value) with reference to the value after storage for 0.5 month was determined. Furthermore, the rate of occurrence of stains on the cigarette paper was studied by the following method.
(Measurement of the Amount of Menthol)
The filter-tipped cigarette in the initial stage after production, and the filter-tipped cigarettes after storage for 0.5, 1.5, and 2.5 months were burned using an automatic smoking machine at a puff volume of 35 mL/2 sec, a puff interval of 60 seconds, and a burning length of 35 mm from the tip of mouthpiece. During burning, the particle phase components in the tobacco smoke were collected using a Cambridge Filter. The components thus obtained were solvent-extracted with methanol, and then subjected to gas chromatography, thereby quantitatively determining the amount of menthol in tobacco smoke.
(The Rate of Occurrence of Stains on Cigarette Paper)
The filter-tipped cigarettes were stored for 1 month in a constant temperature and humidity bath at a temperature of 22° C. and a relative humidity of 60%. Thereafter, stains appeared on the cigarette paper of the tobacco rod were visually observed, and the rate of occurrence of stains was determined. The stain with a size of 0.9 to 1.8 mm as measured by visual observation was rated as “small stain”, and that with a size of greater than 1.8 mm as measured by visual observation was rated as “large stain”.
As is evident from
On the other hand, as is evident from
Furthermore, as is evident from
Based on the above results of Test I, it was found that the use of the filter containing menthol-sorbed activated charcoal with highly activated charcoal having a specific surface area of 1500 m2/g or more but 1700 m2/g or less as measured by the BET method is suitable for the achievement of a filter-tipped cigarette which shows a little change in menthol over time and a low rate of occurrence of stains on cigarette paper during storage, while realizing a high releasability of menthol.
<Test II>
Coconut shell activated charcoal having a specific surface area of 1700 m2/g as measured by the BET method and an average particle size of 400 μm (prototype prepared by changing the specific surface area of Kuraraycoal GGS manufactured by Kuraray Chemical Co., Ltd., through the change of the activation conditions) was provided. A menthol flavorant (manufactured by Fuji Flavor Co., Ltd.) was sorbed to the coconut shell activated charcoal at the sorption rates of 80 to 100% with reference to the saturated amount of menthol for the coconut shell activated charcoal, thereby preparing six particulate menthol-sorbed activated charcoals. The saturated amount of menthol for the coconut shell activated charcoal having a specific surface area of 1700 m2/g as measured by the BET method and an average particle size of 400 μm is 60 parts by weight of menthol with reference to 100 parts by weight of activated charcoal. Therefore, the sorption rate was defined as follows: activated charcoal:menthol=100:48 to 60.
Filter-tipped cigarettes were made using the menthol-sorbed activated charcoal obtained above in the same manner as in Test I. The amount of menthol in tobacco smoke during smoking released from the filter-tipped cigarettes in the initial stage (without storage) was measured in the same manner as in Test I. The results are shown in
As is evident from
<Test III>
Coconut shell activated charcoal having a specific surface area of 1700 m2/g as measured by the BET method and an average particle size of 400 μm (prototype prepared by changing the specific surface area of Kuraraycoal GGS manufactured by Kuraray Chemical Co., Ltd., through the change of the activation conditions) was provided. A menthol flavorant (manufactured by Fuji Flavor Co., Ltd.) was sorbed to the coconut shell activated charcoal at sorption rates of 92, 95, and 100% with reference to the saturated amount of menthol for the coconut shell activated charcoal, thereby preparing three particulate menthol-sorbed activated charcoal.
Filter-tipped cigarettes were made using the menthol-sorbed activated charcoal obtained above, in the same manner as in Test I. These filter-tipped cigarettes were measured for the amount of menthol in tobacco smoke during smoking after storage for 0.5, 1.5, 2.5, and 3.5 months under high temperature conditions (maximum temperature 55° C., humidity 35% RH) in the same manner as in Test I, and the amount of menthol (relative value) was determined, setting the value after storage for 0.5 month as 100%. The results are shown in
As is evident from
On the other hand, it is seen that in the cigarette including the menthol-sorbed activated charcoal having a sorption rate of 92%, the amount of menthol in tobacco smoke was kept at about 85% even after storage for 3.5 months under the high temperature conditions with reference to the amount of menthol in tobacco smoke during smoking at the time of 0.5 month storage.
Based on the above results of Tests II and III, it was found that the use of the filter containing the menthol-sorbed activated charcoal in which menthol is sorbed to highly activated charcoal having a specific surface area at a sorption rate of 80% or more and 92% or less with reference to the saturated amount of menthol for the highly activated charcoal is suitable for providing a filter-tipped cigarette which shows a little change in menthol over time during storage, which realizing a high releasability of menthol.
Examples of the present invention are described below.
EXAMPLE 1Coconut shell activated charcoal having a specific surface area of 1700 m2/g as measured by the BET method and an average particle size of 400 μm (prototype prepared by changing the specific surface area of Kuraraycoal GGS manufactured by Kuraray Chemical Co., Ltd., through the change of the activation conditions) was provided. A menthol flavorant (manufactured by Fuji Flavor Co., Ltd.) was sorbed to the coconut shell activated charcoal at a sorption rate of 92% with reference to the saturated amount of menthol for the coconut shell activated charcoal, thereby preparing particulate menthol-sorbed activated charcoal. The saturated amount of menthol for the coconut shell activated charcoal having a specific surface area of 1700 m2/g as measured by the BET method and an average particle size of 400 μm is 60 parts by weight of menthol with reference to 100 parts by weight of activated charcoal. Therefore, the sorption rate of 92% was achieved using 100 parts by weight of activated charcoal and 55 parts by weight of menthol.
A filter-tipped cigarette was made using 160 mg of the menthol-sorbed activated charcoal thus obtained, in the same manner as in Test I.
COMPARATIVE EXAMPLE 1A filter-tipped cigarette was made in the same manner as in Test I, except that 4.0 mg of menthol was sorbed to the cut tobacco in the tobacco rod, instead of placing the menthol-sorbed activated charcoal in the filter.
The filter-tipped cigarettes of Example 1 and Comparative Example 1 were measured for the amount of menthol in tobacco smoke during smoking in the initial stage after production (without storage), in the same manner as in Test I. As a result, the amount of menthol in tobacco smoke from the cigarette of Example 1 was 0.41 mg/cig, and the amount of menthol in tobacco smoke from the cigarette of Comparative Example 1 was 0.4 mg/cig.
Furthermore, the filter-tipped cigarettes of Example 1 and Comparative Example 1 were measured for the amount of menthol in tobacco smoke during smoking after storage for 1, 5, and 9 weeks under high temperature conditions (maximum temperature 55° C., humidity 35% RH), in the same manner as in Test I. The results are shown in
As is evident from
Furthermore, the filter-tipped cigarettes of Example 1 and Comparative Example 1 were stored in a constant temperature and humidity bath at a temperature of 22° C. and a relative humidity of 60% for one month, and stains occurred on the cigarette paper of the tobacco rod were visually observed, and the rate of occurrence of stains was determined. The stain with a size of 0.9 to 1.8 mm as measured by visual observation was rated as “small stain”, and that with a size of greater than 1.8 mm as measured by visual observation was rated as “large stain”. The results are shown in
As is evident from
The same menthol-sorbed activated charcoal (sorption rate 92%) as in Example 1 was provided, and a filter-tipped cigarette was made in the same manner as in Test I using 80 mg of the menthol-sorbed activated charcoal.
COMPARATIVE EXAMPLE 2A filter-tipped cigarette was made in the same manner as in Test I, except that 6.0 mg of menthol was sorbed to the cut tobacco in the tobacco rod, instead of placing menthol-sorbed activated charcoal in the filter.
The filter-tipped cigarettes of Example 2 and Comparative Example 2 were stored for 1.5 months in a constant temperature and humidity bath at a temperature of 22° C. and a relative humidity of 60%, and then the change in the amount of menthol by the puff number was measured by the following method.
More specifically, the filter-tipped cigarette after storage was mounted on an automatic smoking machine, puffed for 2 seconds, and the particle phase components in the puff were collected using Cambridge Filter. The component thus obtained was extracted with a methanol solvent, and then subjected to gas chromatography, thereby determining the amount of menthol in the puff. The puffing was performed seven times in total at intervals of one minute, and the amount of menthol in each puff was determined. The menthol ratio (%) in each puff was determined by summing the amount of menthol in the first to seventh puffs, and dividing the amount of menthol in each puff with the total amount of menthol. The results are shown in
As is evident from
The present invention provides menthol-sorbed activated charcoal which stably holds menthol during storage and smoothly releases menthol only during passage of tobacco smoke, and a cigarette filter containing the menthol-sorbed activated charcoal.
The present invention also provides a filter-tipped cigarette which includes the filter, stably holds menthol over time during storage in the menthol-sorbed activated charcoal in the filter, smoothly releases menthol only when tobacco smoke passes through the filter during smoking, and reduces the occurrence of stains on the cigarette paper.
Claims
1. Menthol-sorbed activated charcoal comprising activated charcoal having a specific surface area of 1500 m2/g or more but 1700 m2/g or less as measured by the BET method, with menthol being sorbed to the activated charcoal at a sorption rate of 80% or more but 92% or less with reference to the saturated amount of menthol for the activated charcoal.
2. A cigarette filter containing a menthol-sorbed activated charcoal according to claim 1.
3. The cigarette filter according to claim 2, wherein the filter has two or more segments, and the menthol-sorbed activated charcoal is contained in a portion thereof.
4. The cigarette filter according to claim 2, wherein the filter material is a cellulose acetate material.
5. A cigarette comprising a cigarette filter according to claim 2.
Type: Application
Filed: Apr 18, 2013
Publication Date: Sep 5, 2013
Applicant: Japan Tobacco Inc. (Tokyo)
Inventor: Yoshinori SAKAI (Tokyo)
Application Number: 13/865,381
International Classification: A24D 3/14 (20060101);