WO2012066656A1 - Granulés à adsorbant supporté et leur procédé de fabrication, filtre à cigarette et cigarette - Google Patents

Granulés à adsorbant supporté et leur procédé de fabrication, filtre à cigarette et cigarette Download PDF

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Publication number
WO2012066656A1
WO2012066656A1 PCT/JP2010/070489 JP2010070489W WO2012066656A1 WO 2012066656 A1 WO2012066656 A1 WO 2012066656A1 JP 2010070489 W JP2010070489 W JP 2010070489W WO 2012066656 A1 WO2012066656 A1 WO 2012066656A1
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Prior art keywords
adsorbent
core material
fine
cigarette
carrying
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PCT/JP2010/070489
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English (en)
Japanese (ja)
Inventor
朋広 小林
憲俊 藤田
正人 宮内
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日本たばこ産業株式会社
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Priority to PCT/JP2010/070489 priority Critical patent/WO2012066656A1/fr
Publication of WO2012066656A1 publication Critical patent/WO2012066656A1/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
    • A24D3/08—Use of materials for tobacco smoke filters of organic materials as carrier or major constituent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28004—Sorbent size or size distribution, e.g. particle size
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • B01J20/28066—Surface area, e.g. B.E.T specific surface area being more than 1000 m2/g
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3202—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the carrier, support or substrate used for impregnation or coating
    • B01J20/3206—Organic carriers, supports or substrates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
    • B01J20/3242—Layers with a functional group, e.g. an affinity material, a ligand, a reactant or a complexing group
    • B01J20/3268—Macromolecular compounds
    • B01J20/327—Polymers obtained by reactions involving only carbon to carbon unsaturated bonds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3291—Characterised by the shape of the carrier, the coating or the obtained coated product
    • B01J20/3293—Coatings on a core, the core being particle or fiber shaped, e.g. encapsulated particles, coated fibers

Definitions

  • the present invention relates to an adsorbent-carrying granule, a production method thereof, a cigarette filter, and a cigarette.
  • the activated charcoal that adsorbs the components in the smoke during smoking is used for the cigarette charcoal filter.
  • Activated carbon uses a specific surface area of 1000 to 1100 g / m @ 2 by carbonization and activation of coconut shells and an acetone adsorption capacity of 26%, and 20-50 mg per cigarette is attached to the filter.
  • the charcoal filter containing activated carbon can adsorb and remove the vapor phase (VOC) component in the smoke, and can provide its unique taste and aroma.
  • the specific surface area of the activated carbon is increased or the amount of the activated carbon added to the filter is increased. It can be mentioned. Further, in order to increase the contact area between the activated carbon and the cigarette smoke flow, it is possible to reduce the particle size of the activated carbon.
  • a porous inorganic material (core material) is mixed with a carbonized material and an inorganic binder, and the core material is coated with the carbonized material together with the inorganic binder, followed by firing.
  • Japanese Patent Application Laid-Open No. 11-241871 has a predetermined particle size, specific surface area and JIS hardness obtained by adding a water-soluble binder to powdered activated carbon and stirring granulation, and has a high adsorption rate and can prevent scattering.
  • a granulated activated carbon for an adsorption-type refrigerator is disclosed.
  • the present invention provides, for example, an adsorbent-carrying granule that adsorbs a VOC component in smoke well and has a larger particle size than activated carbon used in current charcoal filters, and a method for producing the same.
  • the present invention also provides a cigarette filter capable of adsorbing VOC components in smoke well and reducing the airflow resistance.
  • the present invention provides a cigarette that can suppress or prevent the adsorption of flavor during storage, can adsorb the VOC component in the smoke well, and can reduce the ventilation resistance.
  • At least the surface of the non-porous core material is finer adsorbent finer than polyvinyl alcohol, and the blending ratio of polyvinyl alcohol is 6 with respect to the total amount of fine adsorbent and polyvinyl alcohol.
  • An adsorbent-carrying granule supported so as to be 7% by weight or less is provided.
  • a desired amount of a non-porous core material is placed on a rotating dish in a chamber; and the rotating dish is rotated so that the chamber inner surface and the outer peripheral edge of the rotating dish While supplying the air from below to above to cause planetary movement of the core material, spray an aqueous polyvinyl alcohol solution toward the core material, and spray finer particulate adsorbent than the core material.
  • a method for producing an adsorbent-carrying granule is provided.
  • a cigarette filter having the adsorbent-carrying granules of the first aspect.
  • a cigarette provided with the cigarette filter of the third aspect is provided.
  • FIG. 1 is a schematic view showing a centrifugal rolling granulation coating apparatus used for production of an adsorbent-carrying granule according to an embodiment.
  • FIG. 2 is a cross-sectional view showing a cigarette filter according to the embodiment.
  • FIG. 3 is a cross-sectional view showing another cigarette filter according to the embodiment.
  • FIG. 4 is a cross-sectional view showing a cigarette according to the embodiment.
  • FIG. 5 is a cross-sectional view showing another cigarette according to the embodiment.
  • FIG. 6 is a diagram showing the particle size distribution of fine-grained coal and normal coal.
  • FIG. 7 is a graph showing the initial VOC component adsorption rates of evaluation cigarettes equipped with filters containing the adsorbent-carrying granules of Examples 1-1 to 1-3 and fine coal of Example 1-4.
  • FIG. 8 is a graph showing the adsorption rate of the VOC component after the acceleration conditions described above of the cigarette provided with the filter containing the adsorbent-carrying granules of Examples 1-1 to 1-3 and the fine coal of Example 1-4.
  • FIG. 9 shows the adsorption rate of the initial VOC component of the evaluation cigarette equipped with the filter containing the adsorbent-carrying granules of Examples 2-1 to 2-3, the fine coal of Example 2-4, and the normal coal of Example 2-5.
  • FIG. FIG. 10 is a graph showing the adsorption rate of the initial VOC component of the evaluation cigarette provided with the filter containing the adsorbent-carrying granules of Examples 3-1 to 3-3 and the fine coal of
  • the adsorbent-carrying granule according to the embodiment has a fine particle adsorbent finer than polyvinyl alcohol supported on at least a non-porous core material, and the blending ratio of polyvinyl alcohol is the sum of the fine particle adsorbent and polyvinyl alcohol. It is 6.7% by weight or less based on the amount.
  • At least the surface of the non-porous core material means a core material having no open pores on the surface.
  • This core material allows to have pores (closed pores, independent pores) inside.
  • a preferable core material is non-porous inside including the surface.
  • the core material is preferably hygroscopic. Examples of such core materials include granulated sugar, lactose, tri-warm sugar, fine sugar and starch.
  • the core material is preferably spherical.
  • the adsorbent-supporting granules obtained by making the core material spherical to support the fine particle adsorbent on the surface of the core material while moving the planetary planetary motion while supporting the fine particle adsorbent on the core material.
  • the sphericity can be improved. If the spherical adsorbent-carrying granules are selected with a vibration sieve, the particle size distribution can be sharpened.
  • Such adsorbent-carrying granules can improve the filter quality such as adsorption performance and ventilation resistance. It is also possible to increase the filling rate of the adsorbent-carrying granules when filling the filter cavity and to improve the quantitative accuracy of supplying the adsorbent-carrying granules when manufacturing the filter.
  • the fine-grain adsorbent adsorbs the VOC component in the smoke.
  • fine sorbents include activated carbon, hydrotalcite, zeolite, alumina, sepiolite, silica and their surface modifiers, and combinations thereof.
  • activated carbon is preferable.
  • the activated carbon preferably has a specific surface area of 1780 to 1900 m 2 / g by BET method.
  • the blending ratio of polyvinyl alcohol (PVA) By controlling the blending ratio of polyvinyl alcohol (PVA) to 6.7% by weight or less with respect to the total amount of the fine-grain adsorbent and PVA, it is possible to prevent the pores that are the adsorbing portions of the fine-grain adsorbent from being blocked by PVA. Thus, the original adsorption performance of the fine-grain adsorbent can be maintained.
  • the lower limit of the blending ratio of PVA is preferably 0.7% by weight with respect to the total amount of the fine particle adsorbent and PVA from the viewpoint of favorably adhering and supporting the fine particle adsorbent on the surface of the core material.
  • the most preferable blending ratio of PVA is 4.0 wt% or more and 6.3 wt% or less with respect to the total amount of the fine-grain adsorbent and PVA.
  • the adsorbent-carrying granule according to the embodiment is too small, the passage resistance when cigarette smoke passes is increased, and if it is too large, the amount of adhering to the filter is limited, and the adsorption performance of the VOC component in the smoke May decrease. For this reason, it is desirable that the adsorbent-carrying granules have an appropriate size, for example, a particle size of 1000 ⁇ m or less.
  • the core material serving as the core of the adsorbent-carrying granules desirably has a size corresponding to the granules, for example, a particle size of 200 to 900 ⁇ m, more preferably 600 to 900 ⁇ m.
  • the fine particle adsorbent supported on the surface of the core material desirably has a particle size of 50 to 350 ⁇ m, more preferably 75 to 350 ⁇ m in order to adsorb the VOC component in the smoke well.
  • the method for producing an adsorbent-carrying granule includes a step of placing a desired amount of a non-porous core material on a rotating plate of a chamber, a rotating plate, rotating the chamber inner surface and the rotating plate While supplying air from below to above between the outer peripheral edges of the core material to cause planetary movement of the core material, the PVA aqueous solution is sprayed toward the core material, and finer particulate adsorbent is sprayed from the core material. Then, the fine particle adsorbent is supported on the core material so that the blending ratio of PVA is 6.7% by weight or less based on the total amount of the fine particle adsorbent and PVA.
  • centrifugal rolling granulation coating apparatus In such a method for producing an adsorbent-carrying granule, a centrifugal rolling granulation coating apparatus can be used. Centrifugal rolling granulation coating apparatuses are well known in the art and can be obtained, for example, under the name of CF granulator from Freund Sangyo Co., Ltd., Japan.
  • the centrifugal rolling granulation coating apparatus 10 includes a rotating dish (rotor) 11 that rotates in the horizontal direction and a rotating dish 11 that surrounds the rotating dish 11.
  • a cylindrical fixed wall (stator) 12 is provided.
  • the upper opening of the fixed wall 12 is closed by the upper wall 13.
  • the lower opening of the fixed wall 12 is closed by the lower wall 14.
  • a space 16 is provided between the rotating dish 11 and the lower wall 15, and an air supply pipe 17 is provided on the fixed wall 12 so as to communicate with the space 16.
  • a centrifugal rolling chamber 18 is configured by the rotating dish 11 and the fixed wall portion on the upper part of the rotating dish 11.
  • the central part of the rotating dish 11 is raised in a truncated cone shape, and this raised part 31 can move the core particles near the center of the rotating dish 11 to the outer peripheral part and roll the core material on the inclined side surface. .
  • the peripheral edge of the rotating dish 11 is slightly curved upward. The rotating dish 11 is rotated by driving the motor 25 via the shaft 25a.
  • a nuclear material supply pipe (not shown) is provided in the centrifugal rolling chamber 18 through the upper portion of the fixed wall 12, and a nuclear material storage tank (not shown) installed outside the fixed wall 12.
  • the core material 19 is supplied onto the rotating dish 11 through the supply pipe.
  • a fine-particle adsorbent spraying pipe 20 is provided in the centrifugal rolling chamber 18, and the fine-grain adsorbent 21 is sprayed from the storage tank 22 of the fine-grain adsorbent 21 installed outside the fixed wall 12. Is spread on the rotating dish 11.
  • a spray nozzle 24 for spraying the aqueous PVA solution 23 onto the core material 19 on the rotating dish 11 through the upper wall 13 is provided in the centrifugal rolling chamber 18.
  • the core material 19 is placed on the rotating dish 11 from a core material supply pipe (not shown), and the rotating dish 11 is driven to rotate by the motor 25.
  • air 26 is supplied from the air supply pipe 17 into the space 16.
  • the air 26 flows into the centrifugal rolling chamber 18 through a gap 27 between the rotating dish 11 and the fixed wall 12 (slit air 26a). Due to the centrifugal force generated by the rotation of the rotating dish 11 and the action of the slit air 26 a, the core material 19 performs planetary movement (circulating flow) on the rotating dish 11.
  • a PVA aqueous solution 23 is sprayed from the spray nozzle 24 onto the nuclear material 19 in a planetary motion state, and then the fine-particle adsorbent 21 is sprayed from the spray tube 20. That is, spraying of the PVA aqueous solution 23 and spraying of the fine-grain adsorbent 21 are performed intermittently.
  • the coating temperature of PVA on the surface of the core material 19 corresponds to the temperature of the slit air 26a.
  • the PVA aqueous solution penetrates into the core material, and while the spraying of the PVA aqueous solution suppresses the excessive state of moisture on the surface of the core material, the PVA aqueous solution is applied to the core material surface.
  • the uniform adhesion of the dispersed fine particle adsorbent 21 which is uniformly large is promoted.
  • spray conditions such as the number of rotations of the rotating pan 11, the flow rate and temperature of the slit air 26a, the spray amount per spray of the PVA aqueous solution 23, and the spray interval are set so that the core materials do not aggregate. It is preferable to set.
  • the rotational speed of the rotating pan 11 is set to 100 to 1000 rpm
  • the flow rate of the slit air 26a is set to 10 to 100 NL / min
  • the temperature of the slit air 26a is set to 30 to 70 ° C.
  • the spray amount per one time of the aqueous PVA solution is set to 1.
  • the desired spray interval can be set to 0.2 to 5 parts by weight per 100 parts by weight of the core material per minute.
  • the fine particle adsorbent is PVA on each surface of the core material, and the blending ratio of PVA is 6.7% by weight with respect to the total amount of the fine particle adsorbent and PVA.
  • the granules are dried. This drying is preferably performed while the adsorbent-carrying granules are maintained in the planetary motion state described above so that the prepared adsorbent-carrying granules are not aggregated. Drying is preferably performed until the water content of the PVA carrying the fine-grain adsorbent is 1% by weight or less.
  • the pore structure of the fine-grain adsorbent (for example, activated carbon) is covered with the PVA aqueous solution, which may reduce the adsorbent adsorption performance.
  • a fine particle adsorbent (for example, activated carbon) having a minimum particle size of 50 ⁇ m, more preferably 75 ⁇ m, is used during the production of the adsorbent-carrying granules. It is desirable.
  • the upper limit particle size of the fine particle adsorbent is preferably 350 ⁇ m.
  • the cigarette filter according to the embodiment has a structure in which the aforementioned adsorbent-carrying granules are attached to a filter material.
  • cellulose acetate fiber tow can be used as the filter material.
  • a bundle of cellulose acetate fibers can be bound by treating with triacetin.
  • the cigarette filter 41 shown in FIG. 2 is a dual type.
  • One filter material 42 has a structure in which, for example, a filter material 43 formed by bundling or folding acetate fiber or non-woven fabric of pulp is wound into a cylindrical shape with an individual winding paper (not shown).
  • the other filter material 44 has a structure in which a plurality of adsorbent-carrying granules 45 are attached to the same filter material 43 as a whole and wound in a cylindrical shape with an individual web (not shown).
  • These filter materials 42 and 44 are end-butted with each other, and are wound into a cylindrical shape by a common web 46.
  • the cigarette filter 41 shown in FIG. 3 includes two filter materials 47a and 47b in which a filter material 43 formed by bundling or folding non-woven fabrics of acetate fibers or pulp, for example, is wound in a cylindrical shape with individual winding paper (not shown). ing. These filter materials 47a and 47b are arranged at a predetermined interval from each other, and a plurality of adsorbent-carrying granules 45 are filled in the cavity between the filter materials 47a and 47b. Filter members 47 a and 47 b in which the filling portion of the adsorbent-carrying granule 45 is arranged in the middle are wound in a cylindrical shape by a common web 46.
  • the cigarette according to the embodiment includes the filter described above.
  • the cigarette 51 shown in FIG. 4 abuts the end of the cigarette rod 52 and the end of the filter material 44 (attached with the adsorbent-carrying granules 45) of the cigarette filter 41 shown in FIG.
  • the cigarette rod 52 and the filter 41 are integrated by encapsulating the entire outer peripheral surface and the outer peripheral surface portion of the tobacco rod 52 in the vicinity of the butt with a chip paper 53.
  • the tobacco rod 52 is formed by enclosing a tobacco cut 54 in a cylindrical shape with a wrapping paper 55.
  • the cigarette 51 shown in FIG. 5 abuts the end of the cigarette rod 52 and the end of the filter material 47a of the cigarette filter 41 shown in FIG.
  • the outer peripheral surface portion is encapsulated with chip paper 53, and the tobacco rod 52 and the filter 41 are integrated.
  • the surface of the non-porous core material is a fine adsorbent finer than polyvinyl alcohol, and the blending ratio of the polyvinyl alcohol is that of the fine adsorbent and polyvinyl alcohol.
  • the adsorbent-carrying granules of the embodiment show excellent adsorption performance in the fine adsorbent layer on the surface of the core material by supporting the fine particle adsorbent with polyvinyl alcohol (PVA) on the surface of the core material, It has a larger particle size than activated carbon used in charcoal filters.
  • PVA polyvinyl alcohol
  • the adsorbent-supporting granule of the embodiment regulates the upper limit amount of polyvinyl alcohol as a binder, thereby suppressing the pores that are the adsorbing part of the fine adsorbent from being blocked by PVA, and the fine adsorbent It becomes possible to maintain the original adsorption performance.
  • the VOC component in the smoke can be favorably adsorbed.
  • the VOC component in the smoke can be favorably adsorbed.
  • the adsorbent-supported granules contained in the filter have a core-shell structure in which fine adsorbent is supported by PVA on the surface of the core material, and can be made larger in particle size than activated charcoal used in current charcoal filters. Ventilation resistance can be reduced.
  • the cigarette according to the embodiment includes the filter including the adsorbent-carrying granules described above, the VOC component in the smoke can be favorably adsorbed, and the particle size can be increased as compared with the activated carbon used in the current charcoal filter. Ventilation resistance during smoking can be reduced.
  • the adsorbent-carrying granules contained in the filter can be adsorbed by supporting fine adsorbent with polyvinyl alcohol (PVA) at least on the surface of the non-porous core material, that is, the core material that does not have its own adsorption performance.
  • PVA polyvinyl alcohol
  • the field can be limited to the fine sorbent layer on the surface of the core material.
  • the adsorbing ability of the entire adsorbent-supporting granule containing the core material is not expressed, and the adsorbing ability of only the fine-grain adsorbent layer is maintained, thereby exhibiting a high adsorbing ability from the surface of the known example to the entire interior.
  • Adsorption of cigarette flavor during adsorption storage like granulated activated carbon can be suppressed or prevented.
  • Pulverized coal (average particle size 14 ⁇ m, specific surface area 1780 m 2 / g by BET method), 70-200 mesh (75-212 ⁇ m sieve mesh) fine coal (coconut shell activated carbon obtained from Kuraray Chemical Co., Ltd. as an adsorbent. Prepared normal charcoal (average particle size 390 ⁇ m, specific surface area 1800 m 2 / g by BET method) with average particle size 195 ⁇ m, specific surface area 1900 m 2 / g by BET method, and 28-70 mesh (screen interval 212-600 ⁇ m) did.
  • FIG. 6 shows the particle size distribution (A) of the fine coal and the particle size distribution (B) of the normal coal. From FIG. 6, it can be seen that the fine coal has a particle size distribution of 50 to 350 ⁇ m.
  • the average particle diameter and the specific surface area by the BET method were measured by the following methods.
  • ⁇ Particle size distribution of activated carbon, average particle size measurement> The particle size distribution of the powdered activated carbon without pretreatment was measured from the measurement of laser scattering in water by HORIBA LA-920 (manufactured by HORIBA, Ltd.), and the 50% median diameter of the sphere equivalent diameter was calculated as the average particle diameter.
  • Examples 1-1 to 1-3 Using a centrifugal fluid coating device (CF granulator, CF-LABO; manufactured by Freund Sangyo Co., Ltd.), an aqueous binder solution having a concentration of 5% by weight is intermittently injected onto 100 g of granulated sugar (manufactured by Mitsui Sugar Co., Ltd., average particle size 560 ⁇ m) as a core material. Then, 15 g of the above-mentioned three kinds of activated carbon were gradually sprayed to produce adsorbent-carrying granules.
  • CF granulator CF-LABO; manufactured by Freund Sangyo Co., Ltd.
  • Examples 1-1 to 1-3 fine coal was used as activated carbon, and polyvinyl alcohol (PVA), carboxymethyl cellulose (CMC) and tamarind gum (TG) were used as binders, respectively.
  • PVA polyvinyl alcohol
  • CMC carboxymethyl cellulose
  • TG tamarind gum
  • the operating conditions of the centrifugal flow coating apparatus are as follows: the slit air temperature is 55 ° C., the slit air flow rate is 20 NL / min, the rotating plate (rotor) rotational speed is 200 ppm, did.
  • the amount of binder in the adsorbent layer on the surface of the core material of the adsorbent-supported granules obtained under such conditions is shown in Table 1 below. Further, in order to prevent granulation between the adsorbent-carrying granules, the operation was continued for 5 minutes or more after the spraying of the activated carbon, and the granules were sufficiently dried. Table 1 below shows the finished water content and average particle size of the adsorbed and supported granules.
  • Example 2-1 Pulverized coal (Example 2-1), fine coal (Example 2-2), ordinary charcoal (Example 2-3) are used as the activated carbon, PVA is used as the binder, and the spraying speed and spray integration time of the binder aqueous solution are as follows.
  • Adsorbent-carrying granules were produced in the same manner as in Examples 1-1 to 1-3 except that the drying time was changed under the conditions shown in Table 1.
  • Table 1 below shows the ratio of PVA in the adsorbent layer on the surface of the core material of each adsorbent-supported granule, the finished moisture of the adsorbent-supported granule, and the average particle diameter.
  • Example 1-1 Example 1-1, except that fine coal (Example 2-2) was used as the activated carbon, PVA was used as the binder, and the drying time was changed under the conditions shown in Table 1 below for the spray rate and spray integration time of the aqueous binder solution.
  • Adsorbent-carrying granules were produced by the same method as in 1-3. Table 1 below shows the ratio of PVA in the adsorbent layer on the surface of the core material of each adsorbent-supported granule, the finished moisture of the adsorbent-supported granule, and the average particle diameter.
  • the ratio of the binder was calculated from the amount of the binder with respect to the total amount of the adsorbent (activated carbon) and the binder.
  • support granule were measured with the following method.
  • adsorbent-carrying granules were calculated using CAMSIZER (manufactured by HORIBA, Ltd.) or using an incremental-architecture type particle distribution measuring device, and the 50% median diameter of the equivalent sphere diameter was calculated as the average particle diameter.
  • the evaluation cigarette was produced according to the following method.
  • An acetate filter material without addition of triacetin having a length of 5 mm was inserted into a paper tube having an outer diameter of 7.7 mm and a length of 27 mm, and the above-described Examples 1-1 to 1-3 and Examples 2-1 to 2- 3 and the adsorbent-carrying granules obtained in Examples 3-1 to 3-3 were each inserted and filled with 30 mg of activated carbon, and then a 9 mm plasticizer-free acetate filter material was inserted to evaluate 9 types. Filter. Subsequently, the filter of the Salem Alaska menthol product was removed, and this filter was connected to one end of each evaluation filter with an adhesive tape to produce an evaluation cigarette.
  • two acetate filter materials with a length of 5 mm that are not filled with activated carbon and no plasticizer are inserted into the paper tube at a predetermined interval, and the filter of the Salem Alaska menthol product is bonded to one end of the filter for evaluation.
  • Control cigarettes were prepared by connecting with tape.
  • Ventilation Resistance Test The ventilation resistance of the filter was measured according to ISO 6565: 2002 (ISO 6565: 2002 Tobacco and tobacco product “Draw resistance of cigarettes and pressure drop of filter rods” Standard conditions and measurement).
  • Adsorption performance test of nicotine and tar in smoke under accelerated conditions An evaluation cigarette filled with granules of Examples 1-1 to 1-3 was held at a temperature of 22 ° C. and a humidity of 60% for 14 hours, and then a temperature of 55 ° C. and a humidity of 25 After repeating the operation of holding at 10% for 10 hours, it was stored for 1 week. These evaluation cigarettes after the acceleration test were subjected to the adsorption test of 2 above, and the adsorption performance of nicotine and tar in the smoke (nicotine and tar amount per cigarette after passing through the filter) was tested.
  • Table 2 below shows the ventilation resistance of these filters and the adsorption performance of nicotine and tar in low smoke.
  • Examples 1-4, 2-4, and 3-4 are evaluation cigarettes in which fine charcoal is filled in a paper tube instead of granules, and Example 2-5 is ordinary charcoal in paper tubes instead of granules. This is an example using a filled evaluation cigarette.
  • Examples 1-5, 2-6, and 2-5 are examples using control cigarettes.
  • GC was performed using an Agilent 7890 (Agilent Technologies Inc.). MSD was performed using Agilent 5975B (Agilent Technologies Inc.).
  • the adsorption rate (E i ) of the VOC component by each evaluation cigarette was obtained by the following formula by comparing the peak area of the chromatogram of the evaluation cigarette with the peak area of the chromatogram of the control cigarette.
  • E i (A i, in ⁇ A i, out ) / A i, in
  • a i, in and A i, out indicate the peak areas of the VOC component i in the smoke of the evaluation cigarette and the control cigarette, respectively.
  • FIG. 7 shows the adsorption rate of the initial VOC component of the evaluation cigarette equipped with the filter containing the adsorbent-carrying granules of Examples 1-1 to 1-3 and the fine coal of Example 1-4.
  • FIG. 8 shows the adsorption rate of the VOC components after the acceleration conditions described above of cigarettes equipped with filters containing the adsorbent-carrying granules of Examples 1-1 to 1-3 and the fine coal of Example 1-4.
  • FIG. 9 shows the adsorption rate of the initial VOC component of the evaluation cigarette equipped with the filter containing the adsorbent-carrying granules of Examples 2-1 to 2-3, the fine coal of Example 2-4, and the normal coal of Example 2-5. Indicates.
  • FIG. 10 shows the adsorption rate of the initial VOC component of the evaluation cigarette equipped with the filter containing the adsorbent-carrying granules of Examples 3-1 to 3-3 and the fine coal of Example 3-4.
  • the adsorbent-carrying granules of Examples 1-1 to 1-3 using PVA, CMC, and TG as binders are more effective than the fine coal of Example 1-4. It can be seen that the resistance can be reduced.
  • the adsorbent-carrying granules of Example 1-1 of the present invention using PVA as the binder are the adsorbent-carrying examples of Examples 1-2 and 1-3 using CMC and TG as the binder.
  • the adsorption performance of nicotine and tar is higher than that of the granules, and that the adsorption performance of nicotine and tar is almost the same as that of the fine coal of Example 1-4.
  • the adsorbent-carrying granules of Example 1-1 of the present invention using PVA as the binder are the adsorbent-carrying granules of Examples 1-2 and 1-3 using CMC and TG as the binder. It can be seen that the adsorption performance of the VOC component is higher than that of Example 1, and that the adsorption performance of the VOC component is as high as that of the fine coal of Example 1-4 alone. As is apparent from the results of FIG.
  • the adsorbent-carrying granules of Example 1-1 of the present invention using PVA as the binder have a high VOC component adsorption performance equivalent to that of the fine coal of Example 1-4 alone. It can be seen that
  • Example 2-4 As is apparent from the results in Table 2, the adsorbent-carrying granules of Examples 2-1 to 2-3 using PVA as the binder and pulverized coal, fine-grained coal, and ordinary charcoal as the activated carbon were obtained in Example 2-4. It can be seen that the ventilation resistance of the filter can be reduced as compared with fine-grained charcoal alone, and high nicotine and tar adsorption performance is exhibited. As is apparent from the results of FIG. 9, the adsorbent-carrying granules of Example 2-2 using PVA as the binder and fine coal with a particle size of 50 to 350 ⁇ m as the activated carbon are equivalent to the fine coal alone of Example 2-4.
  • the adsorption performance of the VOC component in smoke with a high level of smoke is exhibited.
  • the adsorbent-carrying granules of Example 2-1 using pulverized coal as the activated carbon hardly show the adsorption performance of the VOC component in the smoke. This is presumably because the pores on the surface of the pulverized coal supported on the core material were covered with PVA.
  • the adsorbent-carrying granules of Example 2-3 carrying normal charcoal have a slightly lower adsorption performance of the VOC component in the smoke than the normal charcoal alone of Example 2-5. Since the particle size of normal charcoal is close to that of granulated sugar, which is the core material, there is no merit of supporting normal charcoal on the core material.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Cigarettes, Filters, And Manufacturing Of Filters (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

La présente invention concerne des granulés à adsorbant supporté qui peuvent adsorber un composant COV (composé organique volatil) ou similaire dans la fumée de façon satisfaisante et dont chacun a un diamètre de grain plus grand que celui du charbon actif qui était utilisé dans les filtres à charbon classiques. Selon la présente invention, des granulés à adsorbant supporté peuvent être fournis, lesquels comprennent un adsorbant particulaire fin qui est supporté sur un matériau cœur par l'intermédiaire d'alcool polyvinylique, au moins la surface du matériau cœur étant non poreuse, et l'adsorbant particulaire fin étant plus petit que le matériau cœur et étant supporté sur le matériau cœur d'une manière telle que le rapport des teneurs d'alcool polyvinylique devient 6,7 % en poids ou moins par rapport à la quantité totale de l'adsorbant particulaire fin et de l'alcool polyvinylique.
PCT/JP2010/070489 2010-11-17 2010-11-17 Granulés à adsorbant supporté et leur procédé de fabrication, filtre à cigarette et cigarette WO2012066656A1 (fr)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017168516A1 (fr) * 2016-03-28 2017-10-05 日本たばこ産業株式会社 Filtre pour article à fumer, article à fumer et procédé de production de filtre pour article à fumer
CN113347895A (zh) * 2019-01-25 2021-09-03 日本烟草产业株式会社 吸烟物品用滤嘴
CN113492001A (zh) * 2020-04-03 2021-10-12 万华化学集团股份有限公司 气味吸附剂和制法及粘合剂体系和用途及无醛刨花板和制法
EP3868227A4 (fr) * 2018-10-18 2022-06-01 Japan Tobacco Inc. Produit à fumer, procédé de production dudit produit à fumer et procédé de distinction de charbon actif granulaire

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JPS5795816A (en) * 1980-12-08 1982-06-14 Kyocera Corp Molded body of activated carbon
JPH08506048A (ja) * 1993-01-27 1996-07-02 シラキュース ユニバーシティ 分子設計された活性炭素
JPH10128062A (ja) * 1996-10-25 1998-05-19 Kanegafuchi Chem Ind Co Ltd 焼却設備の排ガス処理剤
JP2009155215A (ja) * 2007-12-25 2009-07-16 Freunt Ind Co Ltd 球形粒及びその製造方法並びに放出制御製剤の製造方法
JP2009263303A (ja) * 2008-04-28 2009-11-12 Freunt Ind Co Ltd 球形顆粒及びその製造方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5795816A (en) * 1980-12-08 1982-06-14 Kyocera Corp Molded body of activated carbon
JPH08506048A (ja) * 1993-01-27 1996-07-02 シラキュース ユニバーシティ 分子設計された活性炭素
JPH10128062A (ja) * 1996-10-25 1998-05-19 Kanegafuchi Chem Ind Co Ltd 焼却設備の排ガス処理剤
JP2009155215A (ja) * 2007-12-25 2009-07-16 Freunt Ind Co Ltd 球形粒及びその製造方法並びに放出制御製剤の製造方法
JP2009263303A (ja) * 2008-04-28 2009-11-12 Freunt Ind Co Ltd 球形顆粒及びその製造方法

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017168516A1 (fr) * 2016-03-28 2017-10-05 日本たばこ産業株式会社 Filtre pour article à fumer, article à fumer et procédé de production de filtre pour article à fumer
JPWO2017168516A1 (ja) * 2016-03-28 2018-08-02 日本たばこ産業株式会社 喫煙物品用フィルター、喫煙物品、および喫煙物品用フィルターの製造方法
EP3868227A4 (fr) * 2018-10-18 2022-06-01 Japan Tobacco Inc. Produit à fumer, procédé de production dudit produit à fumer et procédé de distinction de charbon actif granulaire
CN113347895A (zh) * 2019-01-25 2021-09-03 日本烟草产业株式会社 吸烟物品用滤嘴
CN113492001A (zh) * 2020-04-03 2021-10-12 万华化学集团股份有限公司 气味吸附剂和制法及粘合剂体系和用途及无醛刨花板和制法
CN113492001B (zh) * 2020-04-03 2023-08-11 万华化学集团股份有限公司 气味吸附剂和制法及粘合剂体系和用途及无醛刨花板和制法

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