CN112369671A - Novel heating non-combustion cigarette filter tip rod and preparation method thereof - Google Patents

Novel heating non-combustion cigarette filter tip rod and preparation method thereof Download PDF

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Publication number
CN112369671A
CN112369671A CN202011279760.2A CN202011279760A CN112369671A CN 112369671 A CN112369671 A CN 112369671A CN 202011279760 A CN202011279760 A CN 202011279760A CN 112369671 A CN112369671 A CN 112369671A
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CN
China
Prior art keywords
sodium alginate
composite aerogel
filter tip
silicon dioxide
rod
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202011279760.2A
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Chinese (zh)
Inventor
周顺
王孝峰
王成虎
曹芸
陈鹏鹏
张健
毛昌杰
吴明元
石康中
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Anhui University
China Tobacco Anhui Industrial Co Ltd
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Anhui University
China Tobacco Anhui Industrial Co Ltd
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Publication date
Application filed by Anhui University, China Tobacco Anhui Industrial Co Ltd filed Critical Anhui University
Priority to CN202011279760.2A priority Critical patent/CN112369671A/en
Publication of CN112369671A publication Critical patent/CN112369671A/en
Pending legal-status Critical Current

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    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24DCIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D3/00Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
    • A24D3/06Use of materials for tobacco smoke filters
    • A24D3/14Use of materials for tobacco smoke filters of organic materials as additive
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24DCIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D1/00Cigars; Cigarettes
    • A24D1/20Cigarettes specially adapted for simulated smoking devices
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24DCIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D3/00Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
    • A24D3/02Manufacture of tobacco smoke filters
    • A24D3/0204Preliminary operations before the filter rod forming process, e.g. crimping, blooming
    • A24D3/0212Applying additives to filter materials
    • A24D3/0225Applying additives to filter materials with solid additives, e.g. incorporation of a granular product
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24DCIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D3/00Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
    • A24D3/06Use of materials for tobacco smoke filters
    • A24D3/08Use of materials for tobacco smoke filters of organic materials as carrier or major constituent
    • A24D3/10Use of materials for tobacco smoke filters of organic materials as carrier or major constituent of cellulose or cellulose derivatives

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

Abstract

The invention discloses a novel cigarette filter rod which is not combusted by heating and a preparation method thereof. The filter tip rod is uniformly filled with the sodium alginate-silicon dioxide composite aerogel, the porous structure of the filter tip rod can effectively intercept harmful substances in smoke, and can block heat transfer, so that the smoking experience is well improved, and the filter tip rod has wide application prospect in the field of heating non-combustible tobacco products.

Description

Novel heating non-combustion cigarette filter tip rod and preparation method thereof
Technical Field
The invention belongs to the technical field of adsorption filtering materials and tobacco, and particularly relates to a novel heating non-combustible cigarette filter rod and a preparation method thereof.
Background
Relevant researches show that the generation of various chemical substances in the smoke of the cigarettes is closely related to the combustion temperature of the cigarettes, and the harmfulness index of the cigarettes is increased along with the increase of the combustion temperature of the cigarettes. The smoke generated by the combustion of traditional cigarette products contains dozens of carcinogens. Unlike traditional cigarette, the cigarette without burning is one new kind of low temperature cigarette product designed based on the idea of heating without burning, and can heat tobacco leaf to the degree of giving out smell without igniting the tobacco leaf. Generally, when ordinary cigarettes are smoked, a plurality of harmful substances are generated due to high temperature, and when low-temperature cigarettes are smoked at the temperature of below 400 ℃, the harmful substances are greatly reduced. Under the environment of no smoking and control, the requirements on the retention performance of harmful ingredients in the smoking process of the novel tobacco products are stricter, but the retention performance of the traditional filter rod, such as a cellulose diacetate filter rod, is limited. Therefore, the development of a new type of heating non-combustion cigarette filter rod to improve the retention performance thereof has attracted extensive interest of researchers.
The silica aerogel is a light inorganic solid material with a three-dimensional network framework structure and nano-scale holes, has extremely high porosity and specific surface area, extremely low density and solid content, and simultaneously shows excellent heat insulation and fire prevention characteristics, the heat conductivity coefficient of the silica aerogel can be as low as below 0.011W/m.K, and the silica aerogel is the best one of all solid materials in terms of heat insulation performance, but the pure silica aerogel has extremely high brittleness. The sodium alginate is a polysaccharide natural polymer, has the advantages of wide source, good biocompatibility, biodegradability and the like, is used as a framework supporting material of the silica aerogel, and can effectively improve the toughness of the silica aerogel by preparing the sodium alginate-silica composite aerogel with a three-dimensional network structure by adopting a sol-gel method and a freeze drying technology.
For example, the sodium alginate-silicon dioxide composite aerogel can be compounded with the traditional cellulose diacetate filter rod by a proper method and a proper proportion, or the interception performance of the novel cigarette filter rod which is not combusted by heating can be effectively improved.
Disclosure of Invention
The invention provides a novel cigarette filter rod which is not burnt during heating, so that the interception performance of the filter rod can be improved by adding sodium alginate-silicon dioxide composite aerogel.
In order to achieve the purpose, the invention adopts the following technical scheme:
a novel heating non-combustion cigarette filter tip rod is characterized in that: the filter tip rod is obtained by molding cellulose diacetate tow, and the cellulose diacetate tow is uniformly filled with sodium alginate-silicon dioxide composite aerogel.
Further, the mass percentage of the sodium alginate-silicon dioxide composite aerogel in the filter rod is 5 +/-0.5%.
The preparation method of the novel cigarette filter tip rod which is not combusted by heating comprises the following steps: when the filter tip rod is formed by processing the cellulose diacetate tow, the sodium alginate-silicon dioxide composite aerogel and the cellulose diacetate tow are uniformly mixed and formed together, so that the sodium alginate-silicon dioxide composite aerogel is uniformly distributed in the filter tip rod.
Further, the sodium alginate-silicon dioxide composite aerogel is prepared by the following method:
dissolving 10-13 g of sodium alginate in 30mL of distilled water to form a sodium alginate solution; then adding 5mL of tetraethyl orthosilicate to obtain a layered solution with tetraethyl orthosilicate at the upper layer and sodium alginate solution at the lower layer; dropwise adding oxalic acid solution with the concentration of 0.1mol/L under magnetic stirring, and adjusting the pH to 3-5; stirring the obtained mixture at the temperature of 40-50 ℃ at the speed of 600-650 r/min for reaction for 7-9 h, and gradually converting the solution from two phases into a uniform phase along with the hydrolysis of tetraethyl orthosilicate until a uniform sol is formed;
pouring the obtained sol into a culture dish and aging for 48 hours to form stable gel; performing solvent exchange on the obtained gel by using deionized water, and removing the byproduct ethanol by replacement; and finally, freeze-drying the obtained gel at the temperature of minus 50 +/-2 ℃ by using a freeze dryer, and crushing the gel into powder by using a crusher to obtain the sodium alginate-silicon dioxide composite aerogel.
The invention has the beneficial effects that:
1. the filter tip rod is uniformly filled with the sodium alginate-silicon dioxide composite aerogel, the porous structure of the filter tip rod can effectively intercept harmful substances in smoke, and can block heat transfer so as to avoid the problem of mouth burning caused by overhigh smoke temperature, the sodium alginate is melted at high temperature and can carry away part of heat, the smoking experience is well promoted, and the filter tip rod has wide application prospect in the field of heating non-combustible tobacco products.
2. The sodium alginate-silicon dioxide composite aerogel is uniformly distributed in filter tip tow by a powder embedded adding technology in the process of forming a cellulose diacetate filter tip by using a filter tip forming machine, and has the advantages of simple preparation process, low production cost and lower requirements on equipment and process improvement.
3. The material used in the invention is not only harmless to human body, but also has the advantages of good biocompatibility, safety and environmental protection.
Drawings
Fig. 1 is a scanning electron microscope image of the sodium alginate-silica composite aerogel prepared in example 1 of the present invention;
FIG. 2 is a graph comparing the suction resistance before and after filling the composite aerogel with the cellulose diacetate filter rods of example 1 according to the invention;
FIG. 3 is a test chart of the tar content in the smoke before and after filling the composite aerogel into the cellulose diacetate filter rod in example 1 of the present invention;
fig. 4 is a smoke temperature test chart before and after filling the composite aerogel into the cellulose diacetate filter rod in example 1 of the present invention.
Detailed Description
The following examples are given to illustrate the present invention in detail, and the following examples are carried out on the premise of the technical solution of the present invention, and give detailed embodiments and specific procedures, but the scope of the present invention is not limited to the following examples.
Example 1
Dissolving 12.86g of sodium alginate in 30mL of distilled water at normal temperature to form a uniform sodium alginate solution; then adding 5mL of tetraethyl orthosilicate to obtain a layered solution with tetraethyl orthosilicate at the upper layer and sodium alginate solution at the lower layer; under magnetic stirring, 0.1mol/L oxalic acid solution is added drop by drop, and the pH is adjusted to about 4; stirring the obtained mixture at 40 ℃ at a speed of 600r/min for 8h, gradually converting the solution from two phases into a uniform phase along with the hydrolysis of tetraethyl orthosilicate, and simultaneously gradually converting the solution from light yellow to milky yellow and gradually increasing the viscosity of the solution due to the generation of ethanol until uniform sol is formed; then, pouring the obtained sol into a disposable round culture dish, and aging for 48h to further dehydrate and condense residual hydroxyl groups in the sol to form stable gel; performing solvent exchange on the obtained gel by using deionized water to ensure that a byproduct ethanol in the gel is completely replaced by the deionized water; and finally, freeze-drying the obtained gel at the temperature of-50 ℃ by using a freeze dryer, and crushing the gel into powder by using a crusher to obtain the sodium alginate-silicon dioxide composite aerogel, wherein the porosity of the sodium alginate-silicon dioxide composite aerogel is measured to be 95.3%. Fig. 1 is a scanning electron microscope image of the sodium alginate-silica composite aerogel prepared in this example, and it can be seen from the image that the microstructure of the composite aerogel is a uniform three-dimensional network porous structure, in which sodium alginate is a nano fibrous structure, and silica nanoparticles are attached to the nano fibrous structure.
When the filter tip rod is formed by processing the cellulose diacetate tow, the sodium alginate-silicon dioxide composite aerogel and the cellulose diacetate tow are uniformly mixed and formed together, so that the sodium alginate-silicon dioxide composite aerogel is uniformly distributed in the filter tip rod. The mass percentage of the sodium alginate-silicon dioxide composite aerogel in the filter rod is 5%.
FIG. 2 is a graph comparing the suction resistance before and after filling the composite aerogel with the cellulose diacetate filter rods of this example. The test conditions were: air was passed at a constant flow rate through the filter rods at a temperature of 20+/-3 ℃ and a humidity of 55 +/-3%, and the pressure difference was measured using a standard atmospheric pressure gauge. As can be seen from the figure: before the composite aerogel is not filled, the suction resistance of a standard filter stick of the tobacco product is 2800 Pa; after the composite aerogel is filled, the suction resistance of the novel filter rod is 2830Pa, although the suction resistance of the filter rod is slightly increased, the filter rod does not have obvious change, and the suction experience of a smoker is not influenced.
FIG. 3 is a test chart of the tar content of the smoke before and after the cellulose diacetate filter rod is filled with the composite aerogel (according to the GB/T19609-2004 standard), and it can be seen from the chart that: the tar content in the smoke of the standard filter stick not filled with the composite aerogel is 12.25 mg; the tar content in the smoke of the novel filter stick filled with the sodium alginate-silicon dioxide composite aerogel is 9.38mg, which is reduced by 2.87mg and 23.4% in a same ratio. Therefore, the filling of the composite aerogel can effectively reduce the tar content and reduce the harm to the eaters.
Fig. 4 is a smoke temperature test chart before and after the cellulose diacetate filter tip rod is filled with the composite aerogel, the circumference of a test experiment cigarette is 21.6mm, the total length is 35mm, a thermocouple is used for testing smoke release temperature at a position 2.2mm away from the plane of a filter tip, and the smoke is sucked every 30 s. Compared with a standard filter stick, the novel filter stick filled with the composite aerogel has the advantage that the smoke temperature is obviously reduced.
The above description is only exemplary of the present invention and should not be construed as limiting the present invention, and any modification, equivalent replacement, or improvement made within the principle of the present invention should be included in the protection scope of the present invention.

Claims (4)

1. A novel heating non-combustion cigarette filter tip rod is characterized in that: the filter tip rod is obtained by molding cellulose diacetate tow, and the cellulose diacetate tow is uniformly filled with sodium alginate-silicon dioxide composite aerogel.
2. A novel filter rod for a cigarette which is not burned by heat as set forth in claim 1, wherein: the mass percentage of the sodium alginate-silicon dioxide composite aerogel in the filter rod is 5 +/-0.5%.
3. A method for preparing a novel heating non-combustible cigarette filter rod according to claim 1 or 2, characterized in that: when the filter tip rod is formed by processing the cellulose diacetate tow, the sodium alginate-silicon dioxide composite aerogel and the cellulose diacetate tow are uniformly mixed and formed together, so that the sodium alginate-silicon dioxide composite aerogel is uniformly distributed in the filter tip rod.
4. The preparation method of claim 3, wherein the sodium alginate-silica composite aerogel is prepared by the following method:
dissolving 10-13 g of sodium alginate in 30mL of distilled water to form a sodium alginate solution; then adding 5mL of tetraethyl orthosilicate to obtain a layered solution with tetraethyl orthosilicate at the upper layer and sodium alginate solution at the lower layer; dropwise adding oxalic acid solution with the concentration of 0.1mol/L under magnetic stirring, and adjusting the pH to 3-5; stirring the obtained mixture at the temperature of 40-50 ℃ at the speed of 600-650 r/min for reaction for 7-9 h, and gradually converting the solution from two phases into a uniform phase along with the hydrolysis of tetraethyl orthosilicate until a uniform sol is formed;
pouring the obtained sol into a culture dish and aging for 48 hours to form stable gel; performing solvent exchange on the obtained gel by using deionized water, and removing the byproduct ethanol by replacement; and finally, freeze-drying the obtained gel at the temperature of minus 50 +/-2 ℃ by using a freeze dryer, and crushing the gel into powder by using a crusher to obtain the sodium alginate-silicon dioxide composite aerogel.
CN202011279760.2A 2020-11-16 2020-11-16 Novel heating non-combustion cigarette filter tip rod and preparation method thereof Pending CN112369671A (en)

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Application Number Priority Date Filing Date Title
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103462221A (en) * 2013-05-30 2013-12-25 贵州中烟工业有限责任公司 Cigarette filter containing adsorption filtration layer and application thereof
CN105601983A (en) * 2016-03-10 2016-05-25 云南中烟工业有限责任公司 Natural polysaccharide aerogel, preparation method thereof and application thereof in cigarettes
CN106617287A (en) * 2016-09-18 2017-05-10 广西中烟工业有限责任公司 Preparation method of aerogel particle with smoke reducing function and its application in cigarette filter tip
CN107556516A (en) * 2017-07-27 2018-01-09 广西中烟工业有限责任公司 A kind of Nano-meter SiO_22The preparation method of chitosan three-dimensional gel and the application in cigarette filter
CN107556499A (en) * 2017-07-27 2018-01-09 广西中烟工业有限责任公司 A kind of preparation method of glucose crosslinking plural gel and the application in cigarette
CN111533133A (en) * 2020-04-08 2020-08-14 云南中烟工业有限责任公司 Silicon dioxide aerogel microsphere and preparation method and application thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103462221A (en) * 2013-05-30 2013-12-25 贵州中烟工业有限责任公司 Cigarette filter containing adsorption filtration layer and application thereof
CN105601983A (en) * 2016-03-10 2016-05-25 云南中烟工业有限责任公司 Natural polysaccharide aerogel, preparation method thereof and application thereof in cigarettes
CN106617287A (en) * 2016-09-18 2017-05-10 广西中烟工业有限责任公司 Preparation method of aerogel particle with smoke reducing function and its application in cigarette filter tip
CN107556516A (en) * 2017-07-27 2018-01-09 广西中烟工业有限责任公司 A kind of Nano-meter SiO_22The preparation method of chitosan three-dimensional gel and the application in cigarette filter
CN107556499A (en) * 2017-07-27 2018-01-09 广西中烟工业有限责任公司 A kind of preparation method of glucose crosslinking plural gel and the application in cigarette
CN111533133A (en) * 2020-04-08 2020-08-14 云南中烟工业有限责任公司 Silicon dioxide aerogel microsphere and preparation method and application thereof

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Application publication date: 20210219

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