CN103462221B - Cigarette filter containing adsorption filtration layer and application thereof - Google Patents

Cigarette filter containing adsorption filtration layer and application thereof Download PDF

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Publication number
CN103462221B
CN103462221B CN201310209494.XA CN201310209494A CN103462221B CN 103462221 B CN103462221 B CN 103462221B CN 201310209494 A CN201310209494 A CN 201310209494A CN 103462221 B CN103462221 B CN 103462221B
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tio
nanometer pipe
cigarette
cigarette filter
filtration layer
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CN103462221A (en
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刘剑
聂长春
姬厚伟
惠建权
黄正虹
冯勇
田旭
刘科乾
刘纳纳
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China Tobacco Guizhou Industrial Co Ltd
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China Tobacco Guizhou Industrial Co Ltd
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Abstract

The invention relates to the field of cigarette filters, in particular to a cigarette filter containing a TiO2 aquo-complex nanotube, TiO2 nanometer powder, activated carbon fiber, and SiO2 aerogel. The cigarette filter contains an adsorption filtration layer, wherein the adsorption filtration layer is formed by cellulose acetate fiber, the TiO2 aquo-complex nanotube, the TiO2 nanometer powder, the activated carbon fiber, and the SiO2 aerogel. According to the cigarette filter, the strong capacity of the TiO2 aquo-complex nanotub and the TiO2 nanometer powder on adsorbing ammonia, and the adsorption of the activated carbon fiber on tar and CO are creatively utilized, acetaldehyde, acetic acid and heavy metal ion are removed by the SiO2 aerogel, and the ultralong TiO2 aquo-complex nanotube and the activated carbon fiber can be firmly interweaved and mixed with the cellulose acetate fiber, so that the defects that in the prior art, the degradation of various components in main stream smoke of a cigarette is not obvious, and adsorbing agent is not easily interweaved and mixed with the cellulose acetate fiber are solved.

Description

A kind of cigarette filter containing adsorption filtration layer and uses thereof
Technical field
The present invention relates to cigarette filter field, be specifically related to a kind of containing overlength TiO 2hydrate nanometer pipe, TiO 2nano powder, active carbon fibre peacekeeping SiO 2cigarette filter of aeroge and uses thereof.
Background technology
Publication number CN1302570A discloses a kind of Dotoxicating tip filter for cigarette and production method thereof.Be characterized on the basis of existing filter tip filter course, add the absorption absorbed layer that layer of active carbon and calcium hydroxide mix, make absorption absorbed layer be close to filter course.
Publication number CN1383764A discloses and a kind ofly prepares method containing loess clay mineral cigarette and cigarette product obtained thus.Be characterized in preparing loess homogeneous suspension, this suspension is applied to cigarette filter, filler or encapsulation, dry subsequently.
Publication number CN101637307A discloses a kind of cigarette fiber filter tip of filtering off toxic matters and releasing microelement anions.Be characterized in that the nano-corpuscule made with chitin, tourmaline, medical stone, Organic Selenium, organic germanium, honeybee series of products mixture embeds raw silk rings acetate fiber and makes cigarette filter.
Above-mentioned prior art, has the following disadvantages: (1) degraded to compositions such as the ammonia in cigarette mainstream flue gas is not obvious; (2) adding material is particulate, and being not easy to interweaves with acetate fiber mixes, and is not suitable for the large-scale production of cigarette filter.
Summary of the invention
The object of the invention is to the defect overcoming prior art, provide a kind of containing overlength TiO 2hydrate nanometer pipe, TiO 2nano powder, active carbon fibre peacekeeping SiO 2the cigarette filter of aeroge, in cigarette burning and aspiration procedure, the Multiple components in absorption cigarette mainstream flue gas.
Technical scheme of the present invention is: a kind of cigarette filter, and containing adsorption filtration layer, described adsorption filtration layer is by acetate fiber, TiO 2hydrate nanometer pipe, TiO 2nano powder, NACF and SiO 2aeroge forms.
Cigarette filter of the present invention can also comprise the conventional complete acetate fiber section be made up of acetate fiber.
Preferably, adsorption filtration layer of the present invention is full of whole described cigarette filter; Or described adsorption filtration layer is positioned at the front end of described cigarette filter, middle part or rear end, jointly forms described cigarette filter with the complete acetate fiber section be made up of acetate fiber.Namely cigarette filter of the present invention is made up of the complete acetate fiber section that is made up of acetate fiber and adsorption filtration layer, or is made up of adsorption filtration layer completely.
Preferably, TiO in described adsorption filtration layer 2the content of hydrate nanometer pipe is no less than the 0.01wt% of the total acetate fiber content of cigarette filter; Described TiO 2the content of nano powder is TiO 25 ~ 20wt% of hydrate nanometer pipe, the content of described active carbon is TiO 21 ~ 10wt% of hydrate nanometer pipe; Described SiO 2the content of aeroge is TiO 25 ~ 20wt% of hydrate nanometer pipe.
More excellent, described TiO 2the content of hydrate nanometer pipe is the 0.01wt% ~ 10wt% of the total acetate fiber content of cigarette filter.
Because harm reduction cigarette filter of the present invention both can be made up of adsorption filtration layer completely, also can be spliced by acetate fiber section and adsorption filtration layer; Therefore, when harm reduction cigarette filter is made up of adsorption filtration layer completely, the total acetate fiber content of cigarette filter of the present invention is the acetate fiber content in adsorption filtration layer; When harm reduction cigarette filter is spliced to form by acetate fiber section and adsorption filtration layer, the total acetate fiber content of cigarette filter of the present invention comprises the acetate fiber of acetate fiber section and acetate fiber two parts of adsorption filtration layer.
Preferably, described TiO 2the length of hydrate nanometer pipe is more than or equal to 1 micron, and diameter is 5 ~ 100nm.
More excellent, described TiO 2the length of hydrate nanometer pipe is 5 ~ 25 microns.
TiO of the present invention 2the preparation method of hydrate nanometer pipe is hydrothermal reaction at low temperature, with titanium dioxide and alkali for raw material, stirs hydro-thermal method, prepared the overlength TiO of high dispersive with low temperature 2hydrate nanometer pipe.
Preferably, described TiO 2the preparation method of hydrate nanometer pipe is as follows:
1) by TiO 2be dissolved in aqueous slkali and obtain mixture, at mixture being placed in autoclave 100 ~ 200 DEG C, carry out hydro-thermal reaction 18 ~ 96h with the rotating speed of 5 ~ 20r/min;
2) reaction terminates rear collection white precipitate product, and precipitated product, to neutrality, is soaked 18 ~ 24h by distilled water washing in acid solution, and reaction terminates rear suction filtration and washing precipitation is extremely neutral, dries precipitation, obtains TiO 2hydrate nanometer pipe.
As the TiO of raw material in preparation method of the present invention 2for business level TiO 2.Preferably, described TiO 2for P25 type nano titanium oxide.The described TiO that the present invention obtains 2hydrate is H 2ti 3o 7nH 2o; Preferably, n value 1 or 2.
Preferably, in mixture described in step 1), TiO 2mass percent be 0.1% ~ 10%.
More excellent, in mixture described in step 1), TiO 2mass percent be 0.13% ~ 6.67%.
Preferably, aqueous slkali described in step 1) is the NaOH aqueous solution or the KOH aqueous solution.
More excellent, the concentration of the described NaOH aqueous solution or the KOH aqueous solution is 8 ~ 12M.Most preferably be 10M.
Preferably, step 2) described acid solution is hydrochloric acid or nitric acid (hydrochloric acid or nitric acid are aqueous acid).
More excellent, the concentration of described acid solution is 0.001 ~ 2M.
Preferably, described bake out temperature is 55 ~ 65 DEG C.More excellent, described bake out temperature is 60 DEG C.
Preferably, described TiO 2the particle diameter of nano powder is 6 ~ 30nm.
Preferably, the particle diameter of described NACF is 5 ~ 100 microns.More excellent, the specific area of described NACF is 1000m 2/ more than g (is preferably 1000 ~ 1300m 2/ g).
Preferably, described SiO 2the particle diameter of aeroge is 2 ~ 5nm.More excellent, described SiO 2the specific area of aeroge is 1000m 2/ more than g.
In cigarette filter of the present invention, described TiO 2hydrate nanometer pipe, NACF interweave with acetate fiber and mix, and fill TiO in its gap 2nano powder and SiO 2aeroge nano powder, the common adsorption filtration layer forming cigarette filter.Further, adsorption filtration layer of the present invention both as whole cigarette filter, also as a wherein part for cigarette filter, can be positioned at the front end of cigarette filter, middle part or rear end.
TiO 2hydrate nanometer pipe has the ability of very strong adsorb ammonia; NACF has strong adsorption capacity to tar, CO; Meanwhile, overlength TiO 2nanotube and NACF firmly can interweave with acetate fiber and mix, and in addition, its gap is by TiO ammonia being had to strong adsorption capacity 2nano powder and acetaldehyde, acetic acid, heavy metal ion are had to the SiO of strong adsorption capacity 2aerogel powder is filled, and therefore, not obvious and adsorbent not easily interweaves with acetate fiber the defect mixed to ingredient degradation such as ammonia of main stream smoke of cigarettes to solve existing technology.
Secondly the present invention also discloses aforesaid roll tobacco filters for adsorbing and removing the purposes of Multiple components in cigarette mainstream flue gas.
In described cigarette mainstream flue gas, Multiple components comprises tar, carbon monoxide, ammonia, acetaldehyde, acetic acid and/or heavy metal ion.
The present invention finally also discloses a kind of cigarette, containing aforesaid roll tobacco filters.
TiO 2hydrate nanometer pipe be shorter in length than 1 micron time, not easily mix with acetate fiber, firmly will interweave with acetate fiber and mix, its length needs more than 1 micron, and optimum length is more than 5 microns; TiO 2hydrate nanometer pipe diameter is advisable in 5 to 100 nanometers, when being less than 5 nanometer, and its bad dispersibility, not easy to operate, when being greater than 100 nanometer, its specific area is little, reduces the adsorption capacity of Related Component in main flue gas; TiO in the adsorption filtration layer of cigarette filter 2hydrate nanometer pipe content (weight ratio) is acetate fiber 0.01% to 10% is advisable, and when being less than 0.01%, its content is low, reduces the adsorption capacity of Related Component in main flume, and when being greater than 10%, cost improves.NACF specific area is greater than 1000m 2/ g is suitable, is less than 1000m 2during/g, adsorption capacity declines, and its particle diameter is 5 to 100 microns and is suitable for, and when being less than 5 microns, easily break, not easy to operate, when being greater than 100 microns, specific area is little, and adsorption capacity reduces, and its content (weight ratio) is TiO 21% to 10% of hydrate nanometer pipe is advisable, and when being less than 1%, affecting performance and improve, when being greater than 10%, cost improves.TiO 2when the particle diameter of nano powder is less than 6 nanometer, its bad dispersibility, not easy to operate, when being greater than 30 nanometer, its specific area is little, and adsorption capacity reduces; TiO 2the content (weight ratio) of nano powder is TiO 25% to 20% of hydrate nanometer pipe is advisable, lower than 5% time, gap filling amount is low, affects the raising of absorption property, and when being greater than 20%, powder easily comes off from gap.SiO 2the specific area 1000m of aeroge 2/ more than g is advisable, lower than 1000m 2during/g, affect absorption property, primary particle size 2 to 5 nanometer is advisable, and during lower than 2 nanometer, bad dispersibility, not easy to operate, when being greater than 5 nanometer, specific area reduces, and affect absorption property, its weight ratio is TiO 25% to 20% of hydrate nanometer pipe is advisable, lower than 5% time, gap filling amount is low, affects absorption property, and when being greater than 20%, powder easily comes off from gap.
Beneficial effect of the present invention is: TiO 2hydrate nanometer pipe and TiO 2nano powder all has very strong adsorb ammonia ability, and activated carbon fiber has strong absorption affinity to the tar in flue gas and carbon monoxide; And SiO 2aeroge has strong adsorption capacity to acetaldehyde, acetic acid and heavy metal ion; Four actings in conjunction, solve prior art and not easily to interweave with acetate fiber the defect mixed to the not obvious and adsorbent of Multiple components degraded in cigarette mainstream flue gas.
Accompanying drawing explanation
Fig. 1: TiO 2hydrate nanometer pipe scanning electron microscope (SEM) photograph
Fig. 2: TiO 2hydrate nanometer pipe scanning electron microscope (SEM) photograph
Fig. 3: adsorption filtration layer is as whole cigarette filter
Fig. 4: absorption filtering layer is as a part (front end) for cigarette filter
Fig. 5: adsorption filtration layer is as a part (middle part) for cigarette filter
Fig. 6: adsorption filtration layer is as a part (rear end) for cigarette filter
1. cigarette filter 11. adsorption filtration layer 12. acetate fiber section
Detailed description of the invention
The present invention is set forth further below in conjunction with embodiment.Should be understood that embodiment only for illustration of the present invention, but not limit the scope of the invention.
Embodiment 1TiO 2the preparation of hydrate nanometer pipe
1. preparation method:
Method 1: by 2g business level TiO 2(P25) be dissolved in 75ml10M NaOH solution, mixture moved into 100mL autoclave and put into oil bath pan, hydro-thermal 24h under the rotating speed of the temperature ranges of 150 DEG C and 10r/min.The white precipitate obtained after reaction terminates is washed with distilled water to neutrality, soaks 24h subsequently in acid solution, then suction filtration drip washing is to neutral, 60 DEG C of oven dry, finally obtains TiO 2hydrate nanometer pipe.
Method 2: by 0.1g business level TiO 2(P25) be dissolved in 75ml8M NaOH solution, mixture moved into 100mL autoclave and put into oil bath pan, hydro-thermal 18h under the rotating speed of the temperature ranges of 200 DEG C and 5r/min.The white precipitate obtained after reaction terminates is washed with distilled water to neutrality, soaks 20h subsequently in acid solution, then suction filtration drip washing is to neutral, 55 DEG C of oven dry, finally obtains TiO 2hydrate nanometer pipe.
Method 3: by 5g business level TiO 2(P25) be dissolved in 75ml12M KOH solution, mixture moved into 100mL autoclave and put into oil bath pan, hydro-thermal 72h under the rotating speed of the temperature ranges of 100 DEG C and 20r/min.The white precipitate obtained after reaction terminates is washed with distilled water to neutrality, soaks 18h subsequently in acid solution, then suction filtration drip washing is to neutral, 65 DEG C of oven dry, finally obtains TiO 2hydrate nanometer pipe.
2. product characterizes
To the TiO that preceding method prepares 2hydrate nanometer pipe carries out scanning electron microscope analysis, known TiO 2hydrate nanometer length of tube is 1-25um, and diameter is about 100nm, specifically sees Fig. 1-2.Figure 1 shows TiO prepared by embodiment 1 2eSEM (SEM) photo (multiplication factor 2000 times) of hydrate nanometer pipe, can find out TiO 2hydrate nanometer pipe in tubular construction, favorable dispersibility, length is about 1-25um; Figure 2 shows TiO prepared by embodiment 1 2eSEM (SEM) photo (multiplication factor 30000 times) of hydrate nanometer pipe.TiO can be found out 2in tubular construction, favorable dispersibility, pollution-free on tube wall, diameter is about 100nm to hydrate nanometer pipe.
The preparation of embodiment 2 cigarette filter
1. raw material
Process raw material: TiO 2nano powder, purchased from ISHIHARA SANGYO KAISYA, LTD.; Acetate fiber, purchased from Guizhou Zhong Yan Industrial Co., Ltd; NACF, purchased from Nantong Xin Tong NACF Co., Ltd.
SiO 2aerogel powder, adopt the preparation of soda acid two-step catalysis synthetic method: by ethyl orthosilicate and a certain amount of ethanol mix and blend, add hydrochloric acid and alcohol mixed solution carries out acid catalysis, the mixed solution of ammoniacal liquor and ethanol is added again after ethyl orthosilicate is fully hydrolyzed, carry out base catalysis, agingly finally obtain SiO afterwards 2colloidal sol, gained SiO 2the specific area of colloidal sol is 500m 2/ g, particle diameter to be 6nm(concrete preparation method application reference number be 201010205734.5 patent " a kind of method of preparing super-hydrophobic silica aerogel at normal pressure ").
2. the preparation of cigarette filter
Method one:
By TiO prepared by embodiment 1 2hydrate nanometer pipe and NACF, TiO 2nano powder, SiO 2aerogel powder and acetate fiber mixing: first by TiO 2hydrate nanometer pipe and acetate fiber mixing, finally mix NACF, TiO again 2nano powder and SiO2 aerogel powder, uniform interleaving mixes, and prepares the adsorption filtration layer of cigarette filter.Wherein, TiO in adsorption filtration layer 2the quality of hydrate nanometer pipe is 10%, TiO of the total acetate fiber quality of cigarette filter 2the quality of nano powder is TiO 25% of hydrate nanometer pipe quality, the quality of NACF is TiO 25% of hydrate nanometer pipe quality; SiO 2the quality of aeroge is TiO 210% of hydrate nanometer pipe quality.
Adopt the adsorption filtration layer of previous step to prepare filter stick by the industrialization forming step of filter stick, cutting, obtain cigarette filter.In the inventive method, containing TiO 2as a filter tip part, (middle part, as shown in Figure 5), splices with the complete acetate fiber section be made up of acetate fiber the adsorption filtration layer of hydrate nanometer pipe, obtains cigarette filter.
Method two:
By TiO prepared by embodiment 1 2hydrate nanometer pipe, acetate fiber, TiO 2nano powder, NACF and SiO 2aeroge is mixed with the adsorption filtration layer of cigarette filter, wherein TiO in adsorption filtration layer 2the quality of hydrate nanometer pipe is 1%, TiO of the total acetate fiber quality of cigarette filter 2the quality of nano powder is TiO 210% of hydrate nanometer pipe, the quality of NACF is TiO 210% of hydrate nanometer pipe quality; SiO 2the quality of aeroge is TiO 220% of hydrate nanometer pipe quality.
The adsorption filtration layer of previous step is adopted to prepare filter stick by the industrialization forming step of filter stick, and containing TiO 2as a filter tip part, (front end, as shown in Figure 4), splices with the complete acetate fiber section be made up of acetate fiber the filter course of hydrate nanometer pipe, obtains cigarette filter.
Method three:
By TiO prepared by embodiment 1 2hydrate nanometer pipe, acetate fiber, TiO 2nano powder, NACF and SiO 2aeroge is mixed with the adsorption filtration layer of cigarette filter, wherein, and TiO in adsorption filtration layer 2the quality of hydrate nanometer pipe is 0.01%, TiO of the total acetate fiber quality of cigarette filter 2the quality of nano powder is TiO 220% of hydrate nanometer pipe, the quality of NACF is TiO 21% of hydrate nanometer pipe quality; SiO 2the quality of aeroge is TiO 25% of hydrate nanometer pipe quality.
The adsorption filtration layer of previous step is adopted to prepare filter stick by the industrialization forming step of filter stick, and containing TiO 2as a filter tip part, (rear end, as shown in Figure 6), splices with the complete acetate fiber section be made up of acetate fiber the filter course of hydrate nanometer pipe, obtains cigarette filter.
The detection of embodiment 3 filter tip adsorption filtration effect
1. experimental technique
Experimental subjects: prepare filter tip according to embodiment 2, adsorption filtration layer is positioned at filter stick front end, wherein TiO in adsorption filtration layer 2the quality of hydrate nanometer pipe is 10%, TiO of total acetate fiber quality 2the quality of nano powder is TiO 25% of hydrate nanometer pipe quality, the quality of NACF is TiO 25% of hydrate nanometer pipe quality; SiO 2the quality of aeroge is TiO 210% of hydrate nanometer pipe quality.Prepare cigarette with this filter tip, obtain the cigarette containing adsorption filtration layer in filter tip.
Contrast: adopt the filter tip be made up of acetate fiber completely, prepare cigarette sample in contrast.
Detection method: the detection method reference of filter tip adsorption filtration effect: the mensuration of YC/T377-2010 ammonia of main stream smoke of cigarette; GB/T19609-2004 cigarette conventional analysis smoking machine measures TPM and tar; The mensuration of carbon monoxide in GB/T23356-2009 components in cigarette smoke gas phase; The mensuration of YC/T254-2008 main carbonyl compounds in main stream cigarette smoke.
2. experimental result
See the following form containing the result of the test that the cigarette of adsorption filtration layer is reducing Multiple components burst size in cigarette mainstream flue gas in the filter tip obtained by preceding method:
Containing the adsorption filtration effect of the cigarette of adsorption filtration layer in table 1 filter tip
Experimental result shows: the filter-tip cigarette had containing above-mentioned adsorption filtration layer obviously can reduce the burst size of the Multiple components such as ammonia of main stream smoke of cigarette.

Claims (6)

1. a cigarette filter, containing adsorption filtration layer, is characterized in that, described adsorption filtration layer is by acetate fiber, TiO 2hydrate nanometer pipe, TiO 2nano powder, NACF and SiO 2aeroge forms; TiO in described adsorption filtration layer 2the content of hydrate nanometer pipe is the 0.01wt% ~ 10wt% of the total acetate fiber quality of cigarette filter; Described TiO 2the content of nano powder is TiO 25 ~ 20wt% of hydrate nanometer pipe, the content of described active carbon is TiO 21 ~ 10wt% of hydrate nanometer pipe; Described SiO 2the content of aeroge is TiO 25 ~ 20wt% of hydrate nanometer pipe; Described TiO 2the length of hydrate nanometer pipe is more than or equal to 1 micron, and diameter is 5 ~ 100nm; Described TiO 2the particle diameter of nano powder is 6 ~ 30nm; The particle diameter of described NACF is 5 ~ 100 microns; Described SiO 2the particle diameter of aeroge is 2 ~ 5nm.
2. cigarette filter as claimed in claim 1, is characterized in that, described TiO 2hydrate nanometer pipe is adopted and is prepared with the following method:
1) by TiO 2be dissolved in aqueous slkali and obtain mixture, at mixture being placed in autoclave 100 ~ 200 DEG C, carry out hydro-thermal reaction 18 ~ 96h with the rotating speed of 5 ~ 20r/min;
2) reaction terminates rear collection white precipitate product, and precipitated product, to neutrality, is soaked 18 ~ 24h by distilled water washing in acid solution, and reaction terminates rear suction filtration and washing precipitation is extremely neutral, dries precipitation, obtains TiO 2hydrate nanometer pipe.
3. cigarette filter as claimed in claim 2, is characterized in that, step 1) in described mixture, TiO 2mass percent be 0.1% ~ 10%.
4. cigarette filter described in the arbitrary claim of claim 1-3 is for adsorbing and removing the purposes of Multiple components in cigarette mainstream flue gas.
5. purposes as claimed in claim 4, it is characterized in that, in described cigarette mainstream flue gas, Multiple components comprises tar, carbon monoxide, ammonia, acetaldehyde, acetic acid and/or heavy metal ion.
6. a cigarette, containing cigarette filter described in the arbitrary claim of claim 1-3.
CN201310209494.XA 2013-05-30 2013-05-30 Cigarette filter containing adsorption filtration layer and application thereof Active CN103462221B (en)

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CN104126871A (en) * 2014-07-18 2014-11-05 云南中烟工业有限责任公司 Application of silsesquioxane bridged aerogel containing thioether chain segment and serving as filter-bridged filter tip material
CN105105333B (en) * 2015-07-17 2018-11-09 云南中烟工业有限责任公司 It is a kind of it is effective reduce flue gas metal ion content additives of filter tip and application
US11717018B2 (en) * 2016-02-24 2023-08-08 R.J. Reynolds Tobacco Company Smoking article comprising aerogel
CN108903055B (en) * 2018-08-17 2020-11-27 绍兴恒元机械制造有限公司 Preparation method of paper cigarette filter tip
CN109463796A (en) * 2018-10-10 2019-03-15 湖北中烟工业有限责任公司 A kind of glass fibre toughening composite aerogel and preparation method thereof
CN110250567A (en) * 2019-05-08 2019-09-20 中山市博海精细化工有限公司 A kind of environment-friendly cigarette filter tip filler and preparation method
CN112369671A (en) * 2020-11-16 2021-02-19 安徽中烟工业有限责任公司 Novel heating non-combustion cigarette filter tip rod and preparation method thereof
CN113735556B (en) * 2021-08-13 2022-12-20 红塔烟草(集团)有限责任公司 Silicon-containing aerogel composite material and preparation method and application thereof
CN113944065B (en) * 2021-09-29 2023-03-21 河南中烟工业有限责任公司 Harm-reducing cigarette paper and preparation method thereof

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CN101019692A (en) * 2007-03-22 2007-08-22 何金星 Filter rod and filter tip with mixed active carbon fiber
JP2011517574A (en) * 2008-04-14 2011-06-16 ナノスケール コーポレーション Methods for neutralizing, adsorbing and absorbing toxic or unwanted compounds in tobacco products
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