CN102794154B - Use of amino-functional material for reducing hydrogen cyanide content of cigarette smoke - Google Patents
Use of amino-functional material for reducing hydrogen cyanide content of cigarette smoke Download PDFInfo
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- CN102794154B CN102794154B CN201210299491.5A CN201210299491A CN102794154B CN 102794154 B CN102794154 B CN 102794154B CN 201210299491 A CN201210299491 A CN 201210299491A CN 102794154 B CN102794154 B CN 102794154B
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Abstract
The invention relates a use of a functional material in a cigarette field and especially relates to a use of an amino-functional material for reducing hydrogen cyanide content of cigarette main smoke. The amino-functional material is an amino-functional mesoporous silica adsorption material. The amino-functional mesoporous silica adsorption material MCM41 having a high specific surface area has an effect of obviously reducing hydrogen cyanide content of cigarette main smoke, has an adsorption rate of 20.5%, reduces the damage on a smoker and does not influence a cigarette taste. The amino-functional mesoporous silica adsorption material MCM41 has a high specific surface area of 300 to 550m<2>/g and uniform aperture sizes of 1.2 to 1.8nm, and also has a good hydrogen cyanide adsorption effect. A method for preparing a composite filter tip from the amino-functional mesoporous silica adsorption material MCM41 is simple, is convenient for operation and has a low cost.
Description
Technical field
The present invention relates to the application of the functional material in cigarette field, relate in particular to a kind of application of mesopore silicon oxide sorbing material of the amino functional that reduces hydrogenation cyanogen content in cigarette mainstream flue gas.
Background technology
Hydrogen cyanide is a kind of category-A violent in toxicity, is colourless or light blue liquid or gas under normal temperature, has almond sample smell, mildly bitter flavor, and water soluble, ethanol, be slightly soluble in ether, and its aqueous solution is faintly acid.Hydrogen cyanide, through sucking, can replace the oxygen in ferroheme, generates cyanohemoglobin, hemoglobin is lost and transmit the effect of oxygen, causes histanoxia and poisoning, very large to human health damage.
The mankind's activity can cause the formation of cyanide.As all contained hydrogen cyanide in the smog of vehicle exhaust and cigarette, burn some plastics and wool also can produce hydrogen cyanide.Hydrogen cyanide in cigarette smoke is mainly generated in the lower reaction of high temperature (700-1000 DEG C) by related compounds such as amino acid, content is about 30-200 μ g/ and props up, although content is not high, but studying the security of effective harm reduction technology raising cigarette smoke, is to be related to the healthy important topic of the public.
Up to now, in the cigarette of research reduction both at home and abroad, the method for harmful components mainly comprises: adsorption filtration method, dilution method, direct oxidation method and catalytic oxidation.Filter tip ventilation dilution method is the current external a kind of reducing tar and reducing harm technology extensively adopting, but it is larger on the impact of cigarette flavor amount, and acceptance level is lower at home, in the development of Chinese-style cigarette and application, has certain difficulty.Adsorption filtration method is studied more extensive at home and abroad, loaded metal ion on active carbon and active carbon (WO99/11358 (1999)) can effectively adsorb the harmful substances such as hydrogen cyanide, but larger on the impact of cigarette style, bring offending sensation to smoker.The patented technology such as CN141695A and CN1462652A is used catalytic oxidation effect in hydrogen cyanide in reduction cigarette, show higher catalytic activity, but production cost is higher, in process of production, also have skewness phenomenon in single cigarette, the defect such as wayward.
Meso pore silicon oxide material is the material system rising over nearly 20 years, be characterized in having regular pore passage structure and adjustable aperture, larger specific area and pore volume, good heat endurance and chemical stability, along with going deep into of the preparation research of people to mesopore silicon oxide, obtain the meso pore silicon oxide material of multiple series, as MCM, SBA, the series such as FDU and AMS, the people such as Liu Shaomin " Chinese tobacco journal " have reported that the 20th page to 24 pages of the 12nd the 4th phases of volume of August in 2006 mesopore silicon oxide (M48 and metal-doped M48) material is used for removing cigarette smoke benzo [a] pyrene, the Guo actor playing a martial role in Chinese operas of South China Science & Engineering University has reported in master thesis that in 2010 hexagonal mesoporous silicas (HMS) is to nicotine, tar, CO, the harmful substances such as low molecule group compounds of aldehydes and ketones have certain reducing poison function, the Zhao Na of South China Science & Engineering University has reported in master thesis that in 2010 hexagonal mesoporous silicas (HMS) has certain reducing poison function to nicotine and tar, monarch Shu Li of South China Science & Engineering University has reported in Master's thesis that in 2011 hexagonal mesoporous silicas (HMS) has certain Jiaozhuo that falls and uses.
But the high-specific-surface mesoporous silica adsorbent with amino functional there is not yet bibliographical information for reducing the hydrogen cyanide in cigarette mainstream flue gas, still need to continue to explore suitable technology and method.
Summary of the invention
In view of the shortcoming of above-mentioned prior art, the object of the present invention is to provide the application of a kind of amino functional meso pore silicon oxide material that reduces the hydrogen cyanide content in cigarette mainstream flue gas in cigarette mainstream flue gas, to solve absorption and the removal problem of hydrogenation cyanogen in cigarette mainstream flue gas.
For achieving the above object and other relevant objects, the present invention adopts following technical scheme:
An application for the mesopore silicon oxide adsorbent of the amino functional of high-specific surface area hydrogen cyanide content in reduction cigarette mainstream flue gas, this kind of adsorbent is carry out amino functional on mesopore silicon oxide surface and obtain.
Preferably, described mesopore silicon oxide is MCM41, and its specific area is 500-950m
2/ g, aperture is 1.5-2.5nm.
Preferably, the mesopore silicon oxide MCM41 that the mesopore silicon oxide of described amino functional is amino functional, its specific area is 300-550m
2/ g, aperture is 1.2-1.8nm.
Preferably, in the mesopore silicon oxide MCM41 of described amino functional, the amino amount of contained functionalization is 1.2-2.2mmol/g.
Preferably, the mesopore silicon oxide adsorbent of the amino functional of described high-specific surface area being applied as of hydrogen cyanide content in reduction cigarette mainstream flue gas added the mesopore silicon oxide MCM41 adsorbent of amino functional in cigarette filter to, for reducing the content of hydrogen cyanide in cigarette mainstream flue gas, specifically comprise the steps:
(1) the mesopore silicon oxide MCM41 adsorbent of amino functional is sieved, choose the absorbent particles of 80-100 order particle diameter;
(2) absorbent particles of choosing is placed in to filter-tip intermediate layer, forms the composite filter-tip of sandwich type with the cellulose acetate filter the upper and lower of not adding adsorbent; Or the absorbent particles of choosing is evenly sprayed on to the acetate fibres interfascicular of filter stick, and forms the composite filter-tip of levels structure with the filter stick that does not add absorbent particles; Wherein in every cigarette composite filter tip, the amount of the mesopore silicon oxide MCM41 adsorbent of contained amino functional is 20 ~ 60mg.
In above-mentioned steps (2), the composite filter-tip of sandwich type comprise do not add adsorbent acetate fiber upper strata, be filled with the absorption intermediate layer of absorbent particles and do not add the acetate fiber lower floor of adsorbent.
In above-mentioned steps (2), in the composite filter-tip of levels structure, upper strata is the filter stick layer that does not add absorbent particles, and lower floor is the filter stick lower floor of evenly spraying the absorbent particles of choosing.
The mesopore silicon oxide adsorbent of the amino functional of high-specific surface area of the present invention makes through the method for following steps:
1) preparation of mesopore silicon oxide MCM41: taking cetrimonium bromide (CTABr) as structure directing agent, taking tetraethyl orthosilicate ester (TEOS) as silicon source, first structure directing agent is dissolved in NaOH solution, add again silicon source and stir, then by the mixed liquor of acquisition successively through hydrolysis, aging, filter, the step such as washing, dry and roasting makes the mesopore silicon oxide MCM41 with high specific surface area.
2) preparation of the mesopore silicon oxide MCM41 adsorbent of amino functional: by the mesopore silicon oxide MCM-41 newly making, adding volume ratio is fully to mix in the 3-Propylamino trimethoxy silane (APTMS) of 1:1 and the mixed solution of the new toluene steaming, then in oil bath, at 120 DEG C, stir 3 ~ 6 hours, be cooled to after room temperature, with obtaining intermediate products after sand hopper suction filtration, intermediate products are adopted to toluene and the each washed twice of acetone successively, remove unreacted and be adsorbed on the APTMS in intermediate products duct, again through 120 DEG C of vacuum drying, can obtain amido modified MCM41 material, the i.e. mesopore silicon oxide MCM41 adsorbent of the amino functional of described high-specific surface area, its specific area is 300-550m
2/ g, aperture is 1.2-1.8nm.
Compared with prior art, the present invention has following beneficial effect:
In prior art, also the MCM41 sorbent material of the amino functional of high-specific surface area is not applied to and reduces in cigarette smoke in hydrogenation cyanogen content.The MCM41 adsorbent of the amino functional of the present invention's high-specific surface area used has the feature of hydrogenation cyanogen content in remarkable reduction cigarette mainstream flue gas, and adsorption rate can reach 20.5%; In reducing the harm that smoker is caused, do not affect the mouthfeel of cigarette simultaneously.The mesopore silicon oxide MCM41 adsorbent of prepared amino functional has high-specific surface area, and aperture is even, and its specific area is 300-550m
2/ g, aperture is 1.2-1.8nm, adsorbs the effective of hydrogenation cyanogen.Adopt the preparation method of mesopore silicon oxide MCM41 absorbent preparation composite filter-tip of amino functional of the present invention simple, easy to operate, cost is low.
Brief description of the drawings
Fig. 1 is the powder diffraction spectrum of amination meso pore silicon oxide material.
Fig. 2 is the ESEM phenogram of amination meso pore silicon oxide material.
Fig. 3 is the nitrogen adsorption isotherm of amination meso pore silicon oxide material.
Fig. 4 is amination meso pore silicon oxide material
13c (CP/MAS) NMR solid-state nuclear magnetic resonance collection of illustrative plates.
Detailed description of the invention
Below, by specific instantiation explanation embodiments of the present invention, those skilled in the art can understand other advantages of the present invention and effect easily by the disclosed content of this description.The present invention can also be implemented or be applied by other different detailed description of the invention, and the every details in this description also can be based on different viewpoints and application, carries out various modifications or change not deviating under spirit of the present invention.Should be clear and definite, described embodiment is only a part of embodiment of the present invention, instead of whole embodiment, is intended to illustrate the present invention instead of limitation of the invention.Based on the embodiment in the present invention, the every other embodiment that those skilled in the art obtain under the prerequisite of not making creative work, belongs to the scope of protection of the invention.
The amino functional meso pore silicon oxide material of evaluation of the present invention being removed to hydrogenation cyanogen in cigarette mainstream flue gas is below described in detail.
Embodiment 1
The preparation of the mesopore silicon oxide MCM41 of the amino functional of high-specific surface area:
1, the preparation of mesopore silicon oxide MCM41: by 648g cetrimonium bromide (CTABr), the NaOH solution of the 2mol/L of 3500g water and 320g at room temperature mixes and stirring and dissolving, add again 350g tetraethyl orthosilicate ester (TEOS), continue at room temperature to stir 20 minutes, then be transferred in super constant temperature trough aging 2 days at 100 DEG C, filter, the filtrate of acquisition is washed with distilled water to nearly neutrality, then vacuum drying 24 hours at 80 DEG C, roasting 6 hours at 550 DEG C again, naturally cool to room temperature, obtain meso pore silicon oxide material MCM41.
2, the preparation of the mesopore silicon oxide MCM41 adsorbent of amino functional: get the above-mentioned mesopore silicon oxide MCM-41 newly making of 100g in 5L round-bottomed flask, adding people's volume ratio is the 3-Propylamino trimethoxy silane (APTMS) of 1:l and the mixed solution 2L of toluene (newly steaming), ultrasonic 10 minutes, then stir 4 hours the oil bath of 120 DEG C, be cooled to after room temperature, use sand hopper suction filtration, the intermediate products of acquisition are used to 500mL toluene and the each washed twice of 500mL acetone successively, remove unreacted and be adsorbed on the APTMS in intermediate products duct, again through 120 DEG C of vacuum drying 12 hours, obtain amido modified MCM41 material, it is the mesopore silicon oxide MCM41 adsorbent product of amino functional.
The mesopore silicon oxide MCM41 adsorbent product of the amino functional that the present embodiment is obtained obtains Fig. 1-Fig. 4 after testing, and wherein Fig. 1 is the powder diffraction spectrum of amination meso pore silicon oxide material; Fig. 2 is the ESEM phenogram of amination meso pore silicon oxide material; Fig. 3 is the nitrogen adsorption isotherm of amination meso pore silicon oxide material; Fig. 4 is amination meso pore silicon oxide material
13c (CP/MAS) NMR solid-state nuclear magnetic resonance collection of illustrative plates.
Can calculate specific area and the pore-size distribution of porous material according to nitrogen adsorption isotherm, the specific area of above-mentioned obtained mesopore silicon oxide MCM41 is 500-950m
2/ g, aperture is 1.5-2.5nm.The mesopore silicon oxide of above-mentioned obtained amino functional is the mesopore silicon oxide MCM41 of amino functional, and its specific area is 300-550m
2/ g(detects gained by Fig. 3), aperture is that 1.2-1.8nm(detects gained by Fig. 3).The amino amount that can calculate functionalization contained in the mesopore silicon oxide MCM41 of above-mentioned amino functional according to results of elemental analyses is 1.2-2.2mmol/g.
In Fig. 4
13there are three peaks (Fig. 4) in C (CP/MAS) NMR solid-state nuclear magnetic resonance collection of illustrative plates, respectively three carbon atoms in organic group on corresponding amido modified group
13c NMR signal, further proves that amination is successful.
The mesopore silicon oxide MCM41 adsorbent (hereinafter to be referred as adsorbent) of amino functional is sieved, choose the absorbent particles of 80-100 order particle diameter; Absorbent particles is placed in to common filter-tip intermediate layer, forms sandwich type composite filter tip with the cellulose acetate filter the upper and lower of not adding adsorbent, the amount containing adsorbent in every cigarette is 30mg.According to GB/T16447 requirement, cigarette sample used balance 48 hours at (22 ± 1) DEG C and under the condition of the relative humidity of (60 ± 3) %, through weight and resistance to suction sorting, pick out the experiment cigarette sample of uniformity, in the upper suction of Cerulean SM450 linear pattern smoking machine (Cerulean company of Britain).With diluted sodium hydroxide solution trapping main flume gas gas-phase objects; With cambridge filter trapping flue gas TPM, and extract with sodium hydroxide solution.Detect flue gas, the grain hydrogen cyanide in mutually with continuous-flow instrument respectively, the two measurement result sum is the burst size of cigarette mainstream flue gas hydrogenation cyanogen, concrete detection method is with reference to professional standard YC/T253-2008, result shows, contrast with the filter-tip cigarette that does not add adsorbent, the present invention's adsorbent used can make the content of hydrogen cyanide in main flume decline 20.5%.
Embodiment 2
Prepare the mesopore silicon oxide MCM41 adsorbent of the amino functional of the high-specific surface area of the present embodiment according to the method step of embodiment 1.The mesopore silicon oxide MCM41 adsorbent (hereinafter to be referred as adsorbent) of the amino functional that the present embodiment is obtained sieves, and chooses the absorbent particles of 80-100 order particle diameter; Absorbent particles is placed in to common filter-tip intermediate layer, forms sandwich type composite filter tip with the cellulose acetate filter the upper and lower of not adding adsorbent, the amount containing adsorbent in every cigarette is 20mg.According to GB/T 16447 requirements, cigarette sample used balance 48 hours at (22 ± 1) DEG C and under the condition of the relative humidity of (60 ± 3) %, through weight and resistance to suction sorting, pick out the experiment cigarette sample of uniformity, in the upper suction of Cerulean SM450 linear pattern smoking machine (Cerulean company of Britain).With diluted sodium hydroxide solution trapping main flume gas gas-phase objects; With cambridge filter trapping flue gas TPM, and extract with sodium hydroxide solution.Detect flue gas, the grain hydrogen cyanide in mutually with continuous-flow instrument respectively, the two measurement result sum is the burst size of cigarette mainstream flue gas hydrogenation cyanogen, concrete detection method is with reference to professional standard YC/T253-2008, result shows, contrast with the filter-tip cigarette that does not add adsorbent, the present invention's adsorbent used can make in main flume the content of hydrogen cyanide 20% left and right that declines.
Embodiment 3
Prepare the mesopore silicon oxide MCM41 adsorbent of the amino functional of the high-specific surface area of the present embodiment according to the method step of embodiment 1.The mesopore silicon oxide MCM41 adsorbent (hereinafter to be referred as adsorbent) of the amino functional that the present embodiment is obtained sieves, and chooses the absorbent particles of 80-100 order particle diameter; The absorbent particles of choosing is evenly sprayed on to the acetate fibres interfascicular of filter stick, and (one deck near mouth in composite filter-tip is the filter stick layer that does not add absorbent particles to form the composite filter-tip of levels structure with the filter stick that does not add absorbent particles, another layer is connected with cigarette), the amount containing adsorbent in every cigarette is 60mg.According to GB/T1 6447 requirements, cigarette sample used balance 48 hours at (22 ± 1) DEG C and under the condition of the relative humidity of (60 ± 3) %, through weight and resistance to suction sorting, pick out the experiment cigarette sample of uniformity, in the upper suction of Cerulean SM450 linear pattern smoking machine (Cerulean company of Britain).With diluted sodium hydroxide solution trapping main flume gas gas-phase objects; With cambridge filter trapping flue gas TPM, and extract with sodium hydroxide solution.Detect flue gas, the grain hydrogen cyanide in mutually with continuous-flow instrument respectively, the two measurement result sum is the burst size of cigarette mainstream flue gas hydrogenation cyanogen, concrete detection method is with reference to professional standard YC/T253-2008, result shows, contrast with the filter-tip cigarette that does not add adsorbent, the present invention's adsorbent used can make in main flume the content of hydrogen cyanide 20% left and right that declines.
The above; it is only preferred embodiment of the present invention; not to any formal and substantial restriction of the present invention; should be understood that; for those skilled in the art; do not departing under the prerequisite of the inventive method, also can make some improvement and supplement, these improvement and the supplementary protection scope of the present invention that also should be considered as.All those skilled in the art, without departing from the spirit and scope of the present invention, a little change of making when utilizing disclosed above technology contents, the equivalent variations of modifying and developing, be equivalent embodiment of the present invention; Meanwhile, the change of any equivalent variations that all foundations essence technology of the present invention is done above-described embodiment, modification and differentiation, all still belong in the scope of technical scheme of the present invention.
Claims (3)
1. the application of the mesopore silicon oxide adsorbent of the amino functional of high-specific surface area hydrogen cyanide content in reduction cigarette mainstream flue gas; The mesopore silicon oxide of described amino functional is the mesopore silicon oxide MCM41 of amino functional, and its specific area is 300-550m
2/ g, aperture is 1.2-1.8nm; In the mesopore silicon oxide MCM41 of described amino functional, the amino amount of contained functionalization is 1.2-2.2mmol/g; Described mesopore silicon oxide adsorbent is carry out amino functional on mesopore silicon oxide surface and obtain, and described mesopore silicon oxide is MCM41, and its specific area is 500-950m
2/ g, aperture is 1.5-2.5nm; Described being applied as added the mesopore silicon oxide MCM41 adsorbent of amino functional in cigarette filter to, for reducing the content of hydrogen cyanide in cigarette mainstream flue gas.
2. the mesopore silicon oxide adsorbent of the amino functional of high-specific surface area as claimed in claim 1, reducing the application of hydrogen cyanide content in cigarette mainstream flue gas, is characterized in that, its application process specifically comprises the steps:
(1) the mesopore silicon oxide MCM41 adsorbent of amino functional is sieved, choose the absorbent particles of 80-100 order particle diameter;
(2) absorbent particles of choosing is placed in to filter-tip intermediate layer, forms the composite filter-tip of sandwich type with the cellulose acetate filter the upper and lower of not adding adsorbent; Or the absorbent particles of choosing is evenly sprayed on to the acetate fibres interfascicular of filter stick, and forms the composite filter-tip of levels structure with the filter stick that does not add absorbent particles.
3. the application of the mesopore silicon oxide adsorbent of the amino functional of high-specific surface area as claimed in claim 2 hydrogen cyanide content in reduction cigarette mainstream flue gas, it is characterized in that, in every cigarette composite filter tip, the amount of the mesopore silicon oxide MCM41 adsorbent of contained amino functional is 20～60mg.
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Families Citing this family (5)
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| CN103157448B (en) * | 2013-03-27 | 2016-04-27 | 上海烟草集团有限责任公司 | A kind of preparation method of the amido modified multi-stage porous sorbent material for Harm reduction techniques |
| CN104941606B (en) * | 2015-05-27 | 2018-06-26 | 河南中烟工业有限责任公司 | HCN and the adsorbent of crotonaldehyde release amount in a kind of reduction cigarette mainstream flue gas |
| CN108968148A (en) * | 2018-06-08 | 2018-12-11 | 滁州卷烟材料厂 | A kind of composite filter tip addition material reducing determination of hydrogen cyanide in mainstream cigarette smoke |
| CN109275952B (en) * | 2018-12-06 | 2021-02-02 | 武汉纺织大学 | Preparation method of composite cigarette filter tip |
| CN109275953B (en) * | 2018-12-06 | 2021-02-02 | 武汉纺织大学 | Preparation method of fiber-based cigarette filter |
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| US4300577A (en) * | 1978-05-16 | 1981-11-17 | British-American Tobacco Company Limited | Tobacco-smoke filters |
| CN101194755A (en) * | 2007-12-21 | 2008-06-11 | 湖南中烟工业有限责任公司 | Additive agent selectively reducing aldehydes matter in cigarette flue gas, production method and application thereof |
| CN101669678A (en) * | 2009-09-24 | 2010-03-17 | 中国烟草总公司郑州烟草研究院 | Filter additive material for selectively reducing hydrocyanic acid emission amount in mainstream smoke of cigarette and preparation method thereof |
| CN102499481A (en) * | 2011-11-04 | 2012-06-20 | 湖南中烟工业有限责任公司 | Adsorbent capable of reducing content of hydrocyanic acid in mainstream smoke of cigarette as well as preparation and application of absorbent |
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| US9107455B2 (en) * | 2003-11-21 | 2015-08-18 | Philip Morris Usa Inc. | Cigarette filter |
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| US4300577A (en) * | 1978-05-16 | 1981-11-17 | British-American Tobacco Company Limited | Tobacco-smoke filters |
| CN101194755A (en) * | 2007-12-21 | 2008-06-11 | 湖南中烟工业有限责任公司 | Additive agent selectively reducing aldehydes matter in cigarette flue gas, production method and application thereof |
| CN101669678A (en) * | 2009-09-24 | 2010-03-17 | 中国烟草总公司郑州烟草研究院 | Filter additive material for selectively reducing hydrocyanic acid emission amount in mainstream smoke of cigarette and preparation method thereof |
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