CN110833821B - Liquid phase selective adsorption material and application thereof in cigarette smoke analysis - Google Patents
Liquid phase selective adsorption material and application thereof in cigarette smoke analysis Download PDFInfo
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- CN110833821B CN110833821B CN201911088048.1A CN201911088048A CN110833821B CN 110833821 B CN110833821 B CN 110833821B CN 201911088048 A CN201911088048 A CN 201911088048A CN 110833821 B CN110833821 B CN 110833821B
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- 239000000463 material Substances 0.000 title claims abstract description 38
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 38
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 37
- 239000000779 smoke Substances 0.000 title claims abstract description 36
- 239000007791 liquid phase Substances 0.000 title claims abstract description 25
- 238000004458 analytical method Methods 0.000 title claims abstract description 15
- 239000002105 nanoparticle Substances 0.000 claims abstract description 33
- 229920002401 polyacrylamide Polymers 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 125000003277 amino group Chemical group 0.000 claims abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 12
- 239000011248 coating agent Substances 0.000 claims abstract 2
- 238000000576 coating method Methods 0.000 claims abstract 2
- 239000006185 dispersion Substances 0.000 claims description 20
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 16
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 11
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000003999 initiator Substances 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 238000006116 polymerization reaction Methods 0.000 claims description 8
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical group NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 7
- -1 sulfur peroxide Chemical class 0.000 claims description 7
- 150000001412 amines Chemical class 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 239000000178 monomer Substances 0.000 claims description 5
- 238000000016 photochemical curing Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 239000004408 titanium dioxide Substances 0.000 claims description 4
- 238000005904 alkaline hydrolysis reaction Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 230000002378 acidificating effect Effects 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 238000001723 curing Methods 0.000 claims description 2
- 239000012071 phase Substances 0.000 claims description 2
- 230000000379 polymerizing effect Effects 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- AOHJOMMDDJHIJH-UHFFFAOYSA-N propylenediamine Chemical compound CC(N)CN AOHJOMMDDJHIJH-UHFFFAOYSA-N 0.000 claims description 2
- 239000011593 sulfur Substances 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 12
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 abstract description 6
- 239000003546 flue gas Substances 0.000 abstract description 6
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 6
- 239000001257 hydrogen Substances 0.000 abstract description 6
- HGINCPLSRVDWNT-UHFFFAOYSA-N Acrolein Chemical compound C=CC=O HGINCPLSRVDWNT-UHFFFAOYSA-N 0.000 abstract description 4
- 230000000711 cancerogenic effect Effects 0.000 abstract description 3
- 231100000315 carcinogenic Toxicity 0.000 abstract description 3
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 3
- 150000002500 ions Chemical class 0.000 abstract description 3
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 abstract description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002262 Schiff base Substances 0.000 abstract description 2
- 150000004753 Schiff bases Chemical class 0.000 abstract description 2
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 abstract description 2
- 150000001299 aldehydes Chemical class 0.000 abstract description 2
- 231100000357 carcinogen Toxicity 0.000 abstract description 2
- 239000003183 carcinogenic agent Substances 0.000 abstract description 2
- 230000009920 chelation Effects 0.000 abstract description 2
- MLUCVPSAIODCQM-NSCUHMNNSA-N crotonaldehyde Chemical compound C\C=C\C=O MLUCVPSAIODCQM-NSCUHMNNSA-N 0.000 abstract description 2
- MLUCVPSAIODCQM-UHFFFAOYSA-N crotonaldehyde Natural products CC=CC=O MLUCVPSAIODCQM-UHFFFAOYSA-N 0.000 abstract description 2
- XKLJHFLUAHKGGU-UHFFFAOYSA-N nitrous amide Chemical compound ON=N XKLJHFLUAHKGGU-UHFFFAOYSA-N 0.000 abstract description 2
- 230000000269 nucleophilic effect Effects 0.000 abstract description 2
- 235000019633 pungent taste Nutrition 0.000 abstract description 2
- 239000003205 fragrance Substances 0.000 abstract 1
- 150000002576 ketones Chemical class 0.000 abstract 1
- 230000000717 retained effect Effects 0.000 abstract 1
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 description 24
- 239000000243 solution Substances 0.000 description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 230000000391 smoking effect Effects 0.000 description 12
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 9
- 239000003440 toxic substance Substances 0.000 description 9
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 239000000523 sample Substances 0.000 description 8
- 231100000614 poison Toxicity 0.000 description 7
- 229920001747 Cellulose diacetate Polymers 0.000 description 6
- 230000007062 hydrolysis Effects 0.000 description 6
- 238000006460 hydrolysis reaction Methods 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 238000004817 gas chromatography Methods 0.000 description 4
- 230000001678 irradiating effect Effects 0.000 description 4
- 238000004806 packaging method and process Methods 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000002144 chemical decomposition reaction Methods 0.000 description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 3
- NBBJYMSMWIIQGU-UHFFFAOYSA-N Propionic aldehyde Chemical compound CCC=O NBBJYMSMWIIQGU-UHFFFAOYSA-N 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 2
- 231100000167 toxic agent Toxicity 0.000 description 2
- 235000013162 Cocos nucifera Nutrition 0.000 description 1
- 244000060011 Cocos nucifera Species 0.000 description 1
- 241000208125 Nicotiana Species 0.000 description 1
- 244000061176 Nicotiana tabacum Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- WPKYZIPODULRBM-UHFFFAOYSA-N azane;prop-2-enoic acid Chemical compound N.OC(=O)C=C WPKYZIPODULRBM-UHFFFAOYSA-N 0.000 description 1
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N butyric aldehyde Natural products CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229960002089 ferrous chloride Drugs 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 239000013074 reference sample Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
-
- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
Abstract
The application discloses a liquid phase selective adsorption material and application thereof in cigarette smoke analysis. The liquid phase selective adsorption material is formed by coating inorganic nano particles with polyacrylamide with side-connected amino groups; wherein the polyacrylamide is associated with water. The liquid phase selective adsorption material is a low-viscosity sol state, can directionally adsorb aldehyde substances such as formaldehyde, acetaldehyde, acrolein, crotonaldehyde and the like in the flue gas through Schiff base reaction, and greatly reduces the pungent taste in the flue gas; the phenol carcinogenic substances in the smoke are directionally adsorbed through the action of nucleophilic hydrogen bonds; nitrosamine carcinogens in the smoke are directionally adsorbed through the action of hydrogen bonds; selectively adsorbing particles of heavy metal ions in the flue gas through chelation; in addition, the adsorption component in the product is repelled from the ketone and ester aromatic components in the smoke, so that the fragrance of the smoke can be retained to the maximum extent.
Description
Technical Field
The invention relates to the technical field of cigarette materials, in particular to a liquid-phase selective adsorption material and application thereof in cigarette smoke analysis.
Background
China is a large tobacco producing and consuming country, smokers reach 3 hundred million people, and tobacco consumed each year accounts for 1/3 of the total world sales. The smoke contains various harmful substances, such as strong carcinogenic substances, such as formaldehyde, toluene, catechol, resorcinol, heavy metal ions and the like. For this reason, methods for reducing toxic substances in cigarette smoke have been sought. The method mainly adopted at present is to filter toxic substances in cigarette smoke through physical adsorption and chemical adsorption.
For example, chinese patent CN109894078A discloses a coconut shell activated carbon adsorption material for cigarette filters, which adsorbs toxic substances in cigarettes by activated carbon with large specific surface area. Patent CN106824061A discloses a filter with natural zeolite particles added in cellulose diacetate tow, which is also used for adsorbing toxic substances in smoke by zeolite with large specific surface. However, the simple physical adsorption mode has a general adsorption effect, and poor selectivity leads to easy adsorption saturation. The chemical method is mainly to selectively adsorb one or more harmful substances through chemical bonds or polarity. For another example, patent CN109316830A discloses a smoke filtering composite material, which selectively adsorbs polar substances such as formaldehyde and propionaldehyde in cigarette smoke through polar elements contained in the material. For another example, patent CN106894283A discloses a functional alcoholizing paper material for cigarette, which also adsorbs toxic substances in cigarette through hydrogen bonding of hydroxyl group. However, the reaction of the polar hydrogen bond to the toxic substance is slow, and the toxic substance cannot be efficiently and rapidly adsorbed.
Disclosure of Invention
In order to solve the problems, the application provides a liquid-phase selective adsorption material and application thereof, which can quickly adsorb toxic substances in cigarette smoke.
The inventors of the present application have surprisingly found that polyacrylamide is capable of forming a highly efficient chemical reaction area upon association with water. After the amino is laterally connected with the polyacrylamide, the amino can be subjected to chemical degradation in the following four aspects, on one hand, aldehyde substances such as formaldehyde, acetaldehyde, acrolein, crotonaldehyde and the like in the flue gas can be directionally adsorbed through Schiff base reaction, and the pungent taste in the flue gas is greatly reduced; on the other hand, the phenol carcinogenic substances in the smoke are directionally adsorbed through the nucleophilic hydrogen bond; in the third aspect, nitrosamine carcinogens in the smoke are directionally adsorbed through hydrogen bond action; and fourthly, selectively adsorbing the particles of the heavy metal ions in the flue gas through chelation. It can be seen that the polyacrylamide of the present application provides a reaction site for chemical degradation after associating, and the amino group participates in chemical degradation of toxic substances, and the two functionally support each other. Based on this, the invention of the present application has been completed.
According to a first embodiment of the present application, a selective adsorbent material in liquid phase, formed by supporting a porous mineral clay with a polyacrylamide having pendant amino groups; wherein the polyacrylamide is associated with water.
It is understood that "associate" as used herein refers to a weak chemical bond between molecules, either identical or not, that can be constantly dissociated and re-associated, including but not limited to molecular hydrogen bonding. For the association between polyacrylamide and water in the present application, the disassociation may be achieved by heating.
The source of the amino group is preferably one or at least two of ethylenediamine, 1, 2-propylenediamine and hexamethylenediamine.
Specific examples of the inorganic nanoparticles include one or at least two of alumina, silica, and titania. The particle size is preferably 50 to 400nm, more preferably 100 to 300 nm.
The mass of the polyacrylamide, inorganic nanoparticles, amino group, and water is preferably 1:0.05 to 0.2:0.05 to 0.1:50 to 200, more preferably 1:0.08 to 0.15:0.06 to 0.08:100 to 180.
The liquid phase adsorption material can be prepared by the following method; the preparation method comprises the following steps:
(1) sequentially carrying out alkaline hydrolysis and acidic reaction on an acrylamide monomer and inorganic nanoparticles in a water phase to form a monomer dispersion liquid of the acrylamide monomer coated inorganic nanoparticles;
(2) polymerizing the monomer dispersion liquid to obtain polyacrylamide-coated inorganic nanoparticles;
(3) reacting the polyacrylamide coated inorganic nanoparticles with amine to obtain polyacrylamide coated inorganic nanoparticles with side amino groups;
(4) the polyacrylamide-coated inorganic nanoparticles flanked by amino groups are allowed to adsorb water.
The alkaline hydrolysis in the step (1) specifically means that the amide group of the acrylamide monomer is hydrolyzed to obtain sodium carboxylate. The pH value of the hydrolysis can be 8-10, and the hydrolysis time can be 1-5 min. The pH value of the acid reaction can be 4-6, and the time can be 2-4 h.
The polymerization temperature in step (2) is preferably 60 to 80 ℃, preferably 65 to 75 ℃, the reaction time may be 1 to 2, preferably 1.5 hours, and the mass ratio of the initiator to the monomer in the polymerization reaction is 1:0.01 to 0.05, preferably 1:0.06 to 0.03.
The initiator used in the reaction is preferably a sulfur peroxide initiator, such as potassium persulfate, potassium persulfate-ferrous chloride. The mass ratio of the acrylamide monomer to the initiator is preferably 1:0.01 to 0.05, more preferably 1:0.02 to 0.04.
The reaction in the step (3) is preferably a photocuring reaction, preferably an ultraviolet reaction, and the reaction time is 0.5-2 h. The intensity of the ultraviolet irradiation can be adjusted according to actual needs.
Here, the curing agent for the photocuring reaction may be, for example, a common azo initiator.
The amine may be added in the form of an aqueous solution, and the concentration thereof may be 10 to 20wt%, preferably 12 to 18 wt%.
According to a second embodiment of the present application, there is provided the use of a liquid phase adsorbent material for analysis of cigarette smoke.
The material is low-viscosity sol, good in fluidity and small in gas adsorption flow resistance. In addition, the ammonium acrylate polymer supported by the nanoparticles is formed, the nanoparticles can support a functional material framework structure, the polyacrylamide can absorb 200-300 times of water to form a high-efficiency reaction area, and the side chain of the primary amino micromolecule plays a selective absorption function. Compared with the existing solution type adsorption material, the material has the characteristics of high reaction speed and strong adsorption selectivity.
Detailed Description
The following are specific examples of the present application and further describe the technical solutions of the present application, but the present application is not limited to these examples.
Example 1
(1) Dissolving bisacrylamide in deionized water, adding alumina particles with the particle size distribution of 200-300nm, adjusting the pH value of the solution to 8-10 by using 10wt% of sodium hydroxide solution, adjusting the pH value of the solution to 4-6 by using 10wt% of hydrochloric acid after hydrolysis for 5min, generating alumina nano particles with positive potential, and stirring for 2h to obtain aqueous dispersion of a sol structure in which the bisacrylamide with the reverse potential is coated on the nano particles, wherein the mass ratio of the bisacrylamide to the inorganic nano particles is 1: 0.05;
(2) adding potassium persulfate into the aqueous dispersion obtained in the step (1) to initiate bisacrylamide polymerization, and reacting at 60-80 ℃ for 1-2 hours to obtain an aqueous dispersion with a structure of polyacrylamide coated alumina, wherein the mass ratio of bisacrylamide to potassium persulfate is 1: 0.01;
(3) adding azodiisobutyronitrile and 10wt% of ethylenediamine solution into the aqueous dispersion obtained in the step (2), irradiating for 0.5-2h by using ultraviolet light to graft ethylenediamine micromolecules onto polyacrylamide, and controlling the mass ratio of the bisacrylamide to the ethylenediamine micromolecules to the azodiisobutyronitrile to be 1:0.05: 0.005;
(4) replenishing deionized water to the water content involved, such that the ratio of polyacrylamide: the weight ratio of the aluminum oxide to the ethylenediamine micromolecule to the water is 1:0.05:0.05:50, and the liquid phase selective adsorption material is obtained.
Pouring the selective adsorption material prepared in the example into a cylinder with the bottom surface diameter of 1cm and the height of 2cm, and packaging two sides by using a polytetrafluoroethylene film; the resulting cylinder was added to a cigarette with a cellulose diacetate tow filter to make sample A. Cigarette with cellulose diacetate tow filter was used as reference. And (3) smoking in a constant-temperature and constant-humidity smoking room by using an SM 450 linear smoking machine, and respectively collecting the cigarette smoke of the sample A and the reference sample. Qualitative and quantitative detection is carried out on the collected cigarette smoke through gas chromatography, and the table 1 shows the test results.
Example 2
(1) Dissolving bisacrylamide in deionized water, adding alumina particles with the particle size distribution of 200-300nm, adjusting the pH value of the solution to 8-10 by using 10wt% of sodium hydroxide solution, adjusting the pH value of the solution to 4-6 by using 10wt% of hydrochloric acid after hydrolysis for 5min, generating positive-potential alumina nano particles, and stirring for 2h to obtain aqueous dispersion of a sol structure in which the nano particles are coated with the bisacrylamide with reverse potential, wherein the mass ratio of the bisacrylamide to the inorganic nano particles is 1: 0.1;
(2) adding potassium persulfate into the aqueous dispersion obtained in the step (1) to initiate bisacrylamide polymerization, and reacting at 60-80 ℃ for 1-2 hours to obtain an aqueous dispersion with a structure of polyacrylamide coated alumina, wherein the mass ratio of bisacrylamide to potassium persulfate is 1: 0.01;
(3) adding azodiisobutyronitrile and a 10wt% ethylenediamine solution into the aqueous dispersion obtained in the step (2), irradiating for 0.5-2h by using ultraviolet light to graft ethylenediamine micromolecules onto polyacrylamide, and controlling the mass ratio of the bisacrylamide to the ethylenediamine micromolecules to the azodiisobutyronitrile to be 1:0.075: 0.0075;
(4) replenishing deionized water to the water content involved, such that the ratio of polyacrylamide: the weight ratio of the alumina particles to the ethylenediamine micromolecules to the water is 1:0.1:0.075:100, and the liquid-phase selective adsorption material is obtained.
Pouring the selective adsorption material prepared in the example into a cylinder with the bottom surface diameter of 1cm and the height of 2cm, and packaging two sides by using a polytetrafluoroethylene film; the obtained cylinder was added to a cigarette having a cellulose diacetate tow filter to prepare a sample B. And (4) in a constant-temperature and constant-humidity smoking room, smoking by using an SM 450 linear smoking machine, and collecting the cigarette smoke of the sample B. Qualitative and quantitative detection is carried out on the collected cigarette smoke through gas chromatography, and the table 1 shows the test results.
Example 3
(1) Dissolving bisacrylamide in deionized water, adding silica particles with the particle size distribution of 200-300nm, adjusting the pH value of the solution to 8-10 by using 10wt% of sodium hydroxide solution, adjusting the pH value of the solution to 4-6 by using 10wt% of hydrochloric acid after hydrolysis for 5min, generating silica nanoparticles with positive potential, and stirring for 2h to obtain aqueous dispersion of a sol structure in which the bisacrylamide with the reverse potential is coated on the nanoparticles, wherein the mass ratio of the bisacrylamide to the inorganic nanoparticles is 1: 0.2;
(2) adding potassium persulfate into the aqueous dispersion obtained in the step (1) to initiate bisacrylamide polymerization, and reacting at 60-80 ℃ for 1-2 hours to obtain an aqueous dispersion with a structure of polyacrylamide coated alumina, wherein the mass ratio of bisacrylamide to potassium persulfate is 1: 0.01;
(3) adding azodiisobutyronitrile and 10wt% of hexamethylenediamine solution into the aqueous dispersion obtained in the step (2), irradiating for 0.5-2h by using ultraviolet light to graft the ethylenediamine micromolecule onto polyacrylamide, and controlling the mass ratio of the bisacrylamide to the hexamethylenediamine micromolecule to the azodiisobutyronitrile to be 1:0.1: 0.01;
(4) replenishing deionized water to the water content involved, such that the ratio of polyacrylamide: the weight ratio of the silicon dioxide to the hexamethylene diamine micromolecules to the water is 1:0.2:0.1:150, and the liquid phase selective adsorption material is obtained.
Pouring the selective adsorption material prepared in the example into a cylinder with the bottom surface diameter of 1cm and the height of 2cm, and packaging two sides by using a polytetrafluoroethylene film; the obtained cylinder was added to a cigarette having a cellulose diacetate tow filter, and the resulting mixture was designated as sample C. And (4) in the constant-temperature and constant-humidity smoking chamber, smoking by using an SM 450 linear smoking machine, and collecting the cigarette smoke of the sample C. Qualitative and quantitative detection is carried out on the collected cigarette smoke through gas chromatography, and the table 1 shows the test results.
Example 4
(1) Dissolving bisacrylamide in deionized water, adding titanium dioxide particles with the particle size distribution of 200-300nm, adjusting the pH value of the solution to 8-10 by using 10wt% of sodium hydroxide solution, adjusting the pH value of the solution to 4-6 by using 10wt% of hydrochloric acid after hydrolysis for 5min, generating titanium dioxide nanoparticles with positive potential, stirring for 2h, and obtaining aqueous dispersion of a sol structure in which the bisacrylamide with the reverse potential is coated on the nanoparticles, wherein the mass ratio of the bisacrylamide to the inorganic nanoparticles is 1: 0.2;
(2) adding potassium persulfate into the aqueous dispersion obtained in the step (1) to initiate bisacrylamide polymerization, and reacting at 60-80 ℃ for 1-2 hours to obtain an aqueous dispersion with a structure of polyacrylamide coated alumina, wherein the mass ratio of bisacrylamide to potassium persulfate is 1: 0.01;
(3) adding azodiisobutyronitrile and 10wt% of hexamethylenediamine solution into the aqueous dispersion obtained in the step (2), irradiating for 0.5-2h by using ultraviolet light to graft the ethylenediamine micromolecule onto polyacrylamide, and controlling the mass ratio of the bisacrylamide to the hexamethylenediamine to the azodiisobutyronitrile to be 1:0.1: 0.01;
(4) replenishing deionized water to the water content involved, such that the ratio of polyacrylamide: the weight ratio of titanium dioxide to hexamethylene diamine micromolecules to water is 1:0.2:0.1:200, and the liquid phase selective adsorption material is obtained.
Pouring the selective adsorption material prepared in the example into a cylinder with the bottom surface diameter of 1cm and the height of 2cm, and packaging two sides by using a polytetrafluoroethylene film; the resulting cylinder was added to a cigarette with a cellulose diacetate tow filter to make sample D. And (4) in the constant-temperature and constant-humidity smoking chamber, smoking by using an SM 450 linear smoking machine, and collecting the cigarette smoke of the sample D. Qualitative and quantitative detection is carried out on the collected cigarette smoke through gas chromatography, and the table 1 shows the test results.
The test results for the examples and comparative examples are given in the following table:
the specific embodiments described herein are merely illustrative of the spirit of the application. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the present application as defined by the appended claims.
Claims (9)
1. The application of the liquid phase selective adsorption material in cigarette smoke analysis is characterized in that the liquid phase selective adsorption material is formed by coating inorganic nano particles with polyacrylamide with side-connected amino groups; wherein the polyacrylamide is associated with water; the adsorption material is applied to cigarette smoke analysis.
2. The application of the liquid phase selective adsorption material in cigarette smoke analysis according to claim 1, wherein the inorganic nanoparticles are one or at least two of alumina, silica and titanium dioxide.
3. The application of the liquid phase selective adsorption material in cigarette smoke analysis according to claim 1, wherein the amine providing the amino group is one or at least two of ethylenediamine, 1, 2-propylenediamine and hexamethylenediamine.
4. The application of the liquid phase selective adsorption material to cigarette smoke analysis according to claim 1, wherein the mass ratio of the polyacrylamide to the inorganic nanoparticles to the amino group to the water is 1: 0.05-0.2: 0.05-0.1: 50-200.
5. The application of the liquid phase selective adsorption material in cigarette smoke analysis according to claim 1, wherein the liquid phase selective adsorption material is prepared by the following method; the preparation method comprises the following steps:
(1) sequentially carrying out alkaline hydrolysis and acidic reaction on an acrylamide monomer and inorganic nanoparticles in a water phase to form a monomer dispersion liquid of the acrylamide monomer coated inorganic nanoparticles;
(2) polymerizing the monomer dispersion liquid to obtain polyacrylamide-coated inorganic nanoparticles;
(3) reacting the polyacrylamide coated inorganic nanoparticles with amine to obtain polyacrylamide coated inorganic nanoparticles with side amino groups;
(4) the polyacrylamide-coated inorganic nanoparticles flanked by amino groups are allowed to adsorb water.
6. The application of the liquid phase selective adsorption material in cigarette smoke analysis according to claim 5, wherein the particle size of the inorganic nanoparticles in the step (1) is 50-400 nm.
7. The application of the liquid phase selective adsorption material in cigarette smoke analysis according to claim 5, wherein the temperature of the polymerization reaction in the step (2) is 60-80 ℃, the reaction time is 1-2, the mass ratio of the initiator of the polymerization reaction to the acrylamide monomer is 1: 0.01-0.05, and the initiator is a sulfur peroxide initiator.
8. The application of the liquid phase selective adsorption material to cigarette smoke analysis according to claim 5, wherein the reaction in the step (3) is a photocuring reaction, the curing agent of the photocuring reaction is an azo initiator, and the photocuring reaction is carried out for 0.5-2 hours.
9. The application of the liquid phase selective adsorption material to cigarette smoke analysis according to claim 5, wherein the amine is added in the form of an aqueous solution with a mass concentration of 10-20 wt%.
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| CN201848253U (en) * | 2010-11-04 | 2011-06-01 | 滁州友林科技发展有限公司 | Adsorption high-polymer hydrogel |
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| CN201848253U (en) * | 2010-11-04 | 2011-06-01 | 滁州友林科技发展有限公司 | Adsorption high-polymer hydrogel |
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