CN103865217B - A kind of have polyvinyl alcohol mould material detecting formaldehyde effect and preparation method thereof - Google Patents
A kind of have polyvinyl alcohol mould material detecting formaldehyde effect and preparation method thereof Download PDFInfo
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- CN103865217B CN103865217B CN201410093477.9A CN201410093477A CN103865217B CN 103865217 B CN103865217 B CN 103865217B CN 201410093477 A CN201410093477 A CN 201410093477A CN 103865217 B CN103865217 B CN 103865217B
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- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 239000004372 Polyvinyl alcohol Substances 0.000 title claims abstract description 34
- 229920002451 polyvinyl alcohol Polymers 0.000 title claims abstract description 34
- 239000000463 material Substances 0.000 title claims abstract description 15
- 230000000694 effects Effects 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 239000002105 nanoparticle Substances 0.000 claims abstract description 28
- 239000000523 sample Substances 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 10
- 229920001059 synthetic polymer Polymers 0.000 claims abstract description 8
- 238000001338 self-assembly Methods 0.000 claims abstract description 5
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 60
- 239000000243 solution Substances 0.000 claims description 38
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 15
- 239000000047 product Substances 0.000 claims description 14
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 14
- 239000012498 ultrapure water Substances 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 8
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 7
- 239000005695 Ammonium acetate Substances 0.000 claims description 7
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 7
- 238000013019 agitation Methods 0.000 claims description 7
- 229940043376 ammonium acetate Drugs 0.000 claims description 7
- 235000019257 ammonium acetate Nutrition 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 7
- 239000000376 reactant Substances 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 7
- 238000000967 suction filtration Methods 0.000 claims description 7
- 238000004090 dissolution Methods 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 206010039424 Salivary hypersecretion Diseases 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 208000026451 salivation Diseases 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000005266 casting Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 27
- 238000001514 detection method Methods 0.000 description 8
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229930040373 Paraformaldehyde Natural products 0.000 description 3
- 238000004737 colorimetric analysis Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 229920002866 paraformaldehyde Polymers 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000000589 high-performance liquid chromatography-mass spectrometry Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 235000019633 pungent taste Nutrition 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a kind of polyvinyl alcohol mould material with formaldehyde examination effect and preparation method thereof, first synthetic polymer P (St-alt-Man) and formaldehyde probe molecule KD-XA01, P (St-alt-Man) nano-particle solution that load has probe molecule is obtained by Macromolecular self-assembly technology, joined in polyvinyl alcohol film forming liquid, casting method obtains the polyvinyl alcohol mould material with formaldehyde examination effect.
Description
Technical field
The invention belongs to macromolecule member material and chemical sensor field, be specifically related to a kind of to there is polyvinyl alcohol mould material detecting formaldehyde effect and preparation method thereof.
Background technology
Formaldehyde is at normal temperatures for having pungency and asphyxiant colourless gas, and to person injury greatly, be one of environmental pollutant day by day come into one's own, at China's noxious chemical priority acccess control list, formaldehyde occupies second.Therefore set up easy to operate, the method for determining formaldehyde that precision is high is even more important.The method detecting formaldehyde the most frequently used is colorimetry, can be divided into off-color acid method again, acetylacetone method, AHMT colorimetry etc.; Detect textiles in national standard, food, the prefered method of formaldehyde in air is exactly colorimetry, most widely used general wherein again with acetylacetone method.In recent years, along with the progress of detection technique, the raising of detecting instrument commercialized degree, gas-chromatography, high performance liquid chromatography and gas chromatography mass spectrometry etc. are sensitive, and detection method has also been applied in the detection of formaldehyde efficiently.But, above detection method complex operation, strongly professional, be not suitable for the general population and use.
Formaldehyde test paper is a kind of method checking formaldehyde more easily, it is simple to operate, what play detection effect in formaldehyde test paper is the micromolecular compound of PARA FORMALDEHYDE PRILLS(91,95) sensitivity, but micromolecular compound has certain transport property, along with the migration of micromolecular compound after long storage time, its Detection results will inevitably reduce, and life cycle also can shorten.
Summary of the invention
The object of this invention is to provide and a kind of there is polyvinyl alcohol mould material detecting formaldehyde effect and preparation method thereof, solve the problems such as existing formaldehyde sensor complex operation, life cycle be short.
For solving the problem, the invention provides a kind of polyvinyl alcohol mould material with detection formaldehyde effect, it is characterized in that, comprise the component of following mass fraction: polyvinyl alcohol water solution 8-9 part, P (St-alt-Man) nano-particle solution 1-2 part of carrying probe molecule
P (St-alt-Man) nano-particle solution of described carrying probe molecule is obtained by following methods:
(1) synthesising probing needle molecule KD-XA01
Be dissolved in 60ml benzene by 3.24g1-phenyl-1,3-dimethyl diketone, add ammonium acetate 3.08g and acetic acid 1ml, in nitrogen atmosphere, at 80 DEG C, backflow obtains product in 12 hours, by reactant washing, drying, and except desolventizing; (2) synthetic polymer P (St-alt-Man)
Take 6.24g vinylbenzene, 7.06g maleic anhydride is dissolved in 180ml toluene, adds 0.06gAIBN, logical N
215min, sealing, reacts 20h. product suction filtration and uses hot toluene drip washing at oil bath 65 DEG C,
(3) nano-particle solution is prepared in self-assembly
Take P (St-alt-Man) 0.5g, KD-XA010.03g, be dissolved in the DMF of 10ml, vigorous stirring, slowly drips ultrapure water, when there is blue-opalescent simultaneously, this solution is under agitation slowly dripped in 100ml ultrapure water, obtains this nano-particle solution.
Wherein, polyvinyl alcohol water solution mass concentration is 4-8%.
The above-mentioned preparation method with the polyvinyl alcohol mould material of formaldehyde examination effect comprises the following steps:
(1) synthesising probing needle molecule KD-XA01
Be dissolved in 60ml benzene by 3.24g1-phenyl-1,3-dimethyl diketone, add ammonium acetate 3.08g and acetic acid 1ml, in nitrogen atmosphere, at 80 DEG C, backflow obtains product in 12 hours, by reactant washing, drying, and except desolventizing; (2) synthetic polymer P (St-alt-Man)
Take 6.24g vinylbenzene, 7.06g maleic anhydride is dissolved in 180mL toluene, add 0.06gAIBN, logical N2 gas 15min, sealing, reacts 20h. product suction filtration and uses hot toluene drip washing, then being dissolved in acetone at oil bath 65 DEG C, use toluene precipitate and separate. repeatedly after dissolution precipitation three times, dry in 30 DEG C of vacuum drying ovens and obtain P (St-alt-Man);
(3) nano-particle solution is prepared in self-assembly
Take P (St-alt-Man) 0.5g, KD-XA010.03g, be dissolved in the DMF of 10ml, vigorous stirring, slowly drips ultrapure water, when there is blue-opalescent simultaneously, this solution is under agitation slowly dripped in 100ml ultrapure water, obtains this nano-particle solution;
(4) polyvinyl alcohol film is prepared
Weighing polyvinyl alcohol aqueous solution 8-9 part, P (St-alt-Man) nano-particle solution 1-2 part of carrying probe molecule, mixes to obtain film forming liquid under stirring, film forming liquid is evenly poured on film forming device, salivation film forming, puts into 40 DEG C of baking ovens, takes out and take off film after 48 hours.
Beneficial effect of the present invention: a kind of thin film sensor of invention, film forming matrix is macromolecular material polyvinyl alcohol, the nano-particle solution of PARA FORMALDEHYDE PRILLS(91,95) sensitivity is added in film forming liquid, this nanoparticle with parents notion P (St-alt-Man) for carrier, there is satisfactory stability effect to probe molecule, the shortcoming of probe molecule migration can be overcome.And the polar group carboxyl of maleic anhydride primitive imparting nanoparticle surface can form intermolecular hydrogen bonding effect with the hydroxyl in polyvinyl alcohol segments, the consistency that the system that reaches is good in polymer P (St-alt-Man).Obtained thin-film material is a kind of thin film sensor, easy to use, whether can convert the existence of formaldehyde to color signal and express, carry out qualitative analysis, judge formaldehyde content height by shade simultaneously, also by film by instrumental characterizing, quantitative analysis can be carried out.
Accompanying drawing illustrates:
Fig. 1 probe molecule KD-XA01 nuclear magnetic spectrogram
Fig. 2 polymer P (St-alt-Man) nuclear magnetic spectrogram
P (St-alt-Man) the nanoparticle transmission electron microscope picture of Fig. 3 carrying probe molecule
Fig. 4 mould material PARA FORMALDEHYDE PRILLS(91,95) Detection results
Embodiment
Below utilize embodiment to further describe the present invention, but can not think to limit scope of invention.
Embodiment 1
Configuration quality concentration is the polyvinyl alcohol water solution of 4%, takes in 4g polyvinyl alcohol 96g water, stirring and dissolving.(1) synthesising probing needle molecule KD-XA01
Be dissolved in 60ml benzene by 3.24g1-phenyl-1,3-dimethyl diketone, add ammonium acetate 3.08g and acetic acid 1ml, in nitrogen atmosphere, at 80 DEG C, backflow obtains product in 12 hours, by reactant washing, drying, and except desolventizing; (2) synthetic polymer P (St-alt-Man)
Take 6.24g vinylbenzene, 7.06g maleic anhydride is dissolved in 180mL toluene, adds 0.06gAIBN, logical N
215min, sealing, reacts 20h. product suction filtration use hot toluene drip washing, then is dissolved in acetone, use toluene precipitate and separate at oil bath 65 DEG C. and repeatedly after dissolution precipitation three times, in 30 DEG C of vacuum drying ovens, oven dry obtains P (St-alt-Man);
(3) nano-particle solution is prepared
Take P (St-alt-Man) 0.5g, KD-XA010.03g, be dissolved in the DMF of 10ml, vigorous stirring, slowly drips ultrapure water, when there is blue-opalescent simultaneously, this solution is under agitation slowly dripped in 100ml ultrapure water, obtains this nano-particle solution;
(4) polyvinyl alcohol film is prepared
The weighing polyvinyl alcohol aqueous solution 9 parts, P (St-alt-Man) nano-particle solution 1 part of carrying probe molecule, mixes to obtain film forming liquid under stirring, film forming liquid is evenly poured on film forming device, salivation film forming, puts into 40 DEG C of baking ovens, takes out and take off film after 48 hours.
Embodiment 2
Configuration quality concentration is the polyvinyl alcohol water solution of 5%, takes in 5g polyvinyl alcohol 95g water, stirring and dissolving.(1) synthesising probing needle molecule KD-XA01
Be dissolved in 60ml benzene by 3.24g1-phenyl-1,3-dimethyl diketone, add ammonium acetate 3.08g and acetic acid 1ml, in nitrogen atmosphere, at 80 DEG C, backflow obtains product in 12 hours, by reactant washing, drying, and except desolventizing; (2) synthetic polymer P (St-alt-Man)
Take 6.24g vinylbenzene, 7.06g maleic anhydride is dissolved in 180mL toluene, adds 0.06gAIBN, logical N
2gas 15min, sealing, reacts 20h. product suction filtration use hot toluene drip washing, then is dissolved in acetone, use toluene precipitate and separate at oil bath 65 DEG C. and repeatedly after dissolution precipitation three times, in 30 DEG C of vacuum drying ovens, oven dry obtains P (St-alt-Man);
(3) nano-particle solution is prepared
Take P (St-alt-Man) 0.5g, KD-XA010.03g, be dissolved in the DMF of 10ml, vigorous stirring, slowly drips ultrapure water, when there is blue-opalescent simultaneously, this solution is under agitation slowly dripped in 100ml ultrapure water, obtains this nano-particle solution;
(4) polyvinyl alcohol film is prepared
The weighing polyvinyl alcohol aqueous solution 8 parts, P (St-alt-Man) nano-particle solution 2 parts of carrying probe molecule, mixes to obtain film forming liquid under stirring, film forming liquid is evenly poured on film forming device, salivation film forming, puts into 40 DEG C of baking ovens, takes out and take off film after 48 hours.
Embodiment 3
Configuration quality concentration is the polyvinyl alcohol water solution of 8%, takes in 8g polyvinyl alcohol 92g water, stirring and dissolving.(1) synthesising probing needle molecule KD-XA01
Be dissolved in 60ml benzene by 3.24g1-phenyl-1,3-dimethyl diketone, add ammonium acetate 3.08g and acetic acid 1ml, in nitrogen atmosphere, at 80 DEG C, backflow obtains product in 12 hours, by reactant washing, drying, and except desolventizing; (2) synthetic polymer P (St-alt-Man)
Take 6.24g vinylbenzene, 7.06g maleic anhydride is dissolved in 180mL toluene, adds 0.06gAIBN, logical N
2gas 15min, sealing, reacts 20h. product suction filtration use hot toluene drip washing, then is dissolved in acetone, use toluene precipitate and separate at oil bath 65 DEG C. and repeatedly after dissolution precipitation three times, in 30 DEG C of vacuum drying ovens, oven dry obtains P (St-alt-Man);
(3) nano-particle solution is prepared
Take P (St-alt-Man) 0.5g, KD-XA010.03g, be dissolved in the DMF of 10ml, vigorous stirring, slowly drips ultrapure water, when there is blue-opalescent simultaneously, this solution is under agitation slowly dripped in 100ml ultrapure water, obtains this nano-particle solution;
(4) polyvinyl alcohol film is prepared
The weighing polyvinyl alcohol aqueous solution 9 parts, P (St-alt-Man) nano-particle solution 1 part of carrying probe molecule, mixes to obtain film forming liquid under stirring, film forming liquid is evenly poured on film forming device, salivation film forming, puts into 40 DEG C of baking ovens, takes out and take off film after 48 hours.
Claims (3)
1. there is a polyvinyl alcohol mould material for formaldehyde examination effect, it is characterized in that:
Comprise the component of following mass fraction: polyvinyl alcohol water solution 8-9 part, P (St-alt-Man) nano-particle solution 1-2 part of carrying probe molecule, P (St-alt-Man) nano-particle solution of described carrying probe molecule is obtained by following methods:
(1) synthesising probing needle molecule KD-XA01
Be dissolved in 60ml benzene by 3.24g1-phenyl-1,3-dimethyl diketone, add ammonium acetate 3.08g and acetic acid 1ml, in nitrogen atmosphere, at 80 DEG C, backflow obtains product in 12 hours, by reactant washing, drying, and except desolventizing;
(2) synthetic polymer P (St-alt-Man)
Take 6.24g vinylbenzene, 7.06g maleic anhydride is dissolved in 180mL toluene, adds 0.06gAIBN, logical N
215min, sealing, reacts 20h at oil bath 65 DEG C, product suction filtration use hot toluene drip washing, then is dissolved in acetone, uses toluene precipitate and separate, and repeatedly after dissolution precipitation three times, in 30 DEG C of vacuum drying ovens, oven dry obtains P (St-alt-Man);
(3) nano-particle solution is prepared in self-assembly
Take P (St-alt-Man) 0.5g, KD-XA010.03g, be dissolved in the DMF of 10ml, vigorous stirring, slowly drips ultrapure water, when there is blue-opalescent simultaneously, this solution is under agitation slowly dripped in 100ml ultrapure water, obtains this nano-particle solution.
2. there is the polyvinyl alcohol mould material of formaldehyde examination effect as claimed in claim 1, it is characterized in that: polyvinyl alcohol water solution mass concentration is 4-8%.
3. there is the preparation method of the polyvinyl alcohol mould material of formaldehyde examination effect as claimed in claim 1 or 2, it is characterized in that comprising the following steps:
(1) synthesising probing needle molecule KD-XA01
Be dissolved in 60ml benzene by 3.24g1-phenyl-1,3-dimethyl diketone, add ammonium acetate 3.08g and acetic acid 1ml, in nitrogen atmosphere, at 80 DEG C, backflow obtains product in 12 hours, by reactant washing, drying, and except desolventizing; (2) synthetic polymer P (St-alt-Man)
Take 6.24g vinylbenzene, 7.06g maleic anhydride is dissolved in 180mL toluene, adds 0.06gAIBN, logical N
215min, sealing, reacts 20h at oil bath 65 DEG C, product suction filtration use hot toluene drip washing, then is dissolved in acetone, uses toluene precipitate and separate, and repeatedly after dissolution precipitation three times, in 30 DEG C of vacuum drying ovens, oven dry obtains P (St-alt-Man);
(3) nano-particle solution is prepared in self-assembly
Take P (St-alt-Man) 0.5g, KD-XA010.03g, be dissolved in the DMF of 10ml, vigorous stirring, slowly drips ultrapure water, when there is blue-opalescent simultaneously, this solution is under agitation slowly dripped in 100ml ultrapure water, obtains this nano-particle solution;
(4) polyvinyl alcohol film is prepared
Weighing polyvinyl alcohol aqueous solution 8-9 part, P (St-alt-Man) nano-particle solution 1-2 part of carrying probe molecule, mixes to obtain film forming liquid under stirring, film forming liquid is evenly poured on film forming device, salivation film forming, puts into 40 DEG C of baking ovens, takes out and take off film after 48 hours.
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR101683037B1 (en) * | 2015-06-26 | 2016-12-06 | 한국화학연구원 | Composition for eliminating formaldehyde and formaldehyde-eliminating method using the same |
| CN109001193B (en) * | 2018-06-10 | 2020-11-27 | 盐城舒云新材料有限公司 | Preparation method of formaldehyde detection membrane |
| CN108753186B (en) * | 2018-06-10 | 2021-06-08 | 江苏佳饰家新材料集团股份有限公司 | Formaldehyde detection film paste and use method thereof |
| CN108802025B (en) * | 2018-06-10 | 2020-11-24 | 盐城舒云新材料有限公司 | Preparation method of test paper for formaldehyde detection |
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Effective date of registration: 20180514 Address after: 214000 Jiangsu Wuxi Beitang District North Shanbei Street North Community Community 105 Wan Li Patentee after: Tang Weicheng Address before: 214122 College of chemistry and materials engineering, Jiangnan University 1800, Lihu Avenue, Wuxi, Jiangsu Patentee before: Jiangnan University |
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Effective date of registration: 20240325 Address after: 124-5, 1st Floor, Office Area, No. 35-301 Changjiang South Road, Xinwu District, Wuxi City, Jiangsu Province, 214000 Patentee after: Wuxi Huisheng Hongcheng Environmental Protection Technology Co.,Ltd. Country or region after: China Address before: 214000 Jiangsu Wuxi Beitang District North Shanbei Street North Community Community 105 Wan Li Patentee before: Tang Weicheng Country or region before: China |