CN103865217A - Polyvinyl alcohol membrane material with formaldehyde detection effect and preparation method thereof - Google Patents
Polyvinyl alcohol membrane material with formaldehyde detection effect and preparation method thereof Download PDFInfo
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- CN103865217A CN103865217A CN201410093477.9A CN201410093477A CN103865217A CN 103865217 A CN103865217 A CN 103865217A CN 201410093477 A CN201410093477 A CN 201410093477A CN 103865217 A CN103865217 A CN 103865217A
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- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 239000004372 Polyvinyl alcohol Substances 0.000 title claims abstract description 34
- 229920002451 polyvinyl alcohol Polymers 0.000 title claims abstract description 34
- 230000000694 effects Effects 0.000 title claims abstract description 16
- 239000000463 material Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000001514 detection method Methods 0.000 title abstract description 10
- 239000012528 membrane Substances 0.000 title abstract description 4
- 239000002105 nanoparticle Substances 0.000 claims abstract description 29
- 239000000523 sample Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 10
- 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 63
- 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
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- 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
- 239000007788 liquid Substances 0.000 claims description 11
- 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
- 238000004090 dissolution Methods 0.000 claims description 7
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 7
- 239000002244 precipitate Substances 0.000 claims description 7
- 238000001556 precipitation Methods 0.000 claims description 7
- 239000000376 reactant Substances 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 7
- 238000000967 suction filtration Methods 0.000 claims description 7
- 229920001059 synthetic polymer Polymers 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 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
- 229920000642 polymer Polymers 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000007766 curtain coating Methods 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 239000010408 film Substances 0.000 description 26
- 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
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 230000005012 migration Effects 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
- 229920001577 copolymer Polymers 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
- 239000000203 mixture 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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Abstract
The invention discloses a polyvinyl alcohol membrane material with a formaldehyde detection effect and a preparation method thereof. The preparation method comprises the following steps: firstly synthesizing a polymer P(St-alt-Man) and formaldehyde probe molecules KD-XA01, preparing a P(St-alt-Man) nanoparticle solution loaded with probe molecules by a macromolecular self-assembly technology, adding the P(St-alt-Man) nanoparticle solution into a polyvinyl alcohol film-forming solution, and preparing the polyvinyl alcohol membrane material with the formaldehyde detection effect by adopting a curtain coating method.
Description
Technical field
The invention belongs to macromolecule member material and chemical sensor field, be specifically related to a kind of polyvinyl alcohol mould material with formaldehyde examination effect and preparation method thereof.
Background technology
Formaldehyde, at normal temperatures for having pungency and asphyxiant colourless gas, to person injury greatly, is one of environmental pollutant that day by day come into one's own, and preferentially controls list at China's noxious chemical, and formaldehyde occupies second.Therefore set up easy to operately, the method for determining formaldehyde that precision is high is even more important.Detecting the most frequently used method of formaldehyde is colorimetry, can be divided into again off-color acid method, acetylacetone method, AHMT colorimetry etc.; In national standard, detect textiles, food, in air, the prefered method of formaldehyde is exactly colorimetry, wherein most widely used general with acetylacetone method again.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 that checks more easily formaldehyde, it is simple to operate, what in formaldehyde test paper, play detection effect is the micromolecular compound of PARA FORMALDEHYDE PRILLS(91,95) sensitivity, but micromolecular compound has certain transport property, after long storage time along with the migration of micromolecular compound, its detection effect will inevitably reduce, and life cycle also can shorten.
Summary of the invention
The object of this invention is to provide a kind of polyvinyl alcohol mould material with formaldehyde examination effect and preparation method thereof, solve the problems such as existing formaldehyde sensor complex operation, life cycle be short.
For addressing the above problem, the invention provides a kind of polyvinyl alcohol mould material with 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 load probe molecule
P (St-alt-Man) nano-particle solution of described load probe molecule is made by following methods:
(1) synthesising probing needle molecule KD-XA01
By 3.24g1-phenyl-1,3-dimethyl diketone is dissolved in 60ml benzene, adds ammonium acetate 3.08g and acetic acid 1ml, and in nitrogen atmosphere, at 80 ℃, reflux and within 12 hours, obtain product, by reactant washing, dry, 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 use hot toluene drip washing, then being dissolved in acetone at 65 ℃ of oil baths, use toluene precipitate and separate. and after dissolution precipitation three times, in 30 ℃ of vacuum drying ovens, oven dry obtains P (St-alt-Man) repeatedly;
(3) nano-particle solution is prepared in self-assembly
Take P (St-alt-Man) 0.5g, KD-XA01 0.03g, is dissolved in the DMF of 10ml, vigorous stirring slowly drips ultrapure water, in the time there is blue-opalescent simultaneously, this solution is under agitation slowly dripped in 100ml ultrapure water, obtain this nano-particle solution.
Wherein, polyvinyl alcohol water solution mass concentration is 4-8%.
The preparation method of the above-mentioned polyvinyl alcohol mould material with formaldehyde examination effect comprises the following steps:
(1) synthesising probing needle molecule KD-XA01
By 3.24g1-phenyl-1,3-dimethyl diketone is dissolved in 60ml benzene, adds ammonium acetate 3.08g and acetic acid 1ml, and in nitrogen atmosphere, at 80 ℃, reflux and within 12 hours, obtain product, by reactant washing, dry, 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 65 ℃ of oil baths, use toluene precipitate and separate. repeatedly, after dissolution precipitation three times, in 30 ℃ of vacuum drying ovens, dry and obtain P (St-alt-Man);
(3) nano-particle solution is prepared in self-assembly
Take P (St-alt-Man) 0.5g, KD-XA01 0.03g, is dissolved in the DMF of 10ml, vigorous stirring slowly drips ultrapure water, in the time there is blue-opalescent simultaneously, this solution is under agitation slowly dripped in 100ml ultrapure water, obtain this nano-particle solution;
(4) prepare polyvinyl alcohol film
Weighing polyvinyl alcohol aqueous solution 8-9 part, P (St-alt-Man) nano-particle solution 1-2 part of load 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 ℃ of baking ovens, after 48 hours, takes out and takes off film.
Beneficial effect of the present invention: this patent has been invented a kind of thin film sensor, becoming membrane matrix is macromolecular material polyvinyl alcohol, in film forming liquid, add the nano-particle solution of PARA FORMALDEHYDE PRILLS(91,95) sensitivity, this nanoparticle is take parents' copolymer p (St-alt-Man) as carrier, probe molecule is had to satisfactory stability effect, can overcome the shortcoming of probe molecule migration.And in polymer P (St-alt-Man) maleic anhydride primitive give nanoparticle surface polar group carboxyl can with polyvinyl alcohol segments on hydroxyl form intermolecular hydrogen bonding effect, the consistency that the system that reaches is good.The thin-film material making is a kind of thin film sensor, easy to use, can whether convert the existence of formaldehyde to color signal and express, carry out qualitative analysis, can judge formaldehyde content height by shade simultaneously, also can, by film by instrumental characterizing, carry out quantitative analysis.
Accompanying drawing explanation:
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 load probe molecule
Fig. 4 mould material PARA FORMALDEHYDE PRILLS(91,95) detects effect
Embodiment
Below utilize embodiment to further describe the present invention, but can not think to limit scope of invention.
Configuration quality concentration is 4% polyvinyl alcohol water solution, takes in 4g polyvinyl alcohol 96g water stirring and dissolving.(1) synthesising probing needle molecule KD-XA01
By 3.24g1-phenyl-1,3-dimethyl diketone is dissolved in 60ml benzene, adds ammonium acetate 3.08g and acetic acid 1ml, and in nitrogen atmosphere, at 80 ℃, reflux and within 12 hours, obtain product, by reactant washing, dry, 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 use hot toluene drip washing, then being dissolved in acetone at 65 ℃ of oil baths, use toluene precipitate and separate. and after dissolution precipitation three times, in 30 ℃ of vacuum drying ovens, oven dry obtains P (St-alt-Man) repeatedly;
(3) prepare nano-particle solution
Take P (St-alt-Man) 0.5g, KD-XA01 0.03g, is dissolved in the DMF of 10ml, vigorous stirring slowly drips ultrapure water, in the time there is blue-opalescent simultaneously, this solution is under agitation slowly dripped in 100ml ultrapure water, obtain this nano-particle solution;
(4) prepare polyvinyl alcohol film
9 parts of the weighing polyvinyl alcohol aqueous solution, 1 part of P (St-alt-Man) nano-particle solution of load 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 ℃ of baking ovens, after 48 hours, takes out and takes off film.
Configuration quality concentration is 5% polyvinyl alcohol water solution, takes in 5g polyvinyl alcohol 95g water stirring and dissolving.(1) synthesising probing needle molecule KD-XA01
By 3.24g1-phenyl-1,3-dimethyl diketone is dissolved in 60ml benzene, adds ammonium acetate 3.08g and acetic acid 1ml, and in nitrogen atmosphere, at 80 ℃, reflux and within 12 hours, obtain product, by reactant washing, dry, 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 and use hot toluene drip washing, then being dissolved in acetone at 65 ℃ of oil baths, use toluene precipitate and separate. and after dissolution precipitation three times, in 30 ℃ of vacuum drying ovens, oven dry obtains P (St-alt-Man) repeatedly;
(3) prepare nano-particle solution
Take P (St-alt-Man) 0.5g, KD-XA01 0.03g, is dissolved in the DMF of 10ml, vigorous stirring slowly drips ultrapure water, in the time there is blue-opalescent simultaneously, this solution is under agitation slowly dripped in 100ml ultrapure water, obtain this nano-particle solution;
(4) prepare polyvinyl alcohol film
8 parts of the weighing polyvinyl alcohol aqueous solution, 2 parts of P (St-alt-Man) nano-particle solution of load probe molecule, mix to obtain film forming liquid under stirring, film forming liquid is evenly poured on film forming device, salivation film forming, puts into 40 ℃ of baking ovens, after 48 hours, takes out and takes off film.
Configuration quality concentration is 8% polyvinyl alcohol water solution, takes in 8g polyvinyl alcohol 92g water stirring and dissolving.(1) synthesising probing needle molecule KD-XA01
By 3.24g1-phenyl-1,3-dimethyl diketone is dissolved in 60ml benzene, adds ammonium acetate 3.08g and acetic acid 1ml, and in nitrogen atmosphere, at 80 ℃, reflux and within 12 hours, obtain product, by reactant washing, dry, 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 and use hot toluene drip washing, then being dissolved in acetone at 65 ℃ of oil baths, use toluene precipitate and separate. and after dissolution precipitation three times, in 30 ℃ of vacuum drying ovens, oven dry obtains P (St-alt-Man) repeatedly;
(3) prepare nano-particle solution
Take P (St-alt-Man) 0.5g, KD-XA01 0.03g, is dissolved in the DMF of 10ml, vigorous stirring slowly drips ultrapure water, in the time there is blue-opalescent simultaneously, this solution is under agitation slowly dripped in 100ml ultrapure water, obtain this nano-particle solution;
(4) prepare polyvinyl alcohol film
9 parts of the weighing polyvinyl alcohol aqueous solution, 1 part of P (St-alt-Man) nano-particle solution of load 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 ℃ of baking ovens, after 48 hours, takes out and takes off film.
Claims (3)
1. a polyvinyl alcohol mould material with formaldehyde examination effect, is characterized in that, comprises the component of following mass fraction: polyvinyl alcohol water solution 8-9 part, and P (St-alt-Man) nano-particle solution 1-2 part of load probe molecule,
P (St-alt-Man) nano-particle solution of described load probe molecule is made by following methods:
(1) synthesising probing needle molecule KD-XA01
By 3.24g1-phenyl-1,3-dimethyl diketone is dissolved in 60ml benzene, adds ammonium acetate 3.08g and acetic acid 1ml, and in nitrogen atmosphere, at 80 ℃, reflux and within 12 hours, obtain product, by reactant washing, dry, 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 65 ℃ of oil baths, and product suction filtration also use hot toluene drip washing, then be dissolved in acetone, uses toluene precipitate and separate, and after dissolution precipitation three times, in 30 ℃ of vacuum drying ovens, oven dry obtains P (St-alt-Man) repeatedly;
(3) nano-particle solution is prepared in self-assembly
Take P (St-alt-Man) 0.5g, KD-XA01 0.03g, is dissolved in the DMF of 10ml, vigorous stirring slowly drips ultrapure water, in the time there is blue-opalescent simultaneously, this solution is under agitation slowly dripped in 100ml ultrapure water, obtain this nano-particle solution.
2. the polyvinyl alcohol mould material with formaldehyde examination effect as claimed in claim 1, is characterized in that: polyvinyl alcohol water solution mass concentration is 4-8%, is preferably 4%.
3. the preparation method of the polyvinyl alcohol mould material with formaldehyde examination effect as claimed in claim 1 or 2, is characterized in that comprising the following steps:
(1) synthesising probing needle molecule KD-XA01
By 3.24g1-phenyl-1,3-dimethyl diketone is dissolved in 60ml benzene, adds ammonium acetate 3.08g and acetic acid 1ml, and in nitrogen atmosphere, at 80 ℃, reflux and within 12 hours, obtain product, by reactant washing, dry, 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 65 ℃ of oil baths, and product suction filtration also use hot toluene drip washing, then be dissolved in acetone, uses toluene precipitate and separate, and after dissolution precipitation three times, in 30 ℃ of vacuum drying ovens, oven dry obtains P (St-alt-Man) repeatedly;
(3) nano-particle solution is prepared in self-assembly
Take P (St-alt-Man) 0.5g, KD-XA01 0.03g, is dissolved in the DMF of 10ml, vigorous stirring slowly drips ultrapure water, in the time there is blue-opalescent simultaneously, this solution is under agitation slowly dripped in 100ml ultrapure water, obtain this nano-particle solution;
(4) prepare polyvinyl alcohol film
Weighing polyvinyl alcohol aqueous solution 8-9 part, P (St-alt-Man) nano-particle solution 1-2 part of load 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 ℃ of baking ovens, after 48 hours, takes out and takes off film.
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| KR101683037B1 (en) * | 2015-06-26 | 2016-12-06 | 한국화학연구원 | Composition for eliminating formaldehyde and formaldehyde-eliminating method using the same |
| CN108753186A (en) * | 2018-06-10 | 2018-11-06 | 孝感亿云新材料科技有限公司 | A kind of formaldehyde examination film patch and its application method |
| CN108802025A (en) * | 2018-06-10 | 2018-11-13 | 孝感亿云新材料科技有限公司 | A kind of preparation method of formaldehyde examination test paper |
| CN109001193A (en) * | 2018-06-10 | 2018-12-14 | 孝感亿云新材料科技有限公司 | A kind of preparation method of formaldehyde examination film patch |
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