CN1974609A - Electronic beam radiopolymerization process of directly synthesizing pH sensitive polymer hydrogel - Google Patents
Electronic beam radiopolymerization process of directly synthesizing pH sensitive polymer hydrogel Download PDFInfo
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- CN1974609A CN1974609A CN 200610144008 CN200610144008A CN1974609A CN 1974609 A CN1974609 A CN 1974609A CN 200610144008 CN200610144008 CN 200610144008 CN 200610144008 A CN200610144008 A CN 200610144008A CN 1974609 A CN1974609 A CN 1974609A
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- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 26
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- 230000000996 additive effect Effects 0.000 claims abstract description 22
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- 238000010894 electron beam technology Methods 0.000 claims description 19
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- 239000003795 chemical substances by application Substances 0.000 claims description 16
- MPNXSZJPSVBLHP-UHFFFAOYSA-N 2-chloro-n-phenylpyridine-3-carboxamide Chemical compound ClC1=NC=CC=C1C(=O)NC1=CC=CC=C1 MPNXSZJPSVBLHP-UHFFFAOYSA-N 0.000 claims description 11
- 238000009835 boiling Methods 0.000 claims description 11
- 238000001291 vacuum drying Methods 0.000 claims description 11
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 9
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 9
- LEJBBGNFPAFPKQ-UHFFFAOYSA-N 2-(2-prop-2-enoyloxyethoxy)ethyl prop-2-enoate Chemical compound C=CC(=O)OCCOCCOC(=O)C=C LEJBBGNFPAFPKQ-UHFFFAOYSA-N 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 239000002202 Polyethylene glycol Substances 0.000 claims description 6
- 125000004386 diacrylate group Chemical group 0.000 claims description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims description 6
- GWZMWHWAWHPNHN-UHFFFAOYSA-N 2-hydroxypropyl prop-2-enoate Chemical compound CC(O)COC(=O)C=C GWZMWHWAWHPNHN-UHFFFAOYSA-N 0.000 claims description 5
- 229920002401 polyacrylamide Polymers 0.000 claims description 5
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 4
- 229920001661 Chitosan Polymers 0.000 claims description 4
- CNCOEDDPFOAUMB-UHFFFAOYSA-N N-Methylolacrylamide Chemical compound OCNC(=O)C=C CNCOEDDPFOAUMB-UHFFFAOYSA-N 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
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- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- AGPVCXSFAVEGFP-UHFFFAOYSA-N C(C(=C)C)(=O)N.[N] Chemical compound C(C(=C)C)(=O)N.[N] AGPVCXSFAVEGFP-UHFFFAOYSA-N 0.000 description 1
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 1
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- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
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- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 description 1
- PBSASXNAZJHOBR-UHFFFAOYSA-N n-(2-methylpropyl)prop-2-enamide Chemical compound CC(C)CNC(=O)C=C PBSASXNAZJHOBR-UHFFFAOYSA-N 0.000 description 1
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Abstract
The present invention is electronic beam radiopolymerization process of synthesizing pH sensitive hydrogel directly, and belongs to the field of pH sensitive hydrogel preparing technology. Material monomer, cross-linking agent and additive in the weight ratio of 75-99.7 to 0.1- 25 to 0.1-10 are dissolved in deionized water and polymerized through electron radiation to form cross-linked polymer. The cross-linked polymer is then extracted in a Soxhlet extractor with boiled deionized water for 24 hr and dried in a vacuum oven to obtain the pH sensitive hydrogel. The present invention has the features of low power consumption, simple technological process, high polymerization efficiency, no waste water pollution, low cost, normal temperature and normal pressure operation, etc.
Description
Technical field
The present invention relates to the directly method of synthetic pH sensitive polymer hydrogel of a kind of electron beam irradiation polymerization, belong to pH sensitive polymer hydrogel preparation method technical field.
Background technology
The multicomponent system that hydrogel is made of jointly the superpolymer and the medium of three-dimensional crosslinked network structure, because of its unique stimuli responsive behavior, show good prospects for application in fields such as drug delivery system, memory cell switch, chemical material separation, chemical machinery, artificial-muscles, thereby caused domestic and international many scholars' extensive concern.The stimulating responsive hydrogel be a class for external environment small physics or chemical stimulation, the hydrogel of considerable change can take place in himself character.It is a kind of water insoluble, can be in water swollen hydrophilic cross-linking polymkeric substance.External environment factors vary such as the stimulating responsive hydrogel can response temperature, pH, light, electric field and magnetic field.
Utilize the deformation behavior of stimulating responsive hydrogel under environmental stimulus, people dream up various chemical energy-mechanical energy conversion system, as artificial muscle model, chemical valve, shape-memory material, medicine controlled releasing, sewage disposal etc.The stimulating responsive hydrogel is increasing in the application of bio-science fields such as the activity control of cell culture substrate, enzyme, target administration in recent years.The basis of stimulating responsive macromolecule hydrogel researchdevelopment is the gel swelling theory of Flory PJ, utilizes factors such as the intermolecular interaction field of force, ion electric field and photochemical effect to make the volume of hydrogel produce response.From the selection of hydrogel matrix, mostly adopt synthetic polymer both at home and abroad, promptly by system in response such as homopolymer, grafting or segmented copolymer, blend, interpenetrating polymer networks and polymer microsphere.In view of the huge applications of stimulating responsive hydrogel at biological field is worth, obtained suitable attention to have the good and biodegradable chitosan of the natural macromolecular material of gel phase transformation characteristic, particularly biocompatibility for the research of the hydrogel on basis.Current have the throwing oneself into research of synthetic, structure, performance and Response Mechanism of hydrogel of many scholars, believes that in the near future we can realize the huge convenience that work that the stimulating responsive hydrogel is given us and life bring.
Contain a large amount of facile hydrolysiss or protonated acid, base groups in the pH sensitive aqueous gel, as carboxyl and amino, dissociating of these groups is subjected to the influence of extraneous pH.When the pH of extraneous solution changed, the corresponding change of the dissociation degree of these groups caused the inside and outside ionic concn of hydrogel to change.Dissociating of these groups also can be destroyed corresponding hydrogen bond in the gel in addition, and the cross-linking set of hydrogel cross-linked network is reduced, and causes the hydrogel network structure to change, thereby causes the variation of swelling behavior ability.
The pH susceptibility of hydrogel is found during the earliest by polyacrylamide gel swelling ratio after measuring ageing of the T.Tanaka of U.S. Massachusetts Institute of Technology.This gellike contains a large amount of facile hydrolysiss and the protonated group that dissociates, when extraneous pH changed, the corresponding change of the dissociation degree of these groups caused the variation of the inside and outside ionic concn of gel, and cause and the generation or the fracture of hydrogen bond in the network cause the discontinuous volume phase transformation of gel.N such as the E.O.Akala of U.S. Howard University, N-DMAA, N-isobutyl-acrylamide, vinylformic acid, 4,4-two (Methacrylamide) nitrogen benzide and N-fatty group-O-methacryloyl hydroxylamine has synthesized a kind of pH sensitive aquagel of novelty.They have studied the chain length of fatty group (proyl, hexyl, dodecyl) and content to the swelling effect of kinetics, find that the hydrolysis rate of side chain depends on the chain length and the content of hydrolyzable comonomer in network structure of fatty group.The Chiu H.C. of Taiwan National ChungHsing University etc. has studied vinylformic acid to the preparation of the responsive dextran hydrogel of pH and the influence of swelling behavior.The cross-linking density of methacrylic acid dextran ester and acrylic copolymer is because acrylic acid bridging action and increasing with the increase of acrylic acid content, thereby causes this hydrogel to have bigger swelling capacity.The Cheng Y.F. of U.S. University of New Mexico etc. has studied radiation synthesis and has prepared hydrogel and response performance and swelling kinetics.The Zhuo Renxi of Wuhan University etc. has synthesized the polymkeric substance of the molecule interpenetrating(polymer)networks of vinylformic acid with temperature and pH sensitivity and N-N-isopropylacrylamide, and has studied its swelling behavior and the application on the biomacromolecule controlled release.
At present, the method for preparing the pH sensitive aqueous gel both at home and abroad is based on traditional thermopolymerization and gamma-radiation radio polymerization, and the directly synthetic pH sensitive aqueous gel of electron beam irradiation polymerization is a kind of new method, present domestic any patent report that still do not have.
Summary of the invention
The purpose of this invention is to provide the directly method of synthetic pH sensitive polymer hydrogel of a kind of electron beam irradiation polymerization.Utilize electron beam as source of radiation, the directly synthetic pH sensitive aqueous gel of radiation polymerization is a kind of new technology.This technology has that energy consumption is low, polymerization velocity is fast, reaction efficiency is high, can react at normal temperatures and pressures and open system in characteristics such as operate, greatly simplified polymerization technique, shortcomings such as high energy consumption in the traditional preparation process method, response procedures complexity, polymerization time length and waste liquor contamination have been avoided, for suitability for industrialized production pH sensitive aqueous gel has been opened up new approach.The raw material of this polymerization process comprises monomer, linking agent and additive etc., can form stable homogeneous system in the aqueous solution, and the polymerization process three-waste free pollution is a kind of method for preparing hydrogel of efficient and environmental protection.
The electron beam irradiation polymerization is the method for synthetic pH sensitive polymer hydrogel directly, it is characterized in that this method may further comprise the steps:
(1) starting monomer, linking agent, additive are dissolved in the deionized water by following quality percentage composition (not comprising deionized water),
Monomer 75～99.7wt%,
Linking agent 0.1～25wt%,
Additive 0.1～10wt%,
The quality percentage composition 100% of three kinds of raw materials;
Described monomer is any or multiple composition in vinylformic acid and 2-methylacryoyloxyethyl trimethyl ammonium chloride, methacrylic acid, the MALEIC ANHYDRIDE;
Described linking agent is N, any in N '-methylene-bisacrylamide, diethylene glycol diacrylate, three polyethyleneglycol diacrylates, four polyethyleneglycol diacrylates, Hydroxyethyl acrylate, the Propylene glycol monoacrylate;
Described additive is one or more in n-methylolacrylamide, N-N-isopropylacrylamide, polyvinyl alcohol, chitosan, acrylamide, the polyacrylamide;
(2) solution that step (1) is disposed aggregates into cross-linked polymer through electron beam irradiation;
(3) the described cross-linked polymer of step (2) is put into apparatus,Soxhlet's with the deionized water extracting 24 hours of boiling; After the taking-up, it is dry to put into vacuum drying oven, promptly obtains described pH sensitive polymer hydrogel.
Its radio polymerization response path is as follows:
Utilize the directly synthetic temperature-sensitive hydrogel method of above-mentioned electron beam irradiation polymerization, can prepare the hydrogel of multiple different performance.The swelling ability of such pH sensitive aqueous gel in solution changes with the pH value variation of solution, is in the scope of 6-8 in the pH of solution value, the swelling ability maximum of hydrogel.By regulating the kind and the content of additives in raw materials, make the equilibrium swelling multiple of hydrogel and physical strength to some extent difference to be suitable for various Application Areas and purposes.This preparation method has that energy consumption is low, technology is simple, polyreaction efficient height, normal temperature and pressure open operation, no waste liquor contamination and characteristics such as with low cost.
Description of drawings
Fig. 1 is a radio polymerization response path synoptic diagram of the present invention.
Embodiment
Specify the present invention below in conjunction with embodiment.
The embodiment radiation devices is a linear electron accelerator.
Embodiment 1
5g monomer (vinylformic acid), 1.3g monomer (2-methylacryoyloxyethyl trimethyl ammonium chloride), 0.35g monomer (methacrylic acid), 0.45g monomer (MALEIC ANHYDRIDE), 0.25g linking agent (four polyethyleneglycol diacrylates), 0.05g additive (n-methylolacrylamide), 0.025g additive (chitosan) are dissolved in the 16mL deionized water.The solution for preparing is placed beaker, obtain cross-linked polymer through electron beam irradiation.Cross-linked polymer is put into apparatus,Soxhlet's with the deionized water extracting 24 hours of boiling, put into the vacuum drying oven drying after the taking-up, obtain the pH sensitive aqueous gel.
Embodiment 2
5g monomer (vinylformic acid), 2.53g monomer (2-methylacryoyloxyethyl trimethyl ammonium chloride), 0.33g monomer (methacrylic acid), 0.52g monomer (MALEIC ANHYDRIDE), 0.018g linking agent (N, N '-methylene-bisacrylamide), 0.053g additive (n-methylolacrylamide) are dissolved in the 15mL deionized water.The solution for preparing is placed beaker, obtain cross-linked polymer through electron beam irradiation.Cross-linked polymer is put into apparatus,Soxhlet's with the deionized water extracting 24 hours of boiling, put into the vacuum drying oven drying after the taking-up, obtain the pH sensitive aqueous gel.
Embodiment 3
5g monomer (vinylformic acid), 1.2g monomer (2-methylacryoyloxyethyl trimethyl ammonium chloride), 0.23g monomer (methacrylic acid), 0.51g monomer (MALEIC ANHYDRIDE), 0.24g linking agent (three polyethyleneglycol diacrylates), 0.05g additive (polyvinyl alcohol), 0.015g additive (N-N-isopropylacrylamide) are dissolved in the 16mL deionized water.The solution for preparing is placed beaker, obtain cross-linked polymer through electron beam irradiation.Cross-linked polymer is put into apparatus,Soxhlet's with the deionized water extracting 24 hours of boiling, put into the vacuum drying oven drying after the taking-up, obtain the pH sensitive aqueous gel.
Embodiment 4
5g monomer (vinylformic acid), 1.36g monomer (2-methylacryoyloxyethyl trimethyl ammonium chloride), 0.25g monomer (methacrylic acid), 0.23g monomer (MALEIC ANHYDRIDE), 0.58g linking agent (Hydroxyethyl acrylate), 0.05g additive (N-N-isopropylacrylamide), 0.05g additive (acrylamide) are dissolved in the 15mL deionized water.The solution for preparing is placed beaker, obtain cross-linked polymer through electron beam irradiation.Cross-linked polymer is put into apparatus,Soxhlet's with the deionized water extracting 24 hours of boiling, put into the vacuum drying oven drying after the taking-up, obtain the pH sensitive aqueous gel.
Embodiment 5
5g monomer (vinylformic acid), 2.2g monomer (2-methylacryoyloxyethyl trimethyl ammonium chloride), 0.33g monomer (MALEIC ANHYDRIDE), 0.15g linking agent (diethylene glycol diacrylate), 0.02g additive (N-N-isopropylacrylamide) are dissolved in the 15mL deionized water.The solution for preparing is placed beaker, obtain cross-linked polymer through electron beam irradiation.Cross-linked polymer is put into apparatus,Soxhlet's with the deionized water extracting 24 hours of boiling, put into the vacuum drying oven drying after the taking-up, obtain the pH sensitive aqueous gel.
Embodiment 6
5g monomer (vinylformic acid), 0.83g monomer (2-methylacryoyloxyethyl trimethyl ammonium chloride), 0.46g monomer (methacrylic acid), 0.25g monomer (MALEIC ANHYDRIDE), 0.52g linking agent (Propylene glycol monoacrylate), 0.05g additive (N-N-isopropylacrylamide), 0.02g additive (polyacrylamide) are dissolved in the 13mL deionized water.The solution for preparing is placed beaker, obtain cross-linked polymer through electron beam irradiation.Cross-linked polymer is put into apparatus,Soxhlet's with the deionized water extracting 24 hours of boiling, put into the vacuum drying oven drying after the taking-up, obtain the pH sensitive aqueous gel.
Embodiment 7
5g monomer (vinylformic acid), 1.83g monomer (2-methylacryoyloxyethyl trimethyl ammonium chloride), 0.27g monomer (methacrylic acid), 0.14g monomer (MALEIC ANHYDRIDE), 0.59g linking agent (Propylene glycol monoacrylate) are dissolved in the 15mL deionized water.The solution for preparing is placed beaker, obtain cross-linked polymer through electron beam irradiation.Cross-linked polymer is put into apparatus,Soxhlet's with the deionized water extracting 24 hours of boiling, put into the vacuum drying oven drying after the taking-up, obtain the pH sensitive aqueous gel.
Embodiment 8
5g monomer (vinylformic acid), 1.92g monomer (2-methylacryoyloxyethyl trimethyl ammonium chloride), 0.66g linking agent (Propylene glycol monoacrylate), 0.05g additive (N-N-isopropylacrylamide), 0.02g additive (acrylamide) are dissolved in the 16mL deionized water.The solution for preparing is placed beaker, obtain cross-linked polymer through electron beam irradiation.Cross-linked polymer is put into apparatus,Soxhlet's with the deionized water extracting 24 hours of boiling, put into the vacuum drying oven drying after the taking-up, obtain the pH sensitive aqueous gel.
Embodiment 9
5g monomer (vinylformic acid), 2.1g monomer (2-methylacryoyloxyethyl trimethyl ammonium chloride), 0.35g monomer (methacrylic acid), 0.15g linking agent (diethylene glycol diacrylate), 0.02g additive (N-N-isopropylacrylamide), 0.02g additive (polyacrylamide) are dissolved in the 15mL deionized water.The solution for preparing is placed beaker, obtain cross-linked polymer through electron beam irradiation.Cross-linked polymer is put into apparatus,Soxhlet's with the deionized water extracting 24 hours of boiling, put into the vacuum drying oven drying after the taking-up, obtain the pH sensitive aqueous gel.
Claims (1)
1, the method for pH sensitive polymer hydrogel is directly synthesized in the electron beam irradiation polymerization, it is characterized in that this method may further comprise the steps:
(1) starting monomer, linking agent, additive are dissolved in the deionized water by following quality percentage composition (not comprising deionized water),
Monomer 75～99.7wt%,
Linking agent 0.1～25wt%,
Additive 0.1～10wt%,
The quality percentage composition 100% of three kinds of raw materials;
Described monomer is any or multiple composition in vinylformic acid and 2-methylacryoyloxyethyl trimethyl ammonium chloride, methacrylic acid, the MALEIC ANHYDRIDE;
Described linking agent is N, any in N '-methylene-bisacrylamide, diethylene glycol diacrylate, three polyethyleneglycol diacrylates, four polyethyleneglycol diacrylates, Hydroxyethyl acrylate, the Propylene glycol monoacrylate;
Described additive is one or more in n-methylolacrylamide, N-N-isopropylacrylamide, polyvinyl alcohol, chitosan, acrylamide, the polyacrylamide;
(2) solution that step (1) is disposed aggregates into cross-linked polymer through electron beam irradiation;
(3) the described cross-linked polymer of step (2) is put into apparatus,Soxhlet's with the deionized water extracting 24 hours of boiling; After the taking-up, it is dry to put into vacuum drying oven, promptly obtains described pH sensitive polymer hydrogel.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102633949A (en) * | 2012-05-16 | 2012-08-15 | 苏州宜生生物技术有限公司 | Method for preparing semi-interpenetrating network hydrogel |
| CN101708342B (en) * | 2009-12-22 | 2012-10-31 | 上海大学 | Temperature sensitive wound face dressing film and preparation method thereof |
| CN103071181A (en) * | 2013-02-01 | 2013-05-01 | 刘昌桂 | Hydrogel as well as preparation method and purpose of hydrogel |
| CN104894672A (en) * | 2015-06-04 | 2015-09-09 | 常州大学 | Method for preparing pH-value-sensitive crosslinked fiber through low-temperature photopolymerization |
| CN107141407A (en) * | 2017-05-25 | 2017-09-08 | 华南理工大学 | It is a kind of can spontaneous driving polyampholyte hydrogel driver and preparation method thereof and type of drive |
| CN112354530A (en) * | 2020-11-18 | 2021-02-12 | 天津工业大学 | Amphoteric adsorption material with salt resistance and preparation method and application thereof |
-
2006
- 2006-11-24 CN CN 200610144008 patent/CN1974609A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101708342B (en) * | 2009-12-22 | 2012-10-31 | 上海大学 | Temperature sensitive wound face dressing film and preparation method thereof |
| CN102633949A (en) * | 2012-05-16 | 2012-08-15 | 苏州宜生生物技术有限公司 | Method for preparing semi-interpenetrating network hydrogel |
| CN102633949B (en) * | 2012-05-16 | 2014-03-05 | 苏州宜生生物技术有限公司 | Method for preparing semi-interpenetrating network hydrogel |
| CN103071181A (en) * | 2013-02-01 | 2013-05-01 | 刘昌桂 | Hydrogel as well as preparation method and purpose of hydrogel |
| CN103071181B (en) * | 2013-02-01 | 2015-04-29 | 刘昌桂 | Hydrogel as well as preparation method and purpose of hydrogel |
| CN104894672A (en) * | 2015-06-04 | 2015-09-09 | 常州大学 | Method for preparing pH-value-sensitive crosslinked fiber through low-temperature photopolymerization |
| CN107141407A (en) * | 2017-05-25 | 2017-09-08 | 华南理工大学 | It is a kind of can spontaneous driving polyampholyte hydrogel driver and preparation method thereof and type of drive |
| CN107141407B (en) * | 2017-05-25 | 2019-04-09 | 华南理工大学 | It is a kind of can spontaneous driving polyampholyte hydrogel driver and preparation method thereof and driving method |
| CN112354530A (en) * | 2020-11-18 | 2021-02-12 | 天津工业大学 | Amphoteric adsorption material with salt resistance and preparation method and application thereof |
| CN112354530B (en) * | 2020-11-18 | 2021-08-27 | 天津工业大学 | Amphoteric adsorption material with salt resistance and preparation method and application thereof |
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