CN105295077A - Temperature sensitive type polyion liquid gel and preparation method thereof - Google Patents

Temperature sensitive type polyion liquid gel and preparation method thereof Download PDF

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CN105295077A
CN105295077A CN201510859268.5A CN201510859268A CN105295077A CN 105295077 A CN105295077 A CN 105295077A CN 201510859268 A CN201510859268 A CN 201510859268A CN 105295077 A CN105295077 A CN 105295077A
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ionic liquid
gly
glycine
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贺晓凌
赵宇新
金镇栗
苏宇
刘晓
魏东盛
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Tianjin Polytechnic University
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Tianjin Polytechnic University
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Abstract

The invention discloses temperature sensitive type polyion liquid gel and a preparation method thereof, relates to the field of high polymer materials, and particularly relates to temperature responsive polyion liquid gel and a preparation method thereof. The gel can be prepared by the following method: forming ion liquid by glycine of good biocompatibility and choline, and forming vinyl choline-glycine ion liquid monomer by modifying the ion liquid through acrylic acid, and then preparing the temperature sensitive type polyion liquid gel by free radical polymerization with a temperature sensitive material N-isopropyl acrylamide (NIPAAm), taking N,N-methylenebisacrylamide (MBAA) as a cross-linking agent, and potassium persulfate as an initiator. The gel is applied to damage-free desorption of cells.

Description

A kind of temperature sensitive type poly ionic liquid gel and preparation method thereof
Technical field
The present invention relates to polymeric material field, particularly a kind of temperature-responsive poly ion liquid gel and preparation method thereof.
Background technology
In recent years along with the rise of Green Chemistry, the research of " green solvent "-ionic liquid starts global range upsurge, and in national strategy plan of science and technology is listed ionic liquid by the U.S., Europe, Japan etc.Poly ion liquid is the product of ionic liquid and polymer science cross coupled, has the premium properties of ionic liquid and polymkeric substance concurrently, demonstrates the advantage that small molecular ion liquid is incomparable, and the research of related fields also causes the broad interest of people just gradually.But with small molecular ion liquid phase ratio, the research of poly ion liquid is ripe not enough, its kind far away from small molecular ion liquid, therefore, be use for reference with the pass of small molecular ion liquid structure and performance, design and synthesis goes out greater functionality poly ion liquid and has important scientific meaning.In application aspect, small molecular ion liquid in the energy, chemical, biotechnology, industrially enter practical stage, and the application of poly ion liquid in most of field is also in the preliminary study stage, therefore, deeply develop poly ion liquid to have important practical significance in the application of more wide field.The applied research of current poly ion liquid has born first fruit in polymer catalyst, polymer dielectric, gas adsorption/parting material etc., but as the research of biomaterial, there is not been reported in field of tissue engineering technology.Along with the research of ionic liquid enters " ergasia " stage, increasing functional ionic liquids continues to bring out, this greenization being biomaterial and expansion selection range provide possibility, explore the application of poly ion liquid as biologic bracket material aspect, not only can find new biomaterial type, and the Application Areas of poly ion liquid can be widened further.
Hydrogel is the ubiquitous a kind of physical form of occurring in nature, and the mass part (organ such as muscle, blood vessel, eyeball as human body) of living organism is formed by hydrogel.Hydrogel has good biocompatibility, the biological activity being fixed on cell in hydrogel can keep the long period, and hydrogel has the mechanical characteristics that can compare favourably with soft tissue, therefore, there is widespread use in the field such as biological chemistry, medical science in hydrogel.Environment-responsive gel in hydrogel is owing to having optical, electrical, hot, the unique performance such as pH is responsive, biochemistry is responsive, become the focus of current research especially, conduct extensive research in fields such as the Co ntrolled release of cellular segregation and cultivation, materials abstraction, immobilized enzyme, medicine and targeted drugs.The present invention is the Application Areas of exploitation ionic liquid, give its functionalization, ionic liquid is introduced environmental stimulus responsive gel field, with temperature sensitive material PNIPAM (PNIPAAm) connected applications, research and develop a kind of temperature sensitive type poly ionic liquid gel, be applied to the not damaged desorption of cell and cell sheets.
Summary of the invention
The object of the present invention is to provide a kind of temperature sensitive type poly ionic liquid gel, this gel has temperature-responsive, can be applicable to the not damaged desorption of cell and cell sheets.Temperature sensitive type poly ionic liquid gel provided by the present invention can be obtained by following methods:
(1) preparation of ionic liquid
Take glycine (Gly) and choline (Ch) respectively, respectively be dissolved in 5ml distilled water, Gly: Ch=2mol: 1mol ~ 1mol: 1mol, at 3 DEG C ~ 25 DEG C, with constant pressure funnel, choline solution is slowly added glycine solution, magnetic agitation reaction 48h; Reaction terminates rear 60 DEG C of backspins steaming and dewaters, and then pours excess ethyl alcohol into above-mentioned reaction system, to remove unreacted glycine; Vacuum-drying reaction product at 50 DEG C, to remove residual second alcohol and water, obtains pure choline-glycine (Ch-Gly) ionic liquid.
(2) preparation of vinyl ionic liquid monomer
Take vinylformic acid (AAc), be dissolved in 10ml distilled water, add N-hydroxy-succinamide (NHS) and 1-ethyl-3-(3-dimethylamine propyl) carbodiimide (EDC), after room temperature lower magnetic force stirs 2h, add choline-glycine (Ch-Gly) ionic liquid and continue reaction 24h, AAc: Ch-Gly: EDC: NHS=5mol: 5mol: 5mol: 1mol; Pour excess ethyl alcohol after reaction terminates into leave standstill, precipitation to be precipitated is complete, and centrifugation, obtains vinyl choline-glycine ionic liquid monomer (Ch-Gly-AAc).
(3) preparation of temperature sensitive type poly ionic liquid gel
Take vinyl choline-glycine ionic liquid monomer (Ch-Gly-AAc) and N-isopropylacrylamide (NIPAAm) monomer, be dissolved in 10ml distilled water, two monomer total masses are 1g, wherein two monomer weight ratio are Gly-AAc: NIPAAm=0: 1,1: 4,1: 2,1: 1,2: 1,4: 1,1: 0,0.1g ~ 0.5g linking agent N is added under nitrogen protection, N-methylene-bisacrylamide (MBAA), stir 20min, then react 15min under adding 0.01g ~ 0.05g initiator potassium persulfate (KPS) room temperature and obtain coagulant liquid; Pour coagulant liquid into glass mold, dropping 1ml2%N, N, N ', N '-Tetramethyl Ethylene Diamine (TEMED), room temperature reaction 24h, forms gel.
Another object of the present invention is to the preparation method providing a kind of temperature sensitive type poly ionic liquid gel, preparation method comprises the following steps:
(1) preparation of ionic liquid
Take glycine (Gly) and choline (Ch) respectively, respectively be dissolved in 5ml distilled water, Gly: Ch=2mol: 1mol ~ 1mol: 1mol, at 3 DEG C ~ 25 DEG C, with constant pressure funnel, choline solution is slowly added glycine solution, magnetic agitation reaction 48h; Reaction terminates rear 60 DEG C of backspins steaming and dewaters, and then pours excess ethyl alcohol into above-mentioned reaction system, to remove unreacted glycine; Vacuum-drying reaction product at 50 DEG C, to remove residual second alcohol and water, obtains pure choline-glycine (Ch-Gly) ionic liquid.
(2) preparation of vinyl ionic liquid monomer
Take vinylformic acid (AAc), be dissolved in 10ml distilled water, add N-hydroxy-succinamide (NHS) and 1-ethyl-3-(3-dimethylamine propyl) carbodiimide (EDC), after room temperature lower magnetic force stirs 2h, add choline-glycine (Ch-Gly) ionic liquid and continue reaction 24h, AAc: Ch-Gly: EDC: NHS=5mol: 5mol: 5mol: 1mol; Pour excess ethyl alcohol after reaction terminates into leave standstill, precipitation to be precipitated is complete, and centrifugation, obtains vinyl choline-glycine ionic liquid monomer (Ch-Gly-AAc).
(3) preparation of temperature sensitive type poly ionic liquid gel
Take vinyl choline-glycine ionic liquid monomer (Ch-Gly-AAc) and N-isopropylacrylamide (NIPAAm) monomer, be dissolved in 10ml distilled water, two monomer total masses are 1g, wherein two monomer weight ratio are Gly-AAc: NIPAAm=0: 1,1: 4,1: 2,1: 1,2: 1,4: 1,1: 0,0.1g ~ 0.5g linking agent N is added under nitrogen protection, N-methylene-bisacrylamide (MBAA), stir 20min, then react 15min under adding 0.01g ~ 0.05g initiator potassium persulfate (KPS) room temperature and obtain coagulant liquid; Pour coagulant liquid into glass mold, dropping 1ml2%N, N, N ', N '-Tetramethyl Ethylene Diamine (TEMED), room temperature reaction 24h, forms gel.
Beneficial effect
Temperature sensitive type poly ionic liquid gel designed by the present invention and preparation method thereof, provides the preparation method of novel poly ion liquid on the one hand, has widened the Application Areas of poly ion liquid, developed the application potential of poly ion liquid; The gelatinous material that provides has temperature-responsive on the other hand; at 37 DEG C of cell culture temperature; cell can adsorb in gel surface, breed; form cell sheets, moved to low temperature environment (lower than 32 DEG C), PNIPAAm molecular chain stretches; hydrophobic grouping exposes; performance hydrophobicity, can realize the automatic desorption of cell from material surface, Cell protection function is injury-free.
Specific embodiments
Embodiment 1.
(1) preparation of ionic liquid
Take glycine (Gly) and choline (Ch) respectively, be respectively dissolved in 5ml distilled water, Gly: Ch=1.05mol: 1mol, with constant pressure funnel, choline solution added glycine solution lentamente at 3 DEG C, magnetic agitation reaction 48h; Reaction terminates rear 60 DEG C of backspins steaming and dewaters, and then pours excess ethyl alcohol into above-mentioned reaction system, to remove unreacted glycine; Vacuum-drying reaction product at 50 DEG C, to remove residual second alcohol and water, obtains pure choline-glycine (Ch-Gly) ionic liquid.
(2) preparation of vinyl ionic liquid monomer
Take vinylformic acid (AAc), be dissolved in 10ml distilled water, add N-hydroxy-succinamide (NHS) and 1-ethyl-3-(3-dimethylamine propyl) carbodiimide (EDC), after room temperature lower magnetic force stirs 2h, add choline-glycine (Ch-Gly) ionic liquid and continue reaction 24h, AAc: Ch-Gly: EDC: NHS=5mol: 5mol: 5mol: 1mol; Pour excess ethyl alcohol after reaction terminates into leave standstill, precipitation to be precipitated is complete, and centrifugation, obtains vinyl choline-glycine ionic liquid monomer (Ch-Gly-AAc).
(3) preparation of temperature sensitive type poly ionic liquid gel
Take vinyl choline-glycine ionic liquid monomer (Ch-Gly-AAc) and N-isopropylacrylamide (NIPAAm) monomer, be dissolved in 10ml distilled water, two monomer total masses are 1g, wherein two monomer weight ratio are Gly-AAc: NIPAAm=1: 1,0.1g linking agent N is added under nitrogen protection, N-methylene-bisacrylamide (MBAA), stirs 20min, then reacts 15min under adding 0.01g initiator potassium persulfate (KPS) room temperature and obtain coagulant liquid; Pour coagulant liquid into glass mold, dropping 1ml2%N, N, N ', N '-Tetramethyl Ethylene Diamine (TEMED), room temperature reaction 24h, forms gel.
Embodiment 2.
(1) preparation of ionic liquid
Take glycine (Gly) and choline (Ch) respectively, be respectively dissolved in 5ml distilled water, Gly: Ch=1mol: 1mol, with constant pressure funnel, choline solution added glycine solution lentamente at 3 DEG C, magnetic agitation reaction 48h; Reaction terminates rear 60 DEG C of backspins steaming and dewaters, and then pours excess ethyl alcohol into above-mentioned reaction system, to remove unreacted glycine; Vacuum-drying reaction product at 50 DEG C, to remove residual second alcohol and water, obtains pure choline-glycine (Ch-Gly) ionic liquid.
(2) preparation of vinyl ionic liquid monomer
Take vinylformic acid (AAc), be dissolved in 10ml distilled water, add N-hydroxy-succinamide (NHS) and 1-ethyl-3-(3-dimethylamine propyl) carbodiimide (EDC), after room temperature lower magnetic force stirs 2h, add choline-glycine (Ch-Gly) ionic liquid and continue reaction 24h, AAc: Ch-Gly: EDC: NHS=5mol: 5mol: 5mol: 1mol; Pour excess ethyl alcohol after reaction terminates into leave standstill, precipitation to be precipitated is complete, and centrifugation, obtains vinyl choline-glycine ionic liquid monomer (Ch-Gly-AAc).
(3) preparation of temperature sensitive type poly ionic liquid gel
Take vinyl choline-glycine ionic liquid monomer (Ch-Gly-AAc) and N-isopropylacrylamide (NIPAAm) monomer, be dissolved in 10ml distilled water, two monomer total masses are 1g, wherein two monomer weight ratio are Gly-AAc: NIPAAm=1: 2,0.5g linking agent N is added under nitrogen protection, N-methylene-bisacrylamide (MBAA), stirs 20min, then reacts 15min under adding 0.05g initiator potassium persulfate (KPS) room temperature and obtain coagulant liquid; Pour coagulant liquid into glass mold, dropping 1ml2%N, N, N ', N '-Tetramethyl Ethylene Diamine (TEMED), room temperature reaction 24h, forms gel.
Embodiment 3.
(1) preparation of ionic liquid
Take glycine (Gly) and choline (Ch) respectively, be respectively dissolved in 5ml distilled water, Gly: Ch=2mol: 1mol, with constant pressure funnel, choline solution added glycine solution lentamente at 3 DEG C, magnetic agitation reaction 48h; Reaction terminates rear 60 DEG C of backspins steaming and dewaters, and then pours excess ethyl alcohol into above-mentioned reaction system, to remove unreacted glycine; Vacuum-drying reaction product at 50 DEG C, to remove residual second alcohol and water, obtains pure choline-glycine (Ch-Gly) ionic liquid.
(2) preparation of vinyl ionic liquid monomer
Take vinylformic acid (AAc), be dissolved in 10ml distilled water, add N-hydroxy-succinamide (NHS) and 1-ethyl-3-(3-dimethylamine propyl) carbodiimide (EDC), after room temperature lower magnetic force stirs 2h, add choline-glycine (Ch-Gly) ionic liquid and continue reaction 24h, AAc: Ch-Gly: EDC: NHS=5mol: 5mol: 5mol: 1mol; Pour excess ethyl alcohol after reaction terminates into leave standstill, precipitation to be precipitated is complete, and centrifugation, obtains vinyl choline-glycine ionic liquid monomer (Ch-Gly-AAc).
(3) preparation of temperature sensitive type poly ionic liquid gel
Take vinyl choline-glycine ionic liquid monomer (Ch-Gly-AAc) and N-isopropylacrylamide (NIPAAm) monomer, be dissolved in 10ml distilled water, two monomer total masses are 1g, wherein two monomer weight ratio are Gly-AAc: NIPAAm=1: 4,0.3g linking agent N is added under nitrogen protection, N-methylene-bisacrylamide (MBAA), stirs 20min, then reacts 15min under adding 0.03g initiator potassium persulfate (KPS) room temperature and obtain coagulant liquid; Pour coagulant liquid into glass mold, dropping 1ml2%N, N, N ', N '-Tetramethyl Ethylene Diamine (TEMED), room temperature reaction 24h, forms gel.
Embodiment 4.
(1) preparation of ionic liquid
Take glycine (Gly) and choline (Ch) respectively, be respectively dissolved in 5ml distilled water, Gly: Ch=1.05mol: 1mol, at 25 DEG C, with constant pressure funnel, choline solution added glycine solution lentamente, magnetic agitation reaction 48h; Reaction terminates rear 60 DEG C of backspins steaming and dewaters, and then pours excess ethyl alcohol into above-mentioned reaction system, to remove unreacted glycine; Vacuum-drying reaction product at 50 DEG C, to remove residual second alcohol and water, obtains pure choline-glycine (Ch-Gly) ionic liquid.
(2) preparation of vinyl ionic liquid monomer
Take vinylformic acid (AAc), be dissolved in 10ml distilled water, add N-hydroxy-succinamide (NHS) and 1-ethyl-3-(3-dimethylamine propyl) carbodiimide (EDC), after room temperature lower magnetic force stirs 2h, add choline-glycine (Ch-Gly) ionic liquid and continue reaction 24h, AAc: Ch-Gly: EDC: NHS=5mol: 5mol: 5mol: 1mol; Pour excess ethyl alcohol after reaction terminates into leave standstill, precipitation to be precipitated is complete, and centrifugation, obtains vinyl choline-glycine ionic liquid monomer (Ch-Gly-AAc).
(3) preparation of temperature sensitive type poly ionic liquid gel
Take vinyl choline-glycine ionic liquid monomer (Ch-Gly-AAc) and N-isopropylacrylamide (NIPAAm) monomer, be dissolved in 10ml distilled water, two monomer total masses are 1g, wherein two monomer weight ratio are Gly-AAc: NIPAAm=2: 1,0.2g linking agent N is added under nitrogen protection, N-methylene-bisacrylamide (MBAA), stirs 20min, then reacts 15min under adding 0.02g initiator potassium persulfate (KPS) room temperature and obtain coagulant liquid; Pour coagulant liquid into glass mold, dropping 1ml2%N, N, N ', N '-Tetramethyl Ethylene Diamine (TEMED), room temperature reaction 24h, forms gel.
Embodiment 5.
(1) preparation of ionic liquid
Take glycine (Gly) and choline (Ch) respectively, be respectively dissolved in 5ml distilled water, Gly: Ch=1mol: 1mol, at 25 DEG C, with constant pressure funnel, choline solution added glycine solution lentamente, magnetic agitation reaction 48h; Reaction terminates rear 60 DEG C of backspins steaming and dewaters, and then pours excess ethyl alcohol into above-mentioned reaction system, to remove unreacted glycine; Vacuum-drying reaction product at 50 DEG C, to remove residual second alcohol and water, obtains pure choline-glycine (Ch-Gly) ionic liquid.
(2) preparation of vinyl ionic liquid monomer
Take vinylformic acid (AAc), be dissolved in 10ml distilled water, add N-hydroxy-succinamide (NHS) and 1-ethyl-3-(3-dimethylamine propyl) carbodiimide (EDC), after room temperature lower magnetic force stirs 2h, add choline-glycine (Ch-Gly) ionic liquid and continue reaction 24h, AAc: Ch-Gly: EDC: NHS=5mol: 5mol: 5mol: 1mol; Pour excess ethyl alcohol after reaction terminates into leave standstill, precipitation to be precipitated is complete, and centrifugation, obtains vinyl choline-glycine ionic liquid monomer (Ch-Gly-AAc).
(3) preparation of temperature sensitive type poly ionic liquid gel
Take vinyl choline-glycine ionic liquid monomer (Ch-Gly-AAc) and N-isopropylacrylamide (NIPAAm) monomer, be dissolved in 10ml distilled water, two monomer total masses are 1g, wherein two monomer weight ratio are Gly-AAc: NIPAAm=4: 1,0.2g linking agent N is added under nitrogen protection, N-methylene-bisacrylamide (MBAA), stirs 20min, then reacts 15min under adding 0.02g initiator potassium persulfate (KPS) room temperature and obtain coagulant liquid; Pour coagulant liquid into glass mold, dropping 1ml2%N, N, N ', N '-Tetramethyl Ethylene Diamine (TEMED), room temperature reaction 24h, forms gel.
Embodiment 6.
(1) preparation of ionic liquid
Take glycine (Gly) and choline (Ch) respectively, be respectively dissolved in 5ml distilled water, Gly: Ch=2mol: 1mol, at 25 DEG C, with constant pressure funnel, choline solution added glycine solution lentamente, magnetic agitation reaction 48h; Reaction terminates rear 60 DEG C of backspins steaming and dewaters, and then pours excess ethyl alcohol into above-mentioned reaction system, to remove unreacted glycine; Vacuum-drying reaction product at 50 DEG C, to remove residual second alcohol and water, obtains pure choline-glycine (Ch-Gly) ionic liquid.
(2) preparation of vinyl ionic liquid monomer
Take vinylformic acid (AAc), be dissolved in 10ml distilled water, add N-hydroxy-succinamide (NHS) and 1-ethyl-3-(3-dimethylamine propyl) carbodiimide (EDC), after room temperature lower magnetic force stirs 2h, add choline-glycine (Ch-Gly) ionic liquid and continue reaction 24h, AAc: Ch-Gly: EDC: NHS=5mol: 5mol: 5mol: 1mol; Pour excess ethyl alcohol after reaction terminates into leave standstill, precipitation to be precipitated is complete, and centrifugation, obtains vinyl choline-glycine ionic liquid monomer (Ch-Gly-AAc).
(3) preparation of temperature sensitive type poly ionic liquid gel
Take vinyl choline-glycine ionic liquid monomer (Ch-Gly-AAc) and N-isopropylacrylamide (NIPAAm) monomer, be dissolved in 10ml distilled water, two monomer total masses are 1g, wherein two monomer weight ratio are Gly-AAc: NIPAAm=2: 1,0.2g linking agent N is added under nitrogen protection, N-methylene-bisacrylamide (MBAA), stirs 20min, then reacts 15min under adding 0.02g initiator potassium persulfate (KPS) room temperature and obtain coagulant liquid; Pour coagulant liquid into glass mold, dropping 1ml2%N, N, N ', N '-Tetramethyl Ethylene Diamine (TEMED), room temperature reaction 24h, forms gel.

Claims (9)

1. a temperature sensitive type poly ionic liquid gel, is characterized in that described gel has temperature-responsive, realizes cell not damaged desorption by the temperature that controls environment, and described gel can be obtained by following method:
(1) preparation of ionic liquid
Take glycine (Gly) and choline (Ch) respectively, be dissolved in 10ml distilled water, Gly: Ch=2mol: 1mol ~ 1mol: 1mol, at 3 DEG C ~ 25 DEG C lower magnetic force stirring reaction 48h, reaction terminates rear 60 DEG C of backspins steaming and dewaters, and then pours excess ethyl alcohol into above-mentioned reaction system, to remove unreacted glycine, vacuum-drying reaction product at 50 DEG C, to remove residual second alcohol and water, obtains pure choline-glycine (Ch-Gly) ionic liquid;
(2) preparation of vinyl ionic liquid monomer
Take vinylformic acid (AAc), be dissolved in 10ml distilled water, add N-hydroxy-succinamide (NHS) and 1-ethyl-3-(3-dimethylamine propyl) carbodiimide (EDC), after room temperature lower magnetic force stirs 2h, add choline-glycine (Ch-Gly) ionic liquid and continue reaction 24h, AAc: Ch-Gly: EDC: NHS=5mol: 5mol: 5mol: 1mol, pour excess ethyl alcohol after reaction terminates into leave standstill, precipitation to be precipitated is complete, centrifugation, obtains vinyl choline-glycine ionic liquid monomer (Ch-Gly-AAc);
(3) preparation of temperature sensitive type poly ionic liquid gel
Take vinyl choline-glycine ionic liquid monomer (Ch-Gly-AAc) and N-isopropylacrylamide (NIPAAm) monomer, be dissolved in 10ml distilled water, two monomer total masses are 1g, wherein two monomer weight ratio are Gly-AAc: NIPAAm=0: 1, 1: 4, 1: 2, 1: 1, 2: 1, 4: 1, 1: 0, 0.1g ~ 0.5g linking agent N is added under nitrogen protection, N-methylene-bisacrylamide (MBAA), stir 20min, react 15min under adding 0.01g ~ 0.05g initiator potassium persulfate (KPS) room temperature again and obtain coagulant liquid, pour coagulant liquid into glass mold, drip 1ml2%N, N, N ', N '-Tetramethyl Ethylene Diamine (TEMED), room temperature reaction 24h, form gel.
2. gel according to claim 1, is characterized in that having temperature-responsive, realizes cell not damaged desorption by the temperature that controls environment.
3. the preparation method of temperature sensitive type poly ionic liquid gel, comprises the following steps:
(1) preparation of ionic liquid
Take glycine (Gly) and choline (Ch) respectively, be dissolved in 10ml distilled water, Gly: Ch=2mol: 1mol ~ 1mol: 1mol, at 3 DEG C ~ 25 DEG C lower magnetic force stirring reaction 48h, reaction terminates rear 60 DEG C of backspins steaming and dewaters, and then pours excess ethyl alcohol into above-mentioned reaction system, to remove unreacted glycine, vacuum-drying reaction product at 50 DEG C, to remove residual second alcohol and water, obtains pure choline-glycine (Ch-Gly) ionic liquid;
(2) preparation of vinyl ionic liquid monomer
Take vinylformic acid (AAc), be dissolved in 10ml distilled water, add N-hydroxy-succinamide (NHS) and 1-ethyl-3-(3-dimethylamine propyl) carbodiimide (EDC), after room temperature lower magnetic force stirs 2h, add choline-glycine (Ch-Gly) ionic liquid and continue reaction 24h, AAc: Ch-Gly: EDC: NHS=5mol: 5mol: 5mol: 1mol, pour excess ethyl alcohol after reaction terminates into leave standstill, precipitation to be precipitated is complete, centrifugation, obtains vinyl choline-glycine ionic liquid monomer (Ch-Gly-AAc);
(3) preparation of temperature sensitive type poly ionic liquid gel
Take vinyl choline-glycine ionic liquid monomer (Ch-Gly-AAc) and N-isopropylacrylamide (NIPAAm) monomer, be dissolved in 10ml distilled water, two monomer total masses are 1g, wherein two monomer weight ratio are Gly-AAc: NIPAAm=0: 1, 1: 4, 1: 2, 1: 1, 2: 1, 4: 1, 1: 0, 0.1g ~ 0.5g linking agent N is added under nitrogen protection, N-methylene-bisacrylamide (MBAA), stir 20min, react 15min under adding 0.01g ~ 0.05g initiator potassium persulfate (KPS) room temperature again and obtain coagulant liquid, pour coagulant liquid into glass mold, drip 1ml2%N, N, N ', N '-Tetramethyl Ethylene Diamine (TEMED), room temperature reaction 24h, form gel.
4., according to claim 1, a kind of temperature sensitive type poly ionic liquid gel preparation method described in 3, is characterized in that described step (1) middle Gly: Ch=2mol: 1mol ~ 1mol: 1mol.
5., according to claim 1, a kind of temperature sensitive type poly ionic liquid gel preparation method described in 3, is characterized in that in described step (1), temperature of reaction is 3 DEG C ~ 25 DEG C.
6., according to claim 1, a kind of temperature sensitive type poly ionic liquid gel preparation method described in 3, is characterized in that described step (2) middle AAc: Ch-Gly: EDC: NHS=5mol: 5mol: 5mol: 1mol.
7., according to claim 1, a kind of temperature sensitive type poly ionic liquid gel preparation method described in 3, is characterized in that in described step (3), two monomer weight ratio are Gly-AAc: NIPAAm=0: 1,1: 4,1: 2,1: 1,2: 1,4: 1,1: 0.
8., according to claim 1, a kind of temperature sensitive type poly ionic liquid gel preparation method described in 3, is characterized in that in described step (3), linking agent N,N methylene bis acrylamide (MBAA) add-on is 0.1g ~ 0.5g.
9., according to claim 1, a kind of temperature sensitive type poly ionic liquid gel preparation method described in 3, is characterized in that in described step (3), initiator potassium persulfate (KPS) add-on is 0.01g ~ 0.05g.
CN201510859268.5A 2015-11-26 2015-11-26 Temperature sensitive type polyion liquid gel and preparation method thereof Pending CN105295077A (en)

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CN110128589B (en) * 2019-05-31 2021-12-03 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of amino acid modified microspheres and product thereof
CN113956773A (en) * 2021-11-29 2022-01-21 厦门双瑞船舶涂料有限公司 Anti-icing coating for wind power blade and preparation method thereof
CN113956773B (en) * 2021-11-29 2022-06-14 厦门双瑞船舶涂料有限公司 Anti-icing coating for wind power blade and preparation method thereof

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Application publication date: 20160203