CN100480291C - Method for preparing temperature sensitive hydrogel with supramolecular structure - Google Patents
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- CN100480291C CN100480291C CNB2007101189434A CN200710118943A CN100480291C CN 100480291 C CN100480291 C CN 100480291C CN B2007101189434 A CNB2007101189434 A CN B2007101189434A CN 200710118943 A CN200710118943 A CN 200710118943A CN 100480291 C CN100480291 C CN 100480291C
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Abstract
This invention discloses a method for preparing temperature-sensitive hydrogel with supermolecular structure. The present methods have such problems as residual corsslinking agent and pore-forming agent, low biocompatibility and low response speed. The method comprises: dissolving cyclodextrin in deionized water, adding glycidyl methacrylate, and stirring, adding N-isopropyl acrylamide, stirring in N2 atmosphere, adding initiator, sealing the container, heating in a water bath, reacting to prepare hydrogel, and soaking in deionized water after the reaction to obtain temperature-sensitive hydrogel with supermolecular structure. The method has such advantages as no need for corsslinking agent, easy operation, and no need for specific apparatus. The obtained hydrogel has supermolecular structure, and has such advantages as high temperature sensitivity and high biocompatibility.
Description
Technical field
The invention belongs to functional high polymer material field, relate to a kind of preparation method of temperature sensitive hydrogel with supramolecular structure.
Background technology
The intelligent macromolecule hydrogel is that a class can stimulate the hydrogel of making a response to external world.Temperature sensitive hydrogel can be made rapid reaction to the subtle change of temperature because of it, and causes extensive studies and application.Especially to gather the macromolecule hydrogel of (N-N-isopropylacrylamide) (hereinafter to be referred as NIPA).Because PNIPA hydrogel environment subtle change is to external world made the quick response characteristics, thereby is with a wide range of applications.Be widely used in controlled drug delivery system, contact camera lens, chemical machinery valve, sensing element etc.
PNIPA macromolecule hydrogel synthetic mainly contains following method: radical polymerization, interpenetrating polymer networks (IPN) and prepare improving one's methods of quick response water gel.
1, radical polymerization.
The PNIPA macromolecule hydrogel is synthesized in radical polymerization, is method relatively more commonly used.Can adopt the different methods initiated polymerization, mainly contain initiator initiation and x radiation x and cause.According to the is olation difference, initiator can be divided into redox decomposition and thermolysis two classes.Redox initiator is by redox reaction initiated polymerization and crosslinked.The most frequently used redox system has Potassium Persulphate (APS) and Tetramethyl Ethylene Diamine (TEMED).Thermal decomposition initiating mainly contains azo and isopropyl cyanide (AIBN).
2, IPN method.
IPN is meant that the component that two different chemicals are formed forms separately independently network respectively, and the mutual mat of two networks constitutes " topological key " formation interpenetrating polymer networks then.This method is mainly used in the preparation dual responsiveness aquagel.IPN has two kinds: a kind of is semiinterpenetrating polymer network (semi IPN), introduces without crosslinked comonomer synthetic water gel when crosslinked NIPA, can obtain semi IPN hydrogel.Another kind is full interpenetrating polymer networks (full IPN).
3, hydrogel is synthetic fast
According to above-mentioned ordinary method synthetic hydrogel, the variation of environment has slower reaction efficiency to external world.Limited applying of hydrogel.The researchist improves synthetic method, improving the environmental response efficient of hydrogel, comprising syntheticly having the gel of pore structure, introduce grafted chain in gel-in-matrix, gel being carried out method such as post-polymerization treatment.
When the synthetic water gel, add pore former, in gel structure, form macropore or many hollow structures, help the turnover of water molecules, improve the speed of response of hydrogel.Pore former commonly used has polyoxyethylene glycol (PEG) and silica gel particle.The weak point of this method is that remaining pore former is difficult for removing.
Discover that NIPA and some monomer form copolymer hydrogel, some performance of hydrogel can obtain different changes.The monomer that forms copolymer hydrogel with NIPA has following a few class:
1, ionic comonomer.Negatively charged ion and cationic monomer are arranged.The adding of anionic monomer can make swelling behavior than increasing.Cationic monomer, for example the phosphorus chloride humulus of rolling into a ball with different substituents is done the cationic water gel of comonomer, its swelling ratio, phase transition temperature and phase transition temperature range all change.
2, ampholytic monomer.Synthetic NIPA/SPV (1-(3-sulfo-propane)-2-vinylpyridine-trimethyl-glycine) copolymer hydrogel such as Wei for example, because SPV has zwitter-ion electrical in the negative and positive two simultaneously, be referred to as the amphoteric ion type hydrogel, result of study shows: SPV content can influence the transformation temperature of hydrogel.
3, nonionic monomers.For example different hydrophobic long-chain methyl acrylates, ethyl propenoate, butyl acrylate, dodecyl acrylate.Studies show that hydrogel weakens the susceptibility of temperature along with the increase of hydrophobic components acrylate content in the hydrogel, phase transition temperature descend gradually and the hydrophobic chain of ester long more, lowering speed is fast more.
The method of above-mentioned several synthetic NIPA hydrogels and separately defective can all be arranged with the monomer of NIPA copolymerization, for example linking agent and pore former are residual, and biocompatibility is bad, and the speed of response is low etc.This makes it be very restricted in actual applications, promotes difficulty.
Summary of the invention
At the deficiencies in the prior art part, the object of the present invention is to provide a kind of preparation method of temperature sensitive hydrogel with supramolecular structure, this gel has temperature sensitivity preferably, has excellent biological compatibility; This gel process for preparing need not to add linking agent, does not have the linking agent residue problem; This hydrogel preparation method technology is simple, does not need specific installation, industrialization easily.
The invention provides a kind of temperature sensitive hydrogel with supramolecular structure, may further comprise the steps:
1) take by weighing with N-N-isopropylacrylamide mol ratio be the cyclodextrin of 1:4～1:50, the preparation cyclodextrin aqueous solution;
2) adding is the glycidyl methacrylate of 1:2.5～1:30 with N-N-isopropylacrylamide mol ratio, stirs 10～25 minutes;
3) the adding mass concentration is 8%～30% N-N-isopropylacrylamide, under nitrogen atmosphere, continues to stir 10～20 minutes;
4) adding and N-N-isopropylacrylamide mol ratio are 0.1%～5% initiator, keep nitrogen atmosphere, continue to stir 5～15 minutes.
5) sealed vessel places 40～70 ℃ of water-baths, reacts 4～24 hours, and products therefrom is soaked with deionized water wash, promptly obtains required temperature sensitive hydrogel with supramolecular structure.
In order better to realize that the present invention, described cyclodextrin are a kind of in beta-cyclodextrin, hydroxypropyl-beta-cyclodextrin, the methyl-beta-cyclodextrin; Described initiator is a kind of or its mixture in Potassium Persulphate, ammonium persulphate, the Sodium Persulfate.
Can also be in former step 2) the basis on, add with N-N-isopropylacrylamide mol ratio and be: 1:4～1:40 oil-soluble monomer vinylbenzene; Perhaps can add with N-N-isopropylacrylamide mol ratio and be: a kind of in 1:5～1:40 acrylic ester monomer methyl methacrylate, Jia Jibingxisuanyizhi, the butyl methacrylate; Perhaps can add with N-N-isopropylacrylamide mol ratio and be: 1:8～1:50 water-soluble monomer acrylamide, N hydroxymethyl acrylamide.
The present invention is by at room temperature, glycidyl methacrylate stirs in cyclodextrin aqueous solution, form glycidyl methacrylate-cyclodextrin Subjective and Objective compound system, and then react in the N-N-isopropylacrylamide, crosslinked by the epoxide group open loop on the glycidyl methacrylate, make cyclodextrin stay on the macromolecular chain, synthetic temperature sensitive hydrogel with supramolecular structure.The invention has the advantages that because the existence of cyclodextrin, the swelling ratio of hydrogel is improved, temperature sensitivity is greatly improved.The bibliographical information monomer concentration is the swelling ratio about 7 of homopolymerization N-N-isopropylacrylamide hydrogel in the time of 25 ℃ of 15wt%.Among the contrast experiment who is done, when not having cyclodextrin to exist, glycidyl methacrylate and N-N-isopropylacrylamide copolymer hydrogel swelling ratio reach 15, and the swelling behavior that the present invention obtains is than reaching 45 times even higher especially.The prepared hydrogel of the present invention has good temperature sensitivity.In the time of 50 ℃, lose 63% water in the 10min fast, in 20min, lose about 76% water. and as a comparison, glycidyl methacrylate and the corresponding numerical value of N-N-isopropylacrylamide copolymer hydrogel are 8% and 11%.This be because, cyclodextrin have a good wetting ability, the existence of cyclodextrin makes hydrophilic/hydrophobic group on the macromolecular chain than improving greatly, the hydrogen bond number that forms with water increases, so water-intake rate improves.Under the temperature that is higher than LCST (low critical transition temperature), this hydrogen bond is destroyed, and water molecules is discharged rapidly, and swelling ratio reduces rapidly, therefore can make response fast to temperature.Simultaneously, cyclodextrin has very big cavity, has played the effect of pore former in hydrogel.Because cyclodextrin has biocompatibility, so the present invention will have broad application prospects on the biological medicine material.The present invention compared with prior art in preparation process, need not to add linking agent, so technology is simple, and easy handling helps industrialization.
Description of drawings
Fig. 1 hydrogel infrared spectrum
The structural representation of Fig. 2 hydrogel
Fig. 3 hydrogel goes the swelling dynamic curve relatively
Embodiment
Provide specific embodiments of the invention below:
Example 1: the 1.05g hydroxypropyl-beta-cyclodextrin is dissolved in the 10ml deionized water, adds the 0.17g glycidyl methacrylate, stirred 10 minutes under the room temperature.Add 4.29g N-N-isopropylacrylamide, under the nitrogen atmosphere, stirred 20 minutes.Add the 0.01g Potassium Persulphate, keep nitrogen atmosphere, continue to stir 5 minutes.Sealed vessel places 40 ℃ of water-baths, reacts 6 hours.Products therefrom is soaked with deionized water wash, remove small molecules for reaction, promptly obtaining N-N-isopropylacrylamide mass concentration is 30%, hydroxypropyl-beta-cyclodextrin and N-N-isopropylacrylamide mol ratio are 1:50, and glycidyl methacrylate and N-N-isopropylacrylamide mol ratio are the temperature sensitive hydrogel with supramolecular structure of 1:30.In the time of 20 ℃, swelling ratio is 30 times; In the time of 50 ℃, lose 49% water in 10 minutes, lose 61% water in the time of 20 minutes.
Example 2: the 2.18g beta-cyclodextrin is dissolved in the 10ml deionized water, adds the 0.44g glycidyl methacrylate, stirred 25 minutes under the room temperature.Add 0.87g N-N-isopropylacrylamide, under the nitrogen atmosphere, stirred 10 minutes.Add the 0.1g Potassium Persulphate, keep nitrogen atmosphere, continue to stir 10 minutes.Sealed vessel places 70 ℃ of water-baths, reacts 24 hours.Products therefrom is soaked with deionized water wash, remove small molecules for reaction, promptly obtaining N-N-isopropylacrylamide mass concentration is 8%, beta-cyclodextrin and N-N-isopropylacrylamide mol ratio are 1:4, and glycidyl methacrylate and N-N-isopropylacrylamide mol ratio are the temperature sensitive hydrogel with supramolecular structure of 1:2.5.In the time of 20 ℃, swelling ratio is 28.5 times; In the time of 50 ℃, lose 43% water in 10 minutes, lose 59% water in the time of 20 minutes.
Example 3: 1.44g methyl-beta-cyclodextrin is dissolved in the 10ml deionized water, adds the 0.21g glycidyl methacrylate, stirred 15 minutes under the room temperature.Add 2.5g N-N-isopropylacrylamide, under the nitrogen atmosphere, stirred 10 minutes.Add the 0.1g Ammonium Persulfate 98.5, keep nitrogen atmosphere, continue to stir 8 minutes.Sealed vessel places 55 ℃ of water-baths, reacts 10 hours.Products therefrom is soaked with deionized water wash, remove small molecules for reaction, promptly obtaining N-N-isopropylacrylamide mass concentration is 20%, methyl-beta-cyclodextrin and N-N-isopropylacrylamide mol ratio are 1:20, and glycidyl methacrylate and N-N-isopropylacrylamide mol ratio are the temperature sensitive hydrogel with supramolecular structure of 1:15.In the time of 20 ℃, swelling ratio is 39.5 times; In the time of 50 ℃, lose 60% water in 10 minutes, lose 71% water in the time of 20 minutes.
Example 4: the 0.72g hydroxypropyl-beta-cyclodextrin is dissolved in the 10ml deionized water, adds the 0.11g glycidyl methacrylate, stirred 20 minutes under the room temperature.Add 1.76g N-N-isopropylacrylamide, under the nitrogen atmosphere, stirred 15 minutes.Add the 0.055g Sodium Persulfate, keep nitrogen atmosphere, continue to stir 7 minutes.Sealed vessel places 65 ℃ of water-baths, reacts 10 hours.Products therefrom is soaked with deionized water wash, remove small molecules for reaction, promptly obtaining N-N-isopropylacrylamide mass concentration is 15%, hydroxypropyl-beta-cyclodextrin and N-N-isopropylacrylamide mol ratio are 1:30, and glycidyl methacrylate and N-N-isopropylacrylamide mol ratio are the temperature sensitive hydrogel with supramolecular structure of 1:20.In the time of 20 ℃, swelling ratio is 45 times; In the time of 50 ℃, lose 63% water in 10 minutes, lose 76% water in the time of 20 minutes.
Example 5: the 0.72g hydroxypropyl-beta-cyclodextrin is dissolved in the 10ml deionized water, adds the 0.11g glycidyl methacrylate, add 0.41g vinylbenzene, stirred 20 minutes under the room temperature.Add 1.76g N-N-isopropylacrylamide, under the nitrogen atmosphere, stirred 15 minutes.Add 0.06g Sodium Persulfate and Potassium Persulphate mixture, keep nitrogen atmosphere, continue to stir 7 minutes.Sealed vessel places 65 ℃ of water-baths, reacts 10 hours.Products therefrom is soaked with deionized water wash, remove small molecules for reaction, promptly obtaining N-N-isopropylacrylamide mass concentration is 15%, hydroxypropyl-beta-cyclodextrin and N-N-isopropylacrylamide mol ratio are 1:30, glycidyl methacrylate and N-N-isopropylacrylamide mol ratio are 1:20, and vinylbenzene and N-N-isopropylacrylamide mol ratio are the temperature sensitive hydrogel with supramolecular structure of 1:4.In the time of 20 ℃, swelling ratio is 41 times; In the time of 50 ℃, lose 58% water in 10 minutes, lose 70% water in the time of 20 minutes.
Example 6: 1.44g methyl-beta-cyclodextrin is dissolved in the 10ml deionized water, adds the 0.21g glycidyl methacrylate, add 0.057g vinylbenzene, stirred 15 minutes under the room temperature.Add 2.5g N-N-isopropylacrylamide, under the nitrogen atmosphere, stirred 10 minutes.Add the 0.1g Ammonium Persulfate 98.5, keep nitrogen atmosphere, continue to stir 8 minutes.Sealed vessel places 60 ℃ of water-baths, reacts 10 hours.Products therefrom is soaked with deionized water wash, remove small molecules for reaction, promptly obtaining N-N-isopropylacrylamide mass concentration is 20%, methyl-beta-cyclodextrin and N-N-isopropylacrylamide mol ratio are 1:20, glycidyl methacrylate and N-N-isopropylacrylamide mol ratio are 1:15, and vinylbenzene and N-N-isopropylacrylamide mol ratio are the temperature sensitive hydrogel with supramolecular structure of 1:40.In the time of 20 ℃, swelling ratio is 37 times; In the time of 50 ℃, lose 58% water in 10 minutes, lose 71% water in the time of 20 minutes.
Example 7: 1.44g methyl-beta-cyclodextrin is dissolved in the 10ml deionized water, adds the 0.21g glycidyl methacrylate, add the 0.31g acrylamide, stirred 15 minutes under the room temperature.Add 2.5g N-N-isopropylacrylamide, under the nitrogen atmosphere, stirred 10 minutes.Add the 0.1g Sodium Persulfate, keep nitrogen atmosphere, continue to stir 8 minutes.Sealed vessel places 65 ℃ of water-baths, reacts 14 hours.Products therefrom is soaked with deionized water wash, remove small molecules for reaction, promptly obtaining N-N-isopropylacrylamide mass concentration is 20%, methyl-beta-cyclodextrin and N-N-isopropylacrylamide mol ratio are 1:20, glycidyl methacrylate and N-N-isopropylacrylamide mol ratio are 1:15, and acrylamide and N-N-isopropylacrylamide mol ratio are the temperature sensitive hydrogel with supramolecular structure of 1:5.In the time of 20 ℃, swelling ratio is 39 times; In the time of 50 ℃, lose 59% water in 10 minutes, lose 72% water in the time of 20 minutes.
Example 8: the 0.72g hydroxypropyl-beta-cyclodextrin is dissolved in the 10ml deionized water, adds the 0.11g glycidyl methacrylate, add the 0.028g acrylamide, stirred 20 minutes under the room temperature.Add the 1.76gN-N-isopropylacrylamide, under the nitrogen atmosphere, stirred 15 minutes.Add 0.06g Sodium Persulfate and Potassium Persulphate mixture, keep nitrogen atmosphere, continue to stir 7 minutes.Sealed vessel places 65 ℃ of water-baths, reacts 10 hours.Products therefrom is soaked with deionized water wash, remove small molecules for reaction, promptly obtaining N-N-isopropylacrylamide mass concentration is 15%, hydroxypropyl-beta-cyclodextrin and N-N-isopropylacrylamide mol ratio are 1:30, glycidyl methacrylate and N-N-isopropylacrylamide mol ratio are 1:20, and acrylamide and N-N-isopropylacrylamide mol ratio are the temperature sensitive hydrogel with supramolecular structure of 1:40.In the time of 20 ℃, swelling ratio is 40 times; In the time of 50 ℃, lose 61% water in 10 minutes, lose 74% water in the time of 20 minutes.
Example 9: the 0.72g hydroxypropyl-beta-cyclodextrin is dissolved in the 10ml deionized water, adds the 0.11g glycidyl methacrylate, add the 0.079g N hydroxymethyl acrylamide, stirred 20 minutes under the room temperature.Add 1.76g N-N-isopropylacrylamide, under the nitrogen atmosphere, stirred 15 minutes.Add 0.06g Sodium Persulfate and Potassium Persulphate mixture, keep nitrogen atmosphere, continue to stir 7 minutes.Sealed vessel places 65 ℃ of water-baths, reacts 10 hours.Products therefrom is soaked with deionized water wash, remove small molecules for reaction, promptly obtaining N-N-isopropylacrylamide mass concentration is 15%, hydroxypropyl-beta-cyclodextrin and N-N-isopropylacrylamide mol ratio are 1:30, glycidyl methacrylate and N-N-isopropylacrylamide mol ratio are 1:20, and acrylamide and N-N-isopropylacrylamide mol ratio are the temperature sensitive hydrogel with supramolecular structure of 1:20.In the time of 20 ℃, swelling ratio is 40 times; In the time of 50 ℃, lose 63% water in 10 minutes, lose 73% water in the time of 20 minutes.
Example 10: the 0.72g hydroxypropyl-beta-cyclodextrin is dissolved in the 10ml deionized water, adds the 0.11g glycidyl methacrylate, add the 0.28g methyl methacrylate, stirred 20 minutes under the room temperature.Add 1.76g N-N-isopropylacrylamide, under the nitrogen atmosphere, stirred 15 minutes.Add the 0.06g Potassium Persulphate, keep nitrogen atmosphere, continue to stir 7 minutes.Sealed vessel places 65 ℃ of water-baths, reacts 10 hours.Products therefrom is soaked with deionized water wash, remove small molecules for reaction, promptly obtaining N-N-isopropylacrylamide mass concentration is 15%, hydroxypropyl-beta-cyclodextrin and N-N-isopropylacrylamide mol ratio are 1:30, glycidyl methacrylate and N-N-isopropylacrylamide mol ratio are 1:20, and methyl methacrylate and N-N-isopropylacrylamide mol ratio are the temperature sensitive hydrogel with supramolecular structure of 1:5.In the time of 20 ℃, swelling ratio is 41 times; In the time of 50 ℃, lose 62% water in 10 minutes, lose 74% water in the time of 20 minutes.
Example 11: 1.44g methyl-beta-cyclodextrin is dissolved in the 10ml deionized water, adds the 0.21g glycidyl methacrylate, add the 0.058g Jia Jibingxisuanyizhi, stirred 15 minutes under the room temperature.Add 2.5g N-N-isopropylacrylamide, under the nitrogen atmosphere, stirred 10 minutes.Add the 0.1g Sodium Persulfate, keep nitrogen atmosphere, continue to stir 8 minutes.Sealed vessel places 65 ℃ of water-baths, reacts 14 hours.Products therefrom is soaked with deionized water wash, remove small molecules for reaction, promptly obtaining N-N-isopropylacrylamide mass concentration is 20%, methyl-beta-cyclodextrin and N-N-isopropylacrylamide mol ratio are 1:20, glycidyl methacrylate and N-N-isopropylacrylamide mol ratio are 1:15, and Jia Jibingxisuanyizhi and N-N-isopropylacrylamide mol ratio are the temperature sensitive hydrogel with supramolecular structure of 1:40.In the time of 20 ℃, swelling ratio is 39 times; In the time of 50 ℃, lose 58% water in 10 minutes, lose 70% water in the time of 20 minutes.
Example 12: 1.44g methyl-beta-cyclodextrin is dissolved in the 10ml deionized water, adds the 0.21g glycidyl methacrylate, add the 0.15g butyl methacrylate, stirred 15 minutes under the room temperature.Add 2.5g N-N-isopropylacrylamide, under the nitrogen atmosphere, stirred 10 minutes.Add the 0.1g Sodium Persulfate, keep nitrogen atmosphere, continue to stir 8 minutes.Sealed vessel places 65 ℃ of water-baths, reacts 14 hours.Products therefrom is soaked with deionized water wash, remove small molecules for reaction, promptly obtaining N-N-isopropylacrylamide mass concentration is 20%, methyl-beta-cyclodextrin and N-N-isopropylacrylamide mol ratio are 1:20, glycidyl methacrylate and N-N-isopropylacrylamide mol ratio are 1:15, and butyl methacrylate and N-N-isopropylacrylamide mol ratio are the temperature sensitive hydrogel with supramolecular structure of 1:20.In the time of 20 ℃, swelling ratio is 38 times; In the time of 50 ℃, lose 60% water in 10 minutes, lose 72% water in the time of 20 minutes.
Fig. 1 is the infrared spectrum of supramolecular structured hydrogel, and the peak (3670cm of cyclodextrin is arranged from spectrogram as can be seen
-1), prove in good existence of cyclodextrin and the hydrogel.
Fig. 2 is the internal structure mimic diagram of hydrogel.Glycidyl methacrylate stirs in cyclodextrin aqueous solution, cyclodextrin is nested on the glycidyl methacrylate, form glycidyl methacrylate-cyclodextrin Subjective and Objective compound system, and then react in the N-N-isopropylacrylamide, crosslinked by the epoxide group open loop on the glycidyl methacrylate, make cyclodextrin stay on the macromolecular chain, synthetic temperature sensitive hydrogel with supramolecular structure.
The hydrogel that Fig. 3 obtains for example 4 goes the swelling kinetic curve relatively with glycidyl methacrylate that does not contain cyclodextrin and N-N-isopropylacrylamide copolymer hydrogel.A is glycidyl methacrylate and N-N-isopropylacrylamide copolymer hydrogel, and b is the hydrogel of example 4, and swelling ratio reaches 45 times.In the time of 50 ℃, lose 63% water in the 10min fast, in 20min, lose about 76% water. and as a comparison, glycidyl methacrylate and the corresponding numerical value of N-N-isopropylacrylamide copolymer hydrogel are 8% and 11%.
Claims (6)
1, a kind of preparation method of temperature sensitive hydrogel with supramolecular structure is characterized in that, comprises the steps:
1) take by weighing with N-N-isopropylacrylamide mol ratio be the cyclodextrin of 1:4～1:50, the preparation cyclodextrin aqueous solution;
2) adding is the glycidyl methacrylate of 1:2.5～1:30 with N-N-isopropylacrylamide mol ratio, stirs 10～25 minutes;
3) the adding mass concentration is 8%～30% N-N-isopropylacrylamide, under nitrogen atmosphere, continues to stir 10～20 minutes;
4) adding and N-N-isopropylacrylamide mol ratio are 0.1%～5% initiator, keep nitrogen atmosphere, continue to stir 5～15 minutes;
5) sealed vessel places 40～70 ℃ of water-baths, reacts 4～24 hours, and products therefrom is soaked with deionized water wash, promptly obtains required temperature sensitive hydrogel with supramolecular structure.
2, the preparation method of temperature sensitive hydrogel with supramolecular structure according to claim 1 is characterized in that: described cyclodextrin is one of beta-cyclodextrin, hydroxypropyl-beta-cyclodextrin, methyl-beta-cyclodextrin.
3, the preparation method of temperature sensitive hydrogel with supramolecular structure according to claim 1 is characterized in that: described initiator is a kind of or its mixture in Potassium Persulphate, ammonium persulphate, the Sodium Persulfate.
4, the preparation method of temperature sensitive hydrogel with supramolecular structure according to claim 1 is characterized in that: in step 2) in add with N-N-isopropylacrylamide mol ratio be the oil-soluble monomer vinylbenzene of 1:4～1:40.
5, the preparation method of temperature sensitive hydrogel with supramolecular structure according to claim 1, it is characterized in that: in step 2) in add with N-N-isopropylacrylamide mol ratio be the acrylic ester monomer of 1:5～1:40, described acrylic ester monomer is a kind of in methyl acrylate, Jia Jibingxisuanyizhi, the butyl methacrylate.
6, the preparation method of temperature sensitive hydrogel with supramolecular structure according to claim 1, it is characterized in that: in step 2) in add with N-N-isopropylacrylamide mol ratio be the water-soluble monomer of 1:8～1:50, described water-soluble monomer is acrylamide or N hydroxymethyl acrylamide.
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| β-环糊精大分子单体/N-异丙基丙烯酰胺共聚水凝胶. 刘郁杨，范晓东.高分子材料科学与工程，第20卷第2期. 2004 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103755967A (en) * | 2013-12-31 | 2014-04-30 | 中科院广州化学有限公司 | Thermo-sensitive chiral separation additive and thermo-sensitive polysulfone chiral separation membrane |
| CN103755967B (en) * | 2013-12-31 | 2016-01-20 | 中科院广州化学有限公司 | A kind of Thermo-sensitive chiral separation additive and Thermo-sensitive polysulfones chiral separation film |
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