CN1730515A - A hydrogel preparation method - Google Patents
A hydrogel preparation method Download PDFInfo
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- CN1730515A CN1730515A CN 200510092974 CN200510092974A CN1730515A CN 1730515 A CN1730515 A CN 1730515A CN 200510092974 CN200510092974 CN 200510092974 CN 200510092974 A CN200510092974 A CN 200510092974A CN 1730515 A CN1730515 A CN 1730515A
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- microwave
- hydrogel
- structural formula
- linking agent
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Abstract
The invention provides a process for preparing aqueous gel comprising the following steps, mixing and dissolving alkene group monomer, cross linking agent and initiating agent by the ratio of 100:2-50:0.2-1:1-10, using microwave having a frequency of 2450MHz or frequency changed microwave of 300MHz-300GHz for radiation to the reaction system.
Description
Technical field
The invention belongs to chemical material technical field, particularly prepare the method for hydrogel
Background of invention
Hydrogel can swelling in water, can not dissolve, and is extremely similar to tissue.Hydrogel has broad application prospects in fields such as biology, medical science and pharmaceutical preparations.
When the preparation hydrogel, for example preparation gathers (N-N-isopropylacrylamide) and poly-(N-caprolactam), document J.Polym.Sci., PartA:Polym.Chem., 1992,30 (10), 2121-2129 and Macromol.Chem.Phys., 1996,197,1973-1982 adopts conventional oil bath heating.Conventional heating, for example oil bath, airbath and sand bath heating or the like belong to traditional conduction-type heating.This heating is complicated operation not only, and required heat-up time is long, and heats inhomogeneously, and temperature reduces from outside to inside, has thermograde.More unfortunately conventional heating efficiency is low, and a large amount of heat energy are wasted.Yet microwave heating belongs to " body heating ", is a kind of internal heating, homogeneous heating not only, and also energy-efficient.
Summary of the invention
The objective of the invention is for overcoming the weak point of prior art, propose a kind of new method for preparing hydrogel, adopt the microwave heating reaction system, not only rate of heating is fast, and homogeneous heating, the efficient height, the valuable energy can be saved, the swelling behavior of hydrogel can also be improved.
The present invention proposes a kind of method for preparing hydrogel, it is characterized in that:
1) make reaction system in the solvent with being dissolved in after vinyl monomer, linking agent and the initiator mixing, the weight ratio of each composition is in this reaction system: monomer: linking agent: initiator: solvent=100: 2-50: 0.2-1: 1-10.
2) utilize frequency reaction system to be carried out obtaining after the irradiated heat for microwave or the 300MHz-300GHz variable frequency microwave of 2450MHz.
Characteristics of the present invention and effect
The heating of the present invention's tradition conduction-type changes microwave heating into, not only can accelerate to prepare the speed of hydrogel, and homogeneous heating, and the efficient height can be saved the valuable energy, belongs to the category of Green Chemistry.The more important thing is that microwave heating can improve some performance of hydrogel, for example the hydrogel that makes of microwave heating often has higher swelling ratio and swelling rate faster.These performances, for example degree of swelling, swelling rate as key index, have determined the purposes of hydrogel.
Embodiment
The method for preparing hydrogel of the present invention is described in detail as follows in conjunction with the embodiments:
Method of the present invention may further comprise the steps:
1) make reaction system in the solvent with being dissolved in after vinyl monomer, linking agent and the initiator mixing, the weight ratio of each composition is in this reaction system: monomer: linking agent: initiator: solvent=100: 2-50: 0.2-1: 1-10;
2) utilize frequency reaction system to be carried out obtaining after the irradiated heat for microwave or the 300MHz-300GHz variable frequency microwave of 2450MHz.
The power of described microwave or variable frequency microwave can be 75 watts to 10,000 watts, irradiated heat 1-30 minute.
Described vinyl monomer structural formula can be a or b:
R1=H wherein, CH
3R2=OR4, NR4R5; The structural formula of R3 is e, f or g:
Wherein
R4，R5＝H，CH
3，CH
2CH
3，CH
2CH
2OH，CH
2CH
2CH
3，CH
2CH
2CH
2OH，CH(CH
3)
2，CH
2CH
2CH
2CH
3，CH
2CH(CH
3)
2，C(CH
3)
3。
Described linking agent structural formula can be c and d:
For structural formula c, n=1-6; For structural formula d, n=1-30.
Described solvent can be has the water that polarity can effectively absorb microwave, methyl alcohol, and ethanol, acetone, tetrahydrofuran (THF), acetonitrile, Virahol, dioxane, DMSO, DMF, ethylene glycol, glycerol, polyoxyethylene glycol 350-2000, and their mixed solvent is a kind of.
Embodiment 1
The 10g acrylamide, 0.5g N, N '-methylene diacrylamine and 10mg Diisopropyl azodicarboxylate are dissolved in 40ml water, blast high pure nitrogen, vacuumize, and repeat to outgas tube sealing under the vacuum three times.Then tube sealing is put into frequency and be the microwave oven of 2450MHz and select 340 watts of output rating irradiation 2 minutes.The hydrogel washing that obtains, oven dry.Yield 90%.
Embodiment 2
The 10g acrylamide, 2g vinylformic acid, 0.5g N, N '-methylene diacrylamine mixes with the 10mg Diisopropyl azodicarboxylate, is dissolved in 50ml water, with the high purity nitrogen degassing three times, tube sealing under the vacuum, then tube sealing is put into microwave oven with frequency the 75W of 300MHz-300GHz scope microwave exposure 20 minutes.Washing, oven dry.Yield 88%.
Embodiment 3
100g N-vinyl pyrrolidone, 5g N, the mixture of N '-methylene diacrylamine and 0.1g Diisopropyl azodicarboxylate is dissolved in 400ml ethanol/water (1: 1v/v), feed argon gas, outgas three times, tube sealing under the vacuum, the microwave oven of then tube sealing being put into frequency and be 2450NHz irradiation 10 minutes under 800W power microwave.The hydrogel water thorough washing that obtains, oven dry.Yield 89%.
Embodiment 4
5g N-N-isopropylacrylamide, 1g hydroxyethyl methyl acrylate, 0.25g N, N '-methylene diacrylamine and 10mg Diisopropyl azodicarboxylate are dissolved in 20ml ethanol/water (1: 1v/v), use argon-degassed, tube sealing, in frequency is irradiation 3 minutes under the 2450MHz170W microwave, washing, and 40 ℃ of vacuum-dryings are to constant weight.Yield 96%.
Embodiment 5
5g N-caprolactam, 0.25g N, N '-methylene diacrylamine and 10mg Diisopropyl azodicarboxylate are dissolved in 20ml ethanol/water (1: 1v/v), feed high purity nitrogen bubbling 3min, vacuumize 5min, repeat to outgas three times, tube sealing under the vacuum, changing frequency then over to is 2450MHz microwave oven 1000W microwave exposure 1min.The water thorough washing, vacuum is dried to constant weight for 40 ℃.Yield 60%.
Embodiment 6
10g N-N-isopropylacrylamide, the 2g acrylamide, 0.5g O, O '-glycol diacrylate and 20mg Diisopropyl azodicarboxylate and the abundant mixing of 50ml ethylene glycol place microwave oven, select the 340W output rating, irradiation 5min.Washing, vacuum-drying.Yield 92%.
Embodiment 7
10g N-caprolactam, 2g N-vinyl pyrrolidone, 0.5g O, O '-glycol diacrylate and 20mg Diisopropyl azodicarboxylate and the abundant mixing of 50ml glycerol, with the high purity nitrogen degassing at least three times, tube sealing, place the variable frequency microwave stove 340W irradiation 10min of frequency in the 300MHz-300GHz scope, the hydrogel water thorough washing that obtains, vacuum drying.Yield 63%.
Embodiment 8
100g N-N-isopropylacrylamide, 5g N, N '-methylene diacrylamine and 0.1g Diisopropyl azodicarboxylate and 200ml polyoxyethylene glycol-400 be mixing fully, with the high purity nitrogen degassing at least three times, tube sealing, place the variable frequency microwave stove of frequency in the 300MHz-300GHz scope, select output rating 5000W, continuous irradiation 2 minutes, washing, oven dry.Yield 95%.
Claims (8)
1. method for preparing hydrogel is characterized in that:
1) make reaction system in the solvent with being dissolved in after vinyl monomer, linking agent and the initiator mixing, the weight ratio of each composition is in this reaction system: monomer: linking agent: initiator: solvent=100: 2-50: 0.2-1: 1-10;
2) utilize frequency reaction system to be carried out obtaining after the irradiated heat for microwave or the 300MHz-300GHz variable frequency microwave of 2450MHz.
2. as claims 1 described method for preparing hydrogel, it is characterized in that the power of described microwave or variable frequency microwave is 75 watts to 10,000 watts, irradiated heat 1-30 minute.
3. as claims 1 described method for preparing hydrogel, it is characterized in that described vinyl monomer structural formula is a or b:
R1=H wherein, CH
3R2=OR4, NR4R5; The structural formula of R3 is e, f or g:
Wherein
R4，R5＝H，CH
3，CH
2CH
3，CH
2CH
2OH，CH
2CH
2CH
3，CH
2CH
2CH
2OH，CH(CH
3)
2，CH
2CH
2CH
2CH
3，CH
2CH(CH
3)
2，C(CH
3)
3。
4. as claims 1 described method for preparing hydrogel, it is characterized in that described linking agent structural formula is c and d:
For structural formula c, n=1-6; For structural formula d, n=1-30.
5. as claims 1 described method for preparing hydrogel, it is characterized in that described solvent is to have the water that polarity can effectively absorb microwave, methyl alcohol, ethanol, acetone, tetrahydrofuran (THF), acetonitrile, Virahol, dioxane, DMSO, DMF, ethylene glycol, glycerol, polyoxyethylene glycol 350-2000, and their mixed solvent is a kind of.
6. as claims 1 described method for preparing hydrogel, it is characterized in that described initiator adopts Diisopropyl azodicarboxylate.
7. as claims 3 described methods that prepare hydrogel, it is characterized in that described monomer is a vinylformic acid, methyl acrylate, ethyl propenoate, methyl methacrylate, Hydroxyethyl acrylate, Jia Jibingxisuanyizhi, hydroxyethyl methylacrylate, acrylamide, N,N-DMAA, the N-ethyl acrylamide, N-propyl group acrylamide, N-N-isopropylacrylamide, the N-vinyl pyrrolidone, any of N-caprolactam and composition thereof.
8. as claims 5 described methods that prepare hydrogel, it is characterized in that, described linking agent is N, N '-methylene diacrylamine, N, N '-ethylene group diacrylamine, O, O '-glycol diacrylate, among the different molecular weight polyethylene glycol diacrylate of 300-1000 any.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100929748A CN100390220C (en) | 2005-08-26 | 2005-08-26 | A hydrogel preparation method |
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|---|---|---|---|
| CNB2005100929748A CN100390220C (en) | 2005-08-26 | 2005-08-26 | A hydrogel preparation method |
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| CN1730515A true CN1730515A (en) | 2006-02-08 |
| CN100390220C CN100390220C (en) | 2008-05-28 |
Family
ID=35962939
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|---|---|---|---|
| CNB2005100929748A Active CN100390220C (en) | 2005-08-26 | 2005-08-26 | A hydrogel preparation method |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102617787A (en) * | 2012-03-21 | 2012-08-01 | 东南大学 | Hydrogel contact lens material and preparation method thereof |
| CN103282458A (en) * | 2011-01-06 | 2013-09-04 | 积水化成品工业株式会社 | Composition for adhesive hydrogel and use thereof |
| CN105169465A (en) * | 2015-07-13 | 2015-12-23 | 广州新诚生物科技有限公司 | Medical anti-adhesion hydrogel dressing and preparation method thereof |
| CN106421934A (en) * | 2016-09-29 | 2017-02-22 | 成都德信安创新医疗技术有限公司 | Preparation method of Hydrophile ultra-slippery coating for medical apparatus |
| CN108467464A (en) * | 2018-04-02 | 2018-08-31 | 常熟理工学院 | Hydrogel of visible-light curing containing azelaic acid and preparation method thereof |
| WO2019085362A1 (en) * | 2017-10-30 | 2019-05-09 | 广州新诚生物科技有限公司 | Self-expansion-fixing artificial nasolacrimal duct |
| WO2019085363A1 (en) * | 2017-10-30 | 2019-05-09 | 广州新诚生物科技有限公司 | Hydrogel and application thereof |
| CN110256718A (en) * | 2019-07-22 | 2019-09-20 | 四川大学 | A method of foamed material is prepared using hydrogel microwave foaming |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56129208A (en) * | 1980-03-17 | 1981-10-09 | Mitsubishi Chem Ind Ltd | Drying of water-soluble acrylamide type polymer hydrogel |
| CN1065771C (en) * | 1998-11-17 | 2001-05-16 | 苏州医学院 | Method for radio-grafting medical high molecular aquagel membrane |
-
2005
- 2005-08-26 CN CNB2005100929748A patent/CN100390220C/en active Active
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103282458A (en) * | 2011-01-06 | 2013-09-04 | 积水化成品工业株式会社 | Composition for adhesive hydrogel and use thereof |
| CN103282458B (en) * | 2011-01-06 | 2015-05-13 | 积水化成品工业株式会社 | Composition for adhesive hydrogel and use thereof |
| CN102617787A (en) * | 2012-03-21 | 2012-08-01 | 东南大学 | Hydrogel contact lens material and preparation method thereof |
| CN102617787B (en) * | 2012-03-21 | 2014-07-09 | 东南大学 | Hydrogel contact lens material and preparation method thereof |
| CN105169465A (en) * | 2015-07-13 | 2015-12-23 | 广州新诚生物科技有限公司 | Medical anti-adhesion hydrogel dressing and preparation method thereof |
| CN106421934A (en) * | 2016-09-29 | 2017-02-22 | 成都德信安创新医疗技术有限公司 | Preparation method of Hydrophile ultra-slippery coating for medical apparatus |
| WO2019085362A1 (en) * | 2017-10-30 | 2019-05-09 | 广州新诚生物科技有限公司 | Self-expansion-fixing artificial nasolacrimal duct |
| WO2019085363A1 (en) * | 2017-10-30 | 2019-05-09 | 广州新诚生物科技有限公司 | Hydrogel and application thereof |
| CN108467464A (en) * | 2018-04-02 | 2018-08-31 | 常熟理工学院 | Hydrogel of visible-light curing containing azelaic acid and preparation method thereof |
| CN110256718A (en) * | 2019-07-22 | 2019-09-20 | 四川大学 | A method of foamed material is prepared using hydrogel microwave foaming |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100390220C (en) | 2008-05-28 |
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Address after: 221007 Xuzhou Economic Development Zone, Jiangsu, Yang Road, No. 18 Patentee after: Jiangsu Nhwa Pharmaceutical Co., Ltd. Address before: 221007 Zhongshan North Road, Jiangsu, No. 289, Patentee before: Jiangsu Nhwa Pharmaceutical Co., Ltd. |