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Preparation method of double-hydrophilic temperature response polymer

A temperature-responsive polymer technology, which is applied in the direction of medical preparations of non-active ingredients, pharmaceutical formulas, genetic material components, etc., can solve problems such as high experimental conditions, complex preparation process of stimuli-responsive polymers, and difficulties in industrialization. Achieve the effect of abundant sources, low price, and simple synthetic route

Inactive Publication Date: 2012-09-12
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In view of the above reasons, the research on double-hydrophilic temperature-responsive polymers is of great significance. The current research literature and patents, stimuli-responsive polymers have shortcomings such as complicated preparation process, high experimental conditions, and difficulties in industrialization.

Method used

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  • Preparation method of double-hydrophilic temperature response polymer
  • Preparation method of double-hydrophilic temperature response polymer
  • Preparation method of double-hydrophilic temperature response polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) Synthesis of divinyl adipate:

[0036] Mix 28g of adipic acid with 150mL of vinyl acetate, add 0.4g of copper sulfate catalyst, and react at 70°C to obtain 30g of divinyl adipate, with a yield of 78%;

[0037] (2) Enzymatic synthesis of polymerizable glucose divinyl adipate:

[0038] Add 13.14g of divinyl adipate (0.066mol), 3.96g of glucose, 1.0g of subtilisin and 100mL of anhydrous pyridine into a 250mL Erlenmeyer flask, and put it in a constant temperature shaking incubator at 50°C for 4 days at a speed of 210rpm . The reaction process was qualitatively monitored by thin-layer chromatography (TLC), and the developing solvent was ethyl acetate / methanol / water (17:3:1 by volume), and I 2 color. After the reaction was finished, the subtilisin was removed by filtration and most of the pyridine was removed by distillation under reduced pressure, and the crude product was purified by column chromatography, the eluent was pure ethyl acetate, and the developer was ethy...

Embodiment 2

[0040] Add 3.96g of N-isopropylacrylamide, 2.34g of glucose divinyl adipate and 0.126g of AIBN into a flask equipped with a magnetic stirring rotor and an adapter, completely dissolve in 5mL of DMF, seal it, and repeatedly evacuate it. After several times of nitrogen gas, the reaction system was placed at 60°C and stirred for 24 hours under the protection of nitrogen gas, and then the viscous colorless and transparent polymer solution obtained from the reaction was precipitated in a large amount of ether, and the ether was poured out, and the white solid precipitate was again Dissolve in a small amount of ethanol, repeatedly precipitate and dissolve until all unreacted monomers are washed out, and dry in a vacuum oven at 37°C for 24 hours to obtain a white solid powder.

Embodiment 3

[0042] Add 7.92g of N-isopropylacrylamide, 2.34g of glucose divinyl adipate and 0.206g of AIBN into a flask equipped with a magnetic stirring rotor and an adapter, dissolve it completely in 10mL of DMF, seal it, and repeatedly evacuate it. After several times of nitrogen gas, the reaction system was placed at 60°C and stirred for 24 hours under the protection of nitrogen gas, and then the viscous colorless and transparent polymer solution obtained from the reaction was precipitated in a large amount of ether, and the ether was poured out, and the white solid precipitate was again Dissolve in a small amount of ethanol, repeatedly precipitate and dissolve until all unreacted monomers are washed out, and dry in a vacuum oven at 37°C for 24 hours to obtain a white solid powder.

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Abstract

The invention relates to a preparation method of a double-hydrophilic temperature response polymer. The method comprises the following steps of: (1) preparing aliphatic diacid divinyl ester; (2) dissolving the aliphatic diacid divinyl ester and glucose into an organic solvent, and adding bacillus subtilis alkali protease or lipase AY30 to obtain a polymerizable saccharine hydrophilic monomer; and (3) dissolving the polymerizable saccharine hydrophilic monomer, an N-isopropylacrylamide monomer and an initiator into an organic solvent, performing a polymerization reaction under the protection of nitrogen gas at the temperature of 50-80 DEG C to obtain a polymer, repeatedly precipitating, and performing vacuum drying on an obtained precipitant to obtain the double-hydrophilic temperature response polymer. The method is simple, has mild reaction conditions, is easy, convenient and practicable for operating, and is easy for industrializing; and the obtained double-hydrophilic temperature response polymer can be applied in the fields of medicament targeted conveying, gene delivery, biological separation, membrane science and the like.

Description

technical field [0001] The invention belongs to the field of preparation of temperature-responsive polymers, in particular to a method for preparing double-hydrophilic temperature-responsive polymers. Background technique [0002] Biomedical polymer is an interdisciplinary research field between polymer science and life science, medicine and material science. It is a polymer material used for diagnosis, treatment or repair, and replacement of tissues and organs. It has been widely used in the fields of drug controlled release, artificial organs, dental materials and tissue engineering in clinical practice. The application of biomedical polymers can be traced back to the 1930s, when synthetic polymethacrylates began to be used as dental materials. After the 1970s, the huge clinical demand led to the rapid development of the new branch of biomedical polymers, and various new biomedical polymer materials came out one after another. After more than 30 years of development, bio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/54C08F218/14C12P19/44A61K47/32A61K48/00
Inventor 朱利民娄少峰权静张婳田利强张培培
Owner DONGHUA UNIV
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