Temperature response-type polyhydroxyethyl methacrylate and preparation method thereof

A polyhydroxyethyl methacrylate, temperature-responsive technology, applied in coating and other directions, can solve the problems of inability to repeat molding, lack of polymerization process control ability, etc., to broaden the synthesis method and application range, the reaction system is simple and stable, System stabilization effect

Active Publication Date: 2020-07-10
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of these polymers have UCST temperature response phenomenon only when the cross-linked hydrogel is swollen in water, and the formation of cross-linked structure means that it cannot be molded repeatedly
[0005] Poly(hydroxyethyl methacrylate) (PHEMA) has the advantages of high light transmission, high water absorption, non-toxicity, etc., but the ability to control its polymerization process is insufficient at present, so most of the synthesized products are low molecular weight linear PHEMA or cross-linked PHEMA hydrogel

Method used

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  • Temperature response-type polyhydroxyethyl methacrylate and preparation method thereof
  • Temperature response-type polyhydroxyethyl methacrylate and preparation method thereof
  • Temperature response-type polyhydroxyethyl methacrylate and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0027] According to [HEMA]:[MEMA]:[BPO]=40:1:1 ratio to prepare polyhydroxyethyl methacrylate by inverse emulsion polymerization, the specific process is: add hydroxyethyl methacrylate (0.0400mol) Dissolve in water (300wt% hydroxyethyl methacrylate) to prepare a hydroxyethyl methacrylate aqueous solution (25wt%). Add the aqueous solution of hydroxyethyl methacrylate to the reaction bottle with toluene (400wt% hydroxyethyl methacrylate), Span85 (5wt% toluene), Tween80 (5wt% toluene), reducing agent monomer MEMA (0.0010mol) , after stirring evenly and vacuuming to exhaust oxygen, the oxidant BPO (0.0010mol) was added, placed in a water bath at 25°C for 8 hours, and the conversion rate of hydroxyethyl methacrylate was measured to be 94.3%. Demulsify with tetrahydrofuran, wash with water three times and then dry, then purify three times and then dry to obtain polymer. The absolute weight-average molecular weight M of the polymer was measured by dynamic and static light scattering...

Embodiment 2

[0031] Press [HEMA]:[MEMA]:[BPO]=200:1:1 ratio to prepare polyhydroxyethyl methacrylate (others are the same as in Example 1) by inverse emulsion polymerization, and measure the polymer by dynamic and static light scattering The absolute weight average molecular weight M w.MALLS= 1605000 g / mol. Weigh 1 mg of polymer and dissolve it in isopropanol to make a 1 mg / mL solution, weigh and record the solution mass. The solution was placed in an oven at 60°C for more than 24 hours to ensure that the polymer was fully dissolved in the solvent isopropanol, and weighed at any time to replenish the volatilized solvent to keep the solution concentration unchanged. After equilibrating at 18°C ​​for 1 h, the absorbance was measured using a UV-Vis spectrophotometer. Afterwards, the temperature was gradually lowered, and after equilibrating at each temperature for 10 minutes, the absorbance was measured. The test found that the absorbance of the solution suddenly increased in the range of ...

Embodiment 3

[0033] Press [HEMA]:[MPAEMA]:[BPO]=80:1:1 ratio to prepare polyhydroxyethyl methacrylate (others are the same as embodiment 1) by inverse emulsion polymerization, and measure polymer by dynamic and static light scattering The absolute weight average molecular weight M w.MALLS =2442000 g / mol. Weigh 1 mg of polymer and dissolve it in isopropanol to make a 1 mg / mL solution, weigh and record the solution mass. The solution was placed in an oven at 60°C for more than 24 hours to ensure that the polymer was fully dissolved in the solvent isopropanol, and weighed at any time to replenish the volatilized solvent to keep the solution concentration unchanged. After equilibrating at 20°C for 1 h, the absorbance was measured using a UV-Vis spectrophotometer. Afterwards, the temperature was gradually lowered, and after equilibrating at each temperature for 10 minutes, the absorbance was measured. The test found that the absorbance of the solution suddenly increased in the range of 16°C-...

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Abstract

The invention belongs to the field of polymer synthesis, and particularly relates to temperature response-type polyhydroxyethyl methacrylate and a preparation method thereof. The dibenzoyl peroxide isused as an oxidizing agent, and 2-methyl-N-[3-(methyl-phenyl-amino)-propyl]-acrylamide or 2-methyl-N-[3-(methyl-phenyl-amino)-propyl]-propanamide is used as a reducing agent monomer to form a redox initiation system; water and methylbenzene are used as media, a nonionic surfactant is used as an emulsifier, and hydroxyethyl methylacrylate is used as a monomer, a polymerization reaction is carriedout at room temperature and normal pressure to obtain polyhydroxyethyl methylacrylate, and an alcoholic solution of polyhydroxyethyl methylacrylate has a high critical phase transition temperature; the method is simple and stable in polymerization system, low in polymerization cost, easy to operate, mild in condition, small in influence on the environment and low in energy consumption, and the molecular weight and the high critical phase transition temperature of the product are controllable within a certain range. The method is of great significance to theoretical research and large-scale application of temperature-responsive polymers.

Description

technical field [0001] The invention belongs to the field of preparation of functional polymers in polymer synthesis, and in particular relates to a temperature-responsive polyhydroxyethyl methacrylate and a preparation method. Background technique [0002] Smart materials are materials that can perceive and respond to the environment, and are new materials that integrate the functions of self-detection, self-judgment and self-processing. As an important and potential smart material, temperature-responsive polymers have been widely developed and utilized in the fields of drug release, tissue engineering and separation and purification. Temperature-responsive polymers can be divided into two categories: low critical phase transition temperature (LCST) type and high critical phase transition temperature (UCST) type. [0003] LCST type polymer refers to a type of polymer that changes from dissolving and clarifying to insoluble and turbid polymer solution, or from swelling to s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/20C08F220/60C08F4/40C08F2/32C08F120/20
CPCC08F220/20C08F4/40C08F2/32C08F120/20C08F220/60C09D139/06C08F4/34C08L33/14C08F20/20C08F2500/01
Inventor 朱迪范怡黄文艳蒋必彪薛小强杨宏军江力蒋其民
Owner CHANGZHOU UNIV
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