Temperature-responsive poly(hydroxyethyl methacrylate) and preparation method thereof

A poly(hydroxyethyl methacrylate) temperature-responsive technology, which is applied in the coating and other directions, can solve the problems of insufficient control ability of the polymerization process and the inability to repeat molding, etc., so as to broaden the synthesis method and application range, and the reaction system is simple and stable , the effect of mild reaction conditions

Active Publication Date: 2021-04-30
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of these polymers exhibit UCST temperature response only when the cross-linked hydrogel swells in water, which means that remolding is not possible
[0005] Poly(hydroxyethyl methacrylate) (PHEMA) has the advantages of high light transmittance, high water absorption, non-toxicity, etc., but the ability to control its polymerization process is insufficient at present, so most of the synthesized ones are low molecular weight linear PHEMA or cross-linked PHEMA hydrogel

Method used

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  • Temperature-responsive poly(hydroxyethyl methacrylate) and preparation method thereof
  • Temperature-responsive poly(hydroxyethyl methacrylate) and preparation method thereof
  • Temperature-responsive poly(hydroxyethyl methacrylate) and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] According to the ratio of [HEMA]:[MEMA]:[BPO]=40:1:1, poly(hydroxyethyl methacrylate) was prepared by inverse emulsion polymerization. The specific process was: adding hydroxyethyl methacrylate (0.0400 mol) Dissolve in water (300 wt% hydroxyethyl methacrylate) to make an aqueous solution of hydroxyethyl methacrylate (25 wt%). The aqueous solution of hydroxyethyl methacrylate was added to a mixture of toluene (400 wt% hydroxyethyl methacrylate), Span85 (5 wt% toluene), Tween80 (5 wt% toluene), reducing agent monomer MEMA (0.0010mol) After stirring evenly and vacuuming the oxygen, add the oxidant BPO (0.0010mol), put it in a 25 ºC water bath for 8 hours, and the conversion rate of hydroxyethyl methacrylate is 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 of the polymer was measured by dynamic and static light scattering, Mw.MALLS=133000 ...

Embodiment 2

[0029]Poly(hydroxyethyl methacrylate) was prepared by inverse emulsion polymerization according to the proportion of [HEMA]:[MEMA]:[BPO]=200:1:1 (others are the same as in Example 1), and the polymer was measured by dynamic and static light scattering The absolute weight average molecular weight Mw.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 mass of the solution. The solution was placed in a 60 ºC oven 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 volatile solvent to keep the solution concentration constant. After equilibrating at 18 ºC for 1 h, the absorbance was measured using a UV-Vis spectrophotometer. After that, the temperature was gradually lowered, and after equilibrating at each temperature for 10 min, the absorbance was measured. The test found that the absorbance of the solution suddenly increas...

Embodiment 3

[0031] Poly(hydroxyethyl methacrylate) was prepared by inverse emulsion polymerization according to the ratio of [HEMA]:[MPAEMA]:[BPO]=80:1:1 (others are the same as in Example 1), and the polymer was measured by dynamic and static light scattering The absolute weight average molecular weight Mw.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 mass of the solution. The solution was placed in a 60 ºC oven 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 volatile solvent to keep the solution concentration constant. After equilibrating at 20 ºC for 1 h, the absorbance was measured using a UV-Vis spectrophotometer. After that, the temperature was gradually lowered, and after equilibrating at each temperature for 10 min, the absorbance was measured. The test found that the absorbance of the solution suddenly increased ...

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Abstract

The invention belongs to the field of polymer synthesis, and in particular relates to a temperature-responsive polyhydroxyethyl methacrylate and a preparation method. With dibenzoyl peroxide as oxidizing agent, 2-methyl-N-[3-(methyl-phenyl-amino)-propyl]-acrylamide or 2-methyl-N-[3-(methyl ‑Phenyl‑amino)‑propyl]‑propionamide is a reducing agent monomer to form a redox initiation system, water and toluene are media, nonionic surfactants are emulsifiers, and hydroxyethyl methacrylate is a monomer. Polymerization reaction at room temperature and normal pressure to obtain polyhydroxyethyl methacrylate, and its alcohol solution has a high critical phase transition temperature. The polymerization system of the invention is simple and stable, the polymerization cost is low, the operation is easy, the conditions are mild, the impact on the environment is small, the energy consumption is low, and the molecular weight and high critical phase transition temperature of the product are controllable within a certain range. It is of great significance to the 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 polymers refer to a class of polymers in which the polymer solution changes from dissolved and clear to insoluble and turbid, or the hydrogel c...

Claims

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Application Information

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Patent Type & Authority Patents(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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