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A kind of methyl acrylic acid, N, N Two methyl ethyl amide amphiphilic block copolymer of styrene and method

A technology of dimethylaminoethyl ester and methacrylic acid, which is applied in the field of copolymer preparation, can solve problems such as difficult separation, low final conversion rate, and impure products, and achieve efficient and simple preparation methods, pure products, and product separation easy effect

Inactive Publication Date: 2017-01-25
SHANDONG YUHUANG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The prior art has disclosed the preparation method of DMAEMA amphiphilic block copolymer, such as the Chinese invention patent with the application number 201310469745.8 proposing the method of preparing DMAEMA amphiphilic block copolymer by single electron transfer living radical polymerization, but the obtained product is not Pure, difficult to separate, although the polymerization rate is fast, the final conversion rate is low, and the molecular weight distribution is wide, above 1.40

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 78ml of THF, 6.4ml of DMAEMA, 17.3ml of LiCl solution (1mol / L acetone solution) and 12.5ml of 1,1-diphenylhexyl into a 200ml Schlenk polymerization bottle. Lithium (1.6mol / L hexane solution), reacted in a water bath at 30°C for 4h, then added 15.4ml of St monomer to continue the reaction for 4h. After the reaction was completed, 1.2 ml of ethanol was added to terminate, the product solvent was removed, and finally dried in a vacuum oven at 40° C. to constant weight to obtain the target product. The polymer yield was 98.2%. The target product was tested by GPC, and its molecular weight was 2100, and its molecular weight distribution was 1.08. use 1 The results were characterized by H-NMR, and the mass fraction of St was measured to be 29.6%, and the block efficiency was 98.1%.

Embodiment 2

[0022] Add 78ml of THF, 6.4ml of DMAEMA, 17.3ml of LiCl solution (1mol / L acetone solution) and 5.0ml of 1,1-diphenylhexyl into a 200ml Schlenk polymerization bottle. Lithium (1.6mol / L hexane solution), reacted in a water bath at 30°C for 3h, then added 15.4ml of St monomer to continue the reaction for 2h. After the reaction was completed, 1.2 ml of ethanol was added to terminate, the product solvent was removed, and finally dried in a vacuum oven at 40° C. to constant weight to obtain the target product. The polymer yield was 98.3%, and the target product was tested by GPC, the molecular weight was 4900, and the molecular weight distribution was 1.07. use 1 The results were characterized by H-NMR, and the mass fraction of St was measured to be 29.7%, and the block efficiency was 97.9%.

Embodiment 3

[0024] Add 78ml of THF, 6.4ml of DMAEMA, 17.3ml of LiCl solution (1mol / L acetone solution) and 3.1ml of 1,1-diphenylhexyl into a 200ml Schlenk polymerization bottle. Lithium (1.6mol / L hexane solution), reacted in a water bath at 30°C for 2h, then added 15.4ml of St monomer to continue the reaction for 1h. After the reaction was completed, 1.2 ml of ethanol was added to terminate, the product solvent was removed, and finally dried in a vacuum oven at 40° C. to constant weight to obtain the target product. The polymer yield was 89.1%, and the target product was tested by GPC, with a molecular weight of 7200 and a molecular weight distribution of 1.09. use 1 The results were characterized by H-NMR, and the mass fraction of St was measured to be 26.5%, and the block efficiency was 93.2%.

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PUM

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Abstract

The invention relates to the preparation of copolymer technical areas, especially public a kind of methyl acrylic acid, N, N dimethyl amino ethyl ester amphiphilic block copolymer of styrene and preparation methods The preparation method, its character is that: with the method of living anionic polymerization, the initiator of methyl acrylic acid, N, N dimethyl amino ethyl ester solvent additives added to deal with good polymerization with schlenk techniques in a bottle, the reaction condition for 50 to 50 oc 2 5 hours, then add the styrene reaction to 4 hours, after the termination of ethanol, the solvent removal, get the target product The invention of the conversion rate is as high as 99%, product separation easy, narrow molecular weight distribution, and the block rate is high, the product purity, simple preparation method efficiently, to facilitate the future industrial production.

Description

[0001] (1) Technical field [0002] The invention relates to the technical field of copolymer preparation, in particular to a preparation method of N,N-dimethylaminoethyl methacrylate and styrene amphiphilic block copolymer. [0003] (2) Background technology [0004] N,N-dimethylaminoethyl methacrylate (DMAEMA) and styrene (St) amphiphilic block copolymer can be widely used as dispersant, stabilizer, emulsifier, surfactant, etc. PDMAEMA itself has "pH / temperature" responsiveness is likely to become a hotspot in biomedical research in the future. [0005] The prior art has disclosed the preparation method of DMAEMA amphiphilic block copolymer, such as the Chinese invention patent with the application number 201310469745.8 proposing the method of preparing DMAEMA amphiphilic block copolymer by single electron transfer living radical polymerization, but the obtained product is not Pure, difficult to separate, although the polymerization rate is fast, the final conversion rate is...

Claims

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Application Information

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IPC IPC(8): C08F297/02C08F220/34C08F212/08
CPCC08F297/026C08F212/08C08F220/34
Inventor 刘华华焦俊卿王玉强陈双喜王胜伟
Owner SHANDONG YUHUANG CHEM CO LTD
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