Method for preparing DMAEMA based amphiphilic block copolymer through single electron transfer living free radical polymerization

A single-electron transfer, amphiphilic block technology, applied in the field of preparing DMAEMA-based amphiphilic block copolymers, can solve the problems of complex process flow, many catalysts, limited development, etc., and achieves high monomer conversion rate and fast polymerization rate. , the preparation method is simple and easy to implement

Active Publication Date: 2014-01-08
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Amphiphilic block copolymers are usually prepared by anionic polymerization, but the harsh conditions of anionic polymerization limit its development
Atom Transfer Radical Polymerization (ATRP) synthesizes amphiphilic block copolymers under relatively mild reaction conditions, but ATRP requires more catalysts, and the catalysts are transition metals with low oxidation states, typically represented by copper halides and copper salts. Addition makes the polymerization product often very dark in color and requires post-treatment, which not only complicates the process, but also increases its production cost

Method used

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  • Method for preparing DMAEMA based amphiphilic block copolymer through single electron transfer living free radical polymerization
  • Method for preparing DMAEMA based amphiphilic block copolymer through single electron transfer living free radical polymerization
  • Method for preparing DMAEMA based amphiphilic block copolymer through single electron transfer living free radical polymerization

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Experimental program
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Effect test

Embodiment 1

[0026] 0.1gPDMAEMA~Br(M n GPC =7.04×10 4 , PDI=1.30), 10mLBA (n-butyl acrylate) (0.0701mol), 65mL deionized water were added to a 200mL round bottom flask, copper wire Φ0.26mm, L60cm was added, stirred for 20min with nitrogen, and then added under nitrogen protection 0.6823g TREN (0.0047mol), after five cycles of vacuum pumping and nitrogen filling, place the flask in a constant temperature water bath at 60°C, react for 120min, take out the copper wire, dehydrate and vacuum dry to obtain the target product.

[0027] The monomer conversion rate was 64% as measured by gravimetric method, and the polymer M was measured by GPC. n =13.25×10 4 , PDI=1.85.

[0028] the polymer 1 H-NMR analysis, such as figure 1 As shown, the signal peaks in the spectrum completely correspond to the hydrogen protons on the two structural units in the block copolymer. The GPC curve of the macromolecular initiator PDMAEMA~Br and the obtained block copolymer is as follows figure 2 As shown, the ...

Embodiment 2

[0030] 0.1gPDMAEMA~Br(M n GPC =7.04×10 4 , PDI=1.30), 10mLBA (0.0701mol), 15mL deionized water were added to a 50mL round-bottomed flask, copper wire Φ0.50mm, L10cm was added, and after stirring for 20min with nitrogen gas, 0.0351g Cyclam (0.00018mol) was added under nitrogen protection , after five cycles of vacuum pumping and nitrogen filling, the flask was placed in a constant temperature water bath at 30°C, and after 120 minutes of reaction, the copper wire was taken out, and the target product was obtained by dehydration and vacuum drying.

[0031] The monomer conversion rate was 84% ​​as measured by gravimetric method, and the polymer M was measured by GPC. n =24.62×10 4 , PDI=1.50.

Embodiment 3

[0033] 0.1gPDMAEMA~Br(M n GPC =7.04×10 4 , PDI=1.30), 10mLBA (0.0701mol), 40mL deionized water were added to a 100mL round-bottomed flask, copper wire Φ0.08mm, L80cm was added, and after stirring for 20min with nitrogen, 1.0183gTMEDA (0.0088mol) was added under nitrogen protection , after five cycles of vacuuming and nitrogen filling, the flask was placed in a constant temperature water bath at 60°C, and after reacting for 90 minutes, the copper wire was taken out, and the target product was obtained by dehydration and vacuum drying.

[0034] The monomer conversion rate was 88% as measured by gravimetric method, and the polymer M was measured by GPC. n =25.37×10 5 , PDI=1.47.

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Abstract

The invention relates to a method for preparing a DMAEMA based amphiphilic block copolymer through single electron transfer living free radical polymerization. The method comprises the following steps: adding an initiator, a monomer, deionized water and a catalyst into a reactor, filling nitrogen, stirring for 20 min, adding a ligand under the protection of nitrogen, maintaining the nitrogen atmosphere, reacting at 0-90 DEG C for 10-150 min, taking out the catalyst, dewatering and vacuum drying to obtain a target product. The catalyst is a copper wire, and the initiator is active polymethylacrylic acid dimethyl amino ethyl ester; and the monomer is oil soluble acrylate. The preparation method provided by the invention is high in polymerization speed, high in monomer conversion rate (67% can be achieved within 60 min) and narrow in molecular weight distribution (the minimum can be 1.40), and the molecular weight of each segment of the block copolymer is controllable. The preparation method is simple, convenient and easy to realize and is clean and environment-friendly, thereby providing convenience for industrial production.

Description

technical field [0001] The invention relates to a method for preparing a DMAEMA-based amphiphilic block copolymer, in particular to a method for preparing a DMAEMA-based amphiphilic block copolymer by single electron transfer active radical polymerization. Background technique [0002] Amphiphilic block copolymers can be used as dispersants, stabilizers, compatibilizers, and surfactants, and have received a lot of research in recent years. Dimethylaminoethyl methacrylate (DMAEMA) is a water-soluble acrylate with temperature and pH sensitivity, and the amphiphilic block copolymer containing PDMAEMA segment is also environmentally sensitive as a functional polymer, so it has Lots of special uses. PDMAEMA can also have a good affinity for DNA, act as a mediator in different cells, and has biocompatibility and anticoagulant functions. Therefore, DMAEMA-based amphiphilic block copolymers have potential applications in the biological field and medical systems value. [0003] Am...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08F220/34C08F220/14C08F220/18C08F4/50
Inventor 袁金凤殷燕潘明旺郭宏飞张广林
Owner HEBEI UNIV OF TECH
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