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Method for removing catalyst from polymer prepared by atom transferring free-radical polymerization

An atom transfer and free radical technology, applied in the field of catalysts, can solve the problems of increased production costs, large solvent consumption, and large catalyst content, and achieve the effects of low equipment investment costs, easy process, and high extraction efficiency

Inactive Publication Date: 2007-09-05
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Atom transfer radical polymerization technology can be used to synthesize polymers with controllable molecular weight and expected structure, such as block, graft, star, hyperbranched, organic-inorganic hybrid polymers, etc., but due to the use of atom transfer radical polymerization The content of the catalyst is relatively large, resulting in more catalysts in the obtained polymer. Therefore, this will not only affect the color of the product, but more seriously may affect its performance
[0003] Polymers prepared by atom transfer radical polymerization technology contain catalysts, which will not only affect the color of the polymer, but more seriously, may affect its performance
Literature Seong Mu Jo, Hyun-Jong Paik, and Krzysztof Matyjaszewski, Polymer Preprints, 1997, Vol.38, No.1, 695 and Yoshiki Nakagawa, Peter Miller, Cristina Pacis and Krzysztof Matyjaszewski, Polymer Preprints, 1997, Vol.38, No. .1, 701 uses precipitation and alumina column chromatography to remove the catalyst in this kind of polymer system. These two methods can only be used in the laboratory and have no industrial application value. The former needs to consume a lot of solvent and increase equipment investment In addition to increasing equipment investment costs, the latter also needs to frequently replace the packing in the column, which not only increases the production cost, but also causes great difficulties for the industrial continuous production of atom transfer radical polymerization in the future.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Using methyl 2-bromopropionate as an initiator and CuCl / 2,2'-bipyridine complex (the claim is 2,2'-bipyridine?) as a catalyst to initiate atom transfer radical polymerization of methyl acrylate , monomer weight 170g. After the polymerization reaction is terminated, the molecular weight of the polymer measured by GPC is M n =19450, the molecular weight distribution is D=1.35. Add 170g of toluene and 68g of N-methyl-N-ethylhexahydropyridine tetrafluoroborate (the amount used is 20% of the mass of the monomer and solvent) into the polymerization reactor containing the above system, stir and heat up to 90°C, Stir and react at this temperature for 1 hour and then let it stand for 3 hours, then extract the catalyst-containing extraction layer in the lower layer, repeat the above operation three times, and finally directly distill the toluene layer containing the polymer in the upper layer to obtain 160 g of white or yellow polymer , the yield was 94.1% (the percentage of th...

Embodiment 2

[0018] With azobisisobutyronitrile as the initiator, CuBr 2 / N, N'-tetramethylethylenediamine complex is the atom transfer radical polymerization that catalyst initiates methyl methacrylate, monomer weight 200g. After the polymerization reaction is terminated, the molecular weight of the polymer measured by GPC is M n =14800, the molecular weight distribution is D=1.35. Add 200 g of toluene, 20 g of acetonitrile, and 120 g of N-methyl N-hexylmorpholine tetrafluoroborate (amount of 30%) into the polymerization reactor containing the above system, and stir to raise the temperature to 25°C. Stir the reaction for 12 hours and let it stand for 6 hours, then extract the catalyst-containing extraction layer in the lower layer, repeat the above operation twice, and finally directly distill the toluene layer containing the polymer in the upper layer to obtain 186.5 g of white or yellow polymer. The ratio is 93.2%, and the Cu ion content is 4.65ppm according to the fluorescence spectr...

Embodiment 3

[0020] With ethyl 2-bromoisobutyrate as the initiator, Cu 2 SO 4 / N, N', N "-pentamethyldivinyltriamine is the atom transfer radical polymerization of butyl methacrylate initiated by the catalyst, and the weight of the monomer is 142g. After the polymerization reaction is terminated, the molecular weight of the polymer is measured by GPC for M n =22100, the molecular weight distribution is D=1.27. Add 142g of toluene and 142g of N-methyl N-ethylimidazolium tetrafluoroborate (amount of 50%) into the polymerization reactor containing the above system, stir and raise the temperature to 80°C, and then stir and react at this temperature for 1 hour Stand still for 2 hours, extract the lower catalyst-containing extraction layer, repeat the above operation five times, and finally directly distill the upper polymer-containing toluene layer to obtain 134g of white or yellow polymer with a yield of 94.4%. Fluorescence spectrum analysis The Cu ion content was 5.85 ppm.

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Abstract

A method for removing catalyst from atomic-transferring free radical polymer is carried out by taking ion liquid as extracting agent, adding it into atomic-transferring free radical polymerization system under protection of inert gas, agitating while raising temperature, extracting for catalyst while agitating, and separating out extracting agent layer. It's cheap, efficient and re-usable and has no environmental pollution.

Description

technical field [0001] The invention relates to a method for removing catalysts in polymers prepared by atom transfer radical polymerization by using an extraction method. The method uses an ionic liquid as an extraction agent to extract the terminated polymerization system, and the transition metal in the reaction can be combined with the The complexes formed by the ligands are extracted into the extractant. Background technique [0002] Atom transfer radical polymerization technology can be used to synthesize polymers with controllable molecular weight and expected structure, such as block, graft, star, hyperbranched, organic-inorganic hybrid polymers, etc., but due to the use of atom transfer radical polymerization The catalyst content is relatively large, resulting in more catalysts in the obtained polymer, therefore, this will not only affect the color of the product, but more seriously may affect its performance. [0003] Polymers prepared by atom transfer radical pol...

Claims

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Application Information

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IPC IPC(8): C08F6/08C08F6/00
Inventor 洪昕林肖桂林张高勇
Owner WUHAN UNIV