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Lewis acid-base pair catalytic initiator and application thereof

A Lewis acid-base pair and Lewis base technology, applied in physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, chemical instruments and methods, etc., can solve the problem of low catalytic system activity and limited catalytic system activity , low catalytic activity, etc.

Active Publication Date: 2019-05-03
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to its low initiation efficiency and the "slow initiation, fast growth" polymerization mode, the existing catalytic system has low activity and poor controllability.
[0003] In 2016, Feng Xiaoshuang et al. (Zhang, D.; Boopathi, S.K.; Hadjichristidis, N.; Gnanou, Y.; Feng, X. Journal of the American Chemical Society 2016, 138, 11117.) reported a The acid-base pair composed of ethyl boron successfully catalyzed the copolymerization of carbon dioxide and epoxide, but due to the low catalytic activity, the degree of alternation of polycarbonate produced by the copolymerization of carbon dioxide and propylene oxide cannot be 100%, and its conversion frequency (TOF) can only reach 49h -1
However, it is also limited to the activity of the catalytic system, and the conversion frequency (TOF) of the system can only reach 113h -1

Method used

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  • Lewis acid-base pair catalytic initiator and application thereof
  • Lewis acid-base pair catalytic initiator and application thereof
  • Lewis acid-base pair catalytic initiator and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1P

[0074] Embodiment 1PO one-pot method ring-opening polymerization synthesizes polyether

[0075] Before the polymerization reaction, remove the water in a 10mL high-pressure reactor at 110°C for about 2 hours and cool it to room temperature in a desiccator; add several masses of Lewis base 1 triethylamine (TEA) and Lewis acid tri Ethyl boron (TEB), the molar ratio of the two is 1:2; the molar ratio of Lewis base 1 to propylene oxide (PO) is 1 / 1000. Then the autoclave was closed and placed in an oil bath at 60°C for 12 hours under autogenous pressure. Cool to room temperature after the reaction, first dissolve the crude product with tetrahydrofuran, then precipitate the polymer in a mixture of ethanol / deionized water / hydrochloric acid, repeat washing three times, and vacuum-dry to constant weight.

[0076] The content of each chain segment in the polymer was calculated by proton nuclear magnetic spectroscopy, and the molecular weight and molecular weight distribution of the pol...

Embodiment 2

[0077] Embodiment 2PO one-pot method ring-opening polymerization synthesizes polyether

[0078] Before the polymerization reaction, remove the moisture in a 10mL high-pressure reactor at 110°C for about 2 hours and cool it to room temperature in a desiccator; add several masses of Lewis base 2 tributylamine (TBA) and Lewis acid tributylamine to the reactor Ethyl aluminum (TEAl), the molar ratio of the two is 1:4; the molar ratio of Lewis base 2 to propylene oxide (PO) is 1 / 2000. Then the autoclave was closed and placed in an oil bath at 40°C for 10 h under autogenous pressure. Cool to room temperature after the reaction, first dissolve the crude product with tetrahydrofuran, then precipitate the polymer in a mixture of ethanol / deionized water / hydrochloric acid, repeat washing three times, and vacuum-dry to constant weight.

[0079] The content of each chain segment in the polymer was calculated by proton nuclear magnetic spectroscopy, and the molecular weight and molecular we...

Embodiment 3

[0080] Example 3CO 2 / PO one-pot copolymerization into polycarbonate

[0081] Before the polymerization reaction, remove the moisture in a 10mL high-pressure reactor at 110°C for about 2 hours and cool it to room temperature in a desiccator; add a certain amount of Lewis base 3N,N,N',N'-tetraethyl to the reactor Ethylenediamine (E-E) and Lewis acid tributylboron (TBB), the molar ratio of the two is 0.5:1; then add CO 2 、PO(CO 2 With PO molar ratio 1:1) and 3 mL tetrahydrofuran (THF), the molar ratio of Lewis base 3 to propylene oxide (PO) was 1 / 500. Then the autoclave was closed and placed in an oil bath at 40°C for 8 hours under autogenous pressure. Cool to room temperature after the reaction, first dissolve the crude product with tetrahydrofuran, then precipitate the polymer in a mixture of ethanol / deionized water / hydrochloric acid, repeat washing three times, and vacuum-dry to constant weight.

[0082] The content of each chain segment in the polymer was calculated by p...

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PUM

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Abstract

The invention discloses a Lewis acid-base pair catalytic initiator and application thereof. The Lewis acid-base pair catalytic initiator comprises a Lewis acid and a Lewis base, the structural generalformula of the Lewis acid is shown in formula (I), and the structural general formula of the Lewis base is shown in formula (II-1) or (II-2); in the formula, A is selected from an element B or an element Al; R1, R2, R3 and R4 are independently selected from alkyl, alkoxy, aryl or halogen; the carbon number of the alkyl or alkoxy is 1-16; the aryl contains 0-5 substituents selected from methyl, methoxy or halogen; and n is an integer from 1 to 16. The Lewis acid-base pair catalytic initiator can be used for catalyzing epoxide homopolymerization reaction and epoxide copolymerization reaction, and has extremely high catalytic activity.

Description

technical field [0001] The invention relates to the field of catalysts, in particular to a Lewis acid-base pair catalyst initiator and its application in preparing epoxy homopolymers and epoxy copolymers. Background technique [0002] The application of Lewis acid-base pairs (LPs) in the field of catalytic polymerization was first reported by Colorado State University in 2010, initially for the preparation of polyolefin materials from polar vinyl monomers. Due to the characteristics of high activity, strong controllability and easy regulation of polymerization effect of LPs, they have been widely studied at home and abroad. Recent research results have shown that Lewis acid-base pairs can catalyze epoxide / cyclic anhydride copolymerization, epoxide / CO 2 (COS) copolymerization, epoxide / cyclic anhydride copolymerization / carbon dioxide copolymerization reaction to synthesize polyester, polycarbonate, poly(ether-carbonate), polythiocarbonate and poly(carbonate-ester), etc. Howe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/06C08G64/34C08G64/38C08G64/02C08G63/52C08G63/84C08G63/87
CPCC08G64/34C08G63/87C08G63/52C08G63/84C08G64/0208C08G63/58C08G65/10C08G65/2654C08G65/2672C08G65/269C08G65/2603B01J31/0238B01J31/143B01J31/146C08G59/686C08G64/025C08G2650/22
Inventor 张兴宏杨嘉良胡岚方
Owner ZHEJIANG UNIV
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