Catalytic system and synthesis method of multi-block copolymer

A technology of catalytic system and synthesis method, which is applied in the field of chemical synthesis and can solve problems such as the rareness of catalysts

Active Publication Date: 2022-05-10
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, catalysts that can be used to catalyze the synthesis of complex block structures from mixtures of more than three monomers are very rare

Method used

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  • Catalytic system and synthesis method of multi-block copolymer
  • Catalytic system and synthesis method of multi-block copolymer
  • Catalytic system and synthesis method of multi-block copolymer

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Under anhydrous and oxygen-free conditions, mix 0.02mmol of the compound of formula (I) and 0.02mmol of PPNCl with 20mmol of epoxycyclohexane (CHO) in a high-pressure reactor, and place it in an oil bath at 80°C for 48 hours with stirring , take about 0.3mL mixed solution as 300M 1 H NMR NMR samples were characterized, and the results showed that the conversion rate of CHO was 16%, and the reaction products were all cyclohexene carbonate (CHC) (>98% cis, <0.5% trans).

Embodiment 2

[0051] Under anhydrous and oxygen-free conditions, 0.02mmol formula (I) structure compound and 0.02mmol PPNNO 3 Mix it with 20mmol CHO in a high-pressure reactor, place it in an oil bath at 80°C and stir for 48 hours, take about 0.3mL of the mixed solution as 300M 1 The H NMR nuclear magnetic sample was characterized, and the results showed that the conversion rate of CHO was 7.6%, and the reaction product contained 22.2% polycyclohexene carbonate (PCHC) and 77.8% CHC (63.7% cis, 14.1% trans).

Embodiment 3

[0053] Under anhydrous and oxygen-free conditions, mix 0.02mmol of the compound of formula (I), 0.02mmol of PPNOAc and 20mmol of CHO in a high-pressure reactor, place it in an oil bath at 80°C and stir for 48 hours, and take about 0.3mL of the mixed solution as 300M 1 The H NMR nuclear magnetic sample was characterized, and the results showed that the conversion rate of CHO was 18.4%, and the reaction product contained 9.0% PCHC and 91.0% CHC (84.1% cis, 6.9% trans).

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Abstract

The invention belongs to the technical field of chemical synthesis, and particularly relates to a catalytic system and a synthesis method of a multi-block copolymer. The catalytic system provided by the invention comprises a main catalyst with a structure as shown in a formula (I) and a cocatalyst with a structure as shown in a formula (II). The synthesis method provided by the invention comprises the following steps: a) under anhydrous and anaerobic conditions, mixing the catalytic system, acid anhydride, epsilon-caprolactone, carbon dioxide and alicyclic epoxide, and carrying out polymerization reaction; and b) releasing carbon dioxide in the reaction system in the step a), and then continuously carrying out polymerization reaction in an inert gas atmosphere to obtain the multi-block copolymer. The catalytic system provided by the invention has better activity and very high selectivity; according to the synthesis method provided by the invention, alternate copolymerization of epoxide and anhydride, alternate copolymerization of epoxide and carbon dioxide and ring-opening copolymerization of caprolactone can be sequentially realized through a one-pot method, so that the ABC type multi-block copolymer is obtained.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a catalytic system and a synthesis method of a multi-block copolymer. Background technique [0002] Multi-component multi-block copolymers with exquisite and complex sequence structures have been considered to be unique products of nature. Since the emergence of some special polymerization processes, artificial synthesis to produce sequence-controllable block copolymers with simulated natural precision has become a research field that has attracted much attention in recent years. Artificial synthesis strategies are basically based on the active mechanism of polymerization, such as anionic polymerization and some controlled free radical polymerization or chain transfer reactions. In recent years, switchable catalysis has become a research hotspot, because it can synthesize sequence-controllable block copolymers from monomer mixtures in a relatively economic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/83C08G63/87C08G63/64
CPCC08G63/83C08G63/87C08G63/64C08G63/823
Inventor 庞烜杨振杰段然龙胡晨阳周延川陈学思
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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