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A kind of preparation method of crystalline polyester and product thereof

A technology for crystalline polyester and products, applied in the field of preparation of crystalline polyester, can solve the problems of lack of efficient catalytic system reaction conditions, polymers not reported to have crystallinity, difficulty in copolymerizing isobutylene oxide, and the like, achieving no need for post-treatment Purification steps, rich variety, good universal effect

Active Publication Date: 2021-11-16
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Aoshima et al. reported the cross-reaction of isobutylene oxide with vinyl ether (J.Am.Chem.Soc.2013, 135, 9330-9333), but isobutylene oxide requires cationic ring opening at very low temperature (-78°C) , the reaction is difficult to control
[0004] According to the existing research, it is difficult to copolymerize isobutylene oxide with other monomers, and there are very few studies on the copolymerization of isobutylene oxide with cyclic anhydrides
This is mainly due to the lack of a suitable high-efficiency catalytic system and suitable reaction conditions. Even though it has been reported in the literature that oxidized isobutylene-based polyesters have been prepared, only oligomers or copolymers with very low molecular weights have been obtained, and the corresponding polymers are homogeneous. Not reported to be crystalline

Method used

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  • A kind of preparation method of crystalline polyester and product thereof
  • A kind of preparation method of crystalline polyester and product thereof
  • A kind of preparation method of crystalline polyester and product thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Embodiment 1 MA / IBO synthesizes oxidized isobutylene-based crystalline polyester

[0052] Before the polymerization reaction, put the 10mL reactor at 110°C for about 2 hours, remove the water and cool it to room temperature in a desiccator; add indium-cobalt double metal cyanide complex and maleic anhydride (MA) to the reactor in sequence , 1 mL of toluene and isobutylene oxide (IBO); the molar ratio of IBO to MA is 1:1, and the molar ratio of catalyst to IBO is 1 / 500. Then the reactor was closed and placed in an oil bath at 55°C for 12 hours under autogenous pressure. Cool to room temperature after the reaction, first dissolve the crude product with dichloromethane, then precipitate the polymer in ethanol, repeat washing three times, then soak the polymer in ethanol for 12 hours to induce crystallization, and vacuum-dry to constant weight. The molecular weight and molecular weight distribution of the polymer were determined by gel chromatography, and the test results ...

Embodiment 2

[0059] Embodiment 2 MA / IBO synthesizes oxidized isobutylene-based crystalline polyester

[0060] Before the polymerization reaction, the 10mL reaction kettle was dehydrated at 110°C for about 2 hours and cooled to room temperature in a desiccator; zinc-cobalt double metal cyanide complex, maleic anhydride (MA), 1 mL of toluene and isobutylene oxide (IBO); the molar ratio of IBO to MA is 1:1, and the molar ratio of catalyst to IBO is 1 / 500. Then the reactor was closed and placed in an oil bath at 55°C for 12 hours under autogenous pressure. Cool to room temperature after the reaction, first dissolve the crude product with dichloromethane, then precipitate the polymer in ethanol, repeat washing three times, then soak the polymer in methanol for 12 hours to induce crystallization, and vacuum-dry to constant weight. The molecular weight and molecular weight distribution of the polymer were determined by gel chromatography, and the test results are shown in Table 1.

[0061] Afte...

Embodiment 3

[0062] Embodiment 3 MA / IBO synthesizes oxidized isobutylene-based crystalline polyester

[0063] Before the polymerization reaction, the 10mL reaction kettle was dehydrated at 110°C for about 2 hours and cooled to room temperature in a desiccator; zinc-iron double metal cyanide complex, maleic anhydride (MA), 1 mL of toluene and isobutylene oxide (IBO); the molar ratio of IBO to MA is 1:1, and the molar ratio of catalyst to IBO is 1 / 500. Then the reactor was closed and placed in an oil bath at 55°C for 12 hours under autogenous pressure. Cool to room temperature after the reaction, first dissolve the crude product with dichloromethane, then precipitate the polymer in ethanol, repeat washing three times, then soak the polymer in methanol for 12 hours to induce crystallization, and vacuum-dry to constant weight. The molecular weight and molecular weight distribution of the polymer were determined by gel chromatography, and the test results are shown in Table 1.

[0064] After ...

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Abstract

The invention discloses a preparation method of crystalline polyester, which takes isobutylene oxide and cyclic acid anhydride as raw materials, adopts double metal cyanide complex as catalyst, and conducts polymerization reaction and post-treatment to obtain a polymer product; and then the polymer product is placed in a Crystallization is induced in the poor solvent of the polymer product, and the crystalline polyester is obtained after drying. In the preparation method, a crystalline polyester is prepared by selecting a raw material monomer with a specific structure and a suitable catalytic system, and combining with an induced crystallization process after polymerization.

Description

technical field [0001] The invention belongs to the field of polymer material synthesis, and in particular relates to a preparation method of crystalline polyester and a product thereof. Background technique [0002] Isobutylene oxide (also known as methyl propylene oxide) is an important organic intermediate, which can be used to prepare more than 70 kinds of chemical products such as 2-methoxy-2-methyl-1-propanol and isobutylene sulfide. It can be used in the synthesis and production of polyether and medicine, and has great application value. It can be prepared by the epoxidation of olefins, and it can be directly used as a monomer to obtain high value-added polymer materials. However, compared with common epoxy compounds, the special structure of isobutylene oxide, especially two methyl substitutions , making it easy for cationic ring opening and difficult to copolymerize with other monomers. [0003] As early as 1988, some literature (Vysokomol.soyed.A30:No.8,1766-1770...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/58C08G63/42C08G63/682C08G63/84C08G63/82C08G63/83C08J3/00C08L67/02C08L67/06
CPCC08G63/42C08G63/58C08G63/6826C08G63/826C08G63/83C08G63/84C08J3/00C08J2367/02C08J2367/06
Inventor 张兴宏胡岚方曹晓瀚张旭阳
Owner ZHEJIANG UNIV
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