Phthalic anhydride and epoxy compound copolymerization and sequence control method

An epoxy compound and sequence control technology, applied in the field of organic synthesis, can solve the problems of limiting the flexibility of the synthesis method block sequence and the diversity of block copolymer properties, to solve the problem of insufficient polymerization activity and controllability, and simple structure , the effect of simplifying the preparation method

Active Publication Date: 2019-05-21
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, the conventional method can only generate polyether first and regenerate polyester, which greatly limits the flexibility of the synthesis method and the diversity of block sequences and block copolymer properties.

Method used

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  • Phthalic anhydride and epoxy compound copolymerization and sequence control method
  • Phthalic anhydride and epoxy compound copolymerization and sequence control method
  • Phthalic anhydride and epoxy compound copolymerization and sequence control method

Examples

Experimental program
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Embodiment 1

[0035] In this example, the ring-opening copolymerization of phthalic anhydride and ethylene oxide is carried out by using p-phthalic acid as the initiator and the organic Lewis acid-base pair as the catalyst, and the amphiphilic ether ester block copolymer based on phthalic anhydride and ethylene oxide is prepared in one step . The specific operation is as follows:

[0036] Both tetrahydrofuran (THF) and ethylene oxide were used after water removal treatment. In an inert atmosphere, add 1 part of terephthalic alcohol and 100 parts of phthalic anhydride into a dry glass reactor, and add tetrahydrofuran to dissolve. Continue to add phosphazene base t-BuP containing 1 part 1 With 0.3 parts of tetrahydrofuran solution of triethylboron, stir and mix evenly. Add 1000 parts of dry ethylene oxide, seal the glass reactor and react at room temperature (20-25°C) for 18h. In this embodiment, the molar concentration of ethylene oxide is 7mol / L. After the polymerization reaction, it ca...

Embodiment 2

[0040] In this example, ring-opening copolymerization of phthalic anhydride and ethylene oxide is carried out by using water as an initiator and an organic Lewis acid-base pair as a catalyst, and an alternating copolymer based on phthalic anhydride and ethylene oxide is prepared in one step. The specific operation is as follows:

[0041] Both tetrahydrofuran (THF) and ethylene oxide were used after water removal treatment. In an inert atmosphere, add 1 part of pure water and 50 parts of phthalic anhydride into a dry glass reactor, and add tetrahydrofuran to dissolve. Continue to add t-BuP containing 0.05 parts of phosphazene base 1 With 0.01 parts of triethylboron in tetrahydrofuran solution, stir and mix evenly. Add 50 parts of dry ethylene oxide, seal the glass reactor and react at room temperature for 24h. In this embodiment, the molar concentration of ethylene oxide is 3 mol / L. After the reaction is completed, the reactor is opened, and the copolymerized product is take...

Embodiment 3

[0044] In this example, the ring-opening copolymerization of phthalic anhydride and ethylene oxide was carried out by using terephthalmic alcohol as the initiator and organic Lewis acid-base pair as the catalyst, and a random copolymer based on phthalic anhydride and ethylene oxide was prepared in one step. The specific operation is as follows:

[0045] Both tetrahydrofuran (THF) and ethylene oxide were used after water removal treatment. In an inert atmosphere, add 1 part of terephthalic alcohol and 100 parts of phthalic anhydride into a dry glass reactor, and add tetrahydrofuran to dissolve. Continue to add t-BuP containing 1 part of phosphazene base 1 With 5 parts of tetrahydrofuran solution of triethylboron, stir and mix evenly. Add 500 parts of dry ethylene oxide, seal the glass reactor and react at room temperature for 5h. In this embodiment, the molar concentration of ethylene oxide is 6 mol / L. After the reaction is completed, the reactor is opened, and the copolymer...

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Abstract

The invention belongs to the technical field of organic synthesis, and discloses a phthalic anhydride and epoxy compound copolymerization and sequence control method. the phthalic anhydride and an epoxy compound are added into a three-component metal-free catalysis initiating system to react to obtain a copolymer; and the three-component metal-free catalysis initiating system comprises a hydroxy compound, an organic base and triethylborine. The use level and the ratio of the various components in the catalysis initiating system are controlled, the copolymers having alternating, random, gradient, taper, and segmented sequential structures are obtained, and the proportion of the ingredients of a monomer unit and the molecular weight of the copolymer can be accurately controlled. The preparation method is simple, the limit of the traditional preparation means of the ester ether segmented copolymer that polyether is generated first and then polyester is generated is broken, and the segmented copolymer having the microphase separation behavior in a body and having the amphipathic micellization behavior in a (aqueous) solution is prepared in one step.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a method for copolymerization and sequence control of phthalic anhydride and epoxy compounds. Background technique [0002] A copolymer refers to a polymer containing two or more monomer units formed by two or more monomers participating in a polymerization reaction. Copolymers are often significantly different from the corresponding homopolymers in performance, so they are an important supplement to the latter and are widely used in various fields of scientific research and national economy. According to the sequence of monomer units, copolymers can be divided into alternating, random, gradient, tapered, block and graft copolymers, etc. The sequence of monomer units, that is, the sequence structure of the copolymer, is a decisive factor affecting the properties of the copolymer. Therefore, copolymerization, especially the synthesis of sequence-controlled ...

Claims

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Application Information

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IPC IPC(8): C08G63/66C08G65/26
Inventor 赵俊鹏李恒张广照
Owner SOUTH CHINA UNIV OF TECH
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