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A kind of preparation method of tetrahydrofuran copolyether

A technology of tetrahydrofuran copolyether and tetrahydrofuran, which is applied in the chemical industry

Active Publication Date: 2017-10-10
杭州师恩科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, it is mentioned in the literature that PTHF and PCL with a certain molecular weight are mixed in a certain proportion to prepare thermoplastic polyurethane elastomers. There are no literatures and patents that mention the two monomers of tetrahydrofuran and ε-caprolactone in the heteropolyacid system. Using 1,4 butanediol and water as an initiator, the method of copolymerization to generate diols with a certain molecular weight

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A preparation method of tetrahydrofuran copolyether, its preparation method is as follows:

[0031] (1) Premixing of ε-caprolactone and THF

[0032] ①Pre-mix ε-caprolactone and tetrahydrofuran with a mass ratio of 1:5 to obtain a mixture of tetrahydrofuran and ε-caprolactone, and control the water content in tetrahydrofuran to 0.0045% by mass; the antioxidant methyl in ε-caprolactone The mass percentage content of catechol should be less than or equal to 0.03%;

[0033] (2) Preparation of tetrahydrofuran copolyether

[0034] ① Prepare 22 cubic meters of reaction phase in the reaction kettle, the composition of the reaction phase is phosphotungstic acid and tetrahydrofuran with a mass ratio of 1:3, phosphotungstic acid contains 6 crystal water, and the water content in tetrahydrofuran is 0.22% by mass;

[0035] ② Put the mixture of tetrahydrofuran and ε-caprolactone at a flow rate of 3000kg / h, 1,4 butanediol at a flow rate of 150kg / h, and water at a flow rate of 3kg / h ...

Embodiment 2

[0045] A preparation method of tetrahydrofuran copolyether, its preparation method is as follows:

[0046] (1) Premixing of ε-caprolactone and THF

[0047] ① Pre-mix ε-caprolactone and tetrahydrofuran with a mass ratio of 1:5 to obtain a mixture of tetrahydrofuran and ε-caprolactone, and control the water content in tetrahydrofuran to 0.0035% by mass; the antioxidant methyl in ε-caprolactone The mass percentage content of catechol should be less than or equal to 0.04%;

[0048] (2) Preparation of tetrahydrofuran copolyether

[0049] ① Prepare 29 cubic meters of reaction phase in the reaction kettle, the composition of the reaction phase is phosphotungstic acid and tetrahydrofuran with a mass ratio of 1:3, phosphotungstic acid contains 6 crystal water, and the water content in tetrahydrofuran is 0.22% by mass;

[0050] ② Put the mixture of tetrahydrofuran and ε-caprolactone at a flow rate of 3000kg / h, 1,4 butanediol at a flow rate of 150kg / h, and water at a flow rate of 3kg / h...

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Abstract

The present invention relates to a method for preparing tetrahydrofuran copolyether. The preparation method is (1) premixing ε-caprolactone and tetrahydrofuran (2) using tetrahydrofuran, 1,4 butanediol, ε-caprolactone, and water in hetero Preparation of tetrahydrofuran copolyether under the catalysis of polyacid (3) Extraction and purification of tetrahydrofuran copolyether; using phosphotungstic acid as heteropolyacid catalyst, the corrosion of equipment is extremely low; a kind of polyurethane elastomer with superior performance can be obtained The tetrahydrofuran copolyether material, under the premise of the target product molecular weight of 2000, the reaction yield can reach 25%, and the reaction selectivity can reach more than 97%.

Description

technical field [0001] The invention relates to a method for preparing tetrahydrofuran copolyether by using tetrahydrofuran, 1,4 butanediol, ε-caprolactone and water under the catalysis of heteropolyacid. The invention belongs to the technical field of chemical industry. Background technique [0002] Polytetrahydrofuran (PTHF), also known as polytetramethylene ether glycol,. It is mainly used as the soft segment of block polyurethane or block polyether polyester, and can be used as tires, transmission belts, gaskets, etc.; it can also be used in coatings, artificial leather, films, etc. It is the main raw material of polyurethane elastic fibers. It is prepared by cationic polymerization of tetrahydrofuran under acid-catalyzed conditions. [0003] Polyε-caprolactone diol (PCL), used in the preparation of polyurethane coatings, polyurethane elastomers, medical materials, etc., has excellent soft segment properties. The monomer ε-caprolactone is prepared by cationic polymeri...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/28C08G65/30
Inventor 吕涛
Owner 杭州师恩科技有限公司