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Polybutylene terephthalate resin preparation method

A technology of polybutylene terephthalate and terephthalic acid, which is applied in the field of preparation of polybutylene terephthalate resin, and can solve the problems of not being able to well suppress tetrahydrofuran and high production of tetrahydrofuran

Active Publication Date: 2019-04-23
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is that the generation of tetrahydrofuran cannot be well suppressed by using titanium series catalysts in the PBT polymerization process in the past, resulting in a higher problem of tetrahydrofuran generation, and a new polybutylene terephthalate resin is provided. Preparation

Method used

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  • Polybutylene terephthalate resin preparation method
  • Polybutylene terephthalate resin preparation method
  • Polybutylene terephthalate resin preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Preparation of Catalyst A

[0046] Add 12.4 grams (0.2 mol) of ethylene glycol in the reactor that stirrer, condenser and thermometer are equipped with, slowly drop into reactor 28.4 grams (0.1 mol) tetraisopropyl titanate, separate out white precipitate, After reacting at 70°C for 2 hours, the product was centrifuged, and the residue was washed with distilled water three times, and the product was vacuum-dried at 70°C to obtain a white powdery substance.

[0047] Place the dried white powdery substance in a reactor with a stirrer, a condenser and a thermometer, add 90 grams of 1,4-butanediol, 126 grams (0.6 moles) of citric acid monohydrate, and react at 150 ° C After reacting at high temperature for 2 hours, a nearly colorless homogeneous liquid was obtained, which was Catalyst A.

[0048] Preparation of polyester

[0049] With 600 grams of terephthalic acid and 520 grams of 1,4-butanediol and catalyst A (based on the amount of polyester produced, the weight of tita...

Embodiment 2

[0052]The polyester was prepared in the same manner as in Example 1, except that catalyst A was changed (based on the amount of polyester produced, the weight of titanium atoms was changed to 60 ppmw).

[0053] The test results are shown in Table 1.

Embodiment 3

[0055] The polyester was prepared in the same manner as in Example 1, except that the catalyst A was changed (based on the amount of polyester produced, the weight of titanium atoms was changed to 80 ppmw).

[0056] The test results are shown in Table 1.

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Abstract

The invention relates to a polybutylene terephthalate resin preparation method. In the prior art, the PBT polymerization uses the titanium-based catalyst so as not to well inhibit the generation of tetrahydrofuran, such that the generation amount of tetrahydrofuran is high. A purpose of the present invention is mainly to solve the problem in the prior art. According to the technical scheme, the polybutylene terephthalate resin preparation method comprises: carrying out an esterification reaction by using terephthalic acid and 1,4-butanediol as raw materials and using a titanium-based polyestercatalyst to obtain a prepolymer, and carrying out a melt condensation polymerization reaction to obtain the polybutylene terephthalate resin product, wherein the used catalyst is the reaction productof the following raw materials: 1) a titanium compound A, 2) C2-C10 diol B, and 3) at least an aliphatic organic acid C selected from organic acids. With the technical scheme, the problem in the prior art is well solved. The product of the present invention can be used in the industrial production of polybutylene terephthalate resins.

Description

technical field [0001] The invention relates to a preparation method of polybutylene terephthalate resin. Background technique [0002] Polybutylene terephthalate (PBT) is a thermoplastic polyester formed by polycondensation of terephthalic acid (PTA) or methyl terephthalate and butanediol (BDO), which is easy to process, good high temperature resistance , moisture resistance, oil resistance and other properties, have been widely used in automobiles, machinery, instruments, electrical and electronic, household appliances, textile and civil and other fields. [0003] The synthesis process of PBT mainly includes transesterification and direct esterification, and with the emergence of high-purity PTA and the development of efficient catalysts for direct esterification, direct esterification has become the main way of PBT production. At present, the commonly used catalysts for PBT synthesis are organic titanate compounds, such as tetrabutyl titanate, tetraisopropyl titanate, et...

Claims

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Application Information

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IPC IPC(8): C08G63/183C08G63/85
CPCC08G63/183C08G63/85
Inventor 关震宇周文乐熊金根章瑛虹
Owner CHINA PETROLEUM & CHEM CORP