Preparation method of low terminal carboxyl PBT resin

A low-end carboxyl group and resin technology, which is applied in the field of preparation of low-end carboxyl polybutylene terephthalate resin, can solve the problems of reduced chip viscosity, yellow color, difficult control of carboxyl end groups, etc., and achieves the content of carboxyl end groups Low, fast response, good technical effect

Active Publication Date: 2020-05-01
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 terminal carboxyl group is not easy to control in the past PBT polymerization process, which leads to a decrease in the viscosity of the slice and a yellowish color, thereby affecting the quality of the PBT resin.

Method used

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  • Preparation method of low terminal carboxyl PBT resin
  • Preparation method of low terminal carboxyl PBT resin
  • Preparation method of low terminal carboxyl PBT resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Preparation of Catalyst A

[0050]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.

[0051] Place the dried white powdery substance in a reactor with agitator, condenser and thermometer, add 90 grams of 1,4-butanediol, 63 grams of citric acid monohydrate (0.3 mol), 107 grams of magnesium acetate (0.5 mol) was reacted for 2 hours at a reaction temperature of 150° C. to obtain a nearly colorless homogeneous liquid, which was diluted with butanediol to a titanium content of 3%, which was Catalyst A.

[0052] Preparation of polyester

[0053] With 600 grams of terephthalic acid and 520 grams of 1,4-buta...

Embodiment 2

[0056] 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).

[0057] The test results are shown in Table 1.

Embodiment 3

[0059] 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 100 ppmw).

[0060] The test results are shown in Table 1.

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Abstract

The invention relates to a preparation method of low terminal carboxyl PBT resin. In the prior art, the terminal carboxyl group is not easy to control during the PBT polymerization process, the viscosity of slices is reduced, the color becomes yellow, and thus the quality of PBT resin is influenced. The preparation method of the low terminal carboxyl PBT resin is adopted, and a catalyst obtained after reaction of the following raw materials is adopted to prepare the low terminal carboxyl PBT resin: (1) a titanium compound Ti(OR)4 with a general formula shown in the specification; (2) diol B having 2 to 10 carbon atoms; (3) a metal compound C selected from the periodic table IIA of elements; and (4) at least one aliphatic organic acid D. Refined terephthalic acid and 1,4-butanediol are taken as raw materials, the catalyst is added to carry out reactions to obtain the low terminal carboxyl PBT (polybutylene terephthalate) resin, the problems mentioned above are solved, and the preparation method can be applied to industrial production of PBT.

Description

technical field [0001] The invention relates to a preparation method of low-end carboxyl 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, tetraisopr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/183C08G63/85
CPCC08G63/183C08G63/85
Inventor 关震宇王睿章瑛虹熊金根
Owner CHINA PETROLEUM & CHEM CORP
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