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Phosphorus-titanium composite catalyst used for polyester and preparation process of composite catalyst

A composite catalyst and preparation process technology, which is applied in the field of phosphorus-titanium composite catalyst for polyester and its preparation process, and can solve problems such as side reactions, molecular chain breaks, and poor solubility

Active Publication Date: 2018-10-12
福建锦兴环保科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the high activity of such catalysts, more side reactions are often caused, and the molecular chains are broken, resulting in unsatisfactory viscosity of the obtained polyester chips and serious yellowing caused by thermal degradation.
In addition, the dihydric alcohol complexes of titanium are mostly solid, and their solubility is poor, so there are certain difficulties in preparing the slurry
Liquid titanium-based catalysts can avoid dissolution difficulties, but most of the reported liquid titanium-based catalysts are required to be stored away from light and humidity, and the shelf life is shorter than that of solid catalysts

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A kind of preparation method of phosphorus-titanium composite catalyst for polyester, it comprises the following steps:

[0026] 1) React chloroacetone glycidyl and trimethyl phosphite at a molar ratio of 1:2 at 130-135 °C for 4 h under the protection of an inert gas, and then obtain the retained product A by distillation under reduced pressure;

[0027] 2) Dissolve the remaining product A in 70% acetic acid-water mixed solution, stir and react at 10 °C for 12 h, distill off the acetic acid and water in the solution to obtain a crude product; the crude product is purified to obtain product B;

[0028] 3) Dissolve tetraisopropyl titanate in anhydrous n-hexane, then add product B, stir and react at 70 °C for 1 h, and distill under reduced pressure to obtain a solid product, which is the phosphorus-titanium composite catalyst for polyester; titanic acid The reaction feed molar ratio of tetraisopropyl ester and product B is 1:1.5.

Embodiment 2

[0030] A kind of preparation method of phosphorus-titanium composite catalyst for polyester, it comprises the following steps:

[0031] 1) React chloroacetone glycidyl and triethyl phosphite at a molar ratio of 1:4 at 120-125 °C for 5.5 h under the protection of an inert gas, and then obtain the retained product A by vacuum distillation;

[0032]2) Dissolve the remaining product A in 70% acetic acid-water mixed solution, stir and react at 60 °C for 5 h, distill off the acetic acid and water in the solution to obtain a crude product; obtain product B after purification;

[0033] 3) Dissolve tetrabutyl titanate in anhydrous n-hexane, then add product B, stir and react at 10 °C for 7 h, and distill under reduced pressure to obtain a solid product, which is the phosphorus-titanium composite catalyst for polyester; The molar ratio of butyl ester to product B is 1:4.

Embodiment 3

[0035] A kind of preparation method of phosphorus-titanium composite catalyst for polyester, it comprises the following steps:

[0036] 1) React chloroacetone glycidyl and trimethyl phosphite at a molar ratio of 1:6 at 80-85 °C for 8 h under the protection of an inert gas, and then obtain the retained product A by vacuum distillation;

[0037] 2) Dissolve the remaining product A in 30% phosphoric acid-water mixed solution, stir and react at 25 °C for 8 h, distill off the water in the solution, neutralize phosphoric acid with sodium bicarbonate, and filter to remove phosphate to obtain crude product; After the crude product is purified, product B is obtained;

[0038] 3) Dissolve tetrabutyl titanate in anhydrous petroleum ether, then add product B, stir and react at 30 °C for 5 h, and distill under reduced pressure to obtain a solid product, which is the phosphorus-titanium composite catalyst for polyester; The molar ratio of butyl ester to product B is 1:2.

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PUM

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Abstract

The invention discloses a phosphorus-titanium composite catalyst used for polyester. The composite catalyst has a central titanium atom, at least two phosphonate substituent groups and at least two chelate rings; the chelate rings and the central titanium atom are linked through a titanium oxygen bond; structures of the chelate rings are same or different, and the chelate rings are independently selected from a four-membered ring to an eight-membered ring; structures of the phosphonate substituent groups are same or different, and the phosphonate substituent groups are located in any chelate rings and connected with the chelate rings through C1-C4 aliphatic alkylidene; and a substituted site of the alkylidene connected with the phosphonate groups on the rings is optional. The catalyst provided by the invention has excellent catalytic activity and selectivity in addition to good hydrolysis resistance and dispersibility in ethylene glycol, when the titanium catalyst is utilized to prepare a polyester product, thermal degradation in the polycondensation process can be reduced, and the prepared polyester product has the advantages of a low b value, low terminal carboxyl content, and high intrinsic viscosity, and is a titanium catalyst with excellent comprehensive performance.

Description

technical field [0001] The invention relates to the field of polyester synthesis technology, in particular to a phosphorus-titanium composite catalyst for polyester and a preparation process thereof. Background technique [0002] Polyethylene terephthalate (PET) is the most important type of polyester fiber. The synthesis process of its slices is usually based on pure terephthalic acid (PTA) and ethylene glycol. Alcohol (Ethylene glycol, EG for short) is used as a raw material, and it is synthesized by a two-step method of direct esterification (directesterification) and polycondensation (polycondensation). Among them, the esterification reaction can be catalyzed by the acidity of terephthalic acid itself, while the polycondensation reaction needs to add a catalyst to promote molecular weight growth. At present, the catalysts for polycondensation that have been studied more are classified according to the active center, and there are mainly three types: antimony, germanium ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/183C08G63/85C08G63/87
CPCC08G63/183C08G63/85C08G63/87
Inventor 刘洪春刘永滨李伟张慧书孙芳刘斌
Owner 福建锦兴环保科技有限公司