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A kind of phosphorus-titanium composite polyester catalyst and its preparation process

A composite polyester and catalyst technology, applied in the field of phosphorus-titanium composite polyester catalyst and its preparation technology, can solve the problems of yellowing, side reactions, molecular chain breakage and the like

Active Publication Date: 2020-06-30
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

[0024] A kind of preparation method of phosphorus-titanium composite polyester catalyst, it comprises the steps:

[0025] 1) React β-methylepichlorohydrin with tri-n-propyl phosphite in a molar ratio of 1:1 under the protection of an inert gas at 180°C for 2 h, and then obtain the retained product A by distillation under reduced pressure 1 ;

[0026] 2) Will retain product A 1 Soluble in water, react at 1 atmospheric pressure and 98 °C for 3.5 h, remove water to obtain product B 1 ;

[0027] 3) Dissolve tetrabutyl titanate in anhydrous n-hexane, then add product B 1 , stirred and reacted at 30 °C for 4 h, and distilled under reduced pressure to obtain a solid product, which is the phosphorus-titanium composite polyester catalyst I; titanate and product B 1 The reaction feed molar ratio is 1:2.

Embodiment 2

[0029] 1) React epichlorohydrin and diethyl methylphosphonite at a molar ratio of 1:4 under the protection of an inert gas at 115 °C for 6.5 h, and then obtain the retained product A by vacuum distillation 2 ;

[0030] 2) Will retain product A 2 Soluble in water, react at 2 atmospheres and 120°C for 3 h, remove water to obtain product B 2 ;

[0031] 3) Dissolve tetrabutyl titanate in anhydrous n-hexane, then add product B 2 , stirred and reacted at 0 ℃ for 6 h, and distilled under reduced pressure to obtain a solid product, which is the phosphorus-titanium composite polyester catalyst II; titanate and product B 2The reaction feed molar ratio is 1:4.

Embodiment 3

[0033] 1) React β-methylepichlorohydrin with triethyl phosphite at a molar ratio of 1:1.5 at 150°C for 4 h under the protection of an inert gas, and then obtain the retained product A by distillation under reduced pressure 3 ;

[0034] 2) Will retain product A 3 Soluble in water, react at 1 atmosphere and 80 °C for 7 h, remove water to obtain product B 3 ;

[0035] 3) Dissolve tetrabutyl titanate in anhydrous n-hexane, then add product B 3 , stirred and reacted at 60 °C for 2 h, and distilled under reduced pressure to obtain a solid product, namely phosphorus-titanium composite polyester catalyst III; titanate and product B 3 The reaction feed molar ratio is 1:3.

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PUM

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Abstract

The invention discloses a phosphor-titanium composite polyester. The molecular formula of the phosphor-titanium composite polyester 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 bonded through titanium-oxygen bonds; the structures of the chelate rings are similar or dissimilar, and the chelate rings are independently selected from any one from five-membered ring to octatomic ring, the structures of the phosphonate substituent groups are similar or dissimilar, and the phosphonate substituent groups are located on any of the chelate rings and connected with the chelate ring through any one of aliphatic series alkylene from C1 to C7; and the substituent site of alkylene connected with phosphonate group on the chelate ring is random. The prepared catalyst has the excellent catalytic activity and selectivity in addition to excellent hydrolysis resistance and the dispersity in ethylene glycol, thermal degradation in the polycondensation process can be reduced when the titanium-containing catalyst is utilized for preparing a polyester product, and the prepared polyester product has the advantages of being low in b value, low in carboxyl group content and stable in catalysis effect.

Description

technical field [0001] The invention relates to the field of polyester synthesis technology, in particular to a phosphorus-titanium composite polyester catalyst 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 and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/85
CPCC08G63/85
Inventor 孙芳刘斌刘洪春刘永滨张慧书
Owner 福建锦兴环保科技有限公司