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A kind of titanium series catalyst for polyester and its preparation process

A titanium-based catalyst and preparation technology, applied in the field of polyester synthesis technology, can solve the problems of molecular chain breakage, short shelf life, poor solubility, etc.

Active Publication Date: 2020-09-25
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

[0028] A kind of preparation method of titanium series catalyst for polyester, it comprises the steps:

[0029] 1) Glyceryl chlorinated acetone and triethyl phosphite in a molar ratio of 1:1 were stirred and reacted at 150°C for 4 hours under the protection of nitrogen to obtain a crude product, and then the crude product was cooled to room temperature and distilled to obtain the retained product A 1 ;

[0030] 2) will retain the product A 1 Dissolve in 20mL of acetic acid-water mixed solution with a mass ratio of 7:3, then stir and react at 40°C for 9h, then distill off the acetic acid and water in the mixture under reduced pressure to obtain product B 1 ;

[0031]3) Dissolve tetrabutyl titanate in 30 mL of anhydrous cyclohexane, then add 1,3-propanediol and react at 80°C for 1 hour to obtain a crude product, which is distilled to obtain the retained product C 1 ; Wherein, the molar ratio of organic titanate and 1,3 propanediol is 1:1.25;

[0032] 4) will retain the produ...

Embodiment 2

[0034] 1) Glyceryl chlorinated acetone and triethyl phosphite in a molar ratio of 1:5 were stirred and reacted at 105°C under the protection of nitrogen for 7.5 hours to obtain a crude product, and then the crude product was cooled to room temperature and distilled to obtain the retained product A 2 ;

[0035] 2) will retain the product A 2 Dissolve in 20mL of acetic acid-water mixed solution with a mass ratio of 7:3, then stir and react at 60°C for 3h, then distill off the acetic acid and water in the mixture under reduced pressure to obtain product B 2 ;

[0036] 3) Dissolve tetrabutyl titanate in 30 mL of anhydrous cyclohexane, then add ethylene glycol and react at 60°C for 2 hours to obtain a crude product, which is distilled to obtain the retained product C 2 ; Wherein, the molar ratio of organic titanate and ethylene glycol is 1:1.5;

[0037] 4) will retain the product C 2 Dissolve in 40 mL of anhydrous cyclohexane, then add product B 2 React at 40°C for 5 hours to ...

Embodiment 3

[0039] A kind of preparation method of titanium series catalyst for polyester, it comprises the steps:

[0040] 1) Glyceryl chlorinated acetone and triethyl phosphite in a molar ratio of 1:2.5 were stirred and reacted at 80°C for 15 hours under the protection of nitrogen to obtain a crude product, and then the crude product was cooled to room temperature and distilled to obtain the retained product A 3 ;

[0041] 2) will retain the product A 3 Dissolved in 20mL of acetic acid-water mixed solution with a mass ratio of 7:3, then stirred and reacted at 25°C for 12h, then distilled off the acetic acid and water in the mixture under reduced pressure to obtain product B 3 ;

[0042] 3) Dissolve tetrabutyl titanate in 30 mL of anhydrous cyclohexane, then add 1,2-propanediol and react at 45°C for 4 hours to obtain a crude product, which is distilled to obtain the retained product C 3 ; Wherein, the molar ratio of organic titanate and 1,2-propylene glycol is 1:0.8;

[0043] 4) will...

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PUM

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Abstract

The invention discloses a titanium-based catalyst for polyester. The molecular formula of the titanium-based catalyst contains a central titanium atom, a phthalate-substituted group and one or more chelate rings; the chelate rings are bonded with the central titanium atom through titanium-oxygen bonds; the structures of the chelate rings are same or different, and are separately selected from anyone of a four-membered ring to an eight-membered ring; the phthalate-substituted group is positioned on any chelate ring and is connected with the corresponding chelate ring through any alkylidene group of C1-C4; and the substitution site of alkylidene group linking to the phthalate group is arbitrary. The catalyst has the advantages of no toxicity, no harm, low usage amount and stable catalytic performance, and the activity of the catalyst is much higher than the activity of antimony-based catalysts. When the titanium-based catalyst is used for preparing a polyester product, the usage amountof the catalyst is low, the residual amount is low, the influence on subsequent processing of the polyester is small, and the prepared polyester product has the advantages of low b-value, low contentof terminal carboxyl groups and high intrinsic viscosity. The catalyst provided by the invention is a titanium-based catalyst with excellent comprehensive performance.

Description

technical field [0001] The invention relates to the field of polyester synthesis technology, in particular to a titanium-based 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, referred to as EG) as a raw material, through direct esterification (directesterification) and polycondensation (polycondensation) two-step synthesis. 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 titanium. Among them, titanium-b...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/183C08G63/85
CPCC08G63/183C08G63/85
Inventor 刘永滨刘洪春王文立乔玥孙芳刘斌
Owner 福建锦兴环保科技有限公司