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Preparation method and application of titanium phosphorus catalyst for polyester synthesis

A catalyst and polyester technology, applied in the production of bulk chemicals, etc., can solve the problems of unsatisfactory hue and various indicators, etc.

Active Publication Date: 2021-08-31
ZHEJIANG TONGKUN NEW MATERIALS RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although some titanium-based composite catalysts with ligands have been industrialized to a certain extent, the hue and various indicators of the synthesized polyester are still not ideal and need to be further improved and improved.

Method used

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  • Preparation method and application of titanium phosphorus catalyst for polyester synthesis

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preparation example Construction

[0028] Catalyst preparation:

[0029] Dissolve fatty alkyltrimethylammonium halide in deionized water, stir vigorously until a uniform and stable solution is formed; and dissolve titanium compound and phosphorus compound in the above mixed solution at a molar ratio (1:9~9:1) , continuously stirred and reacted at 20-200°C for 1.0-72.0h; filtered the obtained mixed solution, and roasted the solid at 300-800°C for 0.5-8.0h, then washed the roasted product repeatedly with water, dried in vacuum at room temperature, After crushing and grinding, the titanium phosphorus catalyst is obtained.

[0030] Wherein, the titanium compound is at least one of titanium tetrachloride, titanium tetrabromide and titanate compounds. Wherein, the titanate compound has the general formula of Ti(OR)4, and R is an alkyl group with 1-10 carbon atoms.

[0031] The phosphorus compound is at least one of phosphoric acid, polyphosphoric acid, phosphorus pentoxide, phosphorus trichloride and pyrophosphoric...

Embodiment 1

[0037] Catalyst preparation:

[0038] Dissolve 16.5g of octadecyltrimethylammonium bromide in 150ml of deionized water, stir vigorously until a uniform and stable solution is formed; then add phosphoric acid and titanium tetrachloride to the above mixed solution at a molar ratio of 1:1, first Add 9.8 g (0.10 mol) of phosphoric acid, and add 18.9 g (0.10 mol) of titanium tetrachloride under continuous stirring. After continuous stirring for 1.0 h, react at 150 ° C for 48.0 h; roast the resulting mixed solution at 400 ° C for 5.0 h, then the product is filtered out, washed 3 times with deionized water, and vacuum-dried, pulverized and ground at room temperature to obtain a titanium phosphorus catalyst for polyester;

[0039] Synthesis of polyester:

[0040]333.3g purified terephthalic acid, 160g ethylene glycol and titanium phosphorus catalyst 0.13g (10ppm) are added in the 1L reactor, and carry out esterification, precondensation and final polycondensation successively under n...

Embodiment 2

[0042] Catalyst preparation:

[0043] Dissolve 16.5g of cetyltrimethylammonium bromide in 150ml of deionized water and stir vigorously until a uniform and stable solution is formed; then add phosphoric acid and titanium tetrachloride to the above mixed solution at a molar ratio of 0.9:1.1, first Add 8.82g (0.09mol) of phosphoric acid, and add 20.79g (0.11mol) of titanium tetrachloride under continuous stirring, after continuous stirring for 1.0h, react at 50°C for 72.0h; roast the resulting mixed solution at 500°C for 7.0 h, then the product is filtered out, washed 3 times with deionized water, and vacuum-dried, pulverized and ground at room temperature to obtain a titanium phosphorus catalyst for polyester;

[0044] Synthesis of polyester:

[0045] 333.3g purified terephthalic acid, 160g ethylene glycol and titanium phosphorus catalyst 0.06g (5ppm) are added in the 1L reactor, and carry out esterification, precondensation and final polycondensation successively under nitroge...

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Abstract

The invention belongs to the field of polyester synthesis, and relates to a preparation method and application of a titanium-phosphorus catalyst for polyester synthesis. The preparation method comprises the following steps: dissolving fatty alkyl trimethyl ammonium halide in deionized water, and stirring to form a uniform and stable solution; dissolving a phosphorus compound and a titanium compound in the mixed solution according to a certain molar ratio of (1: 9)-(9: 1), continuously stirring, reacting at a constant temperature for 1.0-48.0 hours, and roasting a solid filtered out from the mixed solution at a high temperature; and finally, filtering, washing, drying in vacuum, crushing and grinding to obtain the titanium phosphorus catalyst for polyester. The performance of the catalyst is regulated and controlled by regulating and controlling the molar ratio of the titanium compound to the phosphorus compound. When the catalyst is used for polyester synthesis, the result shows that the catalyst can effectively catalyze transesterification in the polyester synthesis step, and meanwhile, side reactions are remarkably reduced, and the polyester hue is improved.

Description

technical field [0001] The invention relates to the technical field of catalyst and polyester synthesis, in particular to a preparation method and application of a titanium phosphorus catalyst used for polyester synthesis. Background technique [0002] With the rapid economic development, polyester and its related products have become one of the world's largest production, most widely used and fastest growing polymer products. At present, antimony-based catalysts are still the most widely used catalysts in the polyester industry. Since antimony is a heavy metal, its use will cause environmental pollution. Therefore, finding a green catalyst that can replace antimony has become an urgent problem in the industry. [0003] Antimony-free catalysts can be divided into three categories: titanium-based, germanium-based and aluminum-based catalysts. Germanium-based catalysts have high activity, but germanium resources are scarce and expensive, and the application field is severely...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/183C08G63/85C08G63/87
CPCC08G63/85C08G63/87C08G63/183Y02P20/52
Inventor 李圣军唐越超赵晨霞
Owner ZHEJIANG TONGKUN NEW MATERIALS RES INST CO LTD
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