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Antimony/ titanium composite catalyst and application thereof in method for preparing polyethylene glycol terephthalate (PET) copolyesters

A technology of composite catalyst and titanium catalyst, which is applied in the field of highly active antimony/titanium composite catalyst, can solve the problems of large amount of antimony-based catalysts, decreased thermal stability of polyester, and easy graying of products, etc., and achieves the prevention of graying of products, Good thermal stability and low dosage

Active Publication Date: 2012-08-01
MATRIX GUANGZHOU CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is that the amount of antimony-based catalysts in the prior art is large, and the products are prone to graying; the titanium-based catalysts are likely to cause yellowing of the products and reduce the thermal stability of polyester

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Slowly add butyl titanate into ethylene glycol at 70 °C, the molar concentration of butyl titanate is 1.0 mol / L, stir until the mixture is uniform, and under the condition of continuously feeding nitrogen, heat up to 190 °C, and continue After stirring for 12 hours, antimony acetate was added, and after stirring evenly, it was stored at 50° C. for later use, and it was named as catalyst A.

[0020] Dimethyl terephthalate 3880g, ethylene glycol 2400g, polyethylene glycol 8000 310g, catalyst A (based on the amount of generated polymer, the amount of titanium is 15ppm, the amount of antimony is 150ppm), added to the reaction kettle, Under the protection of nitrogen, the temperature in the reactor was maintained at 180 °C, and the reaction was carried out for 100 minutes. Then, 300 ppm of triphenyl phosphite and 50 ppm of di(tetradecyl) thiodipropionate were added. The temperature was raised to 270 °C, and a vacuum was gradually established. The pressure in the reactor was ...

Embodiment 2

[0023] Slowly add isopropyl titanate into ethylene glycol at 70°C, the molar concentration of butyl titanate is 2.0mol / L, stir until the mixture is uniform, and heat up to 190°C under the condition of continuously feeding nitrogen, Continue stirring for 12 hours. Add antimony trioxide, stir evenly, and store at 50°C for later use. Named catalyst B.

[0024] 3880g of dimethyl terephthalate, 2400g of ethylene glycol, 155g of polytetrahydrofuran 2000, catalyst B (based on the amount of the generated polymer, the amount of titanium is 35ppm, the amount of antimony is 100ppm) are added to the reaction kettle, nitrogen protection The temperature in the reactor was maintained at 180° C., and the reaction was performed for 80 minutes. Then add 300 ppm of triphenyl phosphate, 50 ppm of di(dodecyl) thiodipropionate, and heat up to 270 o C, and gradually establish a vacuum, reduce the pressure in the reactor to 60Pa within 45 minutes, and react for 1.5 hours. Filled with nitrogen to ...

Embodiment 3

[0027] Slowly add isopropyl titanate to ethylene glycol at 70 °C, the molar concentration of butyl titanate is 1.5 mol / L, stir until the mixture is uniform, and under the condition of continuously feeding nitrogen, the temperature is raised to 190 °C, Continue stirring for 12 hours. Ethylene glycol antimony was added, stirred evenly, and stored at 50°C for later use. Named catalyst C.

[0028] 3880g of dimethyl terephthalate, 2400g of ethylene glycol, 246g of polyethylene glycol 2000, catalyst C (based on the amount of the generated polymer, the amount of titanium is 50ppm, and the amount of antimony is 70ppm) are added to the reaction kettle, The temperature in the reactor was maintained at 180° C. under nitrogen protection, and the reaction was performed for 80 minutes. Then add 150ppm of trimethyl phosphate and 20ppm of di(tridecyl)thiodipropionate, heat up to 270°C, and gradually establish a vacuum, reduce the pressure in the reactor to 60Pa within 45 minutes, and react ...

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Abstract

The invention discloses a high-activity antimony / titanium composite catalyst, which contains the following components: 1 antimony catalysts, 2 titanium catalysts, 3 first catalyst promoters and 4 second catalyst promoters, wherein the antimony catalysts are oxides and salts of antimony, the titanium catalysts are titanates, the first catalyst promoters are phosphoric acids, phosphorous acids and alkyl groups and / or polyaryl ethers of the phosphorous acids, and the second catalyst promoters are benzothiodiazoles. The antimony / titanium composite catalyst can be used in a method for preparing polyethylene glycol terephthalate (PET) copolyesters, which includes the following steps: 1 mixing and adding the antimony / titanium catalyst, the first catalyst promoters, the second catalyst promoters and binary acids into a reaction system, 2 leading the terephthalic acids, esters of the terephthalic acids and excess ethylene glycol to together perform an esterification reaction at temperature of 240-260 DEG C, at pressure of 0.2-0.4MPa and with reaction time of 1-2 hours, and 3 adding copolymerization glycol monomers for a polycondensation reaction to obtain the copolyesters. The antimony / titanium composite catalyst and the application thereof in the method for preparing the PET copolyesters have the advantages that the catalyst can activate the antimony series catalyst and shortens polycondensation time, and the problem of decreasing of polyester heat stability due to the fact that the antimony series catalyst is apt to yellow products is solved.

Description

technical field [0001] The invention relates to a high-activity antimony / titanium composite catalyst, and also relates to the application of the high-activity antimony / titanium composite catalyst in PET copolyester. Background technique [0002] Antimony trioxide or antimony acetate are generally used as catalysts in polyester production. Although the properties of the polyester products prepared by them, such as viscosity and color, can meet the requirements of general-purpose polyesters, there are still some shortcomings: 1. During the polycondensation process, Sb 3+ It is reduced to metal antimony, which makes the product gray; 2. The amount of antimony catalyst added is relatively large, generally 150~300ppm. Germanium-based catalysts have good stability, cause fewer side reactions in the reaction, and the obtained polyester has a good hue, but due to the lack of resources, the price is expensive; titanium-based catalysts have high activity, but titanium-based catalysts ...

Claims

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Application Information

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IPC IPC(8): C08G63/86C08G63/183C08G63/672
CPCC08G63/672C08G63/86C08G63/85C08G63/183
Inventor 赵巍蔡彤旻曾祥斌徐依斌苑仁旭焦建钟宇科
Owner MATRIX GUANGZHOU CHEM CORP
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