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Method for preparing biodegradable polyester catalyst

A technology of biodegrading polyester and catalyst, applied in the field of polymer materials, can solve the problems of yellowish color and poor transparency of the product, and achieve the effect of good hue

Active Publication Date: 2012-09-05
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the problem of this catalyst is that the color of the prepared product is yellow and the transparency is relatively poor.

Method used

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  • Method for preparing biodegradable polyester catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Preparation of Catalyst A

[0031] Add 18.9 g (0.1 mol) of titanium tetrachloride into a reactor equipped with a stirrer, then dilute with a certain amount of distilled water until no white smoke is generated, and mix well. Add cobaltous chloride 0.39g (0.003mol) in this solution again, stir and dissolve for 2 hours, adjust its pH with ammonia water to be 11, then precipitate and age for 8 hours, filter, and wash with distilled water until the solution does not contain chloride ions (with 0.1mol / L silver nitrate solution), dried, and calcined at 600°C for 4 hours to obtain a titania-cobalt oxide carrier. In a reactor equipped with a stirrer, a condenser and a thermometer, add 34g (0.1mol) of n-butyl titanate, 1.32g (0.005mol) of ethylpropyl orthosilicate, and 0.326g (0.001mol) of triphenyl phosphate The reaction was carried out at 150° C. for 3 hours. Titanium compound B was obtained. Then, 7.8 g of titanium compound B was added to the titanium dioxide-cobalt oxide c...

Embodiment 2

[0036] Preparation of Catalyst B

[0037] Add 18.9 g (0.1 mol) of titanium tetrachloride into a reactor equipped with a stirrer, then dilute with a certain amount of distilled water until no white smoke is generated, and mix well. Add aluminum trichloride 0.4g (0.003mol) in this solution again, stir and dissolve 2 hours, adjust its pH with ammoniacal liquor to be 11, then precipitate and age for 8 hours, filter, and wash with distilled water until the solution does not contain chloride ions ( Use 0.1mol / L silver nitrate solution to detect), dry, and bake at 600°C for 4 hours to obtain a titanium dioxide-alumina carrier. In the reactor equipped with stirrer, condenser and thermometer, add 28.4g (0.1mol) of tetraisopropyl titanate, 1.60g (0.005mol) of n-butyl silicate, 0.326g (0.001mol) of triphenyl phosphate ) was reacted at 150° C. for 3 hours. Titanium compound B was obtained. Then, 7.8 g of titanium compound B was added to the titanium dioxide-alumina carrier, refluxed fo...

Embodiment 3

[0042] Preparation of Catalyst C

[0043] Add 18.9 g (0.1 mol) of titanium tetrachloride into a reactor equipped with a stirrer, then dilute with a certain amount of distilled water until no white smoke is generated, and mix well. Add nickel chloride 0.71g (0.003mol) in this solution again, stir and dissolve for 2 hours, adjust its pH with ammoniacal liquor to be 11, then precipitate and age for 8 hours, filter, and wash with distilled water until the solution does not contain chloride ions (with 0.1mol / L silver nitrate solution), dried, and calcined at 600° C. for 4 hours to obtain a titania-nickel oxide carrier. In a reactor equipped with a stirrer, a condenser and a thermometer, add 22.8g (0.1mol) of tetraethyl titanate, 0.76g (0.005mol) of tetramethyl silicate, and 0.326g (0.001mol) of triphenyl phosphate The reaction was carried out at 150° C. for 3 hours. Titanium compound B was obtained. Then, 7.8 g of titanium compound B was added to the titanium dioxide-nickel oxid...

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Abstract

The invention relates to a method for preparing a biodegradable polyester catalyst and an application, belonging to the field of polymer materials. The method comprises the steps of adopting reaction products of a titanium compound, a silicon compound, a phosphorus compound and a metal compound as raw materials, leading the titanium compound to be reacted with water for obtaining the titanium compound A, leading the titanium compound A to be reacted with the metal compound at the reaction temperature of 0-120 DEG C, and using ammonia for regulating pH value; aging, filtering, washing, then calcining at the temperature of 500-1000 DEG C, and obtaining a titanium dioxide-metal oxide carrier; leading the titanium compound, the silicon compound and the phosphorus compound to react at the reaction temperature of 0-100 DEG C, and obtaining the titanium compound B; and adding the titanium dioxide-metal oxide carrier into 10-20% of ethanol solution of the titanium compound B, suction-filtering, drying and obtaining the composite catalyst. Aliphatic diacid and diol are taken as raw materials, and a polyester product is obtained by esterification and polycondensation routes. Compared with polyester prepared by the traditional catalyst-n-butyl titanate, the adoption of the catalyst can greatly improve the shear viscosity of the polyester and shorten the polymerization time.

Description

technical field [0001] The invention relates to a preparation method of a biodegradable polyester catalyst and a process method of biodegradable aliphatic polyester PBS prepared by using the catalyst, belonging to the technical field of polymer materials. Background technique [0002] In recent years, biodegradable polymer materials have attracted extensive attention from academia and industry due to their environmental friendliness and biomedical applications. Among them, aliphatic polyester is currently one of the most important biodegradable materials. Mainly used in agriculture, packaging, fiber and biomedicine and other fields. Among aliphatic polyesters, polybutylene succinate (PBS) has become a research hotspot due to its excellent comprehensive properties and good industrialization prospects. It is generally prepared by polycondensation of aliphatic diols and dibasic acids. Compared with other aliphatic polyesters, PBS not only has a higher melting point (close to...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/85C08G63/16
Inventor 郭宝华徐军王国利高兵
Owner TSINGHUA UNIV
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