Binary composite catalyst for preparing biodegradable copolyester

A binary composite and catalyst technology, applied in the field of catalyst systems, can solve the problems of easy hydrolysis failure, slow polymerization reaction speed, low molecular weight of products, etc., and achieve the effects of improving polycondensation reaction efficiency, good thermal stability and shortening reaction time.

Inactive Publication Date: 2009-09-09
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to solve several key problems such as many side reactions in polyester catalysts in the prior art, slow polymerization reaction speed, toxicity, easy hydrolysis failure, low mol

Method used

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  • Binary composite catalyst for preparing biodegradable copolyester

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Under the protection of nitrogen, put 0.7mol terephthalic acid, 0.3mol succinic acid and 1.5mol 1,4-butanediol into the reaction kettle, stir slowly to make it a paste, then add 0.50mmol zinc acetate and 0.20 mmol of germanium dioxide, the temperature was gradually raised to 220°C, the stirring rate was 100rpm, the pressure of the reaction system was adjusted to 70kPa, and the esterification reaction was carried out while maintaining the temperature and pressure, and the reaction time was 1.5h. After the esterification is completed, enter the polycondensation stage, raise the temperature to 235 ° C, adjust the reaction pressure, and proceed in two stages. The first stage is the pre-condensation stage, the vacuum is 30kPa, and the time is 1h, and then slowly transition into the second stage , That is, the high vacuum stage, the vacuum degree is 30Pa, the reaction time is 3h, and the PBST copolyester is obtained.

[0021] The weight average molecular weight measured by GP...

Embodiment 2

[0023] Under the protection of nitrogen, put 0.7mol terephthalic acid, 0.3mol succinic acid and 1.5mol 1,4-butanediol into the reaction kettle, stir slowly to make it a paste, and then add 0.30mmol tetrabutyl titanate Ester and 0.30mmol of silicon dioxide, the temperature is gradually raised to 220°C, the stirring rate is 100rpm, the pressure of the reaction system is adjusted to 70kPa, and the esterification reaction is carried out at this temperature and pressure, and the reaction time is 1.5h. After the esterification is completed, enter the polycondensation stage, raise the temperature to 235 ° C, adjust the reaction pressure, and proceed in two stages. The first stage is the pre-condensation stage, the vacuum is 30kPa, and the time is 1h, and then slowly transition into the second stage , That is, the high vacuum stage, the vacuum degree is 30Pa, the reaction time is 2h, and the PBST copolyester is obtained.

[0024] The weight average molecular weight measured by GPC met...

Embodiment 3

[0026] Under the protection of nitrogen, put 0.7mol terephthalic acid, 0.3mol succinic acid and 1.5mol 1,4-butanediol into the reaction kettle, stir slowly to make it into a paste, and then add 0.20mmol tetrapropylene titanate Ester and 0.40mmol tin dioxide, the temperature was gradually raised to 220°C, the stirring rate was 100rpm, the pressure of the reaction system was adjusted to 70kPa, and the esterification reaction was carried out at this temperature and pressure, and the reaction time was 2h. After the esterification is completed, enter the polycondensation stage, raise the temperature to 235 ° C, adjust the reaction pressure, and proceed in two stages. The first stage is the pre-condensation stage, the vacuum is 30kPa, and the time is 1h, and then slowly transition into the second stage , That is, the high vacuum stage, the vacuum degree is 30Pa, the reaction time is 4h, and the PBST copolyester is obtained.

[0027] The weight average molecular weight measured by GP...

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Abstract

The invention belongs to the field of catalyst systems for synthesizing polyester, and provides a binary composite catalyst for preparing biodegradable copolyester. The binary composite catalyst is a binary system consisting of organometallic compounds chosen from cobalt, aluminum, calcium, titanium, magnesium and zinc, and metal oxides chosen from titanium oxide, molybdenum oxide, tin oxide, magnesium oxide, calcium oxide, zinc oxide, manganese oxide, aluminum oxide, silicon oxide, germanium oxide and antimony oxide, and mol ratio of the organometallic compounds to the metal oxides is 1:9-9:1. The catalyst is applicable to preparing aliphatic/aromatic poly (butylene succinate-co-terephthalate), and the binary composite catalyst can effectively inhibit side reactions, and improve polycondensation reaction efficiency and molecular weight of the product.

Description

technical field [0001] The invention belongs to the field of catalyst systems for polyester synthesis, and in particular relates to a binary composite catalyst for preparing biodegradable copolyesters. Background technique [0002] Metal-organic catalysts are generally used in polyester synthesis, and their mechanism of action is to coordinate with the carbonyl oxygen atom in the reactant, so that the reaction continues. Similarly, biodegradable aliphatic / aromatic butylene terephthalate-co-butylene succinate (PBST) is also prepared using organometallic catalysts, and catalysts play a key role in polyester synthesis At present, organic compounds such as titanium and zinc or heavy metal organic compounds such as tin, antimony, cadmium and lead are mostly used as catalysts for the preparation of polyester by condensation polymerization. Although the former has high catalytic activity, it also has high catalytic side reaction activity, serious side reactions, poor thermal stabi...

Claims

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Application Information

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IPC IPC(8): C08G63/82C08G63/83C08G63/84C08G63/85
Inventor 俞建勇李发学罗胜利
Owner DONGHUA UNIV
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