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Method for preparing biodegradable copolyester by direct esterification-polycondensation process

A technology of copolyester and esterification, applied in the field of preparing biodegradable copolyester by direct esterification polycondensation method, can solve the problems of unfavorable industrial production in production route, lack of raw material sources, difficult separation of tetrahydrofuran, etc., and achieve good biodegradation performance , Wide source of raw materials, easy separation effect

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

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to solve several problems existing in the current aliphatic / aromatic PBST copolyester transesterification route: by-product recovery problem, lack of raw material source, by-product methanol and tetrahydrofuran produced in the transesterification stage are difficult to separate and lead to production route Not conducive to industrial production
The invention provides a method for preparing biodegradable PBST copolyester by direct esterification polycondensation method to solve the problems existing in the transesterification route

Method used

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  • Method for preparing biodegradable copolyester by direct esterification-polycondensation process
  • Method for preparing biodegradable copolyester by direct esterification-polycondensation process
  • Method for preparing biodegradable copolyester by direct esterification-polycondensation process

Examples

Experimental program
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Effect test

Embodiment 1

[0032] (1) 0.7mol terephthalic acid, 0.3mol succinic acid, 1.5mol 1,4-butanediol and 0.5mmol dibutyltin oxide catalyst are placed in the reactor under nitrogen protection, and the reaction temperature is 210 °C, the esterification reaction was carried out at a reaction pressure of 40 kPa, a stirring rate of 100 rpm, and a reaction time of 1.5 h. Wherein, the molar ratio of terephthalic acid and succinic acid is 7: 3; The molar ratio of the sum of the moles of terephthalic acid and succinic acid to 1,4-butanediol is 1: 1.5; The ratio of the sum of moles of the two dibasic acids was 0.05%.

[0033] (2) After step (1) finishes, carry out condensation polymerization reaction under the temperature 250 ℃, stirring rate is 100rpm, and precondensation stage reaction pressure is 10kPa, and reaction time is 50min, then slowly transits to high vacuum stage, and reaction pressure is 40Pa, the reaction time is 3h, to obtain PBST copolyester.

[0034] After cooling the product of the abov...

Embodiment 2

[0036] (1) 0.7mol terephthalic acid, 0.3mol succinic acid, 1.5mol 1,4-butanediol and 0.3mmol stannous octoate catalyst are placed in the reactor under nitrogen protection, and the reaction temperature is 200 ° C. The esterification reaction was carried out at a reaction pressure of 75 kPa, a stirring rate of 100 rpm, and a reaction time of 2 h. Wherein, the molar ratio of terephthalic acid and succinic acid is 7: 3; The molar ratio of the sum of the moles of terephthalic acid and succinic acid to 1,4-butanediol is 1: 1.5; The ratio of the sum of moles of the two dibasic acids was 0.03%.

[0037] (2) After step (1) finishes, carry out condensation polymerization reaction under the temperature 245 ℃, stirring rate is 100rpm, and precondensation stage reaction pressure is 15kPa, and reaction time is 60min, then slowly transits to high vacuum stage, and reaction pressure is 30Pa, the reaction time is 3h, to obtain PBST copolyester.

[0038] After cooling the product of the above...

Embodiment 3

[0040](1) 0.7mol terephthalic acid, 0.3mol succinic acid, 1.3mol 1,4-butanediol and 0.3mmol tetraisopropyl titanate catalyst are placed in the reactor under nitrogen protection, and the reaction temperature is The esterification reaction was carried out at 205° C., the reaction pressure was 60 kPa, the stirring rate was 100 rpm, and the reaction time was 1.5 h. Wherein, the mol ratio of terephthalic acid and succinic acid is 7: 3; The molar ratio of the sum of terephthalic acid and succinic acid moles to 1,4-butanediol is 1: 1.3; The ratio of the sum of moles of the two dibasic acids was 0.05%.

[0041] (2) After step (1) finishes, carry out condensation polymerization reaction under the temperature 240 ℃, stirring speed is 100rpm, and precondensation stage reaction pressure is 20kPa, and reaction time is 65min, then slowly transits to high vacuum stage, and reaction pressure is 35Pa, the reaction time is 2.5h, to obtain PBST copolyester.

[0042] After cooling the product o...

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Abstract

The invention belongs to the field of preparing biodegradable copolyester by a condensation polymerization process, and provides a method for preparing biodegradable copolyester by a direct esterification-polycondensation process. The method comprises the following steps: adding three monomers which are terephthalic acid, succinic acid and 1,4-butanediol and a catalyst to a reaction kettle according to a certain proportion, and obtaining poly(butylene succinate-co-terephthalate) (PBST) after two stages which are direct esterification and condensation polymerization at certain reaction temperature, reaction pressure and reaction time. A synthetic route employed by the method is applicable to industrial production, and biodegradable PBST copolyester with higher molecular weight can be synthesized without a chain extension reaction step.

Description

technical field [0001] The invention belongs to the field of preparing biodegradable polyester by condensation polymerization, and in particular relates to a method for preparing biodegradable copolyester by direct esterification and polycondensation. Background technique [0002] In recent years, while various synthetic fiber products have brought convenience to people's lives, a large amount of waste after use has increased day by day, which has caused a non-negligible negative impact on the natural environment and has become a new source of pollution. In recent years, the development of biodegradable polyester has been considered as one of the main ways to solve the increasingly serious "white pollution" problem caused by traditional polyester fiber products. Since aliphatic / aromatic copolyesters have both good biodegradability and good mechanical processing properties, the preparation of aliphatic / aromatic copolyesters by copolymerization of aliphatic polyesters with aro...

Claims

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Application Information

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IPC IPC(8): C08G63/78C08G63/85C08G63/83C08G63/16C08G63/183
Inventor 俞建勇罗胜利李发学
Owner DONGHUA UNIV
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