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Preparation method of degradable glycolic acid copolyester

A technology of glycolic acid copolyester and glycolic acid, which is applied in the field of polymer materials, can solve the problems of poor thermal stability of copolymers, low intrinsic viscosity of products, excessive degradation speed, etc., and achieve low production energy consumption and low production cost. Low, the effect of less side effects in the whole process

Active Publication Date: 2014-07-09
JIANGSU JINJU ALLOY MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The thermal stability of polyglycolic acid itself is poor, and it is easy to degrade when the polymerization temperature is higher than 200 ° C. Therefore, once its melting point becomes high, the polymerization reaction will become very difficult, resulting in a low molecular weight of the final product. Intrinsic viscosity is small
[0004] There are also literatures (Wang Chaoyang et al., Synthesis of polylactic acid-glycolic acid, a biodegradable material for drug sustained release, Fine Chemical Industry, 2003, 20(7):515-518) reporting the preparation of copolymers by melting polycondensation of glycolic acid and lactic acid, but The thermal stability of this copolymer is poor, and when the polymerization temperature reaches above 180°C, severe degradation reactions will occur, and the intrinsic viscosity of the final product is low
In addition, this copolymer has defects such as too fast degradation and poor mechanical properties, so it is difficult to apply to daily necessities such as packaging materials and children's toys
[0005] CN1385452A has reported adopting stannous chloride dihydrate as catalyst to synthesize lactic acid-glycolic acid copolymer, but its used catalyst is more toxic

Method used

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  • Preparation method of degradable glycolic acid copolyester

Examples

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Comparison scheme
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Embodiment 1

[0019] A kind of preparation method of degradable glycolic acid copolyester, preparation steps are as follows: 10mol glycolic acid, 0.05mol adipic acid and 0.045mol ethylene glycol are added in the reactor, add precondensation catalyst 0.038g zinc powder to carry out pretreatment Polycondensation reaction, the precondensation reaction temperature is 100°C, the stirring speed is 5r / min, the precondensation reaction time is 2h, and the precondensation product is obtained; 0.038g of polycondensation catalyst bismuth acetate and 0.0076g of stabilizer phosphoric acid are added to the precondensation product The polycondensation reaction of triphenyl ester is carried out, the stirring speed is 5r / min, the temperature of polycondensation reaction is 170°C, the reaction time is 1h, and the reaction vacuum is 0.1mmHg, and the glycolic acid copolyester with medium molecular weight is obtained. After testing, the glycolic acid copolyester The intrinsic viscosity number of polyester is 0.8...

Embodiment 2

[0021] A kind of preparation method of degradable glycolic acid copolyester, preparation steps are as follows: 10mol glycolic acid, 0.1mol adipic acid and 0.12mol ethylene glycol are added in the reactor, add precondensation catalyst 0.08g tetraisotitanate Propyl ester and 0.02g tetrabutyl titanate were subjected to precondensation reaction, the precondensation reaction temperature was 120°C, the stirring speed was 50r / min, the precondensation reaction time was 4h, and the precondensation product was obtained; 0.18g The polycondensation catalyst antimony acetate and 0.01g stabilizer triphenyl phosphate were used for polycondensation reaction, the stirring speed was 50r / min, the temperature of polycondensation reaction was 190°C, the reaction time was 3h, and the reaction vacuum was 1mmHg to obtain medium molecular weight Glycolic acid copolyester, after testing, the intrinsic viscosity of glycolic acid copolyester is 0.87dl / g; Glycolic acid copolyester produced by polycondensat...

Embodiment 3

[0023]A kind of preparation method of degradable glycolic acid copolyester, preparation steps are as follows: 10mol glycolic acid, 1mol adipic acid and 1.3mol ethylene glycol are joined in the reactor, add precondensation catalyst 0.2g ethylene glycol titanium, 0.6g of titanium butoxide and 0.3g of titanium dioxide were subjected to precondensation reaction, the precondensation reaction temperature was 140°C, the stirring speed was 80r / min, and the precondensation reaction time was 8h to obtain a precondensation product; add 0.9g to the precondensation product The polycondensation catalyst tetraisopropyl titanate and 0.2g stabilizer triphenyl phosphite were used for polycondensation reaction, the stirring speed was 80r / min, the temperature of polycondensation reaction was 200°C, the reaction time was 5h, and the reaction vacuum was 3mmHg. Make the glycolic acid copolyester of medium molecular weight, the intrinsic viscosity number of glycolic acid copolyester is 0.76dl / g throug...

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Abstract

The invention discloses a preparation method of degradable glycolic acid copolyester. Glycolic acid copolyester with high molecular weight is obtained by condensation polymerization of glycollic acid, adipic acid and ethylene glycol. The direct condensation polymerization is adopted, so that the whole process is short in procedure, less in side reaction and low in energy consumption during production; glycollic acid, adipic acid and ethylene glycol are taken as raw materials, so that the cost of the raw materials is low. Thus, the finally obtained glycolic acid copolyester is low in production cost. The prepared glycolic acid copolyester is high in intrinsic viscosity, good in mechanical property and excellent in practicability. In addition, the glycolic acid copolyester is completely prepared by the condensation polymerization of biodegradable monomers, so that the glycolic acid copolyester has the complete biodegradability; catalysts containing stannum, plumbum and the like, which have large toxicity, are not adopted in the preparation process, so that the glycolic acid copolyester is nonhazardous to a human body. As a result, the glycolic acid copolyester disclosed by the invention is a safe and environment-friendly high molecular material.

Description

technical field [0001] The invention relates to a preparation method of degradable glycolic acid copolyester, which belongs to the technical field of polymer materials. Background technique [0002] Polyglycolic acid (also known as polyglycolic acid) is an aliphatic polyester polymer material with the least number of unit carbon atoms, a completely decomposable ester structure, and rapid degradation in the natural environment. The special molecular structure of polyglycolic acid also endows this material with many excellent properties, such as excellent gas barrier properties, excellent mechanical properties, excellent biodegradability and good biocompatibility, etc. Therefore, it has broad application prospects in the fields of packaging materials, biomedical materials, and children's toys. [0003] Polyglycolic acid has been known around 1950, but due to its complicated production process, the production cost of high-quality polyglycolic acid is extremely high. In recent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/60C08G63/80C08G63/85C08G63/83C08G63/86C08K5/526C08K5/523C08K5/521
Inventor 吴晓金翁伟明吴维果毛洪堂
Owner JIANGSU JINJU ALLOY MATERIAL
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