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Catalyst composition for preparing polyglycolide and preparation method of polyglycolide

A polyglycolide and catalyst technology, applied in the field of polyglycolide preparation, can solve the problems of high residual monomer content, decreased mechanical properties, etc., and achieve the advantages of improving intrinsic viscosity and weight average molecular weight, reducing content and achieving good technical effects. Effect

Active Publication Date: 2021-12-10
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved by the present invention is the high content of residual monomers in the preparation of polyglycolide in the prior art, and the problem that the mechanical properties of the polymer after purification and removal of residual monomers are reduced. A method for preparing polyglycolide is provided. The catalyst composition of ester and the preparation method of polyglycolide, the polyglycolide obtained by the method has the advantages of high intrinsic viscosity, high weight-average molecular weight, low residual monomer content and good mechanical properties

Method used

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  • Catalyst composition for preparing polyglycolide and preparation method of polyglycolide

Examples

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Effect test

Embodiment 1

[0057] Preparation of Titanium Complex A

[0058] In a reactor equipped with a stirrer, a condenser and a thermometer, add 18.6 grams (0.3 moles) of ethylene glycol, slowly drop 28.4 grams (0.1 moles) of tetraisopropyl titanate into the reactor, and precipitate a white precipitate , reacted at 80°C for 3 hours, centrifuged the product, washed the residue three times with distilled water, and dried the product in vacuum at 70°C to obtain a white powdery substance. Put the dried white powdery substance in a reactor equipped with a stirrer, a condenser and a thermometer, add 12 grams (0.2 moles) of isopropanol and react at 60°C for 3 hours to obtain a colorless transparent liquid, which is titanium Complex A.

[0059] Preparation of phosphorus complex B

[0060] In a reactor equipped with a stirrer, a condenser and a thermometer, add 14.0 grams (0.1 moles) of trimethyl phosphate and 21.6 grams (1.2 moles) of water, and drop 31.0 grams (0.5 moles) of ethylene glycol into the rea...

Embodiment 2

[0064] Preparation of Titanium Complex C

[0065] In a reactor equipped with a stirrer, a condenser and a thermometer, add 18.6 grams (0.3 moles) of ethylene glycol, slowly drop 28.4 grams (0.1 moles) of tetraisopropyl titanate into the reactor, and precipitate a white precipitate , reacted at 100°C for 2 hours, centrifuged the product, washed the residue three times with distilled water, and dried the product in vacuum at 70°C to obtain a white powdery substance. Put the dried white powdery substance in a reactor equipped with a stirrer, a condenser and a thermometer, add 18.0 grams (0.3 moles) of isopropanol and react at 80 ° C for 4 hours to obtain a colorless transparent liquid, which is titanium Complex C.

[0066] Preparation of polyglycolide

[0067] 1000 grams of glycolide is added in the there-necked flask, and titanium complex C (based on the mass of glycolide monomer, the weight of the titanium atom is 140 mg / kg) is added under the molten state of glycolide, and t...

Embodiment 3

[0069] Preparation of polyglycolide

[0070] 1000 grams of glycolide is added in the there-necked flask, and titanium complex C (based on the mass of glycolide monomer, the weight of the titanium atom is 80 mg / kg) is added under the molten state of glycolide, and the phosphorus complex B (based on the mass of glycolide monomer, the weight of phosphorus atom is 20mg / kg), mixed at 83°C for 8 minutes, after the mixture was cooled and pulverized, it was continuously added to the twin-screw extruder through an autosampler for ring opening Polymerization reaction, reaction temperature 230°C, polymerization residence time 15 minutes, continue to enter the single-screw extruder for on-line removal of residual monomers, single removal temperature 175°C, single removal residence time 6 minutes, to obtain continuously and stably discharged polymer glycolide. The measured intrinsic viscosity of polyglycolide is 1.91dL / g, the weight average molecular weight is 219000, the relative molecul...

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Abstract

The invention discloses a catalyst composition for preparing polyglycolide and a preparation method of the polyglycolide. The catalyst composition comprises a titanium complex and a phosphorus complex. The titanium complex is obtained by reaction of raw materials comprising the following components: (A) a titanium compound with the following general formula: Ti (OR) 4, R being alkyl with 1-10 carbon atoms; and (B) dihydric alcohol with 2-10 carbon atoms. The phosphorus complex is a reaction product obtained by reacting at least one phosphate ester compound with at least one dihydric alcohol with 2-10 carbon atoms. The preparation method comprises the following steps of: carrying out ring opening polymerization on glycolide in the presence of the catalyst composition to obtain polyglycolide, and then removing unreacted residual monomers from the polyglycolide on line. The catalyst composition solves the problems that the residual monomer content of polyglycolide is high and the mechanical property of the polymer is reduced after the residual monomer is purified and removed in the prior art, and can be used for industrial production of polyglycolide.

Description

technical field [0001] The invention relates to the field of polyglycolide preparation, in particular to a catalyst composition for preparing polyglycolide and a preparation method of polyglycolide. Background technique [0002] As an aliphatic polyester, polyglycolide has high biodegradability and good biocompatibility. It can be hydrolyzed in organisms, and can also be metabolized by microorganisms in the natural environment, and finally decomposed into water and carbon dioxide. In addition, polyglycolide has good mechanical properties such as heat resistance and tensile strength, and has good gas barrier properties when used as a film sheet. Therefore, polyglycolide is expected to be used in medical applications instead of general-purpose biodegradable polymers. Polymer materials, agricultural resource materials, various packaging or container materials. Polyglycolide has been used in surgical sutures, artificial skin and blood vessels, bone fixation and repair, control...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/85C08G63/87C08G63/78C08G63/08
CPCC08G63/823C08G63/85C08G63/87C08G63/78C08G63/08
Inventor 周芬王睿章瑛虹熊文韬
Owner CHINA PETROLEUM & CHEM CORP
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