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Synthesis process of ultrahigh-molecular- weight polylactic acid

A technology of ultra-high molecular weight and synthesis process, applied in the field of degradable material synthesis, can solve the problems of wide molecular weight distribution, long process, low molecular weight, etc., and achieve the effects of increasing the degree of polymerization, slowing down the reverse reaction, and increasing the molecular weight

Inactive Publication Date: 2021-01-26
河南龙都天仁生物材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The ring-opening polymerization method is to prepare lactic acid into a ring-shaped dimer lactide. The lactide is purified by recrystallization and then undergoes ring-opening polymerization to obtain polylactic acid. The polylactic acid prepared by this method has a high molecular weight and good quality, but There are problems such as complex synthesis process, long process, low yield and high production cost
The direct polycondensation method is to directly carry out dehydration polycondensation of lactic acid under high temperature and low pressure. It has the advantages of simple synthesis process, short process, high yield, low production cost, and suitable for large-scale industrial production. However, the synthesized polylactic acid usually has a relatively low molecular weight. Low, wide molecular weight distribution, dark product color and other disadvantages

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Take 500 g of L-lactic acid with a mass fraction of 80%, and dehydrate at a temperature of 120°C; then add a catalyst with a molar mass of lactic acid of 0.4% in the reaction flask (wherein the catalyst is manganese acetate with a molar mass ratio of 1:0.3:0.6: to Toluenesulfonic acid: a composite catalyst composed of titanium trichloride), the above-mentioned lactic acid raw material and catalyst are quickly frozen under 77K liquid nitrogen and vacuumized, and then melted, and through three cycles of liquid nitrogen freezing-vacuumizing-thawing operation, Carry out degassing operation on the above system, and then seal the system; heat the above sealed system to 140°C, the heating rate is 2°C / min, and react at constant temperature for 36 hours. Wash with acetone and deionized water to obtain polylactic acid.

Embodiment 2

[0016] Take 500 g of L-lactic acid with a mass fraction of 80%, and dehydrate at a temperature of 140°C; then add a catalyst with a molar mass of lactic acid of 0.6% in the reaction flask (wherein the catalyst is manganese acetate with a molar mass ratio of 1:0.3:0.6: to Toluenesulfonic acid: a composite catalyst composed of titanium trichloride), the above-mentioned lactic acid raw material and catalyst are quickly frozen under 77K liquid nitrogen and vacuumized, and then melted, and through three cycles of liquid nitrogen freezing-vacuumizing-thawing operation, Carry out degassing operation on the above system, and then seal the system; heat the above sealed system to 160°C, the heating rate is 4°C / min, and react at constant temperature for 40 hours. Wash with acetone and deionized water to obtain polylactic acid.

Embodiment 3

[0018] Take 500 g of L-lactic acid with a mass fraction of 80%, and dehydrate at a temperature of 135°C; then add a catalyst with a molar mass of lactic acid of 0.5% in the reaction flask (wherein the catalyst is manganese acetate with a molar mass ratio of 1:0.3:0.6: to Toluenesulfonic acid: a composite catalyst composed of titanium trichloride), the above-mentioned lactic acid raw material and catalyst are quickly frozen under 77K liquid nitrogen and vacuumized, and then melted, and through three cycles of liquid nitrogen freezing-vacuumizing-thawing operation, Carry out degassing operation on the above system, and then seal the system; heat the above sealed system to 160°C, the heating rate is 4°C / min, and react at constant temperature for 48 hours. Wash with acetone and deionized water to obtain polylactic acid.

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Abstract

The invention provides a synthesis process of ultrahigh-molecular-weight polylactic acid, which relates to the technical field of degradable material synthesis. Thesynthesis process comprises the following steps: adding a composite catalyst composed of manganese acetate, p-toluenesulfonic acid and titanium trichloride, and carrying out freezing vacuum degassing and constant-speed heating treatmenton the reaction system to obtain polylactic acid having the weight-average molecular weight reaching up to 208000 and narrowmolecular weight distribution. By adopting the composite catalyst, the problem of incomplete reaction of a single catalyst can be solved, and after the freezing vacuum degassing treatment is adopted, the whole reaction system is in a vacuum state, so that the reaction can becarried out towards the positive reaction direction, the reverse reaction can be slowed down, the yield can be increased, the intermolecular polymerization degree can be improved, and the molecular weight of polycondensate can be increased.

Description

technical field [0001] The invention relates to the field of synthesis of degradable materials, in particular to a synthesis process of ultra-high molecular weight polylactic acid. Background technique [0002] Polylactic acid is a green functional polymer material with very good biocompatibility and biodegradability, which is polymerized from small molecule lactic acid produced by microbial fermentation of biomass raw materials. It can be completely degraded into water and carbon dioxide. It is comparable to petroleum-based general-purpose plastics. Compared with the polylactic acid material, it is more in line with the concept of sustainable development. Not only is the product easy to degrade without causing environmental pollution, but it can fundamentally solve the problems of oil resource depletion and environmental pollution. It has been used in clothing, packaging, agriculture, automobiles, electronics, biological Widely used in medicine and other fields. [0003] A...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/08C08G63/78C08G63/83C08G63/85
CPCC08G63/08C08G63/823C08G63/78
Inventor 汤永彬杨文军何新宇许冬
Owner 河南龙都天仁生物材料有限公司
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