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Method for producing poly-L-lactic acid by using L-lactic acid through oligomerization, melt polycondensation and solid-state polycondensation

A technology of melt polycondensation and solid-state polycondensation, which is applied in the field of deep processing of lactic acid, can solve problems such as unsuitable for industrial application, high cost, and toxicity, and achieve the effects of improving product competitiveness, mild reaction conditions, and reducing costs

Active Publication Date: 2021-02-02
河南金丹乳酸科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The shortcoming of this method is: (1) lactide must be used as raw material, but in industrial production, lactic acid monomer is the cheapest raw material, and the cost of preparing lactic acid oligomerization mixture by lactide is higher; (2) using Solvents such as tetrahydrofuran are toxic and not suitable for industrial applications

Method used

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  • Method for producing poly-L-lactic acid by using L-lactic acid through oligomerization, melt polycondensation and solid-state polycondensation
  • Method for producing poly-L-lactic acid by using L-lactic acid through oligomerization, melt polycondensation and solid-state polycondensation
  • Method for producing poly-L-lactic acid by using L-lactic acid through oligomerization, melt polycondensation and solid-state polycondensation

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Effect test

Embodiment 1

[0108] A method utilizing L-lactic acid to produce poly-L-lactic acid through oligomerization, melt polycondensation and solid phase polycondensation, comprising the steps of:

[0109] (1) Raw material preparation: 45wt% L-lactic acid solution produced by the applicant, the optical purity of L-lactic acid is greater than or equal to 99.5%;

[0110] (2) Dehydration oligomerization to obtain L-lactic acid oligomers;

[0111] Add ethyl pyruvate to the L-lactic acid solution and stir to obtain a mixed solution, the volume ratio of ethyl pyruvate to the L-lactic acid solution is 1:1;

[0112] Simultaneously add cobalt oxide and two-cysteine ​​methyl ester vanadyl as catalyst in mixed solution according to the following steps:

[0113] During the initial reaction (0h): the mass ratio of cobalt oxide and di-cysteine ​​methyl ester vanadyl is 1:1.5, and the amount of cobalt oxide added during the initial reaction is 1 / 2 of the total amount of cobalt oxide added; The reaction tempera...

Embodiment 2

[0119] A method utilizing L-lactic acid to produce poly-L-lactic acid through oligomerization, melt polycondensation and solid phase polycondensation, comprising the steps of:

[0120] (1) Raw material preparation: 60wt% L-lactic acid solution produced by the applicant, the optical purity of L-lactic acid is greater than or equal to 99.5%;

[0121] (2) Dehydration oligomerization to obtain L-lactic acid oligomers;

[0122] Add ethyl pyruvate to L-lactic acid solution and stir to obtain a mixed solution, the volume ratio of ethyl pyruvate to L-lactic acid solution is 1:1; add cobalt oxide and di-cysteine ​​methyl ester to the mixed solution Vanadyl is used as a catalyst; the amount of cobalt oxide used is 0.04% of the mass of L-lactic acid, the amount of di-cysteine ​​methyl ester vanadyl is 0.08% of the mass of L-lactic acid, and the reaction is stirred for 3 hours at room temperature; The preparation method of vanadyl methyl ester is as follows: methyl cysteine ​​and vanadyl...

Embodiment 3

[0125] A method utilizing L-lactic acid to produce poly-L-lactic acid through oligomerization, melt polycondensation and solid phase polycondensation, comprising the steps of:

[0126] (1) Raw material preparation: 50wt% L-lactic acid solution produced by the applicant, the optical purity of L-lactic acid is greater than or equal to 99.5%;

[0127] (2) Dehydration oligomerization to obtain L-lactic acid oligomers;

[0128] Add ethyl pyruvate to the L-lactic acid solution and stir to obtain a mixed solution, the volume ratio of ethyl pyruvate to the L-lactic acid solution is 1:1;

[0129] Simultaneously add cobalt oxide and two-cysteine ​​methyl ester vanadyl as catalyst in mixed solution according to the following steps:

[0130] During the initial reaction (0h): the mass ratio of cobalt oxide and di-cysteine ​​methyl ester vanadyl is 1:1.5, and the amount of cobalt oxide added during the initial reaction is 1 / 2 of the total amount of cobalt oxide added; The reaction tempera...

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Abstract

The invention discloses a method for producing poly-L-lactic acid by using L-lactic acid through oligomerization, melt polycondensation and solid-state polycondensation, comprising the following steps: (1) preparing L-lactic acid oligomers by using L-lactic acid; (2) making L-lactic acid The lactic acid oligomer and the melting polycondensation catalyst are added in the melting polycondensation reactor, and the low molecular weight poly-L-lactic acid is prepared by melting polycondensation, and the addition of the melting polycondensation catalyst is 0.1-1% of the L-lactic acid oligomer quality; (3) The low-molecular-weight poly-L-lactic acid is added into a solid-phase polycondensation reactor to carry out solid-phase polycondensation to prepare high-molecular-weight poly-L-lactic acid. The present invention uses cheap and easy-to-obtain L-lactic acid monomers in actual industrial production as raw materials, and obtains L-lactic acid oligomers with narrow molecular weight distribution. The reaction conditions are mild and easy to control, and the yield of L-lactic acid oligomers is high. , suitable for industrial production; reusing L-lactic acid oligomers to produce poly-L-lactic acid through melt polycondensation and solid-state polycondensation, which greatly reduces costs and improves product competitiveness.

Description

technical field [0001] The invention relates to the technical field of deep processing of lactic acid. More specifically, it relates to a method for producing poly-L-lactic acid by utilizing L-lactic acid through oligomerization, melt polycondensation and solid-state polycondensation. Background technique [0002] Polylactic acid is a polymer with excellent performance, biocompatibility and biodegradability, mainly used in degradable packaging materials and drug microsphere carriers, anti-adhesive films, biological catheters, orthopedic fixtures, orthopedic surgical devices , artificial bone and other medical materials. [0003] In the process of preparing polylactic acid from monomeric lactic acid, lactic acid oligomers are first generated from monomeric lactic acid, and then polylactic acid is prepared by direct polycondensation of lactic acid oligomers; or lactide is prepared from lactic acid oligomers and then lactide Ring-opening polymerization produces polylactic aci...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/08C08G63/78C08G63/80
CPCC08G63/08C08G63/78C08G63/80
Inventor 崔耀军顾永华崔凯宁王浩邢晓霞葛大森李长天范小辉崔浩刘雁
Owner 河南金丹乳酸科技股份有限公司
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