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Method of producing L-lactide with L-lactic acid

A technology of lactide and lactic acid, applied in directions such as organic chemistry, can solve problems such as unsuitable industrial application, high cost, toxic solvent, etc., and achieve the effects of increasing reaction pressure, saving energy, high yield and purity

Active Publication Date: 2018-06-22
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 disadvantages of this method are: (1) Lactide must be used as a raw material, but in industrial production, lactic acid monomer is the cheapest raw material, and the cost of directly preparing lactide from lactic acid monomer is relatively high, so only melting The by-product lactide in the polycondensation is used as a raw material; (2) solvents such as tetrahydrofuran used are poisonous and are not suitable for industrial applications

Method used

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  • Method of producing L-lactide with L-lactic acid
  • Method of producing L-lactide with L-lactic acid
  • Method of producing L-lactide with L-lactic acid

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Embodiment 1

[0029] A method utilizing L-lactic acid to produce L-lactide, comprising the steps of:

[0030] (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%;

[0031] (2) Dehydration oligomerization to obtain L-lactic acid oligomers;

[0032] 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;

[0033] Add cobalt oxide and two-cysteine ​​methyl ester vanadyl as catalyst simultaneously according to the following steps in mixed solution:

[0034] 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 temperature is kept at 5°C from the initial reaction to half of the reaction time; stirring;

...

Embodiment 2

[0049] A method utilizing L-lactic acid to produce L-lactide, comprising the steps of:

[0050] (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%;

[0051] (2) Dehydration oligomerization to obtain L-lactic acid oligomers;

[0052] 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 sulfate are mixed and stirred at room temperature in boric acid solution, and react for ...

Embodiment 3

[0064] A method utilizing L-lactic acid to produce L-lactide, comprising the steps of:

[0065] (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%;

[0066] (2) Dehydration oligomerization to obtain L-lactic acid oligomers;

[0067] 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;

[0068] Add cobalt oxide and two-cysteine ​​methyl ester vanadyl as catalyst simultaneously according to the following steps in mixed solution:

[0069] 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 temperature is kept at 10°C from the initial reaction to half of the reaction time; stirring;

...

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Abstract

The invention discloses a method of producing L-lactide with L-lactic acid. The method comprises the following steps of: (1) performing raw material preparation: 40-60wt% of L-lactic acid solution with optical purity of greater than or equal to 99.5%, (2) performing dehydration and oligomerization to form L-lactic acid oligomer, and (3) depolymerizing the L-lactic acid oligomer to prepare L-lactide. The method of producing L-lactide with L-lactic acid can obtain the lactic acid oligomer with relatively narrow molecular weight distribution, and L-lactide prepared from the lactic acid oligomer as a raw material is very high in productivity and optical purity.

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 L-lactide using L-lactic acid. 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-mucosal 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 acid. Among them, polylactic acid with higher molecular weight can be prepared by ring-opening poly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D319/12
CPCC07D319/12
Inventor 师媛媛张国宣崔洋崔凯宁穆鹏宇王浩张树银邢晓霞范威丁龙龙何腾飞李永香
Owner 河南金丹乳酸科技股份有限公司
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