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Preparation method of medical lactide

A technology of lactide and lactic acid, applied in the direction of organic chemistry, to achieve the effect of improving flow and heat transfer, increasing yield and efficiency, and the reaction color does not turn yellow or black

Active Publication Date: 2020-04-03
SHENZHEN CORLIBER SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The technical problem to be solved by the present invention is to provide a method for preparing medical lactide that improves the yield and purity and can effectively solve the problem of discoloration of the reaction system caused by the above-mentioned high-temperature carbonization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0017] The invention provides a preparation method of medical lactide, which comprises dehydrating lactic acid to obtain dehydrated lactic acid; adding a catalyst to the obtained dehydrated lactic acid to carry out polycondensation reaction to generate lactic acid oligomers; Carry out heating and cracking treatment successively, and then carry out vacuum vacuum distillation to obtain the crude lactide product; then carry out recrystallization and purification on the obtained lactide crude product, obtain the medical lactide; in the polycondensation reaction, the catalyst The ratio of the mass percent to dehydrated lactic acid is 0.1-5%, the reaction temperature of the polycondensation reaction is 120-170°C, and the pressure is 1-30000Pa; the temperature of the thermal cracking treatment is 170-240°C, and the pressure is 1-30000Pa. 3000 Pa.

[0018] As can be seen from the foregoing description, the beneficial effects of the present invention are:

[0019] In the prior art, on...

Embodiment 1

[0036] A method for preparing medical lactide with improved purity and yield, the specific steps are:

[0037] Embodiment 1 is consistent with the two steps of step (1) and step (2) of the comparative example. In step (3), the lactic acid oligomers obtained in step (2) are divided into 3 batches and added to the reactor batch by batch. When the temperature was raised to 180°C, the oil pump started vacuum cracking, and the temperature was gradually raised to 220°C for complete cracking. Finally, 180 g of crude lactide was obtained with a crude yield of 50.0%. The color of lactide changed from colorless to light yellow. The vacuum device and condensing device are still easy to block, and the crude lactide product at the blockage needs to be melted regularly to ensure the smooth flow and vacuum of the system.

[0038] In step (4), the crude lactide was recrystallized and purified three times through ethyl acetate, and a finished lactide product with an optical purity of 97.8% was o...

Embodiment 2

[0040] A method for preparing medical lactide with improved purity and yield, the specific steps are:

[0041] Embodiment 2 is consistent with step (1) and step (2) two-step steps of comparative example, in step (3), the lactic acid oligomer that (2) is obtained is divided into 4 batches, adds in the reactor batch by batch and is heated up to At 180°C, the oil pump starts vacuum cracking, and gradually heats up to 220°C for complete cracking. At the same time, an automatic temperature-regulating heating device is introduced into the condensation receiving device. In the early stage of cracking, the temperature can be adjusted to 80-100°C, and in the later stage of cracking, it can be stabilized at 130-150°C, so as to ensure that lactide will not be blocked by cold precipitated solids, and finally crude lactide will be obtained. 275g, the crude yield was 76.4%, and the color of lactide changed from colorless to pale yellow. There is no blockage in the condensate receiving, and...

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Abstract

The invention relates to a preparation method of medical lactide, which comprises dehydrating lactic acid to obtain dehydrated lactic acid; adding a catalyst to the obtained dehydrated lactic acid to carry out polycondensation reaction to generate lactic acid oligomers; and batching the generated lactic acid oligomers Carry out heating and cracking treatment successively, and then carry out vacuum vacuum distillation to obtain the crude lactide product; and then carry out recrystallization and purification on the obtained crude lactide product to obtain the medical lactide. The preparation method of the medical lactide of the present invention has the advantages of increasing yield and purity, and can effectively solve the problems of easy blockage of the system, reduction of fluidity and heat transfer effect of the system, and discoloration of the reaction system caused by high-temperature carbonization.

Description

technical field [0001] The invention relates to raw materials for medical chemical intermediates of biodegradable materials, in particular to a preparation method of medical lactide. Background technique [0002] Medical lactide is an important raw material for the synthesis of medical polylactic acid. Medical polylactic acid has very good biocompatibility and good mechanical properties, and its degradation products are carbon dioxide and water, so it is a safe and environmentally friendly medical material. Medical polylactic acid has a wide range of applications in surgical sutures, bone fixation materials, drug release, tissue engineering scaffolds and other fields. [0003] There are two main methods for the synthesis of polylactic acid. The first is condensation reaction to obtain polylactic acid, and the other is lactide ring-opening polymerization to obtain polylactic acid. The first is because the water in the reaction product is difficult to remove, so the polylact...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D319/12
CPCC07D319/12
Inventor 向冬
Owner SHENZHEN CORLIBER SCI
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