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Medical lactide and preparation method thereof

A lactide and cracking treatment technology, applied in the direction of organic chemistry, can solve the problems of easy blockage of the system, affect the purity of lactide ring-opening polymerization, increase the cost and difficulty of separation and purification, and achieve the goal of improving yield and purity Effect

Active Publication Date: 2020-06-05
SHENZHEN CORLIBER SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The defect of this method is mainly due to the addition of solvent, which greatly increases the production cost. At the same time, the lactide product often contains added high-boiling point solvents. These high-boiling point reagents must be removed to synthesize high-purity lactide, which greatly increases the cost of separation and purification. Cost and difficulty, ultimately affecting lactide purity and subsequent ring-opening polymerization
[0008] In addition, Chinese patent CN 104710401A discloses a composite catalyst of stannous oxide / zinc oxide, stannous oxide / stannous octoate, stannous oxide / zinc oxide / stannous octoate to improve the yield of lactide crude product, but still The above three problems cannot be solved well, that is, the problem of easy clogging of the system and partial cracking of color, and the use of composite catalyst directly increases the production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0026] 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 percentage of 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.

[0027] As can be seen from the foregoing description, the beneficial effects of the present invention are:

[0028]In the prior art, o...

Embodiment 1

[0045] A method for preparing medical lactide with improved purity and yield, the specific steps are:

[0046] 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.

[0047] 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...

Embodiment 2

[0049] A method for preparing medical lactide with improved purity and yield, the specific steps are:

[0050] 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 medical lactide and a preparation method thereof, and the preparation method comprises the following steps: dehydrating lactic acid to obtain dehydrated lactic acid; adding acatalyst into the obtained dehydrated lactic acid, and carrying out a polycondensation reaction to generate a lactic acid oligomer; sequentially carrying out thermal cracking treatment on the generated lactic acid oligomer in batches, and then carrying out vacuum reduced pressure distillation to obtain a lactide crude product; and recrystallizing and purifying the obtained lactide crude product toobtain the medical lactide. The preparation method of the medical lactide has the advantages that the yield and the purity are improved, and the problems that a system is easy to block, the fluidityand the heat transfer effect of the system are reduced, and a reaction system changes color due to high-temperature carbonization can be effectively solved.

Description

[0001] This application is filed on March 08, 2018 , the application number is 201810189672.X , the name of the invention is medical The preparation method of lactide divisional application of the patent application. technical field [0002] The invention relates to a medical lactide and a preparation method thereof. Background technique [0003] 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. [0004] 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-ope...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D319/12
CPCC07D319/12
Inventor 向冬黄裕程孙杨
Owner SHENZHEN CORLIBER SCI
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