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Method for refining and purifying lactide

A technology for refining and purifying lactide, applied in directions such as organic chemistry, can solve problems such as unsatisfactory yield of lactide, and achieve the effects of reducing the use of organic solvents, reducing costs, and reducing the impact of the environment

Pending Publication Date: 2022-05-06
山东福洋生物制造工程研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when using this method to process lactide with high lactic acid content, the yield of lactide is often not satisfactory, so this method must be used in conjunction with other methods

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The crude lactide used in this example is an L-type lactide prepared from L-lactic acid through polycondensation-depolymerization reaction using zinc oxide as a catalyst.

[0029] A method for refining and purifying lactide, the specific steps are as follows:

[0030] Take 5kg of crude lactide and add it to the water washing tank, add 5kg of distilled water to it, keep the temperature at 25°C, start stirring for water washing, and the washing time is 20min. Separation; the obtained filter cake was put into a vacuum drying oven for vacuum drying at 30°C. Then the preliminary dried crude lactide is added to the vacuum distillation unit, the controlled distillation temperature is 180°C, and the distillation pressure is 5kPa, and the crude lactide distilled passes through the water removal device (the desiccant is calcium chloride, and the temperature maintained 100° C.) to further remove water to finally obtain lactide with a purity of 97.5%, and the yield of lactide is 8...

Embodiment 2

[0032] The crude lactide used in this example is an L-type lactide prepared from L-lactic acid through polycondensation-depolymerization reaction using zinc lactate as a catalyst.

[0033] A method for refining and purifying lactide, the specific steps are as follows:

[0034] Take 5kg of crude lactide and add it to the water washing tank, add 5kg of distilled water to it, keep the temperature at 25°C, start stirring for water washing, and the washing time is 30min. After separation, the obtained filter cake was put into a vacuum drying oven for vacuum drying at 30°C. Then the crude lactide of preliminarily drying is joined in the vacuum distillation unit, and the control distillation temperature is 180 ℃, and distillation pressure is 5kPa, and the crude lactide that distills out passes through dewatering device (desiccant is calcium sulfate, and the temperature that maintains is 120°C) to further remove water to finally obtain lactide with a purity of 98.6%, and the yield of...

Embodiment 3

[0036] The treatment process and operating conditions of this example are the same as those of Example 1, except that the water is washed once and then dehydrated, and the mass ratio of the amount of water to the crude lactide after dehydration is 1:1. After testing, lactide with a purity of 99.3% is finally obtained, and the yield of lactide is 82.6%.

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PUM

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Abstract

The invention discloses a method for refining and purifying lactide, and belongs to the technical field of polylactic acid production. The invention discloses a method for refining and purifying lactide, which comprises the following steps: adding crude lactide into a constant-temperature lactide washing tank, adding a proper amount of water, stirring and washing; filtering or centrifugally dewatering the washed crude lactide; drying the dehydrated crude lactide; and adding the dried crude lactide into a vacuum distillation device, melting the crude lactide, and further purifying and recovering through a water removal device to obtain high-purity lactide. The method for refining and purifying lactide disclosed by the invention can effectively remove impurities such as lactic acid, meracemate lactide and the like in crude lactide, thereby obtaining lactide with high optical purity. According to the method disclosed by the invention, recrystallization is not needed after washing by using an organic solvent, so that the influence on the environment is reduced while the cost is reduced; in addition, the method does not need repeated heating and melting, only one-step distillation is needed, and energy consumption is greatly reduced.

Description

technical field [0001] The invention relates to the technical field of polylactic acid production, in particular to a method for refining and purifying lactide. Background technique [0002] Polylactic acid (PLA) is a green and environmentally friendly bio-based material with environmental protection, non-toxic, antibacterial, flame retardant, good biocompatibility and biodegradability, and can be widely used in clothing, packaging, biomedicine, Disposable products, electronics, civil construction and other fields. At present, the methods of synthesizing polylactic acid mainly include one-step method and two-step method; because the molecular weight of polylactic acid obtained by the one-step method is low, it cannot meet the processing requirements, and its application is limited. Therefore, the more commonly used polylactic acid synthesis method at home and abroad is mainly a two-step method, that is, first synthesize dimer lactide with lactic acid, and then synthesize po...

Claims

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Application Information

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IPC IPC(8): C07D319/12
CPCC07D319/12
Inventor 赵伟朱俊梁金玲齐丹萍时胜伟张雷达
Owner 山东福洋生物制造工程研究院