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Method for purifying lactide

A lactide and solvent technology, applied in organic chemistry methods, organic chemistry, etc., can solve the problems of multiple operation steps and high processing temperature, reduce impurities such as m-lactide, improve product purity, and ensure product yield Effect

Pending Publication Date: 2022-05-13
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The lactide product obtained by this method has high purity and high yield, but after dual-solvent extraction, melting crystallization and constant temperature crystal growth are required, the processing temperature is relatively high, and the operation steps are slightly more

Method used

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  • Method for purifying lactide
  • Method for purifying lactide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Preparation of crude L-lactide: Using zinc oxide and stannous octoate as catalysts, 88% L-lactic acid as raw material, after dehydration, polycondensation and depolymerization of lactic acid, crude L-lactide with a purity of 85.6% was obtained. in, m -The lactide content is 5.8%, the lactic acid content is 5.4%, the lactic acid dimer and trimer content is 2.3%, and a small amount of water and other impurities are also included.

[0039] Take 200g of the above-mentioned crude lactide, use a crusher to crush it to a diameter of 0.5-1.0mm, add it to the reaction kettle at one time, then add 200g of deionized water, keep the system temperature at 5°C, stir at 200rpm for 5min, and then add 100 g of absolute ethanol was added therein, the reaction temperature was maintained at 5° C., and the reaction was continued to stir for 10 minutes, then filtered, washed with water, and dried at 70° C. for 8.0 hours to obtain purified L-lactide. As a result of testing, the product has a...

Embodiment 2

[0041] Preparation of L-lactide: Zinc oxide and stannous octoate are used as catalysts, 88% L-lactic acid is used as raw material, after lactic acid dehydration, polycondensation and depolymerization reactions, lactide with a purity of 79.0% is obtained. in, m -The content of lactide is 6.2%, the content of lactic acid is 6.7%, the content of lactic acid dimer and trimer is 3.1%, and also includes a small amount of water and other impurities.

[0042] Take 200g of the above-mentioned crude lactide, use a crusher to crush it to a diameter of 0.5-1.0mm, add it to the reaction kettle at one time, then add 60g of deionized water, keep the system temperature at 10°C, stir at 100rpm for 3min, and then add 120 g of absolute ethanol was added therein, the reaction temperature was maintained at 15° C., and the reaction was continued to stir for 30 minutes, then filtered, washed with water, and dried at 70° C. for 8 hours to obtain purified L-lactide. As a result of testing, the produc...

Embodiment 3

[0044] Preparation of L-lactide: Zinc oxide and stannous octoate are used as catalysts, 88% L-lactic acid is used as raw material, after dehydration, polycondensation and depolymerization of lactic acid, lactide with a purity of 90.0% is obtained. in, m -The content of lactide is 3.7%, the content of lactic acid is 3.4%, the content of lactic acid dimer and trimer is 1.9%, and also includes a small amount of water and other impurities.

[0045] Take 200g of the above-mentioned crude lactide, crush it with a crusher to a diameter of 0.5-1.0mm, add it to the reaction kettle at one time, then add 600g of deionized water, keep the system temperature at 2°C, and stir at 300rpm for 5min. Then 150 g of absolute ethanol was added thereto, the reaction temperature was maintained at 2° C., and the reaction was continued to stir for 5 minutes, then filtered, washed with water, and dried at 70° C. for 8 hours to obtain purified L-lactide. As a result of testing, the product has a chemica...

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Abstract

The invention relates to a method for purifying lactide, which comprises the following steps of: firstly, pretreating crude lactide, and then adding water to quickly react for less than or equal to 10 minutes at the reaction temperature of lower than 18 DEG C to obtain water extraction feed liquid; and adding a low-carbon alcohol solvent into the water extraction material liquid, and filtering, washing and drying after reaction to obtain purified lactide. According to the method, impurities such as m-lactide in the crude lactide can be efficiently removed, a high-quality lactide product is obtained, and the method is simple, convenient and safe to operate.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a method for purifying lactide. Background technique [0002] While traditional polymer materials bring countless conveniences to people, they also bring a lot of burdens to the environment. "White pollution" is becoming an increasingly serious problem. In this context, polylactic acid, as a fully biodegradable polymer material, has received more and more attention. In 2019, the planned production capacity of polylactic acid in the world and in China has reached one million tons. In recent years, the domestic polylactic acid industry has shown explosive growth. Some enterprises have plans for the construction of polylactic acid plants with a capacity of 50,000 to 300,000 tons. It is expected that the domestic production capacity will reach one million tons in the next five years. As for lactide, the key monomer raw material, currently the main manufacturer...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D319/12
CPCC07D319/12C07B2200/07
Inventor 孙启梅彭绍忠李澜鹏张通白富栋
Owner CHINA PETROLEUM & CHEM CORP
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