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Method for preparing high-purity lactide based on catalytic cracking of organic guanidine complex

A catalytic cracking, organic guanidine technology, applied in organic compound/hydride/coordination complex catalysts, organic chemistry, chemical instruments and methods, etc., can solve problems affecting product yield, high reaction temperature, environmental pollution, etc. Achieve the effect of no cytotoxicity, simple preparation process and high yield

Active Publication Date: 2021-11-02
YANGZHOU HUITONG CHEM ENG TECHN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the problem of high reaction temperature in the process of preparing lactide from lactic acid in the prior art, which affects the product yield and the problem of product pollution and environmental pollution caused by toxic metal catalyst residues in lactide

Method used

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  • Method for preparing high-purity lactide based on catalytic cracking of organic guanidine complex
  • Method for preparing high-purity lactide based on catalytic cracking of organic guanidine complex
  • Method for preparing high-purity lactide based on catalytic cracking of organic guanidine complex

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Mix 0.1mol organic guanidine (CR) and 0.1mol ZnCl 2 Dissolve in 150ml of water and 150ml of methanol respectively, add the zinc chloride methanol solution into the reactor, slowly add the organic guanidine aqueous solution dropwise under continuous stirring, and condense and reflux at 60°C for 8 hours after the dropwise addition; centrifuge, wash, and dry That is, the organic guanidine complex CRZnCl 2 , yield 82.6%.

[0035] (2) Add lactic acid and ZnO (mass ratio to lactic acid: 1:1000) into the reactor, polycondense at 150°C and 1kPa for 8 hours, slowly distill out free water in the reaction system, and finally obtain lactic acid oligomers, molecular weight for 1880.

[0036] Adding organic guanidine complex CRZnCl to lactic acid oligomer 2 (The mass ratio of the oligomer to the oligomer is 1:1000), distilled under reduced pressure at 200°C and a vacuum of 0.5kPa for 2h, and collected white crude lactide with a yield of 91.3%. The chemical purity of the produ...

Embodiment 2

[0039] (1) 0.1mol organic guanidine (CR) and 0.1mol Zn(OAc) 2 Dissolve in 150ml of water and 150ml of ethanol respectively, add zinc acetate ethanol solution into the reactor, slowly add organic guanidine aqueous solution dropwise with continuous stirring, after the dropwise addition is completed, condense and reflux for 12h at 30 °C; centrifuge, wash, and dry. Obtained organic guanidine complex CRZn(OAc) 2 , the yield is 86.5%.

[0040] (2) Add lactic acid and ZnO (the mass ratio to lactic acid is 1:1500) into the reactor, polycondensate at 160 ° C and 2 kPa for 6 hours, and slowly evaporate the free water in the reaction system, and finally obtain lactic acid oligomers with molecular weight. is 1700.

[0041] Addition of organic guanidine complex CRZn(OAc) to lactic acid oligomers 2 (the mass ratio to oligomer is 1:800), under reduced pressure distillation at 190 ° C and a vacuum of 0.4 kPa for 1.5 h, white crude lactide is collected, and the yield is 80.2%. The chemical...

Embodiment 3

[0044] (1) 0.1mol organic guanidine (CR) and 0.1mol Zn(OLa) 2 Dissolve in 150ml of water and 150ml of ethanol respectively, add zinc lactate ethanol solution into the reactor, slowly add organic guanidine aqueous solution dropwise with continuous stirring, after the dropwise addition is completed, condensate and reflux for 10h at 50 °C; centrifuge, wash, and dry. Obtained organic guanidine complex CRZn(OLa) 2 , the yield was 90.6%.

[0045] (2) Add lactic acid and ZnO (mass ratio to lactic acid is 1:1800) into the reactor, polycondensate at 120 ° C and 2 kPa for 5 h, the free water in the reaction system is slowly distilled out, and finally lactic acid oligomers are obtained. is 1330.

[0046] Adding the prepared organic guanidine complex CRZn(OLa) to lactic acid oligomers 2 (1:1200 mass ratio to oligomer), vacuum distillation was carried out at 170 ° C and a vacuum degree of 0.2 kPa for 2.5 h, and white crude lactide was collected, with a yield of 85.5%. The chemical puri...

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Abstract

The invention relates to a method for preparing high-purity lactide based on catalytic cracking of an organic guanidine complex in the field of high polymer material production, which comprises the following steps: (1) preparation of the organic guanidine complex: taking organic guanidine and non-toxic metal salt as raw materials to react to obtain the organic guanidine complex; (2) preparation of crude lactide: carrying out polycondensation on lactic acid and ZnO under heating and pressurizing conditions to obtain a lactic acid oligomer; then carrying out a depolymerization reaction by taking the organic guanidine complex as a depolymerization catalyst to obtain crude lactide; and (3) preparation of high-purity lactide: refining and purifying the crude lactide to obtain the high-purity lactide. The catalyst adopted by the invention is green, environment-friendly and non-toxic, can reduce the depolymerization reaction temperature and shorten the reaction time, can be used for the depolymerization reaction for preparing lactide from lactic acid, and improves the yield of lactide.

Description

technical field [0001] The invention relates to the field of polymer materials, in particular to a method for preparing high-purity lactide. Background technique [0002] White pollution has directly or indirectly affected human life, and it is urgent to prevent and treat it in time. Its treatment is one of the major challenges facing mankind today. Degradable materials that meet the sustainable development strategy are of great significance to improving the ecological environment and improving people's quality of life. In 2020, the National Development and Reform Commission and the Ministry of Ecology and Environment issued the "Opinions on Further Strengthening Plastic Pollution Control" to further promote public attention to biodegradable materials, such as PLA, PBAT, and PBS. Among them, PLA is derived from renewable resources, has good biodegradability, is non-toxic, and has no pollution. Many performance indicators are similar to general-purpose plastics such as polye...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D319/12B01J31/18B01J31/22
CPCC07D319/12B01J31/1805B01J31/182B01J31/2226B01J2531/26B01J2531/22B01J2531/842B01J2531/0213B01J2531/0241
Inventor 包建娜张建纲陈文兴刘雄顾忠辉郑文龚磊柴青立
Owner YANGZHOU HUITONG CHEM ENG TECHN
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