Method for synthesizing polylactic acid by adopting large-channel continuous flow microreactor

A micro-reactor and large-channel technology, applied in the field of organic synthesis, can solve the problems of many side reactions, large molecular weight distribution index, and low production efficiency.

Pending Publication Date: 2021-04-23
上海东庚化工技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] In view of the above-mentioned shortcoming of the prior art, the object of the present invention is to provide a kind of method that adopts large channel continuous flow micro-reactor to synthesize polylactic acid, for solving the polylactic acid synthetic process reaction temperature height in the prior art, reaction time Long, many side reactions, large molecular weight distribution index, low production efficiency and other problems

Method used

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  • Method for synthesizing polylactic acid by adopting large-channel continuous flow microreactor
  • Method for synthesizing polylactic acid by adopting large-channel continuous flow microreactor
  • Method for synthesizing polylactic acid by adopting large-channel continuous flow microreactor

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Experimental program
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Effect test

Embodiment 1

[0037] The loading capacity of catalyst is 1.2mol% of monomer, at reaction temperature-10 ℃, 10 ℃, 30 ℃, residence time 10s, 20s, 30s, 40s, measure its conversion rate C (%), number average molecular weight Mn ( kg / mol) and molecular weight distribution index PDI. The specific data are shown in Table 1:

[0038] Table 1

[0039]

Embodiment 2

[0041] The loading of the catalyst is 0.5mol% of the monomer, at the reaction temperature -10°C, 10°C, 30°C, the residence time is 10s, 20s, 30s, 40s, respectively measure the conversion rate C (%), the number average molecular weight Mn (kg / mol) and molecular weight distribution index PDI. The specific data are shown in Table 2:

[0042] Table 2

[0043]

Embodiment 3

[0045]The load of the catalyst is 0.25mol% of the monomer, at the reaction temperature -10°C, 10°C, 30°C, the residence time is 10s, 20s, 30s, 40s, respectively measure the conversion rate C (%), the number average molecular weight Mn (kg / mol) and molecular weight distribution index PDI. The specific data are shown in Table 3:

[0046] table 3

[0047]

[0048]

[0049] Can find out from embodiment 1-3:

[0050] 1. Under higher catalyst loading (monomer 0.5 mol% and above), the conversion rate of monomer is close to quantitative under all test conditions. When using 1.2mol% catalyst loading, the monomer conversion rate can reach ≥98.5% in the shortest 10s residence time. Residence times in excess of 10 seconds only lead to broadening of the molecular weight distribution.

[0051] 2. At a higher catalyst loading of 1.2mol%, PDI tends to increase, and the optimal reaction parameters can be quickly screened out by using a microreactor. In Example 1, a residence time o...

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Abstract

The invention belongs to the technical field of organic synthesis, and particularly discloses a method for synthesizing polylactic acid by adopting a large-channel continuous flow microreactor, and the method comprises the following steps of: dissolving lactide in an organic solvent, then injecting a lactide solution and a non-metal organic catalyst into the large-channel continuous flow microreactor, and carrying out polymerization reaction to synthesize the polylactic acid. According to the method, the non-metal organic catalyst is combined with the continuous flow microreactor, so that the continuous material ratio, the reaction temperature and the reaction time can be precisely controlled, the reaction realizes rapid mixing and mass transfer, and the obtained product is good in reproducibility, stable in quality, high in monomer conversion rate, high in polymerization degree and low in molecular weight distribution index, and can be controlled to meet the high requirement of 1.1-1.3, the yellow index is low, expanded production in industrial reaction is facilitated, and the problems of high synthesis reaction temperature, many side reactions, long residence time, low production efficiency and the like of polylactic acid in the prior art can be effectively solved.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for synthesizing polylactic acid using a large channel continuous flow microreactor. Background technique [0002] Polylactic acid (PLA) is a synthetic polyester with excellent biodegradability. It is widely used in packaging, disposable tableware, biomedicine and other fields, and its output is increasing year by year. The industrial production of polylactic acid generally adopts a two-step method, that is, firstly synthesize low-molecular-weight polylactic acid through the condensation reaction of 2-hydroxypropionic acid (lactic acid), and then cyclize the low-molecular-weight polylactic acid into lactide, and then lactide High molecular weight polymers are obtained by ring-opening polymerization (ROP). [0003] At present, the main industrial synthesis process of polylactic acid is: use a stirred tank reactor or SMR reactor to react under the action of a me...

Claims

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Application Information

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IPC IPC(8): C08G63/08C08G63/78C08G63/87
CPCC08G63/08C08G63/785C08G63/823
Inventor 康小玲梁勇军唐曦丁永良唐波
Owner 上海东庚化工技术有限公司
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