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Polylactic acid producing process

A production process and technology for polylactic acid, applied in the field of preparing polylactic acid, can solve the problems of complex reaction process, long production cycle, low yield, etc., and achieve the effects of reducing reaction conditions, shortening production process, and easy control of production process

Inactive Publication Date: 2007-04-25
RUGAO FIBERGLASS FACTORY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When using this process for polymerization reaction, the purity of the intermediate monomer lactide is very high, generally it needs to be crystallized 4 to 5 times, and the production cycle is long, about 30 to 40 hours; the reaction process is complicated and the yield is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 1000kg of L-lactic acid and 1kg of strontium-aluminum composite catalyst system catalyst into the reactor, heat to 250°C, the vacuum degree in the reactor is 1500Pa, react for 5h, and fully remove the water to obtain a polymer with a degree of polymerization of 5-20. Lactic acid oligomer 700KG. After the reaction product is purified by solution, 660KG of pure lactic acid oligomers can be obtained.

[0020] After mixing pure lactic acid oligomers and 66g of strontium and aluminum composite catalyst system catalyst in the reactor, replace the air in the reactor with nitrogen, maintain positive pressure, stir and heat to 250°C, Control the pressure at normal pressure, react for 10 hours, and obtain a reaction product containing polylactic acid. After the single treatment, 654 kg of polylactic acid with a molecular weight of about 400,000 can be obtained, and the yield of polylactic acid is above 99%.

Embodiment 2

[0022] Add 1000kg of L-lactic acid and 10kg of strontium-aluminum composite catalyst system catalyst into the reactor, heat to 100°C, the vacuum degree in the reactor is 4500Pa, react for 5h, and fully remove the water to obtain The reaction product of lactic acid oligomers between them is 700KG, and 660KG of pure lactic acid oligomers can be obtained after the reaction product is purified by solution.

[0023] Put the pure lactic acid oligomer and 660g of strontium, aluminum composite catalyst system catalyst into the reactor and mix, replace the air in the reactor with helium, keep the positive pressure, stir and heat to 120°C, the reactor Control the pressure at normal pressure and react for 8 hours to obtain a reaction product containing polylactic acid. After single treatment, 654 kg of polylactic acid with a molecular weight of about 100,000 can be obtained, and the yield of polylactic acid is above 99%.

Embodiment 3

[0025] Add 1000kg of L-lactic acid and 5kg of strontium-aluminum composite catalyst system catalyst into the reactor, heat to 200°C, the vacuum degree in the reactor is 6000Pa, react for 4.5h, and after fully removing water, obtain The reaction product of 20 lactic acid oligomers is 700KG, and the reaction product can be purified by solution to obtain 660KG of pure lactic acid oligomers.

[0026] Put the pure lactic acid oligomer and its 330g strontium-aluminum composite catalyst system catalyst into the reactor and mix them, replace the air in the reactor with neon, keep the positive pressure, stir and heat to 130°C, react The pressure inside the vessel is controlled at normal pressure, and the reaction product containing polylactic acid is obtained after 10 hours of reaction. After the single-off treatment, 654 kg of polylactic acid with a molecular weight of about 350,000 can be obtained, and the yield of polylactic acid is above 99%.

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PUM

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Abstract

The invention discloses a manufacturing technique of polylactic acid, which comprises the following steps: a. adding L-lactic acid and 1 / 100-1 / 1000 strontium and aluminium composite catalyst in the reactor; heating to 100-500 deg.c with vacuum degree at 1500-8000pa; dehydrating completely; obtaining reacting product of oligomer of lactic acid with polymerization degree at 5-20; b. purifying product solution to obtain pure oligomer of lactic acid; c. placing pure oligomer of lactic acid and 1 / 100-1 / 1000 strontium and aluminium composite catalyst into reactor; replacing air in the reactor through inert gas; keeping normal pressure; stirring; heating to 80-250 deg.c; controlling the pressure in the reactor; d. purifying product solution to obtain the polylactic acid.

Description

technical field [0001] The invention belongs to the field of polymer materials, and discloses a homogeneous mixture of L-lactic acid and a catalyst under high temperature and vacuum, after a certain period of dehydration polycondensation reaction, to obtain lactic acid oligomers, and after purification, to obtain pure lactic acid oligomers , and then add a catalyst to prepare the process of polylactic acid. Background technique [0002] At present, many companies and scientific research institutions at home and abroad have conducted in-depth research on the preparation process of polylactic acid, and applied for related patents. The patent documents mainly using the ring-opening polymerization process are: Brit1007374, Fr142533, EP261572 ,JP5813624,DE4412317,U.S.Pat5023349,U.S.Pat5374743,U.S.Pat6383161,CN1167776A,CN1325913A等,美国Cargill-Dow公司开发的丙交酯聚合工艺,可见于U.S.Pat 5142023,U.S.Pat 5247058,U.S.Pat 5247059,U.S.Pat 5258488, U.S.Pat 5274073, U.S.Pat 5357035, U.S.Pat 5484881 and U.S...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/06
Inventor 顾泽波阮刘文沈晓蔚彭春阳陈亚丽
Owner RUGAO FIBERGLASS FACTORY