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Method for catalytically synthesizing polylactic acid by utilizing ionic liquid

A technology of ionic liquid and polylactic acid, which is applied in the field of material chemistry, can solve the problems of poor catalyst selectivity, poor product crystallization performance, and low product optical activity, and achieve the effects of short degradation cycle, improved production efficiency, and thorough degradation cycle

Inactive Publication Date: 2014-01-01
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the catalyst used in this method is a tin-based catalyst, which will leave metal poisons in the product. At the same time, due to the poor selectivity of the catalyst in the reaction, there are more oligomeric by-products in the product, which makes the optical activity of the product lower. , the crystallization performance of the product is poor, therefore, how to prepare products with high molecular weight and high crystallinity under the conditions of the melting method, and to develop a new catalyst system is a very key idea

Method used

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  • Method for catalytically synthesizing polylactic acid by utilizing ionic liquid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027]Firstly, the L-lactic acid to be reacted was dried with 5A molecular sieve for 3 hours, and then placed for use. In a 250 ml reaction bottle, add 200 g of preliminarily dried L-lactic acid, blow nitrogen to drive away oxygen, use an oil bath to control the temperature at 60°C, vacuumize and distill water for 1 hour, add 1,3-dimethylimidazole to 0.1 g of tosylate, the temperature was slowly raised to 100°C, and reacted for 2 hours, the product gradually became viscous, cooled to obtain a white oligomeric solid. Then add the oligomer and 0.15 g of 1,3-dimethylimidazole p-toluenesulfonate into the polymerization tube, heat and melt under the protection of nitrogen, control the reaction temperature at 140 ° C, the reaction pressure at 1000 Pa, stir for 6 hours, and then Slowly cool down to room temperature to obtain a light yellow solid, add 50 ml of chloroform solvent, stir and dissolve the reactant, then add dropwise while stirring with methanol, until turbidity appears, a...

Embodiment 2

[0029] Firstly, the L-lactic acid to be reacted was dried with 5A molecular sieves for 2 hours, and then placed for use. In a 500ml reaction bottle, add 300g of preliminarily dried L-lactic acid, blow nitrogen to drive away oxygen, use an oil bath to control the temperature at 60°C, vacuumize the water for 1 hour, add 1-butyl-3-methyl 0.1 g of pyridinium tetrafluoroborate, the temperature was slowly raised to 100° C., and reacted for 2 hours, the product gradually became viscous, cooled to obtain a white oligomeric solid. Then add the oligomer and 0.2 g of 1-butyl-3-picoline tetrafluoroborate into the polymerization tube, heat and melt under the protection of nitrogen, control the reaction temperature at 140 ° C, the reaction pressure at 800 Pa, and stir for 6 hour, then slowly cool down to room temperature to obtain a light yellow solid, add 100 ml of chloroform solvent, stir and dissolve the reactant, then add dropwise while stirring with methanol, until turbidity appears, a...

Embodiment 3

[0031] Firstly, the L-lactic acid to be reacted was dried with 5A molecular sieve for 3 hours, and then placed for use. In a 500ml reaction bottle, add 300g of pre-dried L-lactic acid, blow nitrogen to drive away oxygen, use an oil bath to control the temperature at 60°C, vacuumize and distill water for 1 hour, add N-methyl-propylpiperidine 0.15 g of hexafluorophosphate, the temperature was slowly raised to 105° C., and reacted for 2 hours, the product gradually became viscous, cooled to obtain a white oligomeric solid. Then add 0.15 g of oligomer and N-methyl-propylpiperidine hexafluorophosphate into the polymerization tube, heat and melt under the protection of nitrogen, control the reaction temperature at 140 ° C, and the reaction pressure at 1000 Pa, stir and react for 6 hours, and then Slowly cool down to room temperature to obtain a light yellow solid, add 100 ml of chloroform solvent, stir and dissolve the reactant, then add dropwise while stirring with methanol, until ...

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Abstract

The invention discloses a method for catalytically synthesizing polylactic acid by utilizing ionic liquid. L-lactic acid as material and the ionic liquid as catalyst are melted to be polymerized, so that the polylactic acid is synthesized. Because the ionic liquid which is utilized by the method to catalyze the polylactic acid has good dissolving property for product polymerization, polymerization reaction can be carried out under the condition of homogeneous reaction, consequently, good catalyzation is achieved, the reaction rate is high, and high-molecular weight product can be obtained within 12 to 15 hours; because soluble substances in the ionic liquid can be completely dissolved in solvent in the final precipitation of the product, no residue exists in the product, and thereby residual toxicant does not need to be considered in the prepared product; the preparation of the ionic liquid can be screened according to needed reaction product, good crystal product can be obtained, the degradation of the product is benefited, the degradation period is short, and degradation is thorough.

Description

technical field [0001] The invention belongs to the technical field of material chemistry, and in particular relates to a method for catalytically synthesizing polylactic acid by using ionic liquid. Background technique [0002] Polylactic acid (PLLA) is a widely used biodegradable biomaterial. There are two main methods for the industrial production of polylactic acid. One is ring-opening polymerization (ROP). This method mainly uses a catalyst represented by stannous octoate and is prepared by coordination polymerization. It can prepare higher molecular weight of polylactic acid. However, this method needs to first synthesize the intermediate lactide, and then, under the action of the initiator, open the ring to obtain polylactic acid. The reaction route is longer, consumes more, and the reaction time is as high as 70-120 hours, resulting in a higher cost of the product obtained. Another method is the direct melt polymerization method. This method is a one-step method, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/06C08G63/87C08G63/84
Inventor 任会学应汉杰
Owner NANJING TECH UNIV