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Preparation method of comb-like copolymer containing poly-hydroxycarboxylic acid

A technology of comb copolymer and hydroxycarboxylic acid, which is applied in the field of preparation of comb copolymer, and can solve the problems of high production cost and low thermal stability of the copolymer

Inactive Publication Date: 2014-03-26
TORAY ADVANCED MATERIALS RES LAB CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the problems of non-biological sources of monomers, high production costs, and low thermal stability of the obtained copolymers in the existing method for preparing polylactic acid copolymers with relatively high Tg, the present invention discloses a method using sulfonic acid as a catalyst for Hydroxycarboxylic acid or hydroxycarboxylic acid oligomers are polycondensed, and polyhydroxycarboxylic acid is capped with a compound containing a polycondensable functional group and a double bond at the same time and only has one double bond and one or more ring structures And the double bond is shared with one of the rings of the ring structure and only one carbon atom is used for free radical polymerization to obtain a comb copolymer; or a compound containing both a polycondensable functional group and a double bond and a compound with only A double bond and one or more than one ring structure, and the double bond is shared with the ring of one of the ring structures and only one carbon atom is used for free-radical copolymerization of olefinic compounds with sulfonic acid as catalyst p-hydroxycarboxylic acid Or hydroxycarboxylic acid oligomers undergo polycondensation product reaction to obtain comb copolymer

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example 1

[0049] After pouring 100 g of 90 wt % L-lactic acid aqueous solution into a 500 mL four-necked flask, the flask was placed in an oil bath. Install a stirrer on the four-neck flask, insert a thermocouple thermometer, connect the vacuum pipeline and the nitrogen pipeline and replace with nitrogen for 3 times, then raise the temperature of the oil bath to 120°C for dehydration. The system pressure gradually decreased from normal pressure to 5KPa within 60 minutes from the start of dehydration; then continued dehydration at 5KPa for 1.5 hours (a total of 2.5 hours of dehydration). Then the temperature of the system was raised to 190°C, the pressure was gradually reduced from normal pressure to 0.3KPa within 2 hours and the pressure was kept at 0.3KPa to obtain a polylactic acid prepolymer after melt polymerization for 28 hours (30 hours in total). By testing the product sample, the number average molecular weight Mn: 2000 was obtained.

preparation example 2

[0051] After pouring 100 g of 90 wt % L-lactic acid aqueous solution into a 500 mL four-necked flask, the flask was placed in an oil bath. Install a stirrer on the four-neck flask, insert a thermocouple thermometer, connect the vacuum pipeline and the nitrogen pipeline and replace with nitrogen for 3 times, then raise the temperature of the oil bath to 120°C for dehydration. The system pressure gradually decreased from normal pressure to 5KPa within 60 minutes from the start of dehydration; then continued dehydration at 5KPa for 1.5 hours (a total of 2.5 hours of dehydration); at this time, after returning the system pressure to normal pressure with nitrogen, add p-toluenesulfonic acid 306mg. Then the temperature of the system was raised to 160°C, the pressure was gradually reduced from normal pressure to 0.3KPa within 1 hour and the pressure was kept at 0.3KPa to obtain a polylactic acid prepolymer after melt polymerization for 0.5 hours (1.5 hours in total). By testing the ...

preparation example 3

[0053] After adding 90 g of L-lactic acid oligomers and 722 mg of methanesulfonic acid to a 500 mL four-necked flask, the flask was placed in an oil bath. Install a stirrer on the four-neck flask, insert a thermocouple thermometer, connect the vacuum pipeline and nitrogen pipeline and replace with nitrogen for 3 times, raise the temperature of the system to 170°C, and gradually reduce the pressure from normal pressure to 0.1KPa within 0.5 hours And keeping the pressure at 0.1KPa, the polylactic acid prepolymer was obtained after melt polymerization for 0.5 hours (1 hour in total). By testing the product sample, the number average molecular weight Mn: 460 was obtained.

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Abstract

The invention discloses a preparation method of a comb-like copolymer containing poly-hydroxycarboxylic acid. The method is characterized in that catalysts are not used or a catalyst is utilized for performing polycondensation on hydroxycarboxylic acid or a hydroxycarboxylic acid oligomer, and then a compound containing a polycondensation functional group and a double-bond is utilized for blocking poly-hydroxycarboxylic acid, an olefin compound containing a double-bond and one or more cyclic structures is utilized for performing free radical polymerization, so as to obtain the comb-like copolymer, wherein the double-bond shares one and only carbon atom with the cycle of one of the cyclic structures. The preparation method of the polylactic acid copolymer has the advantages that the monomer serves as the biogenetic derivation, the production cost is relatively low, and the prepared product has the advantages of high heat stability, high Tg and the like.

Description

technical field [0001] The invention belongs to the field of polymer materials, and in particular relates to a preparation method of a comb copolymer containing polyester. Background technique [0002] Polylactic acid (PLA) is a degradable material derived from renewable resources that has been studied and applied relatively frequently at present. It is a non-toxic and non-irritating material prepared from lactic acid obtained by starch fermentation (or chemical synthesis) as the basic raw material. Environmentally friendly material, it not only has good physical properties, but also has good biocompatibility and degradation performance. At present, there are two main factors that limit the wide application of polylactic acid: one factor is the high production cost and high price. The main reason for the high production cost is that the polymerization route adopted by the vast majority of applied polylactic acid is an indirect (ring-opening) method, that is, the dehydration...

Claims

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Application Information

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IPC IPC(8): C08F283/02C08G63/06C08G63/08C08G63/78
Inventor 左璞晶宋婷婷何勇
Owner TORAY ADVANCED MATERIALS RES LAB CHINA