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Method for preparing polylactic acid group block copolymer

A block copolymer and polylactic acid-based technology, which is applied in the field of preparation of polylactic acid-based block copolymers, can solve the problems of limited wide application, high production cost, insufficient polylactic acid toughness, etc., and achieves simple process and easy industrial production. Effect

Active Publication Date: 2008-02-13
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this kind of polylactic acid has insufficient toughness and relatively high production cost, which limits its wide application.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) 400g of L-lactic acid and 1,4-butanediol carbonate (molecular weight 2000) 20g are joined in the vacuum reactor, add catalyzer stannous octoate 0.5%, vacuumize, the pressure in the reactor is 1500Pa, The temperature is 100°C, react for 2 hours, then reduce the pressure in the reactor to below 100Pa, raise the reaction temperature to 160°C, and continue the reaction for 16h to obtain M w =0.8×10 3 ~3.0×10 4 Lactic acid prepolymer;

[0023] (2) The lactic acid prepolymer obtained in the step (1) is added in the reactor, vacuumized, logical N 2 Gas, add chain extender hexamethylene diisocyanate (HDI) and catalyzer tin protochloride, carry out chain extension reaction, wherein PLA and HDI molar ratio are 3: 1, stannous octoate add-on is 1%; Reaction temperature At 170°C, react for 30 minutes to obtain the desired product, the product weight average molecular weight M w 1×10 5 ~2×10 5 .

Embodiment 2

[0025] (1) 800g of L-lactic acid and 1,4-butanediol polycarbonate (molecular weight 3000) 40g are added in the vacuum reactor, add catalyst stannous chloride 0.7%, vacuumize, the pressure in the reactor is 1000Pa , the temperature was 120°C, reacted for 5 hours, then lowered the pressure in the reactor to below 100Pa, raised the reaction temperature to 200°C, and continued to react for 15 hours to obtain M w =0.8×10 3 ~3.0×10 4 Lactic acid prepolymer;

[0026] (2) The lactic acid prepolymer obtained in the step (1) is added in the reactor, vacuumized, logical N 2 gas, add chain extender hexamethylene diisocyanate (HDI) and catalyst triethylenediamine, carry out chain extension reaction, wherein the molar ratio of PLA and HDI is 2: 1, and the addition of triethylenediamine is 0.5% ; Reaction temperature is 150 ℃, reacts for 50 minutes, promptly obtains desired product, and this product weight-average molecular weight M w 1×10 5 ~2×10 5 .

Embodiment 3

[0028] (1) 800g of L-lactic acid and 1,6-hexanediol polycarbonate (molecular weight 4000) 40g are added in the vacuum reactor, add catalyst stannous bromide 1%, vacuumize, the pressure in the reactor is 1800Pa , the temperature was 110°C, reacted for 3 hours, then lowered the pressure in the reactor to below 100Pa, raised the reaction temperature to 150°C, and continued to react for 20 hours to obtain M w =0.8×10 3 ~3.0×10 4 Lactic acid prepolymer;

[0029] (2) The lactic acid prepolymer obtained in the step (1) is added in the reactor, vacuumized, logical N 2 Gas, add chain extender hexamethylene diisocyanate (HDI) and catalyzer dibutyltin dilaurate, carry out chain extension reaction, wherein PLA and HDI molar ratio are 2.5: 1, dibutyltin dilaurate add-on is 2%; the reaction temperature is 160°C, and after 20 minutes of reaction, the required product is obtained, and the weight average molecular weight of the product is M w 1×10 5 ~2×10 5 .

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Abstract

The invention belongs to the technological field of polymer material, particularly relating to a preparation method of the poly-lactic acid block copolymer. The invention uses the melting and direct polymerization method to prepare the lactic acid prepolymer, and then uses the chain extension method to prepare the poly lactic acid multi-block copolymer with the high molecular weight. The concrete steps are: first the lactic acid and aliphatic polycarbonate diol are used to react under the condition of the presence of the catalyst and to direct polycondensate to synthesize the hydroxyl-terminated p lactic acid prepolymer; then the chain extender and catalyst are added; with the presence of N2, vacuum; the reaction is kept for 10 to 50 minutes at the temperature of 150 to 300 Celsius system; finally the poly lactic acid multi-block copolymer with the high molecular weight can be made. The process of the method of the invention is simple and easy for the industrialized production; the copolymer resin product produced in the invention is completely biodegradable and the application scope is wide.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a preparation method of a polylactic acid-based block copolymer. Background technique [0002] Polylactic acid (Poly lactic acid, PLA) is a type of polymer chemically synthesized from microbial fermentation product lactic acid as a monomer. It is a non-toxic, non-irritating, biocompatible, and biodegradable polymer. Ester linear biodegradable polymer materials. Lactic acid can be obtained by fermenting starch, and starch has a wide range of sources, and renewable natural plants, such as sweet potatoes, corn and other grains can be used as its raw materials. [0003] Patent CN1298892 discloses a method for preparing lactic acid direct condensation polymerization polylactic acid biodegradable material, and the obtained biodegradable polylactic acid has a weight average molecular weight of 100,000. However, this kind of polylactic acid has insufficient toughn...

Claims

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Application Information

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IPC IPC(8): C08G63/91C08G63/64C08G63/80
CPCC08G2261/126C08G63/78C08G63/912C08G63/64C08G63/08
Inventor 任杰杨铭顾书英于涛任天斌
Owner TONGJI UNIV
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