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Preparation method of biodegradation polylactic acid based multicomponent block polymer

A block polymer, polylactic acid-based technology, which is applied in the field of preparation of biodegradable polylactic acid-based multi-block polymers, can solve problems such as no diols involved, achieve fast degradation speed, easy industrialized integrated production, simple conditional effect

Inactive Publication Date: 2007-03-14
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above research involves the influence of two different types of chain extenders on the chain extension reaction, as well as the synergistic effect, but its research is limited to the chain extension reaction of lactic acid copolymer prepolymers, and does not involve diols and dicarboxylic acids or dicarboxylic anhydrides. The introduction of polycondensation reaction prepolymerization products as chain extension units, as well as the formation of new materials and new properties

Method used

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  • Preparation method of biodegradation polylactic acid based multicomponent block polymer
  • Preparation method of biodegradation polylactic acid based multicomponent block polymer
  • Preparation method of biodegradation polylactic acid based multicomponent block polymer

Examples

Experimental program
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Effect test

Embodiment 1

[0038] (1) Put 800g of L-lactic acid purified by vacuum distillation into a vacuum reactor, add 0.8g of stannous chloride, vacuumize, control the pressure of the reactor at 1.0kPa, raise the temperature of the reactor to 100°C, and react for 5 hours ; Then the temperature of the reactor rose to 140°C, the pressure dropped below 60Pa, and the reaction was continued for 15 hours to obtain the weight average molecular weight M W =2×10 4 -5×10 4 lactic acid prepolymer;

[0039] (2) the linear polyester oligomer polybutylene adipate (PBA), the lactic acid prepolymer (PLA) that step (1) obtains, the chain extender hexamethylene diisocyanate (HDI) respectively Add it to the reactor, the molar ratio of PBA to PLA is 1:9, the molar ratio of the sum of PBA and PLA to HDI is 1:1, and fill with N 2 Air, vacuum, after repeated operations several times, the system pressure dropped below 60Pa, and then reacted at 150°C for 10 minutes, N 2 Discharging under air protection, the desired pro...

Embodiment 2

[0041] (1) Add 800 g of D, L-lactic acid purified by vacuum distillation into a vacuum reactor, add 0.4 g of stannous octoate, vacuumize, control the pressure of the reactor at 1.5 kPa, raise the temperature of the reactor to 110 ° C, and react 4 hours; then the temperature of the reactor rose to 160°C, the pressure dropped below 60Pa, and the reaction was continued for 14 hours to obtain the weight average molecular weight M W =2×10 4 -5×10 4 lactic acid prepolymer;

[0042] (2) Lactic acid prepolymer (PLA), linear polyester oligomer polybutylene succinate (PBS), chain extender diphenylmethane diisocyanate (MDI) obtained in step (1) Add to the reaction kettle respectively, the molar ratio of PBS and PLA is 1:1, the molar ratio of the sum of the molar amounts of PBS and PLA to MDI is 1:1.3, and fill with N 2 Gas, vacuum, after repeated operations several times, the system pressure dropped below 60Pa, and then reacted at 180°C for 20 minutes, N 2 Discharging under air prote...

Embodiment 3

[0044] (1) 400g of L-lactic acid purified by vacuum distillation, D, 400g of L-lactic acid are added to a vacuum reactor, 0.8g of germanium chloride is added, vacuumized, the pressure of the reactor is controlled at 2.0KPa, and the temperature of the reactor is raised to 120°C, react for 3 hours; the temperature of the reactor rises to 180°C, the pressure drops below 60Pa, and the reaction continues for 12 hours to obtain the weight average molecular weight M W =2×10 4 -5×10 4 lactic acid prepolymer;

[0045] (2) Lactic acid prepolymer (PLA), linear polyester oligomer polyhexamethylene adipate (PHA) obtained in step (1), chain extender 4,4'-dicyclohexylmethane Add isocyanate (DES) into the reactor respectively, the molar ratio of PHA and PLA is 9:1, the molar ratio of the sum of PHA and PLA to DES is 1:1.5, and fill with N 2 Gas, vacuum, after repeated operations several times, the system pressure dropped below 60Pa, and then reacted at 200°C for 30 minutes, N 2 Dischargin...

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Abstract

The present invention belongs to the field of polymer material technology, and is especially preparation process of biodegradable polylactic acid based polynary block polymer. The preparation process includes the first polycondensation of lactic acid, lactic acid and small molecular dibasic alcohol, or lactic acid and small molecular dibasic carboxylic acid to obtain lactic acid prepolymer in certain molecular weight; and the subsequent adding ester oligomer and chain expander to react under N2 atmosphere at pressure below 60 Pa and temperature of 150-230 deg.c for 10-45 min to obtain the biodegradable resin with high molecular weight. The biodegradable resin has flexibility and heat resistance higher than that of lactic acid homopolymer, adjustable degradation speed, simple preparation process and wide application, and the preparation process is easy use in industrial production.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a preparation method of fully biodegradable polylactic acid-based multi-block polymers. Background technique [0002] Due to its special properties such as good biodegradability, biocompatibility and absorbability, biodegradable polymer materials have developed rapidly in medicine, medicine, and the environment, especially polylactic acid polymers, the main source of lactic acid It is used in renewable resource crops, so it has become a hot spot in the field of materials science. At present, the main methods of preparing polylactic acid are ring-opening polymerization of lactide and direct polycondensation of lactic acid. The lactide ring-opening polymerization method is easy to obtain high molecular weight polylactic acid polymer materials, but the preparation of the cyclic intermediate lactide makes the synthesis route of the polymer lengthy and the cost ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G81/00C08G63/08C08G63/18C08G63/91
Inventor 任杰赵鹏任天斌顾书英
Owner TONGJI UNIV
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