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Method for preparing polyhydroxy fatty acid ester with high thermal stability

A technology of polyhydroxyalkanoate and high thermal stability, which is applied in the field of preparation of high thermal stability polyhydroxyalkanoate, can solve the problems of poor thermal stability and narrow processing window, and achieves good thermal stability, wide processing window, Simple preparation process

Inactive Publication Date: 2008-03-26
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

By using bis(2-oxazoline) as a modifier to prepare polyhydroxyalkanoate with high thermal stability, the problems of poor thermal stability and narrow processing window of polyhydroxyalkanoate are solved, and the existing blending technology is overcome. The influence of the second component on the biological characteristics of polyhydroxyalkanoate makes up for the insufficiency that homopolymer and modified polyhydroxyalkanoate cannot be separated during graft modification, and expands the application of polyhydroxyalkanoate in the field of ordinary plastics and Biomedical and other aspects of the application range

Method used

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  • Method for preparing polyhydroxy fatty acid ester with high thermal stability
  • Method for preparing polyhydroxy fatty acid ester with high thermal stability
  • Method for preparing polyhydroxy fatty acid ester with high thermal stability

Examples

Experimental program
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Effect test

Embodiment 1

[0023]With 40 milliliters of N, N'-dimethylformamide, the weight-average molecular weight and molecular weight distribution are 100,000 and 3.2 respectively, and the HV content is 2.6mol% poly(3-hydroxybutyrate-co-3-hydroxyvaleric acid ester) 1.0 g was added into a 100 ml three-necked round-bottomed flask, and after 5 minutes of feeding nitrogen, heated and stirred in an oil bath at 70°C for 50 minutes to make poly(3-hydroxybutyrate-co-3-hydroxyvalerate) complete Dissolve, then heat to 95°C, add 2 according to the molar ratio of poly(3-hydroxybutyrate-co-3-hydroxyvalerate) to 2,2'-bis(2-oxazoline) is 2.0, 2'-bis(2-oxazoline), react for 3 hours (the reaction is carried out under the condition of nitrogen protection), stop heating, continue to pass nitrogen until the temperature drops below 50°C, take out the reaction product and precipitate it with absolute ethanol, vacuum Suction filtration and vacuum drying at 50° C. for 24 hours. Measured by TGA, the initial degradation tem...

Embodiment 2

[0025] With 20 milliliters of 1,2-dichloroethane, weight average molecular weight and molecular weight distribution are respectively 140,000 and 1.2, and HV content is the poly(3-hydroxybutyrate-co-3-hydroxyvalerate) of 1.0mol%. Add 1.0 g in a 100 ml three-necked round-bottomed flask, feed nitrogen gas for 15 minutes, heat and stir in an oil bath at 60°C for 30 minutes to completely dissolve poly(3-hydroxybutyrate-co-3-hydroxyvalerate) , then heated to 85°C, and added according to the ratio of poly(3-hydroxybutyrate-co-3-hydroxyvalerate) to 1,2-bis(2-oxazoline-2)ethane molar ratio of 1.0 1,2-bis(2-oxazoline-2)ethane, reacted for 6 hours (the reaction was carried out under the condition of nitrogen protection), stopped heating, continued nitrogen flow until the temperature dropped below 50°C, and took out the reaction product with a Precipitate with water and ethanol, vacuum filter, then vacuum dry at 50°C for 24 hours to constant weight. Measured by TGA, the initial degradati...

Embodiment 3

[0027] With 50 milliliters of diethylene glycol dimethyl ether, the weight average molecular weight and molecular weight distribution are respectively 150,000 and 2.8, and the HV content is 15.0mol% poly(3-hydroxybutyrate-co-3-hydroxyvalerate) 1.0 gram was added in the three-neck round-bottomed flask of 100 milliliters, after feeding nitrogen for 8 minutes, 80 ℃ of oil baths were heated and stirred for 1 hour and poly(3-hydroxybutyrate-co-3-hydroxyvalerate) was completely dissolved, and then Heat to 100°C, add 1 according to the molar ratio of poly(3-hydroxybutyrate-co-3-hydroxyvalerate) to 1,4-bis(2-oxazoline-2)butane is 0.7, 4-bis(2-oxazoline-2)butane, reacted for 4 hours (the reaction was carried out under the condition of nitrogen protection), stopped heating, continued nitrogen flow until the temperature dropped below 50°C, and took out the reaction product with anhydrous Precipitate with ethanol, vacuum filter, and then vacuum dry at 50°C for 22 hours. Measured by TGA, ...

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Abstract

The present invention relates to preparation process of high heat stability polyhydroxy fatty acid ester. The preparation process includes dissolving polyhydroxy fatty acid ester in organic solvent, and reacting with modifier bis(2-oxazolinyl) at 85-125 deg.c for 1-16 hr, with the molar ratio between polyhydroxy fatty acid ester and bis(2-oxazolinyl) being 0.5-2.0. The high heat stability polyhydroxy fatty acid ester has high heat stability, wide machining window, and expanded application range in common plastic, biomedicine and other fields.

Description

technical field [0001] The invention belongs to the field of preparation of modified polyhydroxyalkanoate, in particular to a preparation method of polyhydroxyalkanoate with high thermal stability. Background technique [0002] Polyhydroxyalkanoate is a kind of biological polyester synthesized by microorganisms, and it is the only thermoplastic polymer found so far in which the properties of natural polymers are comparable to those of synthetic polymers. Poly(3-hydroxybutyrate) and poly(3-hydroxybutyrate-co-3-hydroxyvalerate) are the most important varieties of polyhydroxyalkanoate, which have been produced industrially. It has good biocompatibility, biodegradability, and renewable resources. However, its (1) stereoregularity is good and the crystallization tendency is large; (2) the glass transition temperature is low, and secondary crystallization is prone to occur during storage; (3) in poly(3-hydroxybutyrate-co-3- (4) In the crystal lattice of poly-3-hydroxybutyrate, t...

Claims

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Application Information

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IPC IPC(8): C08G63/91C08G63/06C08K5/353
Inventor 刘庆生秦宗益朱美芳梁霞吴文华成龙陈彦模
Owner DONGHUA UNIV