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Method for synthesizing poly hydroxy fatty acid ester block copolymers in situ

A technology of polyhydroxyalkanoate and block copolymers, which is applied in the field of preparation of polyhydroxyalkanoate block copolymers, can solve the problems of toxic solvents, etc., and achieve environmental friendliness, widely available raw materials, and simple synthesis process Effect

Inactive Publication Date: 2009-06-10
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation of the above method block copolymers is carried out in a solvent, and the solvents are all toxic

Method used

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  • Method for synthesizing poly hydroxy fatty acid ester block copolymers in situ
  • Method for synthesizing poly hydroxy fatty acid ester block copolymers in situ
  • Method for synthesizing poly hydroxy fatty acid ester block copolymers in situ

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] At 100°C, 30g of poly-3-hydroxybutyrate (number average molecular weight and molecular weight distribution were 4.5×10 4 and 4.8) were dissolved in a four-necked round-bottomed flask containing 300 mL of diethylene glycol dimethyl ether, condensed and refluxed, fed with nitrogen, and the stirring rate was 300 r / min. After the poly-3-hydroxybutyrate was completely dissolved, the liter Add 60mL of ethylene glycol and 0.3g of dibutyltin dilaurate at a high temperature to 140°C, add 0.3g of dibutyltin dilaurate at every hour after the reaction starts, and continue to pass nitrogen after 8 hours of reaction. , take out the reaction product, precipitate the product with ethanol, vacuum filter, and vacuum-dry at 65° C. to constant weight to obtain low-molecular-weight telechelic poly-3-hydroxybutyrate with hydroxyl end groups at both ends. Put telechelic poly-3-hydroxybutyrate and ε-caprolactone in a molar ratio of 1:20, add a total of 15g into a 250mL four-neck round bottom f...

Embodiment 2

[0032] At 100°C, 30g of poly-3-hydroxybutyrate (number average molecular weight and molecular weight distribution were 1.0×10 5 and 2.9) were dissolved in a four-necked round-bottomed flask containing 300 mL of diethylene glycol dimethyl ether, condensed and refluxed, fed with nitrogen, and the stirring rate was 200 r / min. After the poly-3-hydroxybutyrate was completely dissolved, the liter Add 60mL of ethylene glycol and 0.3g of dibutyltin dilaurate at a high temperature to 140°C, add 0.3g of dibutyltin dilaurate at every hour after the reaction starts, and continue to pass nitrogen after 10 hours of reaction. , take out the reaction product, precipitate the product with ethanol, vacuum filter, and vacuum-dry at 65° C. to constant weight to obtain low-molecular-weight telechelic poly-3-hydroxybutyrate with hydroxyl end groups at both ends. Put telechelic poly-3-hydroxybutyrate and D-lactide in a molar ratio of 1:15, add a total of 15g into a 250mL four-necked round-bottomed f...

Embodiment 3

[0035] At 100°C, 30g of poly-3-hydroxybutyrate (number average molecular weight and molecular weight distribution were 2.5×10 5 and 2.4) were dissolved in a four-neck round-bottomed flask with 300 mL of diethylene glycol dimethyl ether, condensed and refluxed, fed with nitrogen, and the stirring rate was 200 r / min. After the poly-3-hydroxybutyrate was completely dissolved, the liter Add 40mL of ethylene glycol and 0.3g of dibutyltin dilaurate at a high temperature to 140°C, add 0.3g of dibutyltin dilaurate at every hour after the reaction starts, and continue to pass nitrogen after 8 hours of reaction. , take out the reaction product, precipitate the product with ethanol, vacuum filter, and vacuum-dry at 65° C. to constant weight to obtain low-molecular-weight telechelic poly-3-hydroxybutyrate with hydroxyl end groups at both ends. Put telechelic poly-3-hydroxybutyrate and 1,5-dioxolan-2-one in a molar ratio of 1:18, add a total of 15g into a 250mL four-necked round-bottomed f...

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Abstract

The invention relates to an in-situ synthesis method for polyhydroxy fatty acid ester block copolymer. The method comprises the following steps of: (1) mixing polyhydroxy fatty acid ester with diethylene glycol dimethyl ether at the bath ratio of 1:30, heating and stirring the materials, raising the temperature to 140 DEG C, adding dibastic alcohol and organic tin catalyst, taking products out after 4 to 10 hours of reaction and performing precipitation, pumping filtration and drying so as to obtain telechelic-type polyhydroxy fatty acid ester; and (2) mixing the telechelic-type polyhydroxy fatty acid ester with intro-cross ester at the molar ratio of 1:10-20, supplying the two with nitrogen and continuing to heat the two to 120 to 140 DEG C, adding the organic tin catalyst, stirring the materials for 3 to 16 hours for reaction, taking out and dissolving reaction products with chloroform, precipitating and drying the reaction products to constant weight so as to obtain the polyhydroxy fatty acid ester block copolymer. The block copolymer synthesized by the method is controllable in molecular weight, components and the length of every block. The synthesis method has the advantages that raw materials used by the method are wide and easy to get, and the method is simple in synthesis process, performs ring-opening polymerization in a state free from solution, and is environment-friendly.

Description

technical field [0001] The invention belongs to the field of preparation of polyhydroxyalkanoate block copolymers, in particular to a method for synthesizing polyhydroxyalkanoate block copolymers in situ. 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-hydroxybuty...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/06C08G63/78C08G63/685
Inventor 秦宗益朱美芳刘庆生翟光照李虎敏陈龙陈彦模
Owner DONGHUA UNIV
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