Chemical synthesizing process of beta-butyrolactone with lactide copolymer

A technology of chemical synthesis and lactide, applied in the field of polymer synthesis, can solve the problems of poor mechanical properties, low impact strength, difficult processing, etc., and achieve the effects of improved crystallinity and processing performance, and narrow relative molecular mass distribution.

Inactive Publication Date: 2009-07-01
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Pure PHB is a highly isotactic, hard and brittle substance with poor mechanical properties, easy thermal decomposition, poor solvent resistance, and difficult processing (PHB has a narrow processing range and can only be carried out at about 190 ° C, melting point 170 -180°C is close to the decomposition temperature of 205°C; the impact strength is low, and its elongation at break is 6%; and the degradation of PHB in vivo is also extremely slow)
Therefore, a single PHB is subject to certain limitations in medical applications.

Method used

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  • Chemical synthesizing process of beta-butyrolactone with lactide copolymer
  • Chemical synthesizing process of beta-butyrolactone with lactide copolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) the catalyst dibutyl tin dichloride of 0.0033g is packed in the reaction vessel and vacuum-dried for 48 hours, (2) the β-butyrolactone of 0.33g is added in the reaction vessel, (3) the L-butyrolactone of 33g is added Lactide was added to the reaction vessel and the reaction vessel was sealed. (4) Reacting at 120° C. for 48 hours under magnetic stirring to obtain a colorless transparent solid. (5) The product obtained in step (4) was dissolved in dichloromethane to obtain solution A. Add A dropwise to excess anhydrous methanol to obtain a white precipitate B, wash and dry the obtained precipitate B to obtain a copolymer of β-butyrolactone and L-lactide, which 1 The H-NMR spectrum is attached figure 1 , 1.25ppm, 2.47ppm, 2.59ppm, and 5.23ppm belong to the characteristic peaks of the poly 3-hydroxybutyrate segment, and 1.56ppm and 5.15ppm belong to the characteristic peaks of the polylactic acid segment. 13 C-NMR attached figure 2 , 19.8ppm, 40.7ppm, 67.7ppm and 1...

Embodiment 2

[0024] (1) the catalyst dibutyl tin dichloride of 0.33g is packed in the reaction vessel, (2) the β-butyrolactone of 33g is added in the reaction vessel, (3) the D of 0.33g, L-lactate The ester was added to the reaction vessel and the reaction vessel was sealed. (4) React at 40° C. for 48 hours under stirring to obtain a colorless transparent solid. (5) The product obtained in step (4) was dissolved in dichloromethane to obtain solution A. Add A dropwise to excess anhydrous methanol to obtain a white precipitate B, wash and dry the obtained precipitate B to obtain a copolymer of β-butyrolactone and L-lactide, the number-average relative molecular mass of the copolymer is 3000.

[0025] In this example, the catalyst can also be one of dibutyltin oxide, dioctyltin oxide and dimethyl tin oxide, triethylaluminum / water, diethylzinc / water, porphyrin aluminum.

Embodiment 3

[0027] (1) the catalyst dibutyltin dichloride of 0.0033g is packed in the reaction vessel and vacuum-dried for 24 hours, (2) the β-butyrolactone of 0.33g is added in the reaction vessel, (3) the L of 0.55g - Lactide is added to the reaction vessel and the reaction vessel is sealed. (4) Reacting at 40° C. for 720 hours under stirring to obtain a colorless transparent solid. (5) The product obtained in step (4) was dissolved in dichloromethane to obtain solution A. Add A dropwise to excess anhydrous methanol to obtain a white precipitate B, wash and dry the obtained precipitate B to obtain a copolymer of β-butyrolactone and L-lactide, the number-average relative molecular mass of the copolymer is 12000.

[0028] In this example, the catalyst can also be one of dibutyltin oxide, dioctyltin oxide and dimethyl tin oxide, triethylaluminum / water, diethylzinc / water, porphyrin aluminum.

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Abstract

The invention is a chemical synthesis method for synthesizing poly-3-hydroxybutyrate by using the technology of beta-butyrolactone and lactide copolymer. The specific method is: preparing reactants; 1-100 parts by weight of β-butyrolactone and 1-100 parts by weight of lactide; coordination polymerization catalyst or anion polymerization catalyst with a total weight of 0.01-1%; Dry in the reaction container for 0-48 hours; put the reactant into the reaction container and seal the reaction container, and react for 24-720 hours under stirring at 40-150°C to obtain a colorless transparent solid product; dissolve the product in an organic solvent , and then added dropwise to the excess precipitant, the precipitate is poly-3-hydroxybutyrate. Utilizing the preparation method of the β-butyrolactone and L-lactide copolymer of the present invention, the number-average relative molecular mass of the β'-butyrolactone and L-lactide copolymer can reach 1000-40000, and the relative molecular mass The mass distribution is narrow.

Description

technical field [0001] The invention belongs to a polymer synthesis method, in particular to a chemical synthesis method for synthesizing poly-3-hydroxybutyrate by using the technology of β-butyrolactone and lactide copolymer. Background technique [0002] Poly 3-hydroxybutyrate (PHB) is a fully biodegradable plastic. Due to the good biocompatibility of PHB, the application of PHB in electronics, optics, especially in high-tech fields such as biomedicine has been highly valued by people. So far, PHB has been used in absorbable sutures, tissue and bone conduction regeneration membranes, Controlled-release preparations with drugs, absorbable fracture retention splints and fixation nails, and composite bone substitute materials have been extensively studied. [0003] PHB is an intracellular product produced by bacterial fermentation, which exists in the cell in a granular state. In order to use PHB, it must first be produced by fermentation, and then PHB is isolated and extra...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/08
Inventor 原续波马沛生刘峻颜成虎盛京
Owner TIANJIN UNIV
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