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Lactide-epsilon-caprolactone copolymerization catalyst and copolymerization method

A technology of co-polymerization catalyst and lactide, which is applied in the field of lactide/ε-caprolactone co-polymerization catalyst, can solve the problems such as uncontrollable microstructure, and achieve the effects of microstructure controllability, simple reaction method and high catalytic activity

Inactive Publication Date: 2012-07-04
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the microstructure of the copolymers obtained by the metal complex-catalyzed copolymerization of lactide and ε-caprolactone reported so far cannot be adjusted, and is completely determined by the nature of the catalyst, and only copolymers with specific structures can be obtained.

Method used

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  • Lactide-epsilon-caprolactone copolymerization catalyst and copolymerization method
  • Lactide-epsilon-caprolactone copolymerization catalyst and copolymerization method
  • Lactide-epsilon-caprolactone copolymerization catalyst and copolymerization method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] C1-catalyzed copolymerization of racemic lactide and ε-caprolactone to form block copolymers

[0028]

[0029]Under the protection of argon, add racemic lactide (0.432g, 3.0mmol) into the polymerization bottle, dissolve it with 3.0mL of toluene, weigh 0.030mmol of aluminum catalyst C1 and 0.090mmol of n-dodecyl alcohol into the polymerization bottle for 70 °C for 24 hours. Weigh ε-caprolactone (0.456 g, 4.0 mmol) into a polymerization bottle, control the reaction temperature to 90° C., react for 2 hours, and add petroleum ether to terminate the reaction. The solvent was removed, the residue was dissolved in dichloromethane, and methanol was added to precipitate the polymer. Vacuum dried for 24h. Caprolactone conversion: 66%, lactide conversion: 100%, M n =7.1×10 3 g / mol, molecular weight distribution PDI=1.35.

Embodiment 2

[0031] C2-catalyzed copolymerization of racemic lactide and ε-caprolactone to form block copolymers

[0032]

[0033] Under the protection of argon, add ε-caprolactone (0.342g, 3.0mmol) into the polymerization bottle, dissolve it with 3.0mL toluene, weigh 0.030mmol of aluminum catalyst C2 and 0.060mmol of isopropanol into the polymerization bottle and polymerize at room temperature 1 Hour. Racemic lactide (0.288 g, 2.0 mmol) was weighed and added into a polymerization bottle, the reaction temperature was controlled at 70° C., and the reaction was carried out for 20 hours, and petroleum ether was added to terminate the reaction. The solvent was removed, the residue was dissolved in dichloromethane, and methanol was added to precipitate the polymer. Vacuum dried for 24h. Caprolactone conversion: 100%, lactide conversion: 90%, M n =1.0×10 4 g / mol, molecular weight distribution PDI=1.16, polymer glass transition temperature and crystallization temperature: 30°C and 98°C, po...

Embodiment 3

[0035] C3 Catalyzed Copolymerization of L-Lactide and ε-Caprolactone to Block Copolymers

[0036]

[0037] Under the protection of argon, add ε-caprolactone (0.342g, 3.0mmol) into the polymerization bottle, dissolve it with 3.0mL toluene, weigh 0.010mmol of aluminum catalyst C3 and 0.010mmol of amyl alcohol, add it to the polymerization bottle and polymerize at room temperature for 4 hours . Weighed L-lactide (0.432g, 3.0mmol) into a polymerization bottle, controlled the reaction temperature to 100°C, reacted for 48 hours, and added petroleum ether to terminate the reaction. The solvent was removed, the residue was dissolved in dichloromethane, and methanol was added to precipitate the polymer. Vacuum dried for 24h. Caprolactone conversion: 100%, lactide conversion: 82%, M n =6.5×10 4 g / mol, molecular weight distribution PDI=1.22.

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Abstract

The invention relates to a lactide-epsilon-caprolactone copolymerization catalyst and a copolymerization method. The lactide-epsilon-caprolactone copolymerization catalyst relates to a nitrogenous bisphenol oxygen-based binuclear aluminum complex. The copolymerization method comprises the following steps of: adding lactide and epsilon-caprolactone into a reaction system sequentially or simultaneously, and carrying out copolymerization in a solvent-free system or an organic solvent medium under the catalysis of an appropriate of alcohol and nitrogenous bisphenol oxygen-based binuclear aluminum complex; and obtaining a lactide and epsilon-caprolactone copolymer through purifying after the copolymerization is finished. The high-efficiency lactide-epsilon-caprolactone copolymerization catalyst can realize synthesis of a lactide / epsilon-caprolactone segmented copolymer, a gradient copolymer, a wedge-shaped copolymer and a random copolymer. The lactide-epsilon-caprolactone copolymerization catalyst has very remarkably advantages of easily-obtained raw materials, simple polymerization method, various copolymer structures, regulating and controlling availability, higher catalysis activity and capabilities of obtaining the lactide and epsilon-caprolactone copolymer with high molecular weight and meeting requirements of the industrial department. A structural formula of the lactide-epsilon-caprolactone copolymerization catalyst is shown in a figure described in the specification.

Description

technical field [0001] The invention relates to a lactide / ε-caprolactone copolymerization catalyst and a method for catalyzing the lactide / ε-caprolactone copolymerization. Background technique [0002] Aliphatic polyester materials have been extensively studied due to their good biocompatibility and degradability. In recent years, it has been widely used in the field of biomedicine, such as slow-release materials for drugs, implanted materials in vivo, surgical sutures, orthopedic enclosure materials, etc.; in addition, it has also achieved certain results in the packaging industry, textile industry and agricultural industry. Progress. The monomers currently used in the research of polylactone materials include lactide, ε-caprolactone, glycolate and butyrolactone; among the above monomers, lactide can be obtained by dimerization of lactic acid, and lactic acid It can be fermented from crops, so the source of raw materials is wide and the price is low. The good machinabili...

Claims

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Application Information

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IPC IPC(8): C08G63/08C08G63/84
Inventor 马海燕王原
Owner EAST CHINA UNIV OF SCI & TECH
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