Method for preparing aliphatic polyesters

A technology of aliphatic polyester and caprolactone, which is applied in the field of biodegradable polymer synthesis, can solve the problems of difficult recycling, difficult to control the properties of aliphatic polyester, and expensive catalysts, etc., and achieve a narrow molecular weight distribution index , high biological safety, the effect of less catalyst consumption

Active Publication Date: 2016-03-02
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, organic catalysts are often used in the preparation of aliphatic polyesters to catalyze the reaction (CN102449027A), but there are still some defects, including expensive catalysts used, difficult to recycle, difficult to control the properties of aliphatic polyesters synthesized, etc.

Method used

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  • Method for preparing aliphatic polyesters
  • Method for preparing aliphatic polyesters
  • Method for preparing aliphatic polyesters

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] In a 5 mL polymerization tube, add valerolactone (0.1812 mL, 2 mmol), 2 mL of dichloromethane, thiourea TU 5 (0.033 g, 0.067 mmol), TFA trifluoroacetic acid (5 microliters, 0.067 mmol), 6.6 microliters (0.067 mmol) of benzyl alcohol were stirred at 20° C. for 37 hours. After the reaction was finished, the reaction was terminated with a small amount of triethylamine. The reaction solution was rotary evaporated, and the obtained crude product was dissolved in a minimum amount of dichloromethane, and then added into a cold methanol solution, and a polymer was precipitated. Centrifuge to obtain a white solid, which is transferred to a vacuum oven for drying. polymer structure through 1 HNMR identification, molecular weight and dispersion of the polymer were determined by GPC. After determination, the transformation rate of polymer is 99%, and productive rate is 61%, M n / M w is 1.30.

Embodiment 2

[0061] In a 5 mL polymerization tube, add caprolactone (0.2134 mL, 2 mmol), dichloromethane 2 mL, thiourea TU 5 (0.033 g, 0.067 mmol), TFA trifluoroacetic acid (5 microliters, 0.067 mmol), 6.6 microliters of benzyl alcohol (0.067 mmol) and stirred at 20° C. for 58 hours. After the reaction was finished, the reaction was terminated with a small amount of triethylamine. The reaction solution was rotary evaporated, and the obtained crude product was dissolved in a minimum amount of dichloromethane, and then added into a cold methanol solution, and a polymer was precipitated. Centrifuge to obtain a white solid, which is transferred to a vacuum oven for drying. polymer structure through 1 HNMR identification, molecular weight and dispersion of the polymer were determined by GPC. After determination, the transformation rate of polymer is 99%, and productive rate is 68%, M n / M w is 1.33.

Embodiment 3

[0063] In a 5 mL polymerization tube, add valerolactone (0.1812 mL, 2 mmol), 2 mL of dichloromethane, thiourea TU 5 (0.033 g, 0.067 mmol), TFA trifluoroacetic acid (5 microliters, 0.067 mmol), 6.6 microliters (0.067 mmol) of benzyl alcohol were stirred at 40° C. for 30 hours. After the reaction was finished, the reaction was terminated with a small amount of triethylamine. The reaction solution was rotary evaporated, and the obtained crude product was dissolved in a minimum amount of dichloromethane, and then added into a cold methanol solution, and a polymer was precipitated. Centrifuge to obtain a white solid, which is transferred to a vacuum oven for drying. polymer structure through 1 HNMR identification, molecular weight and dispersion of the polymer were determined by GPC. After determination, the transformation rate of polymer is 98%, and productive rate is 62%, M n / M w is 1.32.

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Abstract

The invention discloses a method for preparing aliphatic polyesters and belongs to the field of macromolecular synthetic chemistry. According to the method, delta-valerolactone (delta-VL) and epsilon-caprolactone (epsilon-CL) monomers serve as reaction substrates, a combination of thiourea and carboxylic acid serves as a co-catalyst, organic alcohol serves as an initiator, a polymerization reaction is carried out for 25-195 hours in an organic solvent or under solvent-free conditions, and polyvalerolactone and polycaprolactone are obtained after the reaction ends. According to the method provided by the invention, the disadvantage that metal residual is caused due to the fact that polyvalerolactone and polycaprolactone are prepared by using a metal catalyst in the past is overcome, and the preparation rate is accelerated. The method, which is simple in process, low in cost and high in catalysis efficiency and is environment-friendly, is provided for preparing polyvalerolactone and polycaprolactone.

Description

technical field [0001] The invention belongs to the technical field of biodegradable polymer synthesis, and in particular relates to an organocatalytic preparation method of aliphatic polyvalerolactone and polycaprolactone. Background technique [0002] Polyvalerolactone (PVL) and polycaprolactone (PCL), that is, aliphatic polyesters, have attracted widespread attention in recent years due to their good biodegradability and biocompatibility. [0003] Aliphatic polyesters have great application value in the fields of environment-friendly materials and biomedical materials. In industry, polyvalerolactone (PVL) and polycaprolactone (PCL) have excellent biocompatibility and biodegradability as aliphatic polyesters, so materials with special functions can be obtained through modification, thereby It has been widely used in drug carriers, tissue engineering materials, medical sutures, and medical screws. At the same time, aliphatic polyesters are also a class of polymers with go...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/08C08G63/87
Inventor 郭凯李晓佩李振江徐嘉熙陈诚徐松泉赵成旭智绪王慧颖
Owner NANJING UNIV OF TECH
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