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Simple synthesis method of aliphatic series hyperbranched polyester

A technology of hyperbranched polyester and synthesis method, applied in the field of synthesis of hyperbranched polyester, can solve the problems of limited application and development, slow degradation rate, etc., and achieves the effects of wide reaction temperature range, mild conditions and easy removal

Inactive Publication Date: 2018-03-20
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most aliphatic polyesters degrade slowly, which greatly limits their application and development.

Method used

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  • Simple synthesis method of aliphatic series hyperbranched polyester
  • Simple synthesis method of aliphatic series hyperbranched polyester
  • Simple synthesis method of aliphatic series hyperbranched polyester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Into a 250mL three-necked flask were added 0.3mol of hydroxyethyl acrylate, 41mL of acetic anhydride, 85mL of tetrahydrofuran, and 0.3mol of sodium bicarbonate. React the reaction system at 30°C for 12 hours, filter out the solids, add an appropriate amount of dichloromethane, wash with saturated sodium bicarbonate solution, saturated sodium chloride solution, and water three times in sequence, remove water with anhydrous sodium sulfate, and obtain product. figure 1 It is the NMR diagram of the initiator monomer acetoxyethyl methacrylate. It can be seen from the figure that the peak position and integral area of ​​each proton are consistent with the theoretical value. The purity of the synthesized monomer is 99% as measured by high performance liquid chromatography. %, indicating that the initiator monomer with higher purity was successfully synthesized.

Embodiment 2

[0021] Under the protection of argon, 0.2mmol of acetoxyethyl methacrylate, 4mmol of caprolactone, and 0.2mL of toluene were respectively added to a 50mL reaction flask that had been baked repeatedly with a syringe. After freezing-pumping-filling with argon three times, the reaction flask was equilibrated at -30°C for 5 min. Then, under the protection of argon, add 0.2 mmol phosphazene base t-BuP 4 start reacting. After 5 hours, a small amount of benzoic acid was added to terminate the reaction, THF was added to dissolve, the phosphazene base was removed by acidic alumina filtration, n-hexane was settled, and the polymer was obtained by vacuum drying. It is measured that the conversion rate of AcEMA reaches 99.5%, and the conversion rate of caprolactone reaches 99.9%. The number-average molecular weight of gained polymkeric substance is 4900g / mol, and molecular weight distribution is 2.49, by the proton nuclear magnetic spectrogram of product ( figure 2 ) to calculate the ...

Embodiment 3

[0023] Under the protection of argon, 0.2mmol of acetoxyethyl methacrylate, 4mmol of succinic anhydride, and 0.2mL of toluene were respectively added into a 50mL reaction flask that had been baked repeatedly with a syringe. After freezing-pumping-filling with argon three times, the reaction flask was equilibrated at 60°C for 5 minutes. Then, under the protection of argon, add 0.2 mmol phosphazene base t-BuP 4 start reacting. After 1 hour, a small amount of benzoic acid was added to terminate the reaction, THF was added to dissolve, the phosphazene base was removed by acidic alumina filtration, n-hexane was settled, and the polymer was obtained by vacuum drying. It was measured that the conversion rate of AcEMA reached 99.6%, and the conversion rate of succinic anhydride reached 99.0%. The polymer obtained had a number average molecular weight of 6800 g / mol, a molecular weight distribution of 2.01 and a Mark-Howink constant of 0.45.

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Abstract

The invention belongs to the field of synthesis of hyperbranched polyester, and particularly relates to a simple synthesis method of aliphatic series hyperbranched polyester. Firstly, initiator monomers with double bonds at one end and ethyl acetate structure units at the other end are prepared from hydroxyl-containing acrylic ester and acetic anhydride through reaction; then, the initiator monomers are subjected to copolymerization reaction with annular monomers such as lactone, anhydride and cyclic carbonates; the hyperbranched polyester is prepared. Compared with the prior art, the synthesis method of the aliphatic series hyperbranched polyester has the advantages that the synthesis method of the initiator monomers is simple; the polymerization reaction is fast; the conditions are mild;the method is suitable for industrial production and has good application prospects.

Description

technical field [0001] The invention belongs to the synthesis field of hyperbranched polyesters, and in particular relates to a simple synthesis method of aliphatic hyperbranched polyesters. Background technique [0002] Polymer materials are one of the fastest-growing materials in this century, but the use of a large number of polymer materials has brought convenience to people's production and life, but also caused serious environmental pollution. Aliphatic polyester has the characteristics of keeping its performance unchanged during use and rapidly degrading in the natural environment after being discarded, which provides an important way to solve environmental pollution. However, the slow degradation rate of most aliphatic polyesters greatly limits their application and development. Introducing hyperbranched structure into traditional aliphatic polyester is an important method to improve its degradation performance. At present, most hyperbranched polyesters are synthes...

Claims

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Application Information

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IPC IPC(8): C08G63/08C08G63/78C08G63/00
CPCC08G63/08C08G63/00C08G63/78
Inventor 杨宏军左永康黄文艳蒋其民薛小强蒋必彪韩彪
Owner CHANGZHOU UNIV
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