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A kind of preparation method of polyester

A polyester and cyclic ester technology, applied in the field of organic synthesis, can solve the problems of unfavorable material stability, uncontrollable reaction process, wide molecular weight distribution, etc., and achieve great commercial application potential, narrow molecular weight distribution index, and narrow molecular weight distribution. Effect

Active Publication Date: 2022-04-22
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The traditional method of preparing polyester is mainly polycondensation method. This method usually requires high temperature, consumes a lot of energy, and the obtained product has a low molecular weight and a wide molecular weight distribution. The reaction process is uncontrollable, which is not conducive to the stability of the material.

Method used

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  • A kind of preparation method of polyester
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  • A kind of preparation method of polyester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0088] In a 10 mL polymerization tube, add δ-valerolactone (0.27 ml, 3 mmol), squaramide derivative 7 (0.122 g, 0.3 mmol), potassium tert-butoxide (0.011 g, 0.1 mmol), benzyl alcohol (10.34 μL , 0.1mmol), stirred magnetically for 4 hours at 90°C, stopped the reaction, added a small amount of dichloromethane dropwise to the resulting mixture to dissolve, then slowly dropped the resulting solution into cold methanol, and a white polymer was precipitated. After centrifugation, vacuum Dried to obtain the product 0.37g of snow-white color and luster, transformation rate is 95%, the number average molecular weight M of polyvalerolactone n It is 3588g / mol, and the molecular weight distribution PDI is 1.08. The hydrogen spectrum of the product is as figure 1 As shown, the size exclusion chromatogram of the product is shown as figure 2 shown.

Embodiment 2

[0090] In a 10 mL polymerization tube, add D-lactide (0.072 g, 0.5 mmol), squaramide derivative 4 (0.0894 g, 0.3 mmol), sodium tert-butoxide (0.0096 g, 0.1 mmol), pentaerythritol (9.7 μL , 0.1mmol), magnetically stirred for 24 hours under the condition of 200°C, stopped the reaction, added a small amount of dichloromethane dropwise to the resulting mixture to dissolve, then slowly dropped the resulting solution into cold methanol, a white polymer was precipitated, and after centrifugation, vacuum Dry to obtain the product 0.033g of snow-white color and luster, conversion rate is 67.1%, the number average molecular weight M of poly-D-lactide n It is 1300g / mol, and the molecular weight distribution PDI is 1.16.

Embodiment 3

[0092] In a 10 mL polymerization tube, add L-lactide (7.2 g, 50 mmol), squaramide derivative 12 (0.0986 g, 0.3 mmol), lithium tert-butoxide (0.008 g, 0.1 mmol), benzyl alcohol (10.0 μL , 0.1mmol), magnetically stirred at 130°C for 8 hours, stopped the reaction, added a small amount of dichloromethane dropwise to the resulting mixture to dissolve, then slowly dropped the resulting solution into cold methanol, a white polymer was precipitated, and was centrifuged, vacuum Dried to obtain the product 5.6g of snow-white color and luster, conversion rate is 97%, the number average molecular weight M of poly-L-lactide n It is 37000g / mol, and the molecular weight distribution PDI is 1.19. The hydrogen spectrum of the product is as image 3 As shown, the size exclusion chromatogram of the product is shown as Figure 4 shown.

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Abstract

The invention discloses a method for preparing polyester. In the presence of an initiator, a catalytic system composed of a square amide derivative shown in formula I and an alkali metal alkoxide shown in formula II is used to catalyze the ring opening of a cyclic ester monomer Polymerization to obtain polyester compounds. The polyester obtained by the method of the present invention has a narrow molecular weight distribution, no chain transesterification reaction, high yield, white color, great potential for commercial application in the field of biomedicine and microelectronics, and the catalytic efficiency of the catalyst used in the reaction is higher. The response is milder.

Description

technical field [0001] The invention belongs to the field of organic synthesis, in particular to a preparation method of polyester. Background technique [0002] Among many synthetic polymer materials, aliphatic polyester occupies an important position due to its excellent biodegradability, bioabsorbability and biocompatibility, and has become a research hotspot in recent years. Due to the easily hydrolyzed ester group in the molecular structure of this kind of polyester, it is easy to gradually decompose into oligomers or monomers in the presence of water and microorganisms, and then be metabolized into carbon dioxide and water, so it can show certain biodegradability. Compatibility, which has great application potential in biomedicine, tissue engineering and other fields. [0003] The traditional method of preparing polyester is mainly polycondensation method. This method usually requires high temperature, consumes a lot of energy, and the obtained product has a low molec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/685C08G63/78C08G63/83C08G64/30C08G64/16
CPCC08G63/6852C08G63/83C08G63/78C08G64/30C08G64/1641
Inventor 郭凯周方园李振江胡永铸刘博李洁张智浩
Owner NANJING TECH UNIV
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