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Cyclic esters compound polymerization catalyst, preparation method and application thereof

A technology for polymerization catalysts and compounds, which is applied in the fields of polymerization catalysts, preparation methods and applications of cyclic ester compounds, can solve the problems of high energy consumption, low melting point of polymers, high biological toxicity, etc., achieve high reaction efficiency, few reaction steps, easy-to-handle effects

Inactive Publication Date: 2009-09-23
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most initiators initiate the polymerization of cyclic ester monomers under high temperature conditions. This polymerization process has the disadvantages of high energy consumption and easy occurrence of racemization reactions at high temperatures (Macromolecules 2001, 34, 3863-3868), The resulting polymer has a low melting point and poor mechanical properties
At the same time, many initiators themselves have high biological toxicity, and the initiators remain in the polymer after polymerization and are difficult to completely remove, which limits the application of this polymer in the medical and pharmaceutical fields.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1: the synthesis of two (bistrimethylsilyl amino) zinc

[0025] Add 10.5ml of hexamethyldisilazylamine into the three-necked flask, slowly drop in 20ml of LiBu (2.5N hexane solution) under the action of an ice-salt bath (-10°C), stir and react for 10 hours, and pour into the three-necked flask after the reaction Add 3.46g of anhydrous ZnCl 2 , and added 30ml of anhydrous ether, and reacted at 0°C for 10 hours. After the reaction, the excess hexamethyldisilazyl ammonia and the solvent were drained, and then the product was separated by vacuum distillation at 130°C. The total reaction The yield was 82%.

Embodiment 2

[0026] Embodiment 2: the synthesis of two (bistrimethylsilyl amino) zinc

[0027] Add 12ml of hexamethyldisilazylamine into the three-necked flask, slowly add 20ml of LiBu (2.5N hexane solution) dropwise at 0°C, stir and react for 3 hours, and add 3.46g of anhydrous ZnCl to the three-necked flask after the reaction 2 , and added 30ml of anhydrous tetrahydrofuran, and reacted at 70°C for 4 hours. After the reaction, the excess hexamethyldisilazylammonium and solvent were drained, and then the product was separated by vacuum distillation at 130°C. The total reaction The yield was 90%.

Embodiment 3

[0028] Embodiment 3: the synthesis of two (bistrimethylsilyl amino) zinc

[0029] Add 15ml of hexamethyldisilazylamine into the three-necked flask, slowly add 20ml of LiBu (2.5N hexane solution) dropwise at 20°C, stir and react for 10 minutes, and add 3.46g of anhydrous ZnCl to the three-necked flask after the reaction 2 , and added 60ml of anhydrous toluene, and reacted at 100°C for 10 minutes. After the reaction, the excess hexamethyldisilazylammonium and solvent were drained, and then the product was separated by vacuum distillation at 130°C. The total reaction The yield was 76%.

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PUM

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Abstract

The invention belongs to a cyclic esters compound polymerization catalyst, a preparation method and the application thereof. The cyclic esters compound polymerization catalyst has the structure of dual (dual trimethyl silica-based amino) zinc (Zn (N (SiMe3)2)2. Hexamethyl bi-silica-based ammonia is taken as substrate, butyl lithium and anhydrous zinc chloride are taken as reactants, and the dual (dual trimethyl silica-based amino) zinc is synthesized by two-step reaction; the dual (dual trimethyl silica-based amino) zinc is uses as catalyst, an alcohols or phenolic compound is taken as initiator, l-lactide, caprolactone and cyclic carbonate are taken as monomers, polyesters homopolymer or copolymer can be prepared by adopting a way of solution polymerization, bulk polymerization or block copolymerization and being stirred for 5min-48h at the reaction temperature of 0-210 DEG C. The method has rapid speed of polymerization reaction and high monomer conversion rate; the obtained polyester has the number average molecular weight of 10-100 thousands and the molecular weight distribution of 1.1-1.7, is higher in three-dimensional regularity and melting point, and is suitable for the production and the application of high performance polyester materials with multiple specifications.

Description

technical field [0001] The invention relates to a cyclic ester compound polymerization catalyst, a preparation method and an application. Background technique [0002] Polyester compounds (such as L-polylactic acid, polycaprolactone, polycarbonate) are widely used in medical and pharmaceutical fields due to their good biocompatibility and degradability. Their products such as surgical sutures, bone nails, Drug sustained-release capsules, etc.; L-polylactic acid is widely used in daily necessities because of its good mechanical properties and is considered to be an environmentally friendly substitute for traditional polyolefin materials. [0003] The preparation of polyester compounds is mostly carried out by ring-opening polymerization of cyclic monomers initiated by initiators. Different initiation systems and different polymerization conditions will have a significant impact on the structure and properties of polymers. Most initiators initiate the polymerization of cyclic...

Claims

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Application Information

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IPC IPC(8): C08G63/83C08G63/08
Inventor 黄宇彬景遐斌原宇平陈学思
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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