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Method for preparing block polyester polyether copolymer from polyester prepolymer and polyether prepolymer

A technology of polyester polyether copolymerization and polyether prepolymer, which is applied in the field of preparation of block polyester polyether copolymers, can solve the problems of poor thermal stability and low melting point, and achieve low price, low polymerization temperature and wide sources Effect

Inactive Publication Date: 2009-07-29
TORAY FIBER RES INST(CHINA) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0022] The purpose of the present invention is to overcome the shortcomings of low melting point and poor thermal stability of the direct process multi-block polyester polyether copolymers of existing melt polymerization combined with solid phase polymerization, and to provide a solid phase polymerization synthesis with high molecular weight, high melting point and Process for multi-block polyester polyether copolymers with high thermal stability

Method used

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  • Method for preparing block polyester polyether copolymer from polyester prepolymer and polyether prepolymer
  • Method for preparing block polyester polyether copolymer from polyester prepolymer and polyether prepolymer
  • Method for preparing block polyester polyether copolymer from polyester prepolymer and polyether prepolymer

Examples

Experimental program
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Effect test

Embodiment 1

[0070] Add 140g of crystalline polyester prepolymer A1, 7g of polyether prepolymer B2, 0.45g of stannous acetate, 0.6g of p-toluenesulfonic acid and 0.83g of succinic acid into a 500ml three-necked bottle, connect mechanical stirring, nitrogen and vacuum lines. After the system was replaced with nitrogen three times, under the flow of ultra-pure nitrogen, the temperature was raised to 165° C. and after the prepolymer was completely melted, stirring was started at 100 rpm for 10 minutes. After cooling down to 100°C, the mixture was crystallized at 100°C for 2 hours. Take out and crush the mixture, take 50g of 100-250um powder and put it into a vacuum oven, depressurize to 200Pa, perform solid-state polymerization at 145°C for 10 hours, and obtain 45g of block copolymer 1 (DSC and GPC results see attached figure 1 and 2 ). As determined by GPC, the weight average molecular weight Mw is 45000.

Embodiment 2

[0072] Add 160g of crystalline polyester prepolymer A2, 40g of polyether prepolymer B1, and 5.09g of succinic acid into a 500ml three-necked bottle, and connect the mechanical stirring, nitrogen and vacuum pipelines. After the system was replaced with nitrogen three times, under the flow of ultra-pure nitrogen, the temperature was raised to 170° C. and after the prepolymer was completely melted, stirring was started at 100 rpm for 10 minutes. After cooling down to 100°C, the mixture was crystallized at 100°C for 2 hours. Take out and crush the mixture, take 50g of 100-250um powder and put it into a vacuum oven, depressurize to 200Pa, perform solid phase polymerization at 148°C for 10 hours to obtain 46g of block copolymer 2 (see DSC and GPC results in attached figure 1 and 2 ). As determined by GPC, the weight average molecular weight Mw is 85000.

Embodiment 3

[0074] Add 120g of crystalline polyester prepolymer A4, 80g of polyether prepolymer B3, and 4.000g of succinic anhydride into a 500ml three-necked bottle, and connect the mechanical stirring, nitrogen and vacuum pipelines. After the system was replaced with nitrogen three times, under the flow of ultra-pure nitrogen, the temperature was raised to 220° C. and after the prepolymer was completely melted, stirring was started at 100 rpm for 10 minutes. After cooling down to 160°C, the mixture was crystallized at 160°C for 2 hours. Take out and crush the mixture, take 50g of 100-250um powder and put it into a vacuum oven, reduce the pressure to 200Pa, perform solid phase polymerization at 200°C for 16 hours to obtain 46g of block copolymer. As determined by GPC, the weight average molecular weight Mw is 53000.

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Abstract

The invention discloses a method for preparing block polyether polyester copolymer from polyester prepolymer and polyether prepolymer. The polyester prepolymer and the polyether prepolymer are melt in inert atmosphere and under vacuum, even blended, and then the prepolymer mixture are crystallized; later on, the solid phase polymerization is carried out on the crystallized prepolymer mixture in inert atmosphere or under vacuum and in the temperature of lower than the melting point of the prepolymer mixture but higher than glass transition temperature of the prepolymer mixture. The method has the advantages of wide source of materials, low cost, simple technique, environmental protection, low polymerization temperature, high quality of products and being capable of obtaining high molecular weight copolymer, etc.

Description

technical field [0001] The invention belongs to the field of macromolecular materials, and in particular relates to a method for preparing block polyester polyether copolymers by using a solid phase polymerization method. Background technique [0002] Block polyester polyether copolymer is a block copolymer composed of polyester segments and polyether segments bonded together, its structure is: [0003] [0004] or as: [0005] [0006] Wherein: R1, R2, R3 and R4 are independently alkyl, substituted alkyl, aryl or substituted aryl; n and m are integers greater than 1. [0007] Block polyester polyether copolymers have a wide range of applications, such as thermoplastic elastomers, polymer modifiers, biomedical materials, and polyurethane precursors. As a thermoplastic elastomer, block polyester polyether copolymer has high strength, easy processing and molding, wide temperature range, aging resistance, chemical resistance, solvent resistance, oil resistance, etc., an...

Claims

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Application Information

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IPC IPC(8): C08G81/00
Inventor 何勇郭晓朱可新夏天成王枫
Owner TORAY FIBER RES INST(CHINA) CO LTD
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