Method for preparing copolyether ester elastomer

A technology of copolyetherester and elastomer, which is applied in the field of preparation of copolyetherester elastomer, can solve the problems of high price, difficult separation and extraction of tetrahydrofuran, etc., and achieve the effect of low cost and consistent performance

Active Publication Date: 2013-04-03
KINGFA SCI & TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] In summary, the existing methods for preparing copolyetherester elastomers all use dimethyl terephthalate as a raw material, which is expensive; and will produce by-products methanol and tetrahydrofuran, which have similar boiling points and are difficult to separate Tetrahydrofuran

Method used

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  • Method for preparing copolyether ester elastomer
  • Method for preparing copolyether ester elastomer

Examples

Experimental program
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Effect test

Embodiment 1

[0033] A method for preparing copolyetherester elastomer, comprising the following steps:

[0034] (1) Esterification: Add 26g (0.126mol) of terephthalic acid (PTA), 25g (0.278mol) of 1,4-butanediol (BDO) and polytetramethylene ether glycol (Mn= 1000) 10g (0.01mol), at the same time add 10mg tetrabutyl titanate and raise the temperature at 235-240°C and carry out the esterification reaction under the pressure of 80kPa, and the reaction time is two hours. After the reaction is completed, the by-product tetrahydrofuran and water are removed to obtain an esterified product; the mixture of tetrahydrofuran and water is purified by rectification to obtain high-purity tetrahydrofuran;

[0035] (2) Prepolymerization reaction: After the esterification reaction, 10 mg of antioxidant 1010 and 10 mg of tetrabutyl titanate were added to the esterified product, the temperature was 238° C., the pressure was 6 kPa, and the reaction was carried out for 1 hour.

[0036] (3) Polycondensation reac...

Embodiment 2

[0038] A method for preparing copolyetherester elastomer, comprising the following steps:

[0039] (1) Esterification: Add 46g (0.277mol) of PTA, 60g (0.666mol) of BDO and 10g (0.01mol) of polytetramethylene ether glycol (Mn=1000) into the flask, and add 20mg of tetrabutyl titanate at the same time Elevate the temperature at 235-240° C. and carry out the esterification reaction at a pressure of 80 kPa, and the reaction time is two hours. After the reaction is completed, the by-product tetrahydrofuran and water are removed to obtain an esterified product; the mixture of tetrahydrofuran and water is purified by rectification to obtain high-purity tetrahydrofuran;

[0040] (2) Prepolymerization reaction: After the esterification reaction, 20 mg of antioxidant 1010 and 20 mg of tetrabutyl titanate were added to the esterified product, the temperature was 238° C., the pressure was 6 kPa, and the reaction was carried out for 1 hour.

[0041] (3) Polycondensation reaction: transfer ...

Embodiment 3

[0043] A method for preparing copolyetherester elastomer, comprising the following steps:

[0044] (1) Esterification: Add 5.8kg (34.9mol) of PTA, 0.2kg (1.2mol) of isophthalic acid, 7kg (77.8mol) of BDO and 5kg of polytetramethylene ether glycol (Mn=1000) into the flask (5mol), while adding 5g of tetrabutyl titanate, the temperature is raised at 235-240°C and the pressure is 80kPa to carry out the esterification reaction, and the reaction time is two hours. After the reaction is completed, the by-product tetrahydrofuran and water are removed to obtain an esterified product; the mixture of tetrahydrofuran and water is purified by rectification to obtain high-purity tetrahydrofuran;

[0045] (2) Prepolymerization reaction: After the esterification reaction, 10 g of antioxidant 1010 and 20 g of tetrabutyl titanate were added to the esterified product at a temperature of 238° C. and a pressure of 6 kPa for 1 hour of reaction.

[0046] (3) Polycondensation reaction: transfer the ...

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Abstract

The invention discloses a method for preparing copolyether ester elastomer. The method comprises the following steps of mixing aromatic binary acid, polyether glycol and micromolecule glycol to carry out an esterification reaction, removing by-products of tetrahydrofuran and water to obtain carboxylate after the reaction is finished; transferring the obtained carboxylate into a pre-polycondensation reactor, adding an antioxidant and a catalyst to react for 1-2 hours, so as to obtain a prepolymer; transferring the prepolymer to a polycondensation kettle, wherein the polymerization time is 1.5-3 hours and the pressure is 100-200Pa; and obtaining the copolyether ester elastomer after the reaction is finished. By adopting the method disclosed by the invention, the copolyether ester elastomer is prepared from terephthalic acid as a raw material; the cost is low; and the by-product tetrahydrofuran generated by reaction is rectified and purified to obtain the high-purity tetrahydrofuran. The method has no negative effect on the cost of synthetizing TPEE (thermoplastic polyeher ester elastomer); the performance of the synthetized copolyether ester elastomer is consistent with that of the product prepared from dimethyl terephthalate.

Description

technical field [0001] The invention relates to a method for preparing copolyetherester elastomer. Background technique [0002] Polyester thermoplastic elastomer (TPEE for short) has the characteristics of both rubber and thermoplastic engineering plastics. It exhibits the characteristics of rubber at room temperature and the characteristics of thermoplastics at high temperatures. It can be plasticized and molded, and it is easy to process. Its molecular structure is composed of hard segment and soft segment. The hard segment is aromatic polyester (PET or PBT), and the polyether or polyester block with a lower glass transition temperature is used as the soft segment. It is elastic at the use temperature. Partial crystallization of the polyester hard segment of the polyether / polyester forms a crystalline microdomain, and the polyether / polyester soft segment and uncrystallized hard segment form an amorphous phase, and the crystalline microdomain acts as a physical crosslinkin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/672C08G63/688C08G63/78
Inventor 苑仁旭焦健赵巍徐依斌蔡彤旻夏世勇曾祥斌
Owner KINGFA SCI & TECH CO LTD
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