Prepn process of fiber-forming biodegradable fatty copolyester

A technology of aliphatic copolyester and manufacturing method, which is applied in the field of preparation of biodegradable aliphatic copolyester for fiber-forming, can solve the problem of affecting production efficiency, excessive aliphatic diol, and complicated operation of multiple feeding operations, etc. problems, to achieve the effect of color improvement, increase in molecular weight of polymer products, and simplification of operation process

Inactive Publication Date: 2007-03-21
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method usually requires a large excess of aliphatic dihydric alcohol, and the operation of multiple feeding is cumbersome, which affects the production efficiency

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 28.47g of dimethyl succinate, 88.27g of dimethyl terephthalate, 64.35g of 1,4-butanediol and 36.92mg of tetraisopropoxytitanium into a 500ml volume four-neck circle replaced by high-purity nitrogen. in the bottom flask. The four-necked flask is equipped with a high-purity nitrogen gas inlet, a mechanical stirrer, and a condensation water separator. The above reaction system was moved into an oil bath at 180°C, stirred and reacted for 1 to 2 hours with nitrogen gas, and then decompressed slowly, and the temperature of the oil bath was gradually increased to 230°C. The vacuum degree is controlled within 200Pa, and the vacuum polycondensation is carried out for 4 hours. After cooling, the product of the above polymerization reaction was first dissolved in chloroform, and then filtered, and excess cold methanol was added to the obtained filtrate. After separation and drying, aliphatic copolymers are obtained. The resulting product look is slightly yellow, and the wei...

Embodiment 2

[0027] Add 28.47g dimethyl succinate, 88.27g dimethyl terephthalate, 64.35g 1,4-butanediol, 36.92mg titanium tetraisopropoxide and 4.8mg calcium chloride to high-purity nitrogen Replaced in a 500ml volume four-neck round bottom flask. The four-necked flask is equipped with a high-purity nitrogen gas inlet, a mechanical stirrer, and a condensation water separator. The above reaction system was moved into an oil bath at 180°C, stirred and reacted for 1 to 2 hours with nitrogen gas, and then decompressed slowly, and the temperature of the oil bath was gradually increased to 240°C. The vacuum degree is controlled within 200Pa, and the vacuum polycondensation is carried out for 4 hours. After cooling, the product of the above polymerization reaction was first dissolved in chloroform, and then filtered, and excess cold methanol was added to the obtained filtrate. After separation and drying, aliphatic copolymers are obtained. Gained product look is white, and gel permeation chrom...

Embodiment 3

[0031] Add 28.47g dimethyl succinate, 88.27g dimethyl terephthalate, 64.35g 1,4-butanediol, 36.92mg titanium tetraisopropoxide and 7.2mg calcium chloride to high-purity nitrogen Replaced in a 500ml volume four-neck round bottom flask. The four-necked flask is equipped with a high-purity nitrogen gas inlet, a mechanical stirrer, and a condensation water separator. The above reaction system was moved into an oil bath at 180°C, stirred and reacted for 1 to 2 hours with nitrogen gas, and then decompressed slowly, and the temperature of the oil bath was gradually increased to 240°C. The vacuum degree is controlled within 200Pa, and the vacuum polycondensation is carried out for 4 hours. After cooling, the product of the above polymerization reaction was first dissolved in chloroform, and then filtered, and excess cold methanol was added to the obtained filtrate. After separation and drying, aliphatic copolymers are obtained. The resulting product is white in color, and the weigh...

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Abstract

The present invention is preparation process of fiber-forming biodegradable fatty copolyester. In the single kettle operation, the composite catalyst system comprising the main catalyst of metal compound of Ti, Sb or Zn and the co-catalyst of metal ion salt of Ca, Mg, Na or K, or phosphoric acid derivative, and the monomer material are added into the polymerization kettle simultaneously. After esterification or ester exchange reaction for 1-2 hr, the materials are vacuum polycondensated. The preparation process of the present invention has simple operation, fast polymerization reaction speed, raised polymer molecular weight, less side products and improved polymer color.

Description

technical field [0001] The invention relates to a preparation method of biodegradable aliphatic copolyester for fiber formation. The copolyester provided by the invention has relatively high molecular weight and melting point, and is suitable for spinning into fibers. Background technique [0002] Polyesters prepared by condensation polymerization, such as polyethylene terephthalate (PET), polybutylene terephthalate (PBT), polytrimethylene terephthalate (PPT), polysuccinic acid Butylene glycol ester (PBS), etc., have been widely used in various fields of people's daily life as engineering materials, and they can be made into fibers, beverage bottles, films and other materials. These polymers are prepared through two processes: esterification or transesterification of terephthalic acid / succinic acid or its esterification products with aliphatic dihydric alcohols. Usually the esterification process takes place under high pressure, while the transesterification process is car...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/183C08G63/85C08G63/78
Inventor 俞建勇曹阿民李发学王学利程隆棣李婷婷
Owner DONGHUA UNIV
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