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Preparation method of polyethylene terephthalate ethylene glycol copolyester

A technology of poly(trimethylene terephthalate) copolyester and terephthalate, applied in the field of preparation of poly(trimethylene terephthalate) copolyester, capable of solving problems such as difficult direct copolymerization

Inactive Publication Date: 2011-12-14
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, oxalic acid is directly used as a comonomer, and it is difficult to directly copolymerize due to the strong acidity of oxalic acid.

Method used

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  • Preparation method of polyethylene terephthalate ethylene glycol copolyester
  • Preparation method of polyethylene terephthalate ethylene glycol copolyester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Add 182 parts of terephthalic acid (parts by mass), 353 parts of 1,3-propanediol, 194 parts of dimethyl oxalate, 0.12 parts of ethylene glycol antimony and 0.15 parts of tetrabutyl titanate in the batch reactor, at 220 ~ Esterification and transesterification at 250°C and a pressure of 0.25MPa (gauge pressure). The esterification is completed when the water output reaches the theoretical water output. The pressure of the reactor is released to normal pressure. After adding 0.025 parts of trimethyl phosphate, it is transferred to the belt The double-conical polymerization kettle with disc stirring gradually decompresses and heats up. After 45 minutes, the vacuum of the polymerization kettle reaches 90Pa (absolute pressure), and the reaction temperature is maintained at 240-250℃. After 170 minutes of polymerization, the polymerization is completed when the rated stirring power is reached. For polymerization reaction, use nitrogen to eliminate the vacuum, cool with water, a...

Embodiment 2

[0040] Add 330 parts of terephthalic acid, 270 parts of 1,3-propanediol, 12.5 parts of dimethyl oxalate, 0.12 parts of ethylene glycol antimony and 0.15 parts of tetrabutyl titanate into the batch reactor, at 220~250℃, pressure Esterification and transesterification under 0.25MPa (gauge pressure), the esterification is completed when the water output reaches 95% of the theoretical water output, the pressure of the reactor is released to normal pressure, and after adding 0.025 parts of trimethyl phosphate, it is transferred to a Stirring biconical polymerization kettle, gradually decompress and heat up. After 45 minutes, the vacuum of the polymerization kettle reaches 90Pa, and the reaction temperature is maintained at 240-250°C. After 150 minutes of polymerization, the polymerization reaction is completed when the rated stirring power is reached, and the vacuum is eliminated with nitrogen. , after water cooling, pelletizing can obtain a polyethylene terephthalate ethylene glyco...

Embodiment 3

[0042] 83 parts of dimethyl oxalate and 108 parts of 1,3-propanediol, 0.07 parts of manganese acetate are first transesterified at 150-220 ° C, and then with 272 parts of terephthalic acid, 212 parts of 1,3-propanediol, 0.12 parts Ethylene glycol antimony and 0.15 parts of tetrabutyl titanate are esterified at 220-250 ° C and a pressure of 0.25 MPa (gauge pressure). The esterification is completed when the water output reaches 95% of the theoretical water output, and the pressure of the reactor is released to normal. After adding 0.025 parts of triethyl phosphate, transfer to a biconical polymerization kettle with disk stirring, gradually reduce the pressure and increase the temperature. After 45 minutes, the vacuum of the polymerization kettle reaches 90Pa, and the reaction temperature is maintained at 240-250℃. After 160 minutes of polymerization, when the rated stirring power is reached, the polymerization reaction is terminated, and the vacuum is eliminated with nitrogen, c...

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Abstract

The invention discloses a preparation method of polytrimethylene terephthalate oxalate copolyester, that is, oxalate is used as a comonomer to prepare polypylene terephthalate with terephthalic acid and its ester, and 1,3-propylene glycol Propylene glycol dicarboxylate copolyester. The copolyester has a melting point of 180-220°C, an intrinsic viscosity of 0.7-1.5dL / g, and is biodegradable. The preparation method of the invention is simple, the raw material cost is low, and the difference between product performance and PTT is small. Copolyesters can be used in the manufacture of fibers, films and other plastics.

Description

technical field [0001] The invention belongs to the field of polyester preparation, and in particular relates to a preparation method of poly(propylene glycol terephthalate) copolyester. Background technique [0002] At present, with the development of chemical and biological methods for preparing 1,3-propanediol technology, as described in CN96195288, CN97181298, CN97193774, CN99813852, CN200410037692 and CN200510086677, 1,3-propanediol can be obtained cheaply and on a large scale, making large It is possible to produce and apply polytrimethylene terephthalate on a large scale. Polypropylene terephthalate has excellent characteristics. In the field of fiber application, it combines the softness of nylon, the bulkiness of acrylic, the stain resistance of polyester and its own unique resilience; in the field of film, it It overcomes the rigidity of PET and avoids the flexibility of PBT; in the field of plastic applications, it has both the high physical and mechanical proper...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/183C08G63/78C08K5/521C08K3/32
Inventor 魏高富戴志彬夏峰伟
Owner CHINA PETROLEUM & CHEM CORP
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