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Preparation method of polyethylene terephthalate-1,3-propanediol copolyester

A technology of polyethylene terephthalate and propylene glycol copolyester, applied in the field of producing polyethylene terephthalate-1, can solve the problem of low degree of polymerization and achieve high catalytic activity, high intrinsic viscosity, The effect of increased reaction speed

Active Publication Date: 2011-08-31
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Won Sik Yoon and others successfully synthesized polyethylene terephthalate 1,3-propylene glycol copolyester by DMT route, but the degree of polymerization is not high

Method used

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  • Preparation method of polyethylene terephthalate-1,3-propanediol copolyester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Into a 5L stainless steel reaction kettle equipped with nitrogen inlet, condensate outlet and stirrer, add 1000 grams of purified terephthalic acid (PTA), 575 grams of 1,3-propanediol (1,3-PDO), 85 grams of ethylene glycol Alcohol (EG), equivalent to 50ppm titanium n-butyl titanate, 60ppm cobalt cobalt acetate and 70ppm germanium germanium dioxide, then use nitrogen to pressurize to 0.2MPa, keep constant pressure, and the temperature in the reactor rises to 250°C , when the amount of by-product water distilled out in the reactor reaches the theoretical water output, the pressure in the still returns to normal pressure, then adds trimethyl phosphate equivalent to 60ppm phosphorus in the still, and vacuumizes the pressure in the polymerization still to Reduce to below 100Pa within 30 minutes, react under this pressure, control the final temperature of the reaction at 265-275°C, then use nitrogen to restore the reaction system to normal pressure, the polymer melt is cast an...

Embodiment 2

[0036] In a 5 L stainless steel reaction kettle equipped with nitrogen inlet, condensate outlet and stirrer, add 1000 g of purified terephthalic acid (PTA), 575 g of 1,3-propanediol (1,3-PDO), 85 g of ethyl Glycol (EG), make a slurry of n-butyl titanate or tetramethyl titanate equivalent to 25ppm titanium, cobalt nitrate 60ppm and germanium dioxide 70ppm germanium into the reaction kettle, and then pressurize with nitrogen To 0.2MPa, keep a constant pressure, the temperature inside the reactor rises to 250°C, when the by-product water distilled out of the reactor reaches the theoretical amount, the pressure inside the kettle returns to normal pressure, and titanium equivalent to 50ppm titanium is added into the kettle N-butyl acid or tetramethyl titanate, phosphorous acid of 60ppm phosphorus, vacuumize to reduce the pressure to below 100Pa within 20 minutes, maintain the vacuum for 130-140 minutes, and control the final reaction temperature at 265-275°C. Then use nitrogen to e...

Embodiment 3

[0038] In a 5 L stainless steel reaction kettle equipped with nitrogen inlet, condensate outlet and stirrer, add 1000 g of purified terephthalic acid (PTA), 575 g of 1,3-propanediol (1,3-PDO), 85 g of ethyl Glycol (EG), add tetrapropyl titanate or tetraisopropyl titanate equivalent to 20ppm titanium, cobalt phosphate 100ppm cobalt and germanium dioxide 110ppm germanium, then pressurize to 0.2MPa with nitrogen to maintain constant pressure , the temperature in the reactor rises to 250°C, and when the by-product water distilled out of the reactor reaches the theoretical amount, the pressure in the reactor returns to normal pressure, and tetrapropyl titanate or titanate equivalent to 50ppm titanium is added into the reactor Tetraisopropyl ester, 30ppm phosphorus ethyl methyl phosphate or phosphoric acid, vacuumize to reduce the pressure below 100Pa within 30 minutes, maintain this vacuum for 140 minutes, control the final reaction temperature at 265-275°C, and then eliminate it wi...

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Abstract

The invention relates to a preparation method of polyethylene terephthalate-1,3-propanediol copolyester. In the preparation method, terephthalic acid or dimethyl terephthalate, 1,3-propanediol and ethylene glycol are used as raw materials, titanate, germanium compound and cobalt compound are used to form composite catalyst, phosphorus compound is added to be used as stabilizer; under the synergistic catalysis and hue-adjusting functions of the materials, the reaction time can be greatly shortened, the polyester chip of which intrinsic viscosity is 0.75-1.05dL / g is prepared through direct polymerization; and the reaction product has good hue, and the copolyester product can be used in the fields of fiber and engineering plastic.

Description

Technical field: [0001] The invention relates to a method for producing polyethylene terephthalate-1,3-propylene glycol copolyester, and more specifically relates to a synthetic polyethylene terephthalate with intrinsic viscosity above 0.75-1.05dl / g Method for formic acid ethylene glycol 1,3-propanediol copolyester. Background technique: [0002] Polyethylene terephthalate 1,3-propanediol copolyester (copolyester) is made of terephthalic acid (PTA) or dimethyl terephthalate (DMT) and ethylene glycol, 1,3- A long-chain polymer material obtained by condensing the esterification or transesterification product of propylene glycol (1,3-PDO), most of its properties are between polyethylene terephthalate (PET) and polyethylene terephthalate Among them, propylene glycol formate (PTT) can not only improve the disadvantages of PTT, such as poor thermal stability, low strength and poor high-temperature dimensional stability of fibers, but also effectively reduce the cost of PTT. [0...

Claims

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Application Information

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IPC IPC(8): C08G63/183C08G63/86C08G63/85C08G63/82
Inventor 陈颖邹妍朱景利史君温国防李连斌刘冬李彦钧胡亚文王洪星李振忠吴佩华
Owner PETROCHINA CO LTD
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