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Preparation method of semi-dull polytrimethylene terephthalate

A technology of propylene glycol phthalate and terephthalic acid, which is applied in the field of preparation of semi-dull poly(trimethylene terephthalate), can solve problems affecting catalyst activity, and achieve the effect that is not easily affected by adsorption

Inactive Publication Date: 2016-01-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is that the addition of a matting agent in the prior art can affect the catalyst activity

Method used

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  • Preparation method of semi-dull polytrimethylene terephthalate
  • Preparation method of semi-dull polytrimethylene terephthalate
  • Preparation method of semi-dull polytrimethylene terephthalate

Examples

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Effect test

Embodiment 1

[0041] Mix 142g of tetraisopropyl titanate with 46g of ethanol and 90g of lactic acid, and react for 4 hours at a temperature of 100°C in a stirred reactor. Add 36g of magnesium acetate and 91g of triethyl phosphate to the reactant. In the reactor, the reaction was carried out for 4 hours under the temperature condition of 120°C. The reaction product is placed in a reactor equipped with a fractionation device, and ethanol and isopropanol are distilled off to make a catalyst. The catalyst is mixed with 1,3-propanediol, wherein the mass fraction of titanium atoms is 4%.

[0042] 600 grams of terephthalic acid, 440 grams of 1,3 propylene glycol and 1.49 g of catalyst were mixed to form a slurry, which was added to a polymerization kettle for esterification reaction. The esterification temperature was 230 °C and the pressure was 0.25 MPa. The device discharges the water generated by the reaction, reacts for 2 hours, and the esterification rate is 96%. After the esterification is...

Embodiment 2

[0045] Mix 142g of tetraisopropyl titanate with 46g of ethanol and 192g of citric acid, and react for 4 hours at a temperature of 100°C in a stirred reactor, and add 61g of zinc lactate and 91g of triethyl phosphate to the reactant. In a stirred reactor, the reaction was carried out at a temperature of 120° C. for 4 hours. The reaction product is placed in a reactor equipped with a fractionation device, and ethanol and isopropanol are distilled off to make a catalyst. The catalyst is mixed with 1,3-propanediol, wherein the mass fraction of titanium atoms is 4%.

[0046] 600 grams of terephthalic acid, 440 grams of 1,3 propylene glycol and 1.49 g of catalyst were mixed to form a slurry, which was added to a polymerization kettle for esterification reaction. The esterification temperature was 230 °C and the pressure was 0.25 MPa. The device discharges the water generated by the reaction, reacts for 2 hours, and the esterification rate is 96%. After the esterification is comple...

Embodiment 3

[0049] 84g titanium glycolate (Ti(OCH 2 CH 2 O) 2 ) mixed with 46g ethanol, 192g citric acid, in a stirred reactor, reacted for 4 hours under 100°C temperature condition, added magnesium acetate 36g, triethyl phosphate 91g in the reactant, in a stirred reactor, 120 ℃ for 4 hours. The reaction product is placed in a reactor equipped with a fractionation device, and ethanol is distilled off to make a catalyst. The catalyst is mixed with 1,3-propanediol, wherein the mass fraction of titanium atoms is 4%.

[0050] 600 grams of terephthalic acid, 440 grams of 1,3 propylene glycol and 1.49 g of catalyst were mixed to form a slurry, which was added to a polymerization kettle for esterification reaction. The esterification temperature was 230 ° C and the pressure was 0.25 MPa. The device discharges the water generated by the reaction, and reacts for 2 hours, and the esterification rate is 98%. After the esterification is completed, it is lowered to normal pressure, and 4.1 g (55%...

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Abstract

The invention relates to a preparation method of semi-dull polytrimethylene terephthalate to mainly solve the problem of influence of an added dulling agent existing in the prior art on the activity of a catalyst. The method comprises the following steps: 1, adding a titanium catalyst to terephthalic acid and 1,3-propylene glycol adopted as raw materials, and carrying out an esterification reaction at 220-300DEG C under 0.1-0.5MPa to obtain a prepolymer; and 2, carrying out a pre-polycondensation reaction on the obtained prepolymer under vacuum conditions with the temperature of 245-265DEG C and the pressure of 300-1000Pa, and carrying out a fusion polycondensation reaction at 245-265DEG C under a pressure being smaller than 150Pa to obtain a polymerization product. The method well solves the problem, and can be used to produce the semi-dull polytrimethylene terephthalate.

Description

technical field [0001] The invention relates to a preparation method of semi-dull polytrimethylene terephthalate. Background technique [0002] Polypropylene terephthalate was rated as one of the top ten new petrochemical products. Its fiber products have both the advantages of nylon and polyester, and are suitable for the manufacture of high-end clothing, wool-like fabrics, car carpets, etc., and are considered to be expected to replace A new type of polyester product. When used to make fiber products such as semi-dull filaments, it is required to add a matting agent to the polymer during the polymerization process, and titanium dioxide powder is usually used. The matting agent itself usually does not cause the degradation of the catalyst performance. However, in the modern polyester industrial production, the matting agent is usually added in the form of a slurry mixed with ethylene glycol. To ensure the uniformity of the slurry, it is usually necessary to add anti-settl...

Claims

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Application Information

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IPC IPC(8): C08G63/85C08G63/183C08K3/22
Inventor 宋歌熊金根周文乐郁剑乙章瑛虹
Owner CHINA PETROLEUM & CHEM CORP
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