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Preparation method of polybutylene terephthalate

A technology of polybutylene terephthalate and butanediol, which is applied in the field of polyester, can solve the problems of affecting the operation of the reaction equipment system, high catalyst consumption, and fouling of pipeline equipment, etc., so as to suppress the deterioration of the hue and achieve a good hue , The effect of low carboxyl-terminal content

Inactive Publication Date: 2013-10-09
CHINA PETROLEUM & CHEM CORP
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Problems solved by technology

[0013] The technical problem to be solved in the present invention is to disclose a preparation method of polybutylene terephthalate, in particular to a method for preparing polybutylene terephthalate using a liquid titanium catalyst that is resistant to hydrolysis and miscible with 1,4 butanediol. The method of butylene phthalate is to overcome the following defects in the prior art: in the preparation process of PBT, titanates such as tetrabutyl titanate are used as catalysts, and there is a high catalyst consumption caused by easy hydrolysis , Slicing performance is poor, hydrolyzate causes fouling of pipeline equipment, affects the operation of reaction equipment system, etc.

Method used

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  • Preparation method of polybutylene terephthalate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] (A) PBT slices were synthesized in a 2L reactor. Mix 500g of terephthalic acid (PTA) and 569g of 1,4-butanediol (BD) evenly, the molar ratio is PTA:BD=1:2.1, add liquid titanium catalyst 150×10 -6 (Based on the content of titanium atomic mass in the total weight of polyester produced). Gradually raise the temperature from 190°C to 230°C, the absolute reaction pressure is 101325Pa (gauge pressure is 0), and the esterification reaction is carried out, and the reaction time is 1 hour;

[0048] (B) After the esterification reaction is finished, a sufficient amount of distillate is distilled off, and the pre-condensation reaction is started by vacuuming. The reaction temperature is gradually increased from 230°C to 250°C, and the reaction pressure is gradually reduced from an absolute pressure of 101kPa to 600Pa. The polycondensation time is 0.5 hour;

[0049] (C) The final polycondensation reaction was carried out at 260°C and an absolute pressure of 50 Pa. After 30 minut...

Embodiment 2

[0051] (A) PBT slices were synthesized in a 2L reactor. Mix 500g of terephthalic acid (PTA) and 406g of 1,4-butanediol (BD) evenly, the molar ratio is PTA:BD=1:1.5, add liquid titanium catalyst 30×10 -6 (Based on the content of titanium atomic mass in the total weight of polyester produced). Gradually raise the temperature from 190°C to 230°C, the absolute reaction pressure is 101325Pa (gauge pressure is 0), and the esterification reaction is carried out, and the reaction time is 5 hours;

[0052] (B) After the esterification reaction is finished, a sufficient amount of distillate is distilled off, and the pre-condensation reaction is started by vacuuming. The reaction temperature is gradually increased from 230°C to 250°C, and the reaction pressure is gradually reduced from an absolute pressure of 101kPa to 600Pa. The polycondensation time is 1.5 hours;

[0053] (C) The final polycondensation reaction was carried out at 250°C and an absolute pressure of 150 Pa. After 150 mi...

Embodiment 3

[0055] (A) PBT slices were synthesized in a 2L reactor. Mix 500g of terephthalic acid (PTA) and 460g of 1,4-butanediol (BD) evenly, the molar ratio is PTA:BD=1:1.7, add liquid titanium catalyst 50×10 -6 (Based on the content of titanium atomic mass in the total weight of polyester produced). Gradually raise the temperature from 190°C to 230°C, the absolute reaction pressure is 101325Pa (gauge pressure is 0), and the esterification reaction is carried out, and the reaction time is 2 hours;

[0056] (B) After the esterification reaction is finished, a sufficient amount of distillate is distilled off, and the pre-condensation reaction is started by vacuuming. The reaction temperature is gradually increased from 230°C to 250°C, and the reaction pressure is gradually reduced from an absolute pressure of 101kPa to 600Pa. The polycondensation time is 0.5 hour;

[0057] (C) The final polycondensation reaction was carried out at 250°C and an absolute pressure of 70 Pa. After 60 minut...

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Abstract

The invention relates to a preparation method of polybutylene terephthalate. The preparation method comprises the following steps of: with purified terephthalic acid and 1,4-butanediol as base materials, adding hydrolysis-resistant titanium catalyst and carrying out an reaction under esterification reaction conditions of an intermittent or a continuous production way device to obtain an esterified product; carrying out a pre-condensation reaction on the esterified product to obtain a pre-condensed product under the pre-condensation reaction condition of gradually heating up and gradually lowering the pressure; and carrying out a final-condensation reaction on the pre-condensed product for 0.5 hour-2.5 hours to finally obtain a polyester product under the conditions that the reaction temperature is 250 DEG C-260 DEG C and absolute pressure is 150 Pa-50 Pa. The PBT (Polybutylece Terephthalate) resin product obtained by the preparation method disclosed by the invention is excellent in tone, hydrolysis resistance, thermal stability, formability and the like, thereby being suitable for being used as injection-molding parts including electrical parts, electronic parts, car parts and the like, and especially suitable for being used in films, monofilaments, fibers and the like.

Description

technical field [0001] The invention belongs to the field of polyester, and relates to a preparation method of polybutylene terephthalate, in particular to a method for preparing polybutylene terephthalate by using a liquid titanium catalyst which is resistant to hydrolysis and miscible with 1,4 butanediol. Butylene glycol formate method. Background technique [0002] Polybutylene terephthalate (PBT) is famous for its good mechanical properties, heat resistance, electrical properties, processing properties, etc. It is widely used in the fields of automobile industry, electronic and electrical industry, mechanical parts, etc. , thin film and other fields are also expanding. [0003] As the preparation method of PBT, it includes the transesterification method using dimethyl terephthalate (DMT) and 1,4-butanediol as raw materials or the direct method using terephthalic acid and 1,4-butanediol as raw materials. aggregation method. Due to the problem of recovery and treatment ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/183C08G63/78C08G63/85
Inventor 臧国强杨力芳郭灵通马颖涛李云鹏
Owner CHINA PETROLEUM & CHEM CORP
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