Preparation method of catalyst for synthesis of PBT

A technology of catalysts and compounds, applied in the direction of titanium organic compounds, etc., can solve the problems of catalysts not being resistant to hydrolysis, and achieve the effects of inhibiting hydrolysis scaling, reducing the amount of alkyl alcohol, and strong hydrolysis resistance

Inactive Publication Date: 2015-11-25
CHINA PETROCHEMICAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to solve the problem that the currently used tetrabutyl titanate catalyst is not resistant to hydrolysis, convert tetrabutyl titanate into titanium butanedioxide, improve the hydrolysis resistance of the catalyst, and inhibit the hydrolysis of the catalyst

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0010] A kind of preparation method for the catalyst of synthesizing PBT, will structural formula be Ti(OR) 4 The compound is mixed with dihydric alcohol, and reacted for 0.5-10hr under the conditions of absolute pressure 1-95kPa and temperature 60-210°C, and the obtained by-product ROH is removed to obtain a catalyst for synthesizing PBT, wherein dihydric alcohol and Ti(OR) 4 The molar ratio of ≥ 1, preferably dihydric alcohol and Ti(OR) 4 The molar ratio of 4: 1 ~ 120: 1, excess diol can act as a catalyst solvent. Further, the Ti(OR) 4 The R group of the compound includes n-butyl, isopropyl or ethyl, and the dihydric alcohol can be ethylene glycol, propylene glycol or butanediol, preferably 1,4-butanediol.

[0011] The above Ti(OR) 4 Compounds and glycols are mixed and added to the catalyst preparation device. The catalyst preparation device consists of three parts: a stirring conversion tank, an alkyl alcohol recovery tower on the top of the tank and a vacuum system. Th...

Embodiment 1

[0015] Add 18kg of 1,4-butanediol and 1.5kg of tetrabutyl titanate into the catalyst conversion tank. The temperature of the conversion tank is controlled at 120°C and the pressure is controlled at about 12kPa. React for 2 hours, and the butanol produced by the reaction is condensed from the top of the tower After condensing, it is collected in the collection tank. The required catalyst for PBT preparation is obtained in the conversion kettle.

Embodiment 2

[0017] 1,4-butanediol 15kg / hr, tetrabutyl titanate 1.5kg / hr were added to the catalyst conversion tank, the temperature of the conversion tank was controlled at 90°C, the pressure was controlled at about 10kPa, and the residence time was controlled at 2hr. The alcohol collecting tank obtains a water-containing butanol solution, and the butanol flow rate is 0.33kg / hr. The catalyst solution is continuously discharged from the catalyst conversion tank.

[0018] Catalyst hydrolysis performance evaluation:

[0019] For the catalyst samples prepared in Examples 1 and 2, and the tetrabutyl titanate catalyst samples, four water concentration (0.5%, 1%, 2% and 3%) samples containing 0.5% titanium (in terms of titanium elements) were configured respectively, and observed Precipitation occurs in the sample (Table 1), and it can be seen from the table that the catalysts prepared in Examples 1 and 2 have better hydrolysis resistance.

[0020] Table 1 Catalyst Hydrolysis Precipitation Sit...

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PUM

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Abstract

The invention discloses a preparation method of a catalyst for synthesis of PBT, and the method comprises the following steps: a compound whose structural formula is Ti(OR)4 and a dihydric alcohol are mixed, a reaction is carried out for 0.5-10 hours in a condition that the absolute pressure is 1-95kPa and the temperature is 60-210 DEG C, an obtained by-product ROH is removed, and the catalyst for synthesis of PBT is obtained, wherein, the mol ratio between dihydric alcohol and Ti(OR) is equal to or more than 1, and preferably the mol ratio between dihydric alcohol and Ti(OR)4 is 4:1-120:1. According to the invention, the titanium alkoxide catalyst whose traditional structural formula is Ti(OR)4 and dihydric alcohol are reacted, the dihydric alcohol titanium catalyst of which at least of one of the alkyloxy is replaced by dihydric alcohol is obtained; the catalyst has good hydrolysis resistance and catalytic activity, and thereby effectively inhibiting hydrolysis fouling of the catalyst, and reducing the amount of alkyl alcohol brought into the subsequent production along with the catalyst.

Description

technical field [0001] The invention relates to a preparation method of a catalyst for synthesizing PBT, and belongs to the technical field of PBT synthesis. Background technique [0002] Catalysts play a vital role in the production of polybutylene terephthalate (PBT). At present, the esterification step and polycondensation step in the PBT process route at home and abroad generally use alkoxy titanium catalysts, such as tetrabutyl titanate, tetraisopropyl titanate, etc. Although tetrabutyl titanate has a high catalytic activity, there are still the following deficiencies in the actual production process: ① by-product alkyl alcohol, such as butanol produced by the catalysis of tetrabutyl titanate, will accumulate in the reaction tower , affect the normal operation of the reaction tower; ②The discharge of alkyl alcohol from the wastewater will increase the burden of wastewater treatment; ③The alkoxide titanium catalyst is easy to hydrolyze, and the water generated in the es...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/85C08G63/183C07F7/28
Inventor 李仁海张军赵付平黄娟李晶
Owner CHINA PETROCHEMICAL CORP
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