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
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[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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