Catalyst for direct hydrogenation of coal-based 1,4-butynediol at low temperature and low pressure and preparation method thereof

Abstract

The invention relates to a low-temperature and low-pressure direct hydrogenation catalyst for coal-based 1,4-butynediol and a preparation method thereof. The basic structural unit of the catalyst has a monodisperse spherical coating structure, and the catalyst is composed of a uniform silicon oxide core and a metal phyllosilicate shell. The preparation steps are: (1) configure ethanol-water solution, and adjust it with ammonia water; (2) make a mixed solution; (3) centrifuge and filter the above mixed solution, wash with ethanol and deionized water respectively, and dry the filtered items to obtain Uniform layered clad structure SiO 2 @SiO 2 Nanosphere; (4) get the prepared SiO 2 @SiO 2 Disperse 2.0g of nanospheres in water, reflux and stir with metal nickel precursor and urea to deposit nickel phyllosilicate; (5) centrifuge and filter the above solution, wash, filter and dry to obtain Ni‑Si‑PS@SiO 2 precursor; (6) Ni‑X‑Si‑PS@SiO to be obtained 2 Preparation of secondary deposited Ni‑Si‑PS@SiO 2 precursor; (7) the secondary deposition of Ni‑Si‑PS@SiO 2 The precursor is calcined in an air atmosphere to obtain a low-temperature and low-pressure hydrogenation catalyst Ni‑Si‑PS@SiO 2 .

Description

technical field [0001] The invention relates to a low-temperature and low-pressure direct hydrogenation catalyst for coal-based 1,4-butynediol and a preparation method thereof, belonging to the technical field of catalysts. Background technique [0002] At present, the main method for industrial production of 1,4-butanediol is the hydrogenation of coal-based 1,4-butynediol. However, in the hydrogenation process of 1,4-butynediol, its hydrogenation intermediate species 1,4-butenediol is easily isomerized into 2-hydroxytetrahydrofuran with hemiacetal structure, and finally converted into 2-hydroxytetrahydrofuran. Cyclic acetal 2-(4′-hydroxybutoxy)-tetrahydrofuran, the final by-product forms an azeotrope with 1,4-butanediol, which cannot be removed by conventional rectification, thereby seriously reducing 1,4- The purity and color of butanediol products directly affect the quality of 1,4-butanediol and its application in downstream fields. [0003] Chinese patent CN 102145286...

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Problems solved by technology

However, in the hydrogenation process of 1,4-butynediol, its hydrogenation intermediate species 1,4-butenediol is easily isomerized into a by-product of 2-hydroxytetrahydrofuran with a hemiacetal structure, and finally converted to Cyclic acetal 2-(4′-hydroxybutoxy)-tetrahydrofuran, the final by-product forms an azeotrope with 1,4-butanediol, which cannot be removed by conventional rectification, thereby seriously reducing 1,4- The purity and color of butanediol products directly affect the quality of 1,4-butanediol and its application in downstream fields

[0003] Chinese patent CN 102145286 B discloses a Ni-SiO 2 / Al 2 o 3 Catalyst and preparation method, the catalyst can effectively realize the hydrolysis and hydrogenation conversion of cyclic acetal 2-(4'-hydroxybutoxy)-tetrahydrofuran, but its preparation process is relatively cumbersome

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