Low-temperature low-pressure direct hydrogenation catalyst for coal-based 1,4-butynediol and preparation method thereof

Abstract

The invention relates to a low-temperature low-pressure direct hydrogenation catalyst for coal-based 1,4-butynediol and a preparation method thereof. A 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 layer. The preparation method comprises the following steps: (1) preparing an ethanol-aqueous solution, and adjusting with ammonia water; (2) preparing a mixed solution; (3) centrifugally filtering the mixed solution, washing with ethanol and deionized water respectively, and drying the filtered object to obtain uniformly-layered coating-structure SiO2@ SiO2 nanospheres; (4) dispersing 2.0 g of the prepared SiO2@SiO2 nanospheres in water, and carrying out reflux stirring on the SiO2@SiO2 nanospheres, a metal nickel precursor and urea to carry out nickel phyllosilicate deposition; (5) centrifugally filtering the solution, and carrying out washing, filtering anddrying to obtain a Ni-Si-PS@SiO2 precursor; (6) preparing a secondary deposition Ni-Si-PS@SiO2 precursor from the obtained Ni-X-Si-PS@SiO2; and (7) calcining the secondarily deposited Ni-Si-PS@SiO2 precursor in an air atmosphere to obtain the low-temperature low-pressure hydrogenation catalyst Ni-Si-PS@SiO2.

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 of 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 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 disclose...

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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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