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

A technology of hydrogenation catalyst and butynediol, which is applied in the directions of catalyst activation/preparation, hydrogenation preparation, hydroxyl compound preparation, etc., and can solve problems such as reduction, cumbersome preparation process, and impact

Active Publication Date: 2022-05-27
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] ① Prepare an ethanol-water solution with a volume ratio of ethanol:water of 0.5:1, and adjust the pH to 7.5 with ammonia water; raise the temperature to 60°C, slowly add 30 mL / L methyl orthosilicate to the ethanol-water solution, and vigorously Stir for 1 h, continue to add 27 mL / L hexadecyltrimethoxysilane and 85 mL / L methyl orthosilicate, and vigorously stir the mixed solution for 1 h; after centrifugal filtration of the above mixture, wash with ethanol and deionized water respectively 3 times, and the filtered items were dried at 90 °C for 10 h to obtain a uniformly layered coating structure of SiO 2 @SiO 2 Nanospheres.

[0055] ②Take 2.0g of the prepared SiO 2 @SiO 2 The nanospheres were dispersed in 150 mL of water, and 0.005 mol of nickel acetylacetonate and 0.4 mol of urea were respectively dissolved therein, the temperature was raised to 60° C., refluxed and stirred for 4 h, and then centrifuged and filtered, and washed with ethanol and deionized water for 5 ...

Embodiment 2

[0058] ① Prepare an ethanol-water solution with a volume ratio of ethanol:water of 10:1, and adjust the pH to 8.5 with ammonia water; raise the temperature to 40°C, slowly add 80 mL / L ethyl orthosilicate to the ethanol-water solution, and vigorously Stir for 2h, continue to add 22mL / L hexadecyltrimethoxysilane and 70mL / L ethyl orthosilicate, and vigorously stir the mixed solution for 1h; after centrifugal filtration, the mixed solution is washed with ethanol and deionized water, respectively 3 times, and the filtered items were dried at 60 °C for 8 h to obtain a uniformly layered coating structure of SiO 2 @SiO 2 Nanospheres.

[0059] ②Take 2.0g of the prepared SiO 2 @SiO 2 The nanospheres were dispersed in 500 mL of water, and 0.006 mol of nickel acetate and 0.2 mol of urea were dissolved therein, the temperature was raised to 120° C., refluxed and stirred for 2 h, and then centrifuged and filtered, and washed with ethanol and deionized water for 3 times respectively. Aft...

Embodiment 3

[0062] ① Prepare an ethanol-water solution with a volume ratio of ethanol:water of 1:1, and adjust the pH to 9.0 with ammonia water; raise the temperature to 30°C, slowly add 40 mL / L of silica sol to the ethanol-water solution, and stir vigorously for 7h, Continue to add 30mL / L dodecyltrimethoxysilane and 100mL / L silica sol, and stir the mixed solution vigorously for 4h; after centrifugal filtration of the above mixed solution, wash with ethanol and deionized water for 3 times respectively, and filter the items in Dry at 125°C for 12h to obtain a uniformly layered coating structure of SiO 2 @SiO 2 Nanospheres.

[0063] ②Take 2.0g of the prepared SiO 2 @SiO 2 The nanospheres were dispersed in 300 mL of water, and 0.01 mol of nickel acetate and 0.2 mol of urea were dissolved therein, the temperature was raised to 70 ° C, refluxed and stirred for 5 h, and then centrifugally filtered, washed with ethanol and deionized water for 5 times, and the filtered items were placed at 80 ...

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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...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/745B01J35/10B01J37/03C07C29/17C07C31/20
CPCB01J23/745B01J37/031C07C29/172B01J35/397B01J35/615B01J35/647C07C31/207
Inventor 王长真赵永祥李海涛
Owner SHANXI UNIV
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