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

A technology of hydrogenation catalyst and butynediol, which is applied in the direction of catalyst activation/preparation, hydrogenation preparation, hydroxyl compound preparation, etc. It can solve the problems of removal, reduction, and impact, and achieve the effect of curbing conversion

Active Publication Date: 2021-03-12
SHANXI UNIV
View PDF13 Cites 0 Cited by
  • 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

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Low-temperature low-pressure direct hydrogenation catalyst for coal-based 1,4-butynediol and preparation method thereof
  • Low-temperature low-pressure direct hydrogenation catalyst for coal-based 1,4-butynediol and preparation method thereof
  • Low-temperature low-pressure direct hydrogenation catalyst for coal-based 1,4-butynediol 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 30mL / L methyl orthosilicate to the ethanol-water solution, and vigorously Stir for 1h, continue to add 27mL / L hexadecyltrimethoxysilane and 85mL / L methyl orthosilicate, and stir the mixed solution vigorously for 1h; after the above mixed solution is centrifugally filtered, wash with ethanol and deionized water respectively 3 times, the filtered item was dried at 90°C for 10 hours to obtain a uniformly layered coating structure SiO 2 @SiO 2 nanospheres.

[0055] ②Take 2.0g of prepared SiO 2 @SiO 2 Nanospheres were dispersed in 150 mL of water, and 0.005 mol of nickel acetylacetonate and 0.4 mol of urea were dissolved in it respectively, heated to 60°C, refluxed and stirred for 4 hours, then centrifugally filtered, washed with ethanol and deionized water for 5 times, and the filtered items were placed ...

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 80mL / 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 stir the mixed solution vigorously for 1h; after the above mixed solution is centrifugally filtered, wash with ethanol and deionized water respectively 3 times, the filtered item was dried at 60°C for 8 hours to obtain a uniformly layered coating structure SiO 2 @SiO 2 nanospheres.

[0059] ②Take 2.0g of prepared SiO 2 @SiO 2 Disperse the nanospheres in 500mL water, and dissolve 0.006mol of nickel acetate and 0.2mol of urea in it respectively, raise the temperature to 120°C, reflux and stir for 2h, then centrifuge and filter, wash with ethanol and deionized water three times respectively, and filter the items at 100°C ℃ drying for 2...

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 40mL / L silica sol to the ethanol-water solution, and stir vigorously for 7 hours, Continue to add 30mL / L dodecyltrimethoxysilane and 100mL / L silica sol, and stir the mixed solution vigorously for 4h; after centrifuging and filtering the above mixed solution, wash with ethanol and deionized water for 3 times respectively, and filter the items in Dry at 125°C for 12 hours to obtain a uniformly layered coating structure SiO 2 @SiO 2 nanospheres.

[0063] ②Take 2.0g of prepared SiO 2 @SiO 2 Disperse the nanospheres in 300mL water, and dissolve 0.01mol of nickel acetate and 0.2mol of urea in it respectively, raise the temperature to 70°C, reflux and stir for 5h, then centrifuge and filter, wash with ethanol and deionized water for 5 times respectively, and filter the items at 80°C ℃ drying for 8 hours to o...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

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...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): B01J23/745B01J35/10B01J37/03C07C29/17C07C31/20
CPCB01J23/745B01J35/1019B01J35/1061B01J35/008B01J37/031C07C29/172C07C31/207
Inventor 王长真赵永祥李海涛
Owner SHANXI UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap