Supported nickel-based alloy catalyst as well as preparation method and application thereof

A nickel-based catalyst and nickel-based alloy technology, applied in the field of catalysis, can solve the problems of complex preparation process, difficulty in activating ester group, high ratio of reaction hydrogen to ester, etc.

Pending Publication Date: 2019-04-26
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process of DMO hydrogenation to MG, the catalyst needs to activate the ester group and hydrogen at the same time, and the nickel-based catalyst can activate the hydrogen well but it is difficult to activate the ester group, so it shows a poor conversion rate of DMO
[0005] The inventor disclosed a nickel-indium carbide alloy catalyst in the patent CN201710956080.1. By forming a nickel-indium carbide alloy with nickel in carbon and indium elements, the ability of the nickel-based catalyst to hydrogenate and activate the ester group was improved. The patented nickel-indium carbide alloy catalyst InNi 3 C 0.5 / Ni-foam is used in the hydrogenation reaction of dimethyl oxalate to ethylene glycol. Under the high DMO conversion rate, ethylene glycol has high selectivity, but the indium in the catalyst is expensive (In(NO 3 ) 3 .4H2O, nearly 2 million yuan per ton), so the cost of the catalyst is very high. At the same time, the catalyst needs to be used at a higher temperature, and its low-temperature selectivity is poor. Therefore, the catalyst is not conducive to industrial applications
The inventor disclosed a self-supporting nickel phosphide catalyst in the patent CN201710956090.5. The nickel phosphide catalyst in this patent was used in the reaction of dimethyl oxalate hydrogenation to methyl glycolate, and obtained high DMO conversion Methyl glycolate has a high selectivity at a high rate, but the preparation process of this catalyst requires the use of highly toxic phosphine gas and the preparation process is complicated. In addition, the hydrogen-ester ratio of the reaction is also high, which is not conducive to industrial applications.

Method used

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  • Supported nickel-based alloy catalyst as well as preparation method and application thereof
  • Supported nickel-based alloy catalyst as well as preparation method and application thereof
  • Supported nickel-based alloy catalyst as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0080] 1) Weigh 1 gram of foamed nickel (110PPI), put it in a 1% aqueous solution of sodium carbonate and ultrasonically treat it for 30 minutes, remove surface oil stains, wash it with distilled water, and then place the foamed nickel in 1 mol / liter of dilute hydrochloric acid Ultrasonic treatment in the solution for 30 minutes to remove surface oxides, wash with distilled water until the solution is neutral; then transfer the foamed nickel to an autoclave, add 20 mmol of nickel nitrate, 80 mmol of ammonium chloride, and 80 ml of water, At 100°C, hydrothermal reaction for 6 hours, the reaction was completed, the temperature was naturally lowered to room temperature, the distilled water was taken out for ultrasonic cleaning, and dried at 100°C to obtain a supported nickel-based catalyst with a nickel hydroxide crystal layer grown in situ on the carrier precursor;

[0081] 2) Take by weighing 1.73 grams of ferric nitrate nonahydrate and dissolve in 0.7 gram of water to obtain a...

Embodiment 2

[0102] 1) Weigh 1 gram of foamed nickel (110PPI), put it in a 1% aqueous solution of sodium carbonate and ultrasonically treat it for 30 minutes, remove surface oil stains, wash it with distilled water, and then place the foamed nickel in 1 mol / liter of dilute hydrochloric acid The solution was ultrasonically treated for 30 minutes to remove surface oxides, and washed with distilled water until the solution was neutral; then the nickel foam was transferred to an autoclave, and 180 mmol of oxalic acid, 15 mmol of ammonium chloride, and 80 ml of water were added. Under 180°C, hydrothermal reaction for 24 hours, finish the reaction, naturally cool down to room temperature, take out distilled water, ultrasonically clean, and dry at 100°C to obtain a supported nickel-based catalyst precursor with a nickel oxalate crystal layer grown in situ on the carrier ;

[0103] 2) Weigh 0.55 grams of zinc nitrate and dissolve in 0.7 grams of water to obtain an aqueous solution containing zinc ...

Embodiment 3

[0118] 1) Weigh 1 gram of foamed nickel (110PPI), put it in a 1% aqueous solution of sodium carbonate and ultrasonically treat it for 30 minutes, remove surface oil stains, wash it with distilled water, and then place the foamed nickel in 1 mol / liter of dilute hydrochloric acid Ultrasonic treatment in the solution for 30 minutes to remove surface oxides, washing with distilled water until the solution is neutral; then transfer the foamed nickel to an autoclave, add 80 mmoles of terephthalic acid, 80 mmoles of nickel nitrate, 80 ml of di Methylformamide, at 140 ° C, solvothermal reaction time of 24 hours, the reaction is completed, the temperature is naturally cooled to room temperature, the distilled water is taken out and ultrasonically cleaned, and dried at 100 ° C, that is, the in-situ growth of nickel terephthalate on the carrier Supported nickel-based catalyst precursors for crystalline layers;

[0119] 2) Take by weighing 0.52 gram of tin protochloride and be dissolved i...

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Abstract

The invention discloses a supported nickel-based alloy catalyst as well as a preparation method and application thereof. The supported nickel-based alloy catalyst comprises a carrier and a nickel-based alloy supported by the carrier. The nickel-based alloy is a NixMyCz alloy, wherein x is greater than or equal to 1 and less than or equal to 10, y is greater than or equal to 1 and less than or equal to 10, and z is greater than or equal to 0 and less than or equal to 5; M is selected from at least one of iron, copper, cobalt, zinc, molybdenum, palladium, silver, gallium, indium, tin, germanium,bismuth and lead; in addition, when z is greater than 0, M is not indium, the total mass of the nickel-based alloy is 1 to 50 percent, and the balance is a carrier. The catalyst provided by the invention has the advantages of stable structure, good thermal conductivity, high permeability, high conversion rate, high selectivity, high activity, high mechanical strength, easiness in forming and filling, high throughput, low pressure drop and the like. The supported nickel-based alloy catalyst is a good catalyst for reactions for preparing methyl glycollate, ethylene glycol and ethanol by hydrogenation of dimethyl oxalate.

Description

technical field [0001] The present invention relates to a kind of catalyst and its preparation method and application, specifically, relate to a kind of supported nickel base alloy catalyst and its preparation method and its hydrogenation of dimethyl oxalate to produce methyl glycolate reaction, dimethyl oxalate The application of ester hydrogenation to ethylene glycol reaction and dimethyl oxalate hydrogenation to ethanol reaction belongs to the technical field of catalysis. Background technique [0002] With the increasing shortage of petroleum resources and the gradual strengthening of people's awareness of environmental protection, research and search for environmentally friendly alternatives to petroleum energy have become one of the directions of technology development in the world's energy field. In view of this, exploring the efficient and clean utilization of coal resources is an important way to realize the diversification of Sinopec products, optimize the energy s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755B01J23/835B01J23/889B01J27/22C07C29/149C07C67/29C07C69/675C07C31/20C07C31/08
CPCC07C29/149C07C67/29B01J23/755B01J23/835B01J23/8892B01J27/22B01J27/224B01J27/24C07C31/202C07C31/08C07C69/675Y02P20/52
Inventor 路勇朱坚赵国锋刘晔
Owner EAST CHINA NORMAL UNIV
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