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Sulfide catalyst with palladium on nitrogen doped mesoporous carbon, and application of sulfide catalyst

A nitrogen-doped mesoporous carbon and sulfide technology is used in physical/chemical process catalysts, chemical/physical processes, preparation of organic compounds, etc. The effect of improving activity, not easy to be deactivated, and good stability

Inactive Publication Date: 2017-06-30
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although these methods have mature technology and mild reaction conditions, a large amount of waste water and waste residue are produced by-products, and the product quality is low.

Method used

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  • Sulfide catalyst with palladium on nitrogen doped mesoporous carbon, and application of sulfide catalyst
  • Sulfide catalyst with palladium on nitrogen doped mesoporous carbon, and application of sulfide catalyst
  • Sulfide catalyst with palladium on nitrogen doped mesoporous carbon, and application of sulfide catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] (1) Weigh 10g of mesoporous carbon, the particle size of mesoporous carbon is 1000 mesh, and the specific surface area is 1300m 2 / g, the average pore diameter is 3nm, mix it with 2g of urea evenly, and treat it at 800°C for 8h under nitrogen atmosphere to obtain 10g of nitrogen-doped mesoporous carbon;

[0042] (2) Prepare 10 g of nitrogen-doped mesoporous carbon obtained in step (1) in 100 ml of deionized water to prepare a slurry at a temperature of 25 ° C, and slowly add 10 ml of H 2 PdCl 4 Solution (the Pd content is 0.05g / ml, namely 0.47mmol / ml), stirred for 0.5h; the pH value of the solution was adjusted to 8 with 10wt% KOH solution, and the temperature was lowered to room temperature, filtered, and the filter residue was washed with deionized water until Neutral to get filter cake;

[0043] (3) The filter cake obtained in step (2) is configured into 80ml slurry at 80°C, 0.9g of 85wt% hydrazine hydrate solution (23.9mmol) is added dropwise, stirred for 2.5h, fi...

Embodiment 2

[0046] (1) Weigh 10g of mesoporous carbon, the particle size of mesoporous carbon is 800 mesh, and the specific surface area is 1500m 2 / g, the average pore size is 2nm, put it in NH 3 , the gas flow rate is 1L / h, and the treatment is at 200°C for 50h to obtain 9.9g of nitrogen-doped mesoporous carbon;

[0047] (2) Prepare 9.9 g of nitrogen-doped mesoporous carbon obtained in step (1) in 100 ml of deionized water to form a slurry at a temperature of 100 ° C, and slowly add 10 ml of Na 2 PdCl 4 solution (Pd content is 0.01g / ml, namely 0.094mmol / ml), stirred for 2h; the pH value of the solution was adjusted to 8.5 with 10wt% NaOH solution, and the temperature was lowered to room temperature, filtered, and the filter residue was washed with deionized water to medium sex;

[0048] (3) The filter cake obtained in step (2) is configured into a 50ml slurry at 100°C, 14g of 40wt% formaldehyde (186.7mmol) is added dropwise, stirred for 0.5h, filtered, and the filter cake is washed w...

Embodiment 3

[0051] (1) Weigh 10g of mesoporous carbon, the particle size of mesoporous carbon is 100 mesh, and the specific surface area is 1600m 2 / g, with an average pore diameter of 10nm, mix it with 14g of melamine evenly, and treat it at 1500°C for 0.5h under a helium atmosphere to obtain 10.0g of nitrogen-doped mesoporous carbon;

[0052] (2) Prepare 10.0 g of nitrogen-doped mesoporous carbon obtained in step (1) in 100 ml of deionized water to prepare a slurry at a temperature of 40° C., and slowly add 5 ml of Pd(NO 3 ) 2 Solution (the Pd content is 0.2g / ml, namely 1.88mmol / ml), stirred for 10h; the pH value of the solution was adjusted to 9 with ammonia water, and the temperature was lowered to room temperature, filtered, and the filter residue was washed with deionized water until neutral to obtain a filter cake ;

[0053] (3) The filter cake is then configured into a 100ml slurry at 20°C, 30g of 30wt% formic acid (195.7mmol) is added dropwise, stirred for 50 hours, filtered, t...

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Abstract

The invention discloses a sulfide catalyst with palladium on nitrogen doped mesoporous carbon, and application of the sulfide catalyst. The sulfide catalyst is prepared through the following steps: uniformly mixing mesoporous carbon with a nitrogen-containing compound to obtain nitrogen doped mesoporous carbon; enabling the obtained nitrogen doped mesoporous carbon to be made into seriflux; slowly dropwise adding a soluble palladium-containing solution according to the palladium loading capacity; performing thorough uniform stirring; adding an alkaline solution to regulate the pH value of the solution; lowering the temperature to room temperature; performing filtering to obtain a filter cake I and filter residues; performing washing until the filter residues are neutral; enabling the filter cakes I to be made into seriflux; dropwise adding a liquid-phase reduction agent; performing stirring; performing filtering to obtain a filter cake II; washing the filter cake II until the filter cake II is neutral; performing drying. Under inert atmosphere, high-temperature sulfidation is performed on the catalyst with palladium on nitrogen doped mesoporous carbon by adopting a sulphur-containing substance to obtain the sulfide catalyst with palladium on nitrogen doped mesoporous carbon. The sulfide catalyst with palladium on nitrogen doped mesoporous carbon, which is disclosed by the invention, is used for synthesizing sulfo-arylamine through catalytic hydrogenation.

Description

[0001] (1) Technical field [0002] The invention relates to a nitrogen-doped mesoporous carbon supported palladium sulfide catalyst and application thereof. [0003] (2) Background technology [0004] Sulfur is a poison of metal catalysts, and the catalytic hydrogenation of sulfur-containing organic compounds has always been a difficult problem in academia and industry. Ordinary metal catalysts will still have catalyst deactivation even at a high metal catalyst / sulfur-containing feedstock ratio. For example, the literature [E.K.Novakova, L.McLaughlin, et al.J.Catal., 2007, 249:93] reported that 10wt% Pd / C was used as a catalyst to achieve a liquid phase at 75°C and 5MPa hydrogen pressure. Catalytic hydrogenation / hydrogenolysis of 4,4'-dinitrodiphenyl disulfide to 4-aminothiophenol, but it should be pointed out that this is achieved when the mass ratio of Pd / C catalyst to raw material is as high as 1:1.3 (In ordinary hydrogenation reactions, the mass ratio of Pd / C catalyst to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/045B01J27/24C07B43/04C07C315/04C07C319/12C07C319/20C07C323/36C07C323/37C07C323/34C07C317/36B01J35/10
CPCC07B43/04C07C315/04C07C319/12C07C319/20B01J27/045B01J27/24B01J35/617B01J35/618B01J35/647C07C323/36C07C323/37C07C323/34C07C317/36
Inventor 张群峰丰枫马磊卢春山许孝良李康李小年
Owner ZHEJIANG UNIV OF TECH
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