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Transition metal phosphorus sulfide active phase preparation method

A technology of transition metals and phosphorus sulfides, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve problems such as safety problems, and achieve a wide range of applications

Active Publication Date: 2019-12-06
TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But these methods all need the hydrogen gas of higher pressure (generally greater than 1MPa), need or release highly toxic H at the same time. 2 S
The process not only consumes a lot of expensive hydrogen, but also has safety problems

Method used

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  • Transition metal phosphorus sulfide active phase preparation method
  • Transition metal phosphorus sulfide active phase preparation method
  • Transition metal phosphorus sulfide active phase preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Preparation of Ni by In Situ Temperature Programmed Reduction (TPR) of Phosphate Precursor 2 P, MoP and WP catalysts.

[0022] Weigh 6.60g nickel nitrate hexahydrate (Ni(NO 3 ) 2 ·6H 2 O) and 3.00g diammonium hydrogen phosphate ((NH 4 ) 2 HPO 4 ) were dissolved in 10mL and 15mL of deionized water respectively, under the condition of magnetic stirring, the (NH 4 ) 2 HPO 4 The solution was slowly added Ni(NO 3 ) 2 ·6H 2 In the O solution, after the dropwise addition, continue to stir for 0.5h, quickly evaporate a large amount of water, continue drying at 120°C for 12h, and then roast at 500°C for 3h to obtain Ni 2 P phosphate precursor with a Ni / P molar ratio of 1.

[0023] Weigh 4.01g ammonium molybdate ((NH 4 ) 6 Mo 7 o 24 4H 2 O) and 3.00g diammonium hydrogen phosphate ((NH 4 ) 2 HPO 4 ) were dissolved in 10mL and 15mL of deionized water respectively, under the condition of magnetic stirring, the (NH 4 ) 2 HPO 4 The solution was slowly added drop...

Embodiment 2

[0027] According to the method described in Example 1, in-situ reduction prepares Ni 2 After the P catalyst, lower the temperature to 240°C, and pass through the vulcanizing agent to react and vulcanize. The vulcanization liquid raw material used is 1.25% (mass fraction) of 2-phenyl-cyclohexanethiol / decalin solution, and the vulcanization conditions are: Ar pressure 4MPa, Ar flow rate 75mL / min, temperature 240°C, liquid hourly space velocity 54h -1 , The vulcanization treatment time is 2h. XPS spectrum of S2p region ( figure 1 ) shows that S is successfully embedded on the surface of the catalyst, and according to the position of the characteristic peak, the main sulfur species is S δ- (02 Phosphorus sulfide active phase of P.

Embodiment 3

[0029] According to the method described in Example 1, after the MoP catalyst was prepared by in-situ reduction, the temperature was lowered to 240° C., and a vulcanizing agent was introduced to react and vulcanize. The vulcanization liquid raw material used is 1.25% (mass fraction) 2-phenyl-cyclohexanethiol (2-PCHT) / decalin solution, and the vulcanization conditions are: Ar pressure 4MPa, Ar flow rate is 75mL / min, temperature 240 ℃, liquid hourly space velocity 54h -1 , The vulcanization treatment time is 2h. S 2p region XPS spectrum ( figure 2 ) shows that: 2-PCHT can successfully sulfide the surface of MoP in an inert atmosphere to form the phosphorus sulfide active phase of MoP. According to the characteristic peak position, the main sulfur species is S δ- (0<δ≤2). The sulfur content (in atomic percent) was 11.3%.

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Abstract

The invention relates to a transition metal phosphorus sulfide active phase preparation method, which comprises: treating a VI group and VIII group covalent transition metal phosphide catalyst by using an organic sulfur-containing compound containing alkyl or cycloalkyl C-S bond as a vulcanizing agent in an inert atmosphere to prepare the phosphorus sulfide active phase, wherein the transition metal phosphide is prepared by using a transition metal phosphate as a precursor through temperature-programmed reduction in a hydrogen atmosphere. Compared with the existing transition metal phosphorussulfide preparation method, the preparation method of the present invention does not require expensive and dangerous hydrogen, does not require or generate highly toxic H2S gas, and further has advantages of safety, low cost and good application prospect in industry.

Description

technical field [0001] The invention belongs to the technical field of heterogeneous catalysis, and relates to a transition metal phosphorous sulfide catalyst, in particular to a method for preparing a transition metal phosphorous sulfide active phase. Background technique [0002] Transition metal phosphides are a general term for compounds formed by transition metals (Fe, Co, Ni, Mo and W, etc.) and phosphorus. Among them, metal-rich transition metal phosphides (metal / phosphorus molar ratio ≥ 1) not only have the properties of metals, but also have high hardness and stability, so they have attracted attention in many reactions catalyzed by metal catalysts. Studies have shown that Ni 2 Transition metal phosphide catalysts represented by P, MoP and WP have higher intrinsic reactivity in hydrodesulfurization (HDS) and hydrodenitrogenation (HDN) reactions than traditional sulfide catalysts (Chem.Lett., 1998, 3:207), constituting a new type of fuel oil hydrotreating catalyst ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/185B01J27/19B01J27/188C10G45/06C10G45/04
CPCB01J27/1853B01J27/19B01J27/188C10G45/06C10G45/04
Inventor 李翔周学荣王安杰王琳刘盛男
Owner TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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