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Preparation method for tungsten phosphide catalyst

A catalyst and tungsten phosphide technology, applied in physical/chemical process catalysts, chemical instruments and methods, chemical/physical processes, etc., to achieve high hydrodesulfurization activity, reduce desulfurization rate of hydrogenation reaction, and good stability

Inactive Publication Date: 2013-02-20
SHAANXI HI TECH ENERGY DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are few reports on phosphides, especially tungsten phosphide as active components of catalysts

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Will (NH 4 ) 2 W 4 o 13 18H 2 O and (NH 4 ) 2 HPO 4 Dissolve in deionized water, add dropwise to γ-Al 2 o 3 In, make γ-Al 2 o 3 After fully wetting, stir for 0.5 h, then bathe in 363 K water, then dry at 373 K for 3 h, and let it stand overnight; filter the obtained solid to crush, press into tablets, and take a certain number of particles at a flow rate of 300mL / min, at a heating rate of 1K / min to 923 K hydrogen flow for 4 h, then at room temperature at a flow rate of 30 mL / min, containing 0.5% O 2 passivation in nitrogen flow for 2h.

Embodiment 2

[0013] The catalyst prepared in Example 1 was activated with high-purity hydrogen at 400°C for 3 h. Next, put 1.5 mL of the catalyst (20-40 mesh) prepared in Example 1 into a stainless steel reaction tube with an inner diameter of 6 mm, and then use a liquid feed pump to feed 85.00% cyclohexane, 5.0% n-octane, 5.00% thiophene and 5.00% pyridine into it. Control reaction pressure 3.0 MPa, space velocity 4 h -1 , The volume ratio of hydrogen to oil is l 000. After the reaction, the reaction product was collected by condensation, quantified by GC-200 gas chromatograph, and detected by a hydrogen flame detector. The measured thiophene hydrodesulfurization rate was 98.3%.

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PUM

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Abstract

The invention relates to a preparation method for a tungsten phosphide catalyst. The preparation method for the tungsten phosphide catalyst comprises dissolving (NH4)2W4O13-18H2O and (NH4)2HPO4 in deionized water, dropwise adding the deionized water into gamma-Al2O3, mixing after gamma-Al2O3 is fully wetted, performing water bath in 363K water, drying for 3h under 373K, and standing for a night; filtering, smashing and sheeting obtained solid, taking a certain number of particles to perform reduction in 923K hydrogen flow for 4h, and performing passivation in nitrogen flow containing 0.5% of O2 for 2h at room temperature. The preparation method is good in stability, hydrodesulfurization activity is extremely large, and the hydrogenation reaction desulphurization rate of thiophene is reduced.

Description

technical field [0001] The invention relates to a preparation method of a catalyst. Background technique [0002] The contradiction between the increase of organic nitrogen compounds and sulfides in crude oil and the heavy crude oil and strict environmental protection regulations is becoming more and more prominent, so it is necessary to carry out deep hydrorefining of oil products. Studies have shown that although traditional molybdenum sulfide-based catalysts are effective in hydrorefining processes, they are far from meeting the requirements of deep hydrodesulfurization. The current approach is to modify the existing catalysts and find alternative new catalysts to meet the needs of improving the deep hydrotreating of crude oil. Since the 1990s, there have been reports on the synthesis and performance of molybdenum carbide and molybdenum nitride hydrodesulfurization catalysts abroad, as well as the structure and performance of catalysts such as P-Ni-Mo and P-Ni-Co with ph...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/188
Inventor 王耀斌
Owner SHAANXI HI TECH ENERGY DEV