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Method for preparing 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 good stability, high hydrodesulfurization activity, and reduce the desulfurization rate of hydrogenation reaction

Inactive Publication Date: 2013-02-13
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] Amorphous phosphotungstate was pulverized at room temperature and mixed with γ-Al 2 o 3 Mix evenly, then press into tablets and sieve, take 100-mesh particles and reduce them for 4 hours in a hydrogen stream with a purity of 99.999%, a speed of 300mL / min, and a heating rate of 1K / min to 923K, and then at room temperature. Flow rate of 30 mL / min with 0.5% O 2 passivation in a nitrogen stream for 2 h.

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 94.2%.

Embodiment 3

[0015] 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 76.00% cyclohexane, 2.0% n-octane, 2% n-octane Octane, 20% cyclohexene, 0.8% thiophene and 1.2% pyridine were punched in. 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. It is measured that after 105 hours of operation, the denitrification rate and desulfurization rate of the catalyst are only reduced by about 2%, which shows that the catalyst prepared in Example 1 has good stability.

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PUM

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Abstract

The invention discloses a method for preparing a tungsten phosphide catalyst, and relates to a method for preparing the catalyst. The method for preparing the tungsten phosphide catalyst comprises the following steps of: smashing amorphous phosphotungstate at room temperature, uniformly mixing the amorphous phosphotungstate and gamma-Al2O3, pressing, screening, reducing particles of a certain mesh number in 923K hydrogen flow for 4 hours, and carrying out passivating in nitrogen flow with 0.5 percent of O2 at the room temperature for 2 hours. The tungsten phosphide catalyst is relatively high in stability; the hydrodesulfurization activity is extremely high; and the hydrodesulfurization 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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IPC IPC(8): B01J27/188C10G45/04
Inventor 王耀斌
Owner SHAANXI HI TECH ENERGY DEV
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