Preparation method of middle-low temperature coal tar hydrotreating catalyst Ni2P/SiO2 or Ni2P/Al2O3

A low-temperature coal tar and hydrotreating technology, which is applied in the direction of physical/chemical process catalysts, chemical instruments and methods, and petroleum industry, and can solve the problem of low preparation temperature

Inactive Publication Date: 2018-10-30
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention is used in order to solve Ni 2 The preparation of P-loaded catalysts requires high temperature and high consumption of phosphorus sources. To provide a low-temperature, non-toxic, environmentally friendly and low-temperature coal tar hydrotreating catalyst Ni 2 P / SiO 2 and Ni 2 P / Al 2 o 3 preparation method

Method used

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  • Preparation method of middle-low temperature coal tar hydrotreating catalyst Ni2P/SiO2 or Ni2P/Al2O3

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 1. Prepare 0.86 moL / L nickel nitrate hexahydrate solution, and load nickel nitrate to SiO by equal volume impregnation 2 on the carrier.

[0019] 2. Dry the carrier at 80 °C for 12 h. The samples were then calcined at 330 °C in air for 5 h.

[0020] 3. Put 10 g of the calcined product into a tube furnace fed with hydrogen, and the hydrogen flow rate is 60 mL / min. Reduction was carried out at 350°C for 3 h.

[0021] 4. Transfer 4 g of the reduced product into a 1 L reactor and blow nitrogen into it. Weigh 0.105 g red phosphorus into the reactor (1.04 times the theoretical phosphorus consumption). The reactor was heated to 390 °C at a rate of 2 °C / min and then kept for 120 min. After the reaction, the reactor was cooled to room temperature. followed by 0.5 vol% O 2 / N 2 Mixed gas, the passivation time is 2 h, and the medium and low temperature coal tar hydrogenation catalyst with 27wt% Ni 2 P / SiO 2 .

Embodiment 2

[0023] 1. Prepare a 0.7 mol / L nickel acetate solution, and load nickel acetate onto SiO by equal volume impregnation 2 on the carrier.

[0024] 2. Dry the carrier at 100 °C for 10 h. The samples were then calcined at 350 °C for 5 h in air.

[0025] 3. Put 10 g of the calcined product into a tube furnace fed with hydrogen, and the hydrogen flow rate is 32 mL / min. Reduction was carried out at 360 °C for 6 h.

[0026] 4. Transfer 4 g of the reduced product into a 1 L reactor and blow nitrogen into it. Weigh 0.12 g red phosphorus into the reactor (1.06 times the theoretical phosphorus consumption). The reactor was heated to 400 °C at a rate of 3 °C / min and then kept for 100 min. After the reaction, the reactor was cooled to room temperature. followed by 0.5 vol% O 2 / N 2 , the passivation time is 3 h, and the medium and low temperature coal tar hydrogenation catalyst with 21 wt% Ni 2 P / SiO 2 .

Embodiment 3

[0028] 1. Prepare a 1 mol / L nickel acetate solution, and load nickel acetate onto SiO by equal volume impregnation 2 on the carrier.

[0029]2. Dry the carrier at 100 °C for 10 h. The samples were then calcined at 360 °C for 5 h in air.

[0030] 3. Put 10 g of the calcined product into a tube furnace fed with hydrogen, and the hydrogen flow rate is 45 mL / min. The reduction was carried out at 360°C, and the reduction time was 6 h.

[0031] 4. Transfer 4 g of the reduced product into a 1 L reactor and blow nitrogen into it. Weigh 0.13 g red phosphorus into the reactor (1.08 times the theoretical phosphorus consumption). The reaction kettle was heated to 404 °C at a rate of 3 °C / min and then kept for 100 min. After the reaction, the reactor was cooled to room temperature. followed by 0.5 vol% O 2 / N 2 , the passivation time is 4 h, and the medium and low temperature coal tar hydrogenation catalyst with 30wt% Ni 2 P / SiO 2 .

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Abstract

The invention discloses a preparation method of a middle-low temperature coal tar hydrotreating catalyst Ni2P/SiO2 or Ni2P/Al2O3. The preparation method comprises the following steps: impregnating nickel nitrate onto an SiO2 or Al2O3 carrier at equal volume; drying, calcining in air; reducing with hydrogen; reacting a reduction product and red phosphorus at 390-410 DEG C for 30-120 min; after finishing the reaction, cooling a reactor to room temperature; and then, feeding a nitrogen-oxygen gas mixture having an oxygen concentration of 0.5 vol% to 2 vol% for passivation. The preparation methodprovided by the invention has advantages of low cost, no toxicity, environmental protection and low phosphorus consumption.

Description

technical field [0001] The invention relates to a medium and low temperature coal tar hydrotreating catalyst Ni 2 P / SiO 2 or Ni 2 P / Al 2 o 3 method of preparation. Background technique [0002] Most of the current medium and low temperature coal tar hydrotreating catalysts use the traditional NiMoS / Al 2 o 3 catalyst. Since Robinson et al. discovered Ni in 1996 2 P exhibits a stronger performance in hydrodenitrogenation than the conventional industrial catalyst NiMoS / Al 2 o 3 After better results, the researchers then performed Ni 2 P catalysts have given high attention (W. Robinson, J. N. M. van Gestel, T. Koranyi, S. Eijsbouts, A. M. van der Kraan, J. A. van Veen, V. H. de Beer, Journal of Catalysis 1996, 161 , 539-550.). Studies have shown that Ni 2 P catalysts have excellent activity in hydrodenitrogenation, hydrodesulfurization, hydrodeoxygenation, and hydrodechlorination (D. Liu, A. Wang, C. Liu, R.Prins, Catalysis Communications 2016, 77, 13- 17; W. Wang...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/185C10G45/06
CPCB01J27/1853C10G45/06C10L2200/043
Inventor 崔海涛邵明强赵亮富
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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