Method for preparing ternary complex carrier supported nickel phosphide catalyst

A ternary composite and composite support technology, applied in the direction of physical/chemical process catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve the problems of deactivation, catalyst coking and carbon deposition, etc.

Inactive Publication Date: 2012-11-14
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Patent literature (CN101612584B) discloses a TiO 2 -Al 2 o 3 A preparation method of a nickel phosphide catalyst supported by a binary composite carrier. The catalyst has better performance in removing dibenzothiophene, a sulfur-containing compound that is difficult to remove from oil products. During the removal of sulfur compounds and nitrogen-containing compounds, nitrogen-containing compounds are easily adsorbed to the surface of the catalyst and are not easy to desorb, making the catalyst easily deactivated by coking and carbon deposition

Method used

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  • Method for preparing ternary complex carrier supported nickel phosphide catalyst
  • Method for preparing ternary complex carrier supported nickel phosphide catalyst
  • Method for preparing ternary complex carrier supported nickel phosphide catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0022] a. Measure 4ml of deionized water and 12.8ml of ethanol, mix evenly, add nitric acid dropwise to adjust the pH value to about 4, and then add 2.6ml of acetic acid. Use a beaker to weigh 8.48g of butyl titanate and 7.143g of ethyl orthosilicate and mix evenly. After stirring to clarify, a golden transparent solution is obtained; then measure 25ml of ethanol, and add the golden solution and ethanol to the pH=4 solution at the same time. in solution. Weigh 8.0g of powdered γ-Al 2 o 3Add to the golden sol with strong stirring (300r / min), and continue to stir vigorously until a white gel is formed. The above gel was left to age for 5 hours, and then dried at 120° C. for 3 hours. Finally, the light yellow solid was calcined at 500 °C for 5 h to obtain a white composite support (SiO 2 with TiO 2 The introduction amount is 20wt% respectively).

[0023] b. Mix 11.832g of nickel nitrate, 10.649g of diammonium hydrogen phosphate and 30.0g of deionized water to completely dis...

Embodiment 2

[0027] a. Measure 4ml of deionized water and 13ml of ethanol and mix evenly, add nitric acid dropwise to adjust the pH value to about 4, and then add 3.0ml of acetic acid. Use a beaker to weigh 8.48g of butyl titanate and 4.24g of sodium metasilicate and mix them evenly. After stirring and clarification, a golden transparent solution is obtained; then measure 25ml of ethanol, and add the golden solution and ethanol into the solution with pH=4 at the same time . Weigh 8.0g of powdered γ-Al 2 o 3 Add to the vigorously stirred golden sol and continue stirring vigorously until a white gel forms. The above gel was left to age for 4 hours, and then dried at 120° C. for 3 hours. Finally, the light yellow solid was calcined at 550°C for 4h to obtain a white composite support (SiO 2 with TiO 2 The introduction amount is 20wt% respectively).

[0028] b. Mix 11.832g of nickel nitrate, 9.466g of diammonium hydrogen phosphate and 27.0g of deionized water to completely dissolve nickel...

Embodiment 3

[0031] a. Measure 4ml of deionized water and 12.8ml of ethanol, mix evenly, add nitric acid dropwise to adjust the pH value to about 4, and then add 2.6ml of acetic acid. Weigh 8.48g of butyl titanate and 5.8286g of silicon tetrachloride in a beaker and mix them evenly. After stirring and clarification, a golden transparent solution is obtained; then measure 25ml of ethanol, and add the golden solution and ethanol into the solution with pH=4 at the same time . Weigh 8.0g of powdered γ-Al 2 o 3 Add to the vigorously stirred golden sol and continue stirring vigorously until a white gel forms. The above gel was left to age for 6 hours, and then dried at 120° C. for 3 hours. Finally, the light yellow solid was calcined at 500°C for 6h to obtain a white composite support (SiO 2 with TiO 2 The introduction amount is 20wt% respectively).

[0032] b. Mix 11.832g of nickel nitrate, 8.282g of diammonium hydrogen phosphate and 25.0g of deionized water to completely dissolve nickel ...

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Abstract

The invention discloses a method for preparing ternary complex carrier supported nickel phosphide catalyst, comprising the following steps: preparing a SiO2-TiO2-Al2O3 composite support from raw materials including a silicon-containing compound such as the ethyl orthosilicate, activated alumina particles and butyl titanate by adopting the improved sol-gel process, impregnating, drying and calcinating at high temperature to obtain the precursor of the catalyst by using nickel nitrate and diammonium phosphate, and finally carrying out the temperature-programmed reduction to obtain the catalyst. Due to the introduction of the SiO2, the degree of crystallinity of the active phase of nickel phosphide is improved, the acidity of the catalyst is decreased, the adsorption of the nitrogen-containing compound in the oil on the surface of the catalyst is reduced, the problem on the deactivation of the catalyst due to coking and carbon depositing is avoided, and the catalyst has excellent oil hydrodesulfurization and hydrodenitrification performance.

Description

technical field [0001] The invention relates to a method for preparing an oil hydrodesulfurization and hydrodenitrogenation catalyst, in particular to a SiO 2 -TiO 2 -Al 2 o 3 Ni supported on ternary composite carrier 2 Preparation method of P catalyst. Background technique [0002] In recent years, the sulfur content standards of gasoline and diesel in developed countries have been limited to less than 10ppm. Therefore, it is urgent to solve the problem of how to efficiently produce low-sulfur fuels. Hydrodesulfurization is the current main desulfurization technology in the oil desulfurization industry, and the focus of this technology is the development of efficient hydrodesulfurization catalysts. [0003] However, during the hydrodesulfurization process of oil products, the nitrogen compounds in the oil products will seriously affect the progress of the hydrodesulfurization reaction on the catalyst. This is because the adsorption of nitrogen-containing compounds on ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/185C10G45/06
Inventor 杨伯伦陈涛
Owner XI AN JIAOTONG UNIV
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