Preparation method of nickel phosphide catalyst carried by composite carrier

A composite carrier and nickel phosphide technology, which is applied in the direction of catalyst activation/preparation, physical/chemical process catalysts, chemical instruments and methods, etc., can solve problems such as difficult to be widely used, small specific surface area, poor mechanical strength, etc., to achieve The pore structure is suitable, the specific surface area is large, and the effect of improving the dispersion effect

Inactive Publication Date: 2009-12-30
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But TiO 2 As a catalyst carrier, there are also some weaknesses, such as its specific surface area is relatively small, generally not more than 100m 2 g -1 , the active anatase type is not stable enough at high temperature, and it is easy to transform into an inert rutile structure, with poor mechanical strength and weak acidity, making it difficult to be widely used in industry

Method used

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  • Preparation method of nickel phosphide catalyst carried by composite carrier
  • Preparation method of nickel phosphide catalyst carried by composite carrier

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] a. Dissolve 13ml of tetrabutyl titanate in 13ml of ethanol and 1.3ml of glacial acetic acid to form a mixed solution of tetrabutyl titanate, and weigh 7.8g of γ-Al 2 o 3 Place in the mixed solution of tetrabutyl titanate, and disperse the above mixed solution under ultrasonic for 30min, with ultrasonic power of 500W. After aging for half a day, the γ-Al 2 o 3 The surface of the carrier is coated with a layer of TiO 2 . After centrifugal filtration, wash three times with absolute ethanol and deionized water respectively, and dry in a drying oven at 120° C. for 12 hours. Place the dried powder in a muffle furnace, calcinate at 300°C for 5 hours, and cool to room temperature to obtain TiO 2 -Al 2 o 3 Composite carrier.

[0025] b. Weigh 8.25 g of the carrier prepared by the above method, and add it into a three-necked flask with a funnel. Weigh 7.5g nickel nitrate Ni (NO 3 ) 2 ·6H 2 O and 6.5g diammonium hydrogen phosphate (NH 4 ) 2 HPO 4Dissolve in 20g deio...

Embodiment 2

[0029] a. Dissolve 13ml of tetrabutyl titanate in 13ml of ethanol and 3.9ml of glacial acetic acid to form a mixed solution of tetrabutyl titanate, and weigh 5.2g of γ-Al 2 o 3 Put it in the mixed solution of tetrabutyl titanate, and disperse the above mixed solution under ultrasonic for 20min, the ultrasonic power is 700W. After aging for half a day, the γ-Al 2 o 3 The surface of the carrier is coated with a layer of TiO 2 . After centrifugal filtration, wash three times with absolute ethanol and deionized water respectively, and dry in a drying oven at 120° C. for 12 hours. Place the dried powder in a muffle furnace, calcinate at 500°C for 3 hours, and cool to room temperature to obtain TiO 2 -Al 2 o 3 Composite carrier.

[0030] b. Weigh 8.5 g of the carrier prepared by the above method, and add it into a three-necked flask with a funnel. Weigh 7.5g nickel nitrate Ni (NO 3 ) 2 ·6H 2 O and 4.5g diammonium hydrogen phosphate (NH 4 ) 2 HPO 4 Dissolve in 22g deio...

Embodiment 3

[0033] In this example step a composite carrier TiO 2 -Al 2 o 3 In the preparation process of , the traditional mechanical stirring is used instead of ultrasonic dispersion; in the preparation process of the oxidation state nickel phosphide catalyst precursor in step b, the traditional mechanical stirring is also used instead of ultrasonic impregnation, and drying in a 120 °C drying oven instead of microwave oven Drying under the power of 700W, other operating steps are according to embodiment 1, obtain Ni 2 P / TiO 2 -Al 2 o 3 Catalyst, denoted as Catalyst II. The activity evaluation of the catalyst was carried out according to the method of Example 1. When reacting at 340°C, the desulfurization rate of dibenzothiophene is about 95%.

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Abstract

The invention relates to a preparation method of a nickel phosphide catalyst carried by a composite carrier. The method is characterized by comprising the following steps: firstly, using activated alumina and relative enzymes and alcohols as raw materials to prepare a composite carrier of TiO2-Al2O3 by adopting an improved sol-gel method; further, selecting suitable nickel salt and phosphate and carrying out ultrasound dipping and drying in microwaves to obtain a catalyst precursor; and finally, increasing a temperature by a program and reducing to obtain the composite support. The composite carrier of TiO2-Al2O3 prepared by the invention not only can effectively overcome the defect that nickel phosphide is apt to react with gamma-Al2O3 to generate AlP4 to lose the activity, but also overcomes the defect that a specific surface area of single TiO2 is relatively small, effectively exerts the strong metal-support interaction (SMSI) of the TiO2, thereby obtaining a hydrodesulfurization catalyst with remarkable activity efficacy.

Description

technical field [0001] The present invention relates to the preparation of an oil hydrodesulfurization catalyst, in particular to a preparation method of a nickel phosphide catalyst that changes the carrier used for carrying the active component Background technique [0002] As we all know, catalytic hydrodesulfurization (HDS) technology is still the main way to reduce the sulfur content of gasoline and diesel. The activity of traditional hydrodesulfurization catalysts has not reached the new low-sulfur content standard, so it is urgent to find efficient hydrogenation desulfurization catalyst. [0003] Studies have shown that transition metal phosphide catalysts, especially nickel phosphide, have attracted much attention due to their excellent hydrodesulfurization activity, but unsupported Ni 2 The specific surface area of ​​the P catalyst is very small (less than 1m 2 g -1 ), in order to increase its active surface area, Ni 2 P is supported on a carrier with a higher sp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/185B01J37/34B01J37/02B01J37/16C10G45/06
Inventor 杨伯伦王凯乐
Owner XI AN JIAOTONG UNIV
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