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Preparation method of thermometal phosphide hydrofining catalyst

A hydrorefining, bimetallic technology, applied in physical/chemical process catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve the problems of decreased catalyst activity, bimetallic phosphide activity is not as good as single metal phosphide, etc. To achieve the effect of improving catalyst activity

Active Publication Date: 2014-08-27
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the transition metal phosphide is different from the traditional sulfide structure. When the second metal component is introduced, the activity of the catalyst will generally decrease, that is, the activity of the double metal phosphide is not as good as that of the single metal phosphide.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] a. Under stirring at room temperature, mix 8.07 g (NH 4 ) 6 W 7 o 24 .6H 2 O and 4.37 g (NH 4 ) 2 HPO 4 Dissolved in 27 g of deionized water, evaporated to dryness at 120°C to obtain a solid powder, which was calcined in a muffle furnace at 550°C for 2 hours to obtain a precursor of bulk WP. Take 1 gram of bulk WP precursor and place it in a fixed-bed reactor, raise the temperature from room temperature to 650 °C at a rate of 10 °C / min in a 100 mL / min pure hydrogen (99.99%) gas flow and keep it for 2 h, and then decrease to 650 °C. to room temperature, and passivated in nitrogen for 1 hour to obtain bulk WP.

[0017] b. Under stirring at room temperature, 1.60 g of NiCl 2 .6H 2 O and 1.07 g NaH 2 PO 2 .H 2 O was dissolved in 10.15 g of water, then 1.0 g of bulk WP was added, stirred for 4 hours, and dried in an oven at 60°C to obtain bulk bimetallic phosphide WP-Ni 2 Precursor of P catalyst. Take 1 gram of bulk bimetallic phosphide WP-Ni 2 The precursor o...

Embodiment 2

[0019] a. While stirring at room temperature, mix 8.07 grams of ammonium metatungstate (NH 4 ) 6 W 7 o 24 .6H 2 O and 4.37 g (NH 4 ) 2 HPO 4 Dissolve in 60 grams of deionized water, then add 15 grams of superfine silica, soak at room temperature for 10 hours, evaporate to dryness at 120°C to obtain a solid powder, and roast the obtained solid powder in a muffle furnace at 550°C for 2 hours to obtain silica Loaded WP precursor. Take 1 g of silica-supported WP precursor and place it in a fixed-bed reactor, and raise the temperature from room temperature to 650 °C at a rate of 10 °C / min in a 100 mL / min pure hydrogen (99.99%) gas flow and keep it for 2 h , then cooled down to room temperature, and passivated in nitrogen for 1 hour to obtain silica-supported WP.

[0020] b. Under stirring at room temperature, 0.66 g of NiCl 2 .6H 2 O and 0.44 g NaH 2 PO 2 .H 2 O was dissolved in 5 g of deionized water, then 1.0 g of silica-loaded WP was added, stirred for 4 hours, and ...

Embodiment 3

[0023] Catalyst preparation process and condition are the same as embodiment 1, and difference is that the ammonium metatungstate of 8.07 grams (NH 4 ) 6 W 7 o 24 .6H 2 O is replaced by 5.28 g (NH 4 ) 6 Mo 7 o 24 .4H 2 O, the bulk bimetallic phosphide MoP-Ni can be obtained 2 P catalyst.

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PUM

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Abstract

The invention provides a preparation method of a thermometal phosphide hydrofining catalyst. The method comprises the following steps of: firstly, preparing a bulk phase WP or a WP loaded by a porous carrier material by adopting a traditional procedure warming reduction method, then soaking the bulk phase WP or the WP loaded by the carrier in a nickel chloride and sodium hypophosphite solution, drying, carrying out thermal treatment in nitrogen, passivating and washing to obtain the bulk phase thermometal phosphide WP-Ni2P catalyst or the catalyst loaded by the carrier, and bulk phase thermometal phosphide MoP-Ni2P catalyst or the catalyst loaded by the carrier can be obtained by adopting the same method. The method provided by the invention has characteristics that the method effectively utilizes temperature difference between the metal phosphide prepared by the procedure warming reduction method and the metal phosphide prepared by a hypophosphite resolving method, a novel preparation technology of the thermometal phosphide hydrofining catalyst is provided, the method realizes the synergy acceleration action of different metal phosphides, and the catalytic activity of the metal phosphide is effectively improved.

Description

technical field [0001] The invention belongs to the technical fields of catalytic materials, petroleum refining and petrochemical industry, and relates to a preparation method of a bimetallic phosphide catalyst used in oil hydrorefining. Background technique [0002] With the heavy and inferior quality of crude oil, the enhancement of people's awareness of environmental protection and the increasingly stringent environmental protection laws and regulations, the development of clean fuel production technology has become one of the most important challenges and driving forces for petroleum refining technology. To meet this challenge, oil refining technology is developing towards the production of clean petroleum fuels with ultra-low sulfur and ultra-low nitrogen content. The traditional hydrorefining catalysts are supported Ni-Mo, Ni-W or Co-Mo sulfides Catalysts, although sulfide catalysts have been continuously improved, their performance still cannot meet the increasingly s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/19B01J27/188
Inventor 李伟魏入朝
Owner NANKAI UNIV
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