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Process for preparing high dispersion supported type transition metal phosphide catalyst

A transition metal and phosphide technology, which is applied in the field of preparation of highly dispersed supported transition metal phosphide catalysts, can solve problems such as uneven distribution of phosphides, and achieve easy large-scale preparation, improved dispersion degree, and high dispersion degree Effect

Inactive Publication Date: 2008-04-30
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the distribution of phosphides prepared in this way on the surface of the support is not very uniform

Method used

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  • Process for preparing high dispersion supported type transition metal phosphide catalyst
  • Process for preparing high dispersion supported type transition metal phosphide catalyst
  • Process for preparing high dispersion supported type transition metal phosphide catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1MoP / Al 2 o 3

[0020] The pore volume (mlg) of the carrier used was determined in advance -1 ), according to the amount of carrier, determine the water content in the impregnation solution. Al used in this example 2 o 3 The pore volume is 1.1mlg -1 . Weigh ammonium molybdate 0.364g and diammonium hydrogen phosphate 0.276g of target phosphide (MoP) stoichiometric ratio (molybdenum: phosphorus = 1: 1) and be dissolved in 3.3ml water, after completely dissolving, citric acid is added to above solution to obtain impregnation solution. The amount of citric acid and metal molybdenum is 2:1 (molar ratio). Weigh 3.0g Al 2 o 3 Immerse in the immersion solution, let stand for 6 hours, dry at 120°C for 12 hours, and finally calcinate at 500°C for 5 hours under a flowing air atmosphere to obtain a precursor. Under a hydrogen atmosphere, the precursor was raised from room temperature to 350 °C in 0.5 h, then raised to 850 °C at a rate of 5 °C / min, kept at this te...

Embodiment 2

[0023] Example 2 WP / SiO 2

[0024] The preparation method is the same as in Example 1. SiO used in this example 2 The pore volume is 1.5mlg -1 . Weigh 0.567g of ammonium metatungstate with the target phosphide (WP) stoichiometric ratio (tungsten: phosphorus = 1:1), and dissolve 0.275g of diammonium hydrogen phosphate in 4.5ml of water. After completely dissolving, add malic acid to the above solution to obtain an impregnating solution. The amount of malic acid and metal molybdenum is 1:1 (molar ratio). Weigh 3.0g SiO2 2 into the immersion solution. After standing still for 10 hours, it was dried at 140°C for 10 hours, and finally calcined at 450°C for 5 hours under a flowing air atmosphere to obtain a precursor. Under a hydrogen atmosphere, the precursor was raised from room temperature to 350 °C in 0.5 h, then raised to 750 °C at a rate of 5 °C / min, kept at this temperature for 2 h, and then cooled to room temperature. In order to prevent the violent oxidation reacti...

Embodiment 3

[0025] Example 3 Ni 2 P / SiO 2

[0026] Weigh the target phosphide (Ni 2 P) nickel nitrate 3.15g of stoichiometric ratio (nickel: phosphorus = 2: 1) is mixed with diammonium hydrogen phosphate 0.74g and dissolved in 4.5ml water, and a green precipitate is formed; 3:1) was added to the above solution, and after the tartaric acid was completely dissolved, a clear impregnation solution was obtained. Weigh 3.0g SiO2 2 Put it into the immersion solution, let it stand for 10 hours, dry it at 140°C for 10 hours, and finally calcinate it at 450°C for 5 hours under the flowing air atmosphere to obtain the precursor. Under a hydrogen atmosphere, the precursor was raised from room temperature to 350 °C in 0.5 h, then raised to 600 °C at a rate of 5 °C / min, and kept at this temperature for 2 h, then cooled to room temperature. In order to prevent the violent oxidation reaction of phosphide in contact with air, before the sample is exposed to air, use O 2 / N 2 (1% V / V) passivation fo...

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Abstract

The invention relates to a catalyst of supported metal phosphide, in particular to a process for preparing the catalyst of high dispersive supported metal phosphide. The catalyst is composed of two parts of active components and a carrier which can be represented by AP / Z or B2P / Z, wherein the A of the active components is Mo or W, the B of the active components is Ni or Co, and the Z of the carrier is Al2O3 or SiO2. The operation steps of the catalyst are that transient metal salt and mammonium dihydrogen phosphate are dissolved in deionized water according to the stoichiometric ratio of targeted phosphide, and simultaneously moderate hydroxy acid as chelating agent is added to get the impregnating solution for preparing supported transition metal phosphide. The porous carrier is immersed in the impregnating solution, and is rested, the procedure gains temperature and returns after the impregnating solution is dried, roasted and under the atmosphere of hydrogen gas, and finally the supported transition metal phosphide is made. The supported transition metal phosphide prepared by the preparation method has the advantages of high dispersion, simple and convenient operation, low cost, no pollution, good repeatability and easiness of large scale preparation.

Description

technical field [0001] The invention relates to a loaded metal phosphorus compound catalyst, in particular to a preparation method of a highly dispersed loaded transition metal phosphide catalyst. Background technique [0002] Phosphide has noble metal-like catalytic properties, and is a new type of catalytic material after transition metal carbides and nitrides. It has been successfully applied to the deep hydrodesulfurization and hydrodenitrogenation reactions of oil products, and it is a great substitute for the existing Co(Ni)MoS / Al 2 o 3 Potential of catalysts for commercial use (Journal of Catalysis, 216 (2003), 343). On the other hand, this new type of substance can also be widely used in many other hydrogen-related reactions, such as hydrogenation reaction, reduction of NO and electrochemical reduction reaction. [0003] In these catalytic reactions, supported transition metal phosphide catalysts are mostly used (Journal of Catalysis, 218(2003), 78). The supporte...

Claims

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Application Information

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IPC IPC(8): B01J27/185B01J27/187B01J21/04B01J21/08C01B21/02C01C1/02C01B3/04
CPCY02E60/364Y02E60/36Y02P20/52
Inventor 程瑞华张涛李林孙军舒玉瑛王晓东
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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