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Preparation method of molybdenum phosphide catalysts

A molybdenum phosphide catalyst and catalyst technology, applied in the direction of physical/chemical process catalysts, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of cumbersome steps, high temperature required, difficult to reduce phosphate, etc., and achieve simple equipment, Low price, small particle effect

Active Publication Date: 2018-10-09
CHANGZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The P-O bond energy in ammonium phosphate is too strong, and the P-O bond must be destroyed by high temperature, so the required temperature is high and the steps are cumbersome
In addition, the patents (ZL200910070122.7, ZL200910070457.9 and ZL200910070458.3) use the thermal decomposition of hypophosphite precursor in nitrogen atmosphere to produce reducing phosphine gas to reduce molybdenum species to prepare molybdenum phosphide, but all of them need to be washed with water to obtain Pure molybdenum phosphide phase, this is due to the insufficient thermal decomposition of hypophosphite in a nitrogen atmosphere to generate some difficult-to-reduce phosphates, which are introduced into the catalyst system and must be washed with water to obtain a pure molybdenum phosphide phase

Method used

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  • Preparation method of molybdenum phosphide catalysts
  • Preparation method of molybdenum phosphide catalysts

Examples

Experimental program
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Effect test

Embodiment 1

[0022] First, dissolve 9g of molybdenum trioxide and 5.4g of ammonium hypophosphite in 20mL of ammonia water at room temperature, stir for 30 minutes and dissolve to a clear solution. The solution is dried at room temperature for 10 hours and then placed in an oven at 60°C for drying. The obtained white solid was ground into powder and then put into a quartz reactor and reduced by passing hydrogen gas. The hydrogen flow rate was maintained at 100 mL / min. The quartz reactor is heated from room temperature to 550°C with a heating rate of 2°C / min. Hold at 550°C for 3 hours. After the reduction, the unsupported MoP catalyst was obtained by naturally cooling to room temperature.

Embodiment 2

[0024] Firstly, 9g of molybdenum trioxide and 8.1g of ammonium hypophosphite were dissolved in 20mL of ammonia water at room temperature, stirred for 20min and then dissolved into a clear solution. The solution was dried at room temperature for 24 hours and then placed in an oven at 50°C for drying. The obtained white solid was ground into powder and then put into a quartz reactor and reduced by passing hydrogen gas. The hydrogen flow rate was maintained at 100 mL / min. The quartz reactor is heated from room temperature to 600°C with a heating rate of 2°C / min. Hold at 600°C for 3 hours. After the reduction, the unsupported MoP catalyst was obtained by naturally cooling to room temperature.

Embodiment 3

[0026] Firstly, 9g of molybdenum trioxide and 8.1g of ammonium hypophosphite were dissolved in 20mL of ammonia water at room temperature, stirred for 40 minutes, and then dissolved into a clear solution. The solution was dried at room temperature for 6 hours and then dried in an oven at 70°C. The obtained white solid was ground into powder and then put into a quartz reactor and reduced by passing hydrogen gas. The hydrogen flow rate was maintained at 150 mL / min. The quartz reactor was heated from room temperature to 600°C with a heating rate of 1°C / min. Hold at 600°C for 3 hours. After the reduction, the unsupported MoP catalyst was obtained by naturally cooling to room temperature.

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Abstract

The invention discloses a method using hydrogen to reduce molybdenum trioxide and ammonium hypophosphite to prepare supported and non-supported molybdenum phosphide (MoP) catalysts. The method is characterized in that the molybdenum trioxide and the ammonium hypophosphite serving as the reaction raw materials are dissolved in ammonia water, then simple low-temperature drying is performed to obtainprecursor powder, and the precursor powder is subjected to reduction under hydrogen atmosphere and relatively low reduction temperature to obtain the non-supported molybdenum phosphide catalyst; themolybdenum trioxide and the ammonium hypophosphite are added into ammonia water to obtain impregnation liquid, a carrier is impregnated with the impregnation liquid, drying is performed, and then temperature-rising reduction is performed under hydrogen protection to obtain the supported molybdenum phosphide catalyst. The method has the advantages that the method is simple in preparation process, low in synthesis temperature and short in synthesis cycle, and the obtained molybdenum phosphide catalysts do not need washing and are relatively small in particles and high in hydrogenation activity.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation, and relates to a method for preparing a molybdenum phosphide catalyst, and more specifically, to a method for preparing a non-supported and supported molybdenum phosphide catalyst. Background technique [0002] With the continuous decline in the quality of crude oil worldwide, the increase in the proportion of heavy components in crude oil, and the increasingly stringent environmental protection regulations, countries all over the world have put forward new requirements for the quality of oil products. On June 8, 2013, my country issued the national standard "Vehicle Diesel (Ⅴ)". As of January 1, 2018, it is clearly stipulated that the sulfur content in fuel must be less than 10ppm, and the content of polycyclic aromatic hydrocarbons should not exceed 11%. The cetane number is not less than 43. In order to achieve such a high fuel standard, various refineries are looking for a new ty...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/19B01J29/00C01B25/08C10G45/04C10G45/08
CPCB01J27/19B01J29/00C01B25/08C10G45/04C10G45/08C10G2300/202C10G2300/307
Inventor 唐天地赵文博傅雯倩张磊
Owner CHANGZHOU UNIV
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