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Preparation method for vanadium phosphorus oxide catalyst used in selective oxidation of hydrocarbon

A technology of vanadium phosphorus oxide and catalyst, applied in physical/chemical process catalysts, chemical instruments and methods, organic chemistry, etc., can solve the problems of poor strength and poor heat dissipation of VPO catalysts

Active Publication Date: 2016-03-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is that the existing VPO catalyst itself has poor strength and poor heat dissipation. The present invention provides a new preparation method of vanadium phosphorus oxide catalyst. Surface-treated tungsten carbide with a thermal coefficient that improves catalyst thermal characteristics and enhances catalytic performance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 5g of tungsten carbide fine powder into 50ml of 2M phosphoric acid solution, stir and heat to 80°C and maintain for 3h. The resulting precipitate was filtered and washed with water, and then dried at 120° C. for 10 h to obtain phosphoric acid-treated tungsten carbide. Add 25g of vanadium pentoxide and phosphoric acid-treated tungsten carbide powder into a mixed solution of 250ml of isobutanol and 100ml of benzyl alcohol, start stirring and slowly add about 30.8g of 105wt.% phosphoric acid, heat the mixed solution to reflux and then reflux for 16h, stop After heating, the mixed solution was filtered and washed with isobutanol, and the resulting filter cake was dried at 120° C. for 20 h to obtain a precursor. The precursor was calcined at 250°C for 3 hours in an air atmosphere, then heated to 425°C for 3 hours in an atmosphere with a volume ratio of 20% air / 20% nitrogen / 10% carbon dioxide / 50% water vapor, and finally baked at 40% nitrogen / 10% The active catalyst was ...

Embodiment 2

[0036] Add 5g of tungsten carbide fine powder into 50ml of 2M phosphoric acid solution, stir and heat to 80°C and maintain for 3h. The resulting precipitate was filtered and washed with water, and then dried at 120° C. for 10 h to obtain phosphoric acid-treated tungsten carbide. Add 25g of vanadium pentoxide and phosphoric acid-treated tungsten carbide powder into a mixed solution of 300ml of isobutanol and 60ml of benzyl alcohol, start stirring and slowly add about 30.8g of 105wt.% phosphoric acid, heat the mixed solution to reflux and then reflux for 16h, stop After heating, the mixed solution was filtered and washed with isobutanol, and the resulting filter cake was dried at 120° C. for 20 h to obtain a precursor. The precursor was calcined at 250°C for 3 hours in an air atmosphere, then heated to 425°C for 3 hours in an atmosphere with a volume ratio of 20% air / 20% nitrogen / 10% carbon dioxide / 50% water vapor, and finally baked at 40% nitrogen / 10% The active catalyst was obt...

Embodiment 3

[0038] Add 3g of tungsten carbide fine powder into 50ml of 2M phosphoric acid solution, stir and heat to 80°C and maintain for 3h. The resulting precipitate was filtered and washed with water, and then dried at 120° C. for 10 h to obtain phosphoric acid-treated tungsten carbide. Add 25g of vanadium pentoxide and phosphoric acid-treated tungsten carbide powder into a mixed solution of 300ml of isobutanol and 60ml of benzyl alcohol, start stirring and slowly add about 30.8g of 105wt.% phosphoric acid, heat the mixed solution to reflux and then reflux for 16h, stop After heating, the mixed solution was filtered and washed with isobutanol, and the resulting filter cake was dried at 120° C. for 20 h to obtain a precursor. The precursor was calcined at 250°C for 3 hours in an air atmosphere, then heated to 425°C for 3 hours in an atmosphere with a volume ratio of 20% air / 20% nitrogen / 10% carbon dioxide / 50% water vapor, and finally baked at 40% nitrogen / 10% The active catalyst was o...

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Abstract

The present invention relates to a vanadium phosphorus oxide catalyst, and mainly solves the problem that the catalytic performance of a catalyst in the prior art in preparing maleic anhydride by selective oxidation of a hydrocarbon is poor. For well solving the aforementioned technical problem, according to the technical scheme of the present invention, a preparation method of the vanadium phosphorus oxide catalyst comprises the following steps of: 1) mixing tungsten carbide powder with a phosphoric acid solution, raising the temperature of the mixture to 50-100 DEG C and enabling the mixture to react for 1-10 hours, and carrying out filtering and drying to obtain tungsten-carbide subjected to phosphate processing; 2) after mixing a vanadium compound, and the tungsten-carbide subjected to phosphate processing with an organic solvent, carrying out stirring and slowly adding 85wt%-110wt% of phosphoric acid, and performing heating reflux for 8-32 hours; 3) filtering and washing the obtained catalyst precursor solution after cooling, and carrying out drying at 100-150 DEG C to obtain a catalyst precursor; and 4) obtaining an active catalyst by performing calcination activation on the catalyst precursor. The prepared catalyst can be used in the industrial production of maleic anhydride.

Description

technical field [0001] The invention relates to an improved preparation method of a vanadium phosphorus oxide catalyst. The catalyst prepared by the method is especially suitable for the selective oxidation of gas-phase hydrocarbons to prepare maleic anhydride. technical background [0002] Maleic anhydride, referred to as maleic anhydride, also known as maleic anhydride (Maleicanhydride, MA), is a commonly used important organic chemical raw material and the third largest consumption of anhydride in the world. Maleic anhydride is currently mainly used in the production of unsaturated polyester resins, alkyd resins, 1,4-butanediol (BDO), γ-butyrolactone (GBL), tetrahydrofuran (THF) and other chemicals. In addition, it is also widely used in various fine chemicals. [0003] The production of maleic anhydride is mainly divided into two categories. The earliest production method uses benzene as the raw material for production. Decreasing; the current mainstream production met...

Claims

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Application Information

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IPC IPC(8): B01J27/22C07D307/60
Inventor 曾炜顾龙勤杨为民徐俊峰陈亮赵欣
Owner CHINA PETROLEUM & CHEM CORP
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