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Catalyst and preparation method thereof

A technology of catalysts and main catalysts, applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc., can solve the problems that catalysts cannot be used in large-scale industrial production, so as to improve selectivity, yield, and particle size distribution Uniform, chemically active effect

Inactive Publication Date: 2012-01-18
CHANGSHU INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalyst prepared by the preparation method provided by this invention has the advantages of good selectivity and high yield, but due to TiCl 4 It is easy to react violently with water vapor in the air to produce acid mist, and its pretreatment needs to be considered. The prepared catalyst cannot be used in industrial large-scale production at present

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1: Add ammonium metavanadate to the oxalic acid solution, reduce it to vanadium at 80-90°C, add hydrochloric acid dropwise to adjust the pH to 2-3, add an alcohol solution of butyl titanate dissolved in absolute ethanol, making V 2 o 5 and TiO 2 The weight ratio is 0.18:0.80, control the reaction temperature to make V-Ti sol; take the weight basis of the main catalyst as 1, add P 2 o 5 0.017, Sb 2 o 3 0.036, MoO 3 0.002 into a sol spraying liquid, and then spray the spraying liquid on the ￠5-6mm SiC carrier heated to 230-250°C in advance, then put it in a muffle furnace at 250°C for 30 minutes, and then continue to heat up to 480°C Roast for 2 hours. Let cool, remove and set aside.

[0025] Put 50mL of catalyst into a ￠40mm reaction tube, and control the reaction temperature to 430-450°C. Pass through durene, use air for catalytic oxidation, and the space velocity is 4000-4500h -1 , The product yield is measured every 2 hours, and the highest weight...

Embodiment 2

[0026] Example 2: adding ammonium metavanadate to the oxalic acid solution, reducing it to vanadium at 80-90°C, adding hydrochloric acid dropwise to adjust the pH to 2-3, adding an alcohol solution of butyl titanate dissolved in absolute ethanol, making V2 o 5 and TiO 2 The weight ratio of the main catalyst is 0.20:0.82, and the reaction temperature is controlled to make V-Ti sol; the weight basis of the main catalyst is 1, and the P 2 o 5 0.019, Sb 2 o 3 0.038, MoO 3 0.004 to make a spraying liquid, and then spray the spraying liquid on the ￠5-6mm SiC carrier pre-heated to 230-250°C, then put it in a muffle furnace at 250°C for 30 minutes, and then continue to heat up to 480°C for roasting 2 hours. Let cool, remove and set aside. The highest weight yield of the product obtained by the reaction is 99-103%, and the content of pyromellitic dianhydride is about 96%.

Embodiment 3

[0027] Example 3: Ammonium metavanadate is added to the oxalic acid solution, reduced to vanadium at 80-90°C, hydrochloric acid is added dropwise to adjust the pH to 2-3, and an alcohol solution of butyl titanate dissolved in absolute ethanol is added, making V 2 o 5 and TiO 2 The weight ratio of the main catalyst is 0.19:0.81, and the reaction temperature is controlled to make V-Ti sol; the weight basis of the main catalyst is 1, and the P 2 o 5 0.019, Sb 2 o 3 0.038, MoO 3 0.004 to make a spraying liquid, and then spray the spraying liquid on the ￠5-6mm SiC carrier pre-heated to 230-250°C, then put it in a muffle furnace at 250°C for 30 minutes, and then continue to heat up to 480°C for roasting 2 hours. Let cool, remove and set aside. The highest weight yield of the product obtained by the reaction is 98-102%, and the content of pyromellitic dianhydride is about 96%.

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PUM

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Abstract

The invention discloses a catalyst for catalyzing in preparation of pyromellitic acid dianhydride from durene. In the catalyst, V2O5-TiO2-P2O5-Sb2O3-MoO3 is taken as a composition system; a major catalyst consists of V2O5 and TiO2 in the ratio of (0.18-0.20):(0.82-0.80); a catalyst accelerator consists of P2O5, Sb2O3 and MoO3; and when the weight of the major catalyst is set as 1, P2O5 accounts for 0.017-0.019, Sb2O3 accounts for 0.036-0.038, and MoO3 accounts for 0.002-0.004. The invention further discloses a preparation method of the catalyst. The catalyst has the characteristics of high selectivity and high yield, and is suitable to be applied to gas-phase oxidation of durene.

Description

technical field [0001] The invention relates to the technical field of a catalyst for preparing pyromellitic dianhydride by gas-phase oxidation of durene and a preparation method thereof. Background technique [0002] At present, the process of producing pyromellitic dianhydride in one step through air gas phase oxidation using durene as raw material is widely used. Most of the catalysts used in industry are anatase TiO 2 The powder is used as the carrier, with vanadium as the main component (V 2 o 5 -P 2 o 5 -MoO 3 ) of the three-component composite catalyst, the reaction temperature is 380-390 ° C. This method has simple process, saves the process of dehydration into pyromellitic dianhydride, can be produced continuously, and is easy to realize automation. It is currently the main method for producing pyromellitic dianhydride. However, due to the small number of catalyst components and the large particles on the surface of the catalyst produced at the same time, the ...

Claims

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Application Information

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IPC IPC(8): B01J27/228B01J35/02C07D493/04
Inventor 王旭红汤忠俊柴文
Owner CHANGSHU INSTITUTE OF TECHNOLOGY
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