A preparing method of a vanadium phosphorus oxide catalyst for n-butane oxidation to produce maleic anhydride

An anhydride vanadium phosphorus oxygen catalyst, catalyst technology, applied in physical/chemical process catalysts, chemical instruments and methods, organic chemistry, etc., to achieve the best catalytic performance, high maleic anhydride selectivity, and large specific surface area

Active Publication Date: 2016-07-13
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] In the prior art, liquid-phase oxidation is used to precisely adjust the valence state of vanadium in the vanadium-phosphorus-oxygen catalyst, that is, to precisely change the V in the catalyst. 4+ / V 5+ Relative content, to carry out the preparation of the catalyst, and to achieve the technology of controllable catalytic performance has not been reported so far

Method used

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  • A preparing method of a vanadium phosphorus oxide catalyst for n-butane oxidation to produce maleic anhydride
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  • A preparing method of a vanadium phosphorus oxide catalyst for n-butane oxidation to produce maleic anhydride

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preparation example Construction

[0049] (2) Preparation of vanadium phosphorus oxygen catalyst

[0050] The vanadium phosphorus oxide obtained in step (1) is first shaped, and the shape of the obtained vanadium phosphorus oxygen catalyst can be a tablet, a spherical shape, an extruded rod, etc., and the phase of the catalyst precursor is (VOHPO 4 0.5H 2 o).

[0051] (3) Activation of vanadium phosphorus oxygen catalyst

[0052] Take 86g of the Raschig ring-shaped catalyst particles obtained in step (2), impregnate them into 180g of 2.5% tert-butyl hydroperoxide tert-butanol solution, keep the impregnation time for 1-2 hours, filter the catalyst after the impregnation, and put the wet catalyst Dry in a closed drying oven at 100~150°C, recover the evaporated tert-butanol solvent, put the dried catalyst into a tubular reactor, and in an inert gas or nitrogen atmosphere, at a gas volume space velocity of 100~1500h -1 , the heating rate is 1-5°C / min, the activation temperature is raised to 425°C for roasting tr...

Embodiment 1

[0057] exist figure 1 In the shown reaction kettle with stirring device and reflux condensing device, add 649mL of isobutanol and benzyl alcohol mixture, the volume ratio of isobutanol / benzyl alcohol is 10:1, 29.53g of vanadium pentoxide, additive hexahydrate Ferric nitrate 0.3g, additive zirconium nitrate 0.5g, start stirring, increase the reaction temperature and keep it at 100±2°C, carry out reflux reaction, keep reflux time for 4 hours, then add 34.98g of phosphoric acid with a concentration of 100%, phosphorus / vanadium The molar ratio was 1.1, the reflux was continued for 4 hours, and the reaction ended. After the reaction solution was cooled to room temperature, it was vacuum filtered, and the filter cake was rinsed with a small amount of isobutanol three times, then the filter cake was placed in an enamel tray and dried naturally at room temperature, dried in an oven at 100°C for 8 hours, and finally dried in a muffle furnace. Calcined at 250°C for 5 hours to obtain a ...

Embodiment 2

[0063] exist figure 1 In the shown reaction kettle with stirring device and reflux condensing device, add 649mL of isobutanol and benzyl alcohol mixture, the volume ratio of isobutanol / benzyl alcohol is 10:1, 29.53g of vanadium pentoxide, additive hexahydrate Ferric nitrate 0.3g, additive zirconium nitrate 0.5g, start stirring, increase the reaction temperature and keep it at 100±2°C, carry out reflux reaction, keep reflux time for 4 hours, then add 34.98g of phosphoric acid with a concentration of 100%, phosphorus / vanadium The molar ratio was 1.1, the reflux was continued for 4 hours, and the reaction ended. After the reaction solution was cooled to room temperature, it was vacuum filtered, and the filter cake was rinsed with a small amount of isobutanol three times, then the filter cake was placed in an enamel tray and dried naturally at room temperature, dried in an oven at 100°C for 8 hours, and finally dried in a muffle furnace. Calcined at 250°C for 5 hours to obtain a ...

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Abstract

A preparing method of a vanadium phosphorus oxide catalyst is disclosed. The method includes preparing a catalyst precursor in a stirring reaction kettle, dipping the catalyst precursor in an organic peroxide to perform liquid phase oxidation treatment, and calcinating in an inert gas atmosphere so that the crystalline phase in the catalyst precursor is subjected to phase inversion and structured, namely the VOHPO4.<0.5>H2O phase in the precursor is converted into an active (VO)<2>P2O7 phase, and the V<5+> phase is converted into beta-VOPO4 phase. The method can quantificationally control the relative content V<4+>/V<5+> in the catalyst and can adjust synergistic effects between the V<4+> phase and the V<5+> phase so that performance of the catalyst is optimum. The catalyst prepared through the method is large in specific surface area and high in pore volume. When the catalyst is used for a catalytic reaction of oxidizing n-butane to produce maleic anhydride, the conversion ratio of the n-butane is 85-95 mol%, and selectivity of the maleic anhydride can be 72-86 mol%.

Description

technical field [0001] The invention relates to a preparation method of a vanadium-phosphorus-oxygen catalyst, which is suitable for the catalytic reaction process of n-butane oxidation to maleic anhydride. Background technique [0002] Maleic anhydride, also known as maleic anhydride, is an important organic chemical raw material and the third largest organic anhydride in the world after phthalic anhydride and acetic anhydride. It is widely used in petrochemical, food processing, and pharmaceutical industries. , Building materials and other industries. Its specific applications include the manufacture of unsaturated polyester resins, alkyd resins, maleic acid (maleic acid), fumaric acid (fumaric acid), and pesticides, coatings, glass fiber reinforced plastics, lubricating oil additives, paper chemistry Product additives, surfactants, etc. The advent of the new method of maleic anhydride esterification and low-pressure hydrogenation to produce 1,4-butanediol makes it an im...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/198C07D307/60
Inventor 王海波宋丽芝勾连科
Owner CHINA PETROLEUM & CHEM CORP
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