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Method for preparing vanadium phosphorus oxide catalyst

A catalyst, vanadium phosphorus oxygen technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc., can solve the problems of introducing impurities, environmental pollution, etc., and achieve the goal of reducing dosage, reducing environmental pollution, and shortening the diffusion path Effect

Active Publication Date: 2018-11-02
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Aiming at the deficiency of using too much organic solvent in the preparation of vanadium phosphorus oxygen catalyst in the prior art, not only introducing impurities, but also causing environmental pollution, the present invention provides a vanadium phosphorus oxygen catalyst and its preparation method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0045] (1) Preparation of ionic liquid

[0046] Will M 1 and M 2 Add to water, M 1 with M 2 The molar ratio is 1:1~1:2, heated to the reaction temperature under stirring conditions, the reaction temperature is 60~150°C, and the constant temperature reaction is 1~4h. After the reaction is completed, cool to room temperature, centrifuge, and filter to obtain the ionic liquid I .

[0047] Will M 3 and M 4 Mixed, M 3 with M 4 The molar ratio is 1:1~1:2, and the constant temperature reaction is 20~30h at the reaction temperature of 70~100°C to obtain a colorless viscous liquid, which is cooled to room temperature, washed 2~6 times with ether, and heated at 60~100°C Drying at low temperature for 24~50h, the intermediate product was obtained, which was added to acetone, and then M 1 , stirring at room temperature, suction filtration, washing, washing liquid and filtrate combined, with anhydrous MgSO 4 After drying, acetone and water were evaporated by rotary evaporation to ...

Embodiment 1

[0060] Dimethylammonium chloride 300g, ammonium tetrafluoroborate 190g, pure water 450g, mixed, heated to 80°C under stirring, kept at constant temperature for 1 hour, clarified, naturally cooled to about 30°C, centrifuged to filter out the solid to obtain 300g of ionic liquid I , the water content is about 3.5wt%, and the yield is 73wt%.

[0061]Take 1.92 mol of chloroethanol and 1.28 mol of methylimidazole and reflux at 80°C for 24 hours under the condition of microwave heating. After the reaction, a viscous colorless transparent liquid is obtained. Cool to room temperature and wash four times with ether to obtain colorless crystal 1-hydroxyethyl Base-3-methylimidazolium chloride ionic liquid, dried in a vacuum oven at 80°C for 48h. Take 100g (0.6mol) of dried 1-hydroxyethyl-3-methylimidazolium chloride ionic liquid and add it to 600ml acetone, then add 72g (0.68mol) sodium tetrafluoroborate, stir at room temperature for 24h, filter with suction, the filter residue is wax L...

Embodiment 2

[0066] Diethylammonium chloride 250g, ammonium tetrafluoroborate 180g, pure water 400g, mixed, heated to 90°C under stirring, kept at constant temperature for 1.5h, clarified, naturally cooled to about 30°C, centrifuged to filter out the solid to obtain ionic liquid I 260g, water content about 3.5wt%, yield 73wt%.

[0067] The preparation steps of 1-(4′-hydroxy)butyl-3-methylimidazolium fluoroborate ionic liquid are the same as in Example 1.

[0068] In the submerged circulating impingement flow reactor, 250g of ionic liquid I, 30.0g of vanadium pentoxide, 0.3g of ferric nitrate hexahydrate, and 0.5g of auxiliary agent zirconium nitrate were mixed, and put into the reactor from the feeding port, and started. Adjust the rotation speed of the propeller to 900r / min, raise the temperature to 95°C to allow the material to undergo an impact reaction for 2 hours; then feed 35.5g of concentrated phosphoric acid with a concentration of 100% into the reactor, the phosphorus / vanadium mol...

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Abstract

The invention discloses a method for preparing a vanadium phosphorus oxide catalyst. The method comprises the following steps: (1) mixing ionic liquid I and vanadium pentoxide, adding the mixture intoan impinging stream reactor, a boiling-bed reactor or a high gravity reactor, raising the temperature and reacting; (2) introducing concentrated phosphoric acid into the reactor, reacting for 2-4 hours, introducing ionic liquid II for continuously reacting for 2-4 hours, filtering, drying and calcining to obtain a vanadium phosphorus oxide catalyst precursor, and activating and molding, thereby obtaining the catalyst. The vanadium phosphorus oxide catalyst prepared by the method disclosed by the invention has dual pore channel distribution, the ionic liquid serves as the solvent and reducingagent, and the usage amount of the solvent and reducing agent is effectively reduced; with the adoption of the impinging stream reactor, the reaction time is short, the mass transfer effect is excellent, the reaction efficiency is high, and the production cost is saved.

Description

technical field [0001] The invention relates to a preparation method of a vanadium-phosphorus-oxygen catalyst, and the vanadium-phosphorus-oxygen catalyst is suitable as a catalyst for the reaction of n-butane oxidation to maleic anhydride. Background technique [0002] Maleic anhydride, also known as maleic anhydride for short, is an important organic chemical raw material and fine chemical product. It is currently the third largest anhydride in the world after phthalic anhydride and acetic anhydride. Its development and utilization prospects are very broad. . [0003] There are three basic routes for the production of maleic anhydride: benzene oxidation, butane oxidation, butene (C 4 fraction) oxidation method. The technology of using n-butane as raw material to produce maleic anhydride has become the main route of maleic anhydride production due to its advantages of cheap raw material, less environmental pollution and low production cost of maleic anhydride. The select...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/198B01J35/10C07D307/60
CPCC07D307/60B01J27/198B01J35/613B01J35/69B01J35/633B01J35/647
Inventor 薛冬吕振辉白富栋李政张通
Owner CHINA PETROLEUM & CHEM CORP
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