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A method and application of ionic liquid-assisted preparation of vanadium phosphorus oxygen catalyst

An ionic liquid, vanadium phosphorus oxide technology, applied in chemical instruments and methods, catalyst activation/preparation, physical/chemical process catalysts, etc., to achieve the effects of increasing active sites, increasing specific surface area, and simple preparation methods

Active Publication Date: 2021-04-27
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are few reports on the application of vanadium phosphorus oxygen catalysts prepared by ionic liquids in the oxidation of n-butane to maleic anhydride.

Method used

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  • A method and application of ionic liquid-assisted preparation of vanadium phosphorus oxygen catalyst
  • A method and application of ionic liquid-assisted preparation of vanadium phosphorus oxygen catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Weigh V 2 o 5 Put 20g in a 500ml container, add a mixture of isobutanol and benzyl alcohol (160ml / 40ml), then add 2ml of 1-butyl-3-methylimidazolium hexafluorophosphate ionic liquid, stir and mix evenly, at 135°C After reflux for 3 hours under the same conditions, the temperature was lowered to 60 °C, and then slowly added dropwise H2O with a mass fraction of 85%. 3 PO 4 15.5ml, and the temperature was raised to 135°C and the reflux was continued for 16 hours. Filter and wash to obtain a blue precipitate, and dry it in air at 120° C. for 12 hours to obtain a catalyst precursor powder. The obtained catalyst precursor powder was pressed into tablets under a pressure of 15 MPa, crushed, and 20-40 mesh catalyst particles were sieved. The catalyst particles were then placed in a reaction atmosphere (C4H 10 / O 2 / N 2 =1.4 / 19.5 / 79.1) from room temperature to 400°C at a rate of 2°C / min for in-situ activation for 12 hours to obtain an activated vanadium-phosphorus-oxyge...

Embodiment 2

[0034] Weigh V 2 o 5 20g is placed in a 500ml container, add the mixed solution of isobutanol and benzyl alcohol (160ml / 40ml), then add 1.5ml 1-butyl-3-methylimidazolium tetrachloride ionic liquid, mechanically stir and mix evenly, 135 After reflux for 3 hours under the condition of ℃, cool down to 60 ℃, then slowly dropwise add H 3 PO 4 15.5ml, and the temperature was raised to 135°C and the reflux was continued for 16 hours. The gray-green precipitate was obtained by filtering and washing, and dried in air at 120° C. for 12 hours to obtain catalyst precursor powder. The obtained catalyst precursor powder was pressed into tablets under a pressure of 15 MPa, crushed, and 20-40 mesh catalyst particles were sieved. Afterwards, the catalyst particles were placed in the reaction atmosphere (C 4 h 10 / O 2 / N 2 =1.4 / 19.5 / 79.1) from room temperature to 400°C at a rate of 2°C / min for in-situ activation for 12 hours to obtain an activated vanadium-phosphorus-oxygen catalyst. ...

Embodiment 3

[0037] Weigh V 2 o 5 Put 20g in a 500ml high-pressure glass reactor, add a mixture of isobutanol and benzyl alcohol (160ml / 40ml), then add 1ml of 1-sulfobutyl-3-methylimidazolium bisulfate ionic liquid, stir and mix evenly , reflux at 135°C for 3 hours and then cool down to 60°C, then slowly dropwise add 85% H 3 PO 4 16.7ml, and the temperature was raised to 135°C for reflux for 16 hours. Filter and wash to obtain a light green precipitate, and dry it in air at 120° C. for 12 hours to obtain a catalyst precursor powder. The obtained catalyst precursor powder was pressed into tablets under a pressure of 15 MPa, crushed, and 20-40 mesh catalyst particles were sieved. The catalyst particles were then placed in a reaction atmosphere (C4H 10 / O 2 / N 2 =1.4 / 19.5 / 79.1) from room temperature to 400°C at a rate of 2°C / min for in-situ activation for 12 hours to obtain an activated vanadium-phosphorus-oxygen catalyst. The catalyst is mainly composed of vanadyl pyrophosphate phas...

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Abstract

The invention relates to a method for preparing a vanadium-phosphorus-oxygen catalyst assisted by an ionic liquid, which comprises the following steps: placing vanadium pentoxide in a container, adding a mixed solution of isobutanol and benzyl alcohol with a volume ratio of 1 to 8:1, and then Add ionic liquid, heat up to 100-180°C and react for 1-8 hours, then cool to 30-60°C, add phosphoric acid to the container, heat up to 100-200°C and continue to react for 10-24 hours, the product is filtered, washed, Dry to obtain a vanadium-phosphorus-oxygen precursor, roast the vanadium-phosphorus-oxygen precursor at a temperature of 350-550°C for 2-15 hours, and cool to obtain a vanadium-phosphorus-oxygen catalyst; wherein, the structure of the ionic liquid cation and anion is: The structure of the cation is or R 1 , R 2 , R 3 , R 4 for the same or different C n h 2n+1 , 1≤n≤20; the anion is selected from BF 4 ‑ 、PF 6 ‑ 、HCOO ‑ 、CH 3 COO ‑ 、C 2 h 5 COO ‑ 、C 6 h 5 COO ‑ 、HOCH 2 COO ‑ 、HSO 4 ‑ 、CH 3 SO 3 ‑ 、H 2 PO 4 ‑ , FeCl 4 ‑ 、CoCl 4 ‑ , AlCl 3 ‑ , (CH 3 O) 2 PO 2 at least one of the And, the application of the obtained vanadium phosphorus oxygen catalyst in the selective oxidation of n-butane to maleic anhydride is provided.

Description

technical field [0001] The invention belongs to the field of catalytic synthesis, and in particular relates to a method and application of an ionic liquid-assisted preparation of a vanadium-phosphorus-oxygen catalyst. Background technique [0002] Maleic anhydride, referred to as maleic anhydride or maleic anhydride, is an important organic chemical raw material and fine chemical product, and is the third largest anhydride in the world after phthalic anhydride and acetic anhydride. Maleic anhydride is mainly used in the production of fine chemical products such as unsaturated polyester resin and alkyd resin, γ-butyrolactone, 1,4-butanediol, tetrahydrofuran, maleic acid, etc. market demand. At present, the n-butane oxidation method is the main technical route for the production of maleic anhydride. Compared with the benzene oxidation method, the n-butane oxidation method has the advantages of wide source of raw materials, less environmental pollution, lower cost and higher a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/198C07D307/60
CPCC07D307/60B01J27/198B01J37/0018B01J35/50B01J35/613
Inventor 刘瑞霞代飞李自航张瑞锐张锁江
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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