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Preparation method and application of vanadyl phosphate catalyst

A technology of vanadyl phosphate catalyst and vanadium source, applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc., can solve problems such as electronic defects and unstable performance, and achieve low cost, simple operation, and simplified preparation The effect of the process

Active Publication Date: 2018-12-28
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

The method of the present invention uses the heteropolyacid ionic liquid to assist in the synthesis of the vanadyl phosphate catalyst, which can overcome the problems of unstable performance and obvious electronic defects of the traditional vanadyl phosphate catalyst

Method used

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  • Preparation method and application of vanadyl phosphate catalyst
  • Preparation method and application of vanadyl phosphate catalyst
  • Preparation method and application of vanadyl phosphate catalyst

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preparation example Construction

[0026] The invention provides a kind of preparation method of vanadyl phosphate catalyst, it comprises the following steps:

[0027] (1) Vanadium source, heteropolyacid ionic liquid, benzyl alcohol and C 3 ~C 8 The monohydric alcohol is mixed, obtains the mixture, reacts, wherein, the anion general formula of described heteropolyacid ionic liquid is [XM 12 o 40 ] n- or [Y 2 N 18 o 62 ] n- , X is the element Si or P, M is at least one of the elements W, Mo, V and Nb, Y is the element P, and N is at least one of the elements W, Mo and V, and the heteropolyacid ionic liquid The cation is at least one of quaternary ammonium cations and derivatives thereof, alkyl substituent imidazolium cations and pyrrole cations and derivatives thereof;

[0028] (2) Mix the reaction product obtained in step (1) with the phosphorus source, raise the temperature to 100°C to 200°C, and continue the reaction to obtain the vanadyl phosphate precursor;

[0029] (3) Roasting to obtain the vanad...

Embodiment 1

[0053] Preparation of vanadyl phosphate catalyst:

[0054] Weigh 4.54g V 2 o 5 (0.25mol) was placed in a 250mL three-necked flask, and 0.55g [TBA] was added 3 PMo 12 o 40 , 40mL of isobutanol and 10mL of benzyl alcohol, mechanically stirred and mixed evenly, refluxed at 135°C for 3h and then cooled to 70°C. Slowly add 3.61 mL of 85% H 3 PO 4 , and continued to reflux for 16 hours at a temperature of 135° C. The precipitate was filtered, washed with absolute ethanol, and dried in air at 80° C. for 24 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. Afterwards, the catalyst particles were activated in situ in an atmosphere of n-butane / oxygen / nitrogen reaction gas with a volume ratio of 1.5:17:81.5 from room temperature to 430°C at a rate of 2°C / min for 12 hours to obtain a vanadyl phosphate catalyst.

[0055] Detection:

[0056...

Embodiment 2

[0059] Weigh 4.54g V 2 o 5 (0.25mol) was placed in a 250mL three-necked flask, and 0.51g [TBA] was added 4 PMo 11 VO 40 , 40mL of isobutanol and 10mL of benzyl alcohol, mechanically stirred and mixed evenly, refluxed at 135°C for 3h and then cooled to 70°C. Slowly add 3.61 mL of 85% H 3 PO 4 , and continued to reflux for 16 hours at a temperature of 135° C. The precipitate was filtered, washed with absolute ethanol, and dried in air at 80° C. for 24 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. Afterwards, the catalyst particles were activated in situ in an atmosphere of n-butane / oxygen / nitrogen reaction gas with a volume ratio of 1.5:17:81.5 from room temperature to 430°C at a rate of 2°C / min for 12 hours to obtain a vanadyl phosphate catalyst.

[0060] Detection:

[0061] Weigh 2.0g of the vanadyl phosphate catalyst and p...

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Abstract

The invention relates to a preparation method and an application of a vanadyl phosphate catalyst. The method comprises the following steps: 1) mixing a vanadium source, heteropoly acid ionic liquid, benzyl alcohol and C3-C8 monohydric alcohol to obtain a mixture, and performing reaction; 2) mixing a reaction product obtained in the step 1) with a phosphorus source, performing heating to 100-200 DEG C, and continuing reaction to obtain a vanadyl phosphate precursor; 3) performing roasting to obtain the vanadyl phosphate catalyst. According to the method, the heteropolyacid ionic liquid is usedfor strengthening preparation of the vanadyl phosphate catalyst and has a 'multi-site coordination' effect on vanadyl phosphate, catalytic activity is improved, the problems of low yield, poor selectivity and the like are solved, and the defects of high cost and severe pollution of the traditional catalyst improvement method are overcome.

Description

technical field [0001] The invention belongs to the field of chemical catalysis, and relates to a preparation method and application of a vanadyl phosphate catalyst, in particular to a vanadyl phosphate catalyst, a method for strengthening the preparation by using a heteropolyacid ionic liquid, and an application thereof. Background technique [0002] Vanadyl phosphate (VPO) is an important composite oxide, which exhibits excellent catalytic performance in reactions such as selective oxidation of low paraffins and ammonia oxidation. Catalyst for maleic anhydride. [0003] So far, most scholars generally agree that the active phase of the vanadium phosphorus oxygen catalyst is formed by its precursor VOHPO which belongs to the tetragonal crystal system. 4 0.5H 2 O undergoes activated topological transformation into (VO) with an orthorhombic crystal structure 2 P 2 o 7 , in the preparation process of the precursor and the topological transformation process of the crystal ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/188B01J27/199B01J35/10C07D307/60
CPCC07D307/60B01J27/188B01J27/199B01J35/60
Inventor 刘瑞霞张锁江黎康南琳琳李自航代飞
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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