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Preparation method and application of oxyvanadium phosphate catalyst

A vanadyl phosphate catalyst, n-butane technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc., can solve the problems of unstable VPO catalyst batch performance and unclear key factors, and achieve excellent Selectivity and conversion, simplified process, stable performance

Inactive Publication Date: 2020-07-17
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For VPO catalysts, the main focus is on the organic phase method to improve its catalytic performance by adding metal additives, organic additives, and new additives. However, the batch performance of VPO catalysts is not stable, and the key factors in the VPO synthesis process are not unclear

Method used

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

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preparation example Construction

[0021] The embodiment of the present invention provides a kind of preparation method of vanadyl phosphate catalyst, it comprises the following steps:

[0022] S01: set V 2 o 5 Add to the mixture of isobutanol and benzyl alcohol, stir and mix, reflux at 130°C-140°C for 2-5 hours, then cool down to 100°C-120°C.

[0023] S02: Maintain 100°C to 120°C, add H with a mass concentration of 85% to 90% at a rate of 0.6 to 1.6mL / min 3 PO 4 Afterwards, the temperature was raised to 130-140°C and continued to reflux for 10-14 hours, and the product was filtered and washed to obtain the vanadyl phosphate precursor;

[0024] S03: roasting the vanadyl phosphate precursor to obtain the vanadyl phosphate catalyst.

[0025] Preferably, the volume ratio of isobutanol to benzyl alcohol is (3-5):1, such as 3:1, 3.2:1, 3.5:1, 4:1, 4.5:1, 4.7:1, 4.9:1 , or 5:1, etc.

[0026] Preferably, the V 2 o 5 The concentration is 0.02g / mL~0.12g / mL, such as 0.02g / mL, 0.04g / mL, 0.06g / mL, 0.07g / mL, 0.08g / m...

Embodiment 1

[0044] Preparation of vanadyl phosphate catalyst:

[0045] (1) Weigh 10g V 2 o 5 Place in a 250mL three-neck flask, add a mixture of 80mL isobutanol and 20mL benzyl alcohol, stir and mix evenly, reflux at 135°C for 3h and then cool down to 110°C.

[0046] (2) Keeping at 110°C, add 7.53mL of 85% H2 dropwise within 7min 3 PO 4 , and continued to reflux for 12 hours at a temperature of 135° C. The product was filtered, washed with absolute ethanol to obtain a blue precipitate, and dried in air at 120° C. for 24 hours to obtain a vanadyl phosphate precursor.

[0047] (3) The obtained vanadyl phosphate precursor powder is compressed under a pressure of 15MPa, crushed, and 20-40 mesh catalyst particles are sieved, and then the catalyst particles are mixed in n-butane / oxygen at a volume ratio of 1.5:17:81.5 / Nitrogen reaction gas atmosphere from room temperature to 430° C. for 12 hours at a rate of 2° C. / min to obtain the vanadyl phosphate catalyst.

[0048] Detection:

[0049...

Embodiment 2

[0052] Preparation of vanadyl phosphate catalyst:

[0053] (1) Weigh 10g V 2 o 5 Place in a 250mL three-neck flask, add a mixture of 80mL isobutanol and 20mL benzyl alcohol, stir and mix evenly, reflux at 135°C for 3h and then cool down to 110°C.

[0054] (2) Keeping at 110°C, add 7.21mL of 87% H2 dropwise within 6.7min 3 PO 4 , and continued to reflux for 12 hours at a temperature of 135° C. The product was filtered and washed with absolute ethanol to obtain a blue-black precipitate, which was dried in air at 120° C. for 24 hours to obtain a vanadyl phosphate precursor.

[0055] (3) Press the obtained vanadyl phosphate precursor powder into tablets under a pressure of 15MPa, crush it, and sieve the catalyst particles of 20-40 meshes, and then heat the catalyst particles from room temperature at a rate of 2°C / min under a reaction gas atmosphere Raise the temperature to 430°C for in-situ activation for 12 hours to obtain a vanadyl phosphate catalyst.

[0056] Detection: ...

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Abstract

The invention relates to a preparation method of an oxyvanadium phosphate catalyst, which comprises the following steps: adding V2O5 into a mixed solution of isobutanol and benzyl alcohol, stirring and mixing, refluxing at 130-140 DEG C for 2-5 hours, cooling to 100-120 DEG C, keeping the temperature at 100-120 DEG C, adding H3PO4 with the mass concentration of 85-90% at the speed of 0.6-1.5 mL / min, heating to 130-140 DEG C, continuously refluxing for 10-14 hours, and filtering and washing the product to obtain an oxyvanadium phosphate precursor, and roasting the oxyvanadium phosphate precursor to obtain the oxyvanadium phosphate catalyst. According to the method, by controlling the adding process of the phosphorus source, the defect that the performance is improved by adding auxiliaries traditionally can be overcome, secondary pollution is avoided, the cost is reduced, and meanwhile the preparation process is simplified.

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. Background technique [0002] Vanadyl phosphate catalyst (also known as vanadium oxyphosphorus catalyst, referred to as VPO) is currently the most efficient and economical industrial catalyst for the selective oxidation of n-butane to maleic anhydride (MA). Topological transformation into the active phase vanadyl pyrophosphate. [0003] The organic phase method is the most widely used method for the synthesis of VPO catalysts for domestic and foreign industrial applications. For VPO catalysts, the main focus is on the organic phase method to improve its catalytic performance by adding metal additives, organic additives, and new additives. However, the batch performance of VPO catalysts is not stable, and the key factors in the VPO synthesis process are not unclear. Contents of the invention [0004] Aiming ...

Claims

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Application Information

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IPC IPC(8): B01J27/198B01J35/10B01J35/02C07D307/60
CPCB01J27/198C07D307/60B01J35/50B01J35/612
Inventor 张婷刘瑞霞张瑞锐李英葳李自航张永康张锁江
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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