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Oxyvanadium phosphate catalyst and preparation method and application thereof

A technology of vanadyl phosphate catalyst and vanadium source, applied in the direction of physical/chemical process catalysts, organic chemistry, chemical instruments and methods, etc., can solve problems affecting catalyst stability and selectivity, catalyst sintering, and uneven heating of catalysts, etc., to achieve Improve catalyst performance, reduce by-products, and promote uniform heating effects

Inactive Publication Date: 2019-05-10
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] According to the C proposed by Ballarini et al. 4 h 10 +3.5O 2 →C 4 h 2 o 3 +4H 2 O△H 0 298K =-1268kJ / mol, the n-butane oxidation reaction is a reaction of a strong exothermic process, so the catalyst is easy to affect the stability and selectivity of the catalyst due to uneven heating and local overheating during the reaction process, which is very industrially The catalyst is prone to local overheating and sintering

Method used

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  • Oxyvanadium phosphate catalyst and preparation method and application thereof
  • Oxyvanadium phosphate catalyst and preparation method and application thereof
  • Oxyvanadium phosphate catalyst and preparation method and application thereof

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preparation example Construction

[0017] The embodiment of the present invention provides a kind of preparation method of vanadyl phosphate catalyst, it comprises the following steps:

[0018] (1) Mix the vanadium source, benzyl alcohol, C3-C8 monohydric alcohol and heat-conducting material to obtain a mixture, and react;

[0019] (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;

[0020] (3) roasting to obtain the vanadyl phosphate catalyst;

[0021] Wherein, the thermally conductive material is at least one of SiC, graphite, graphene and carbon nanotubes.

[0022] Specifically, the volume ratio of the C3-C8 monohydric alcohol to benzyl alcohol is (3-5):1, such as 3:1, 4:1, 5:1, etc. Preferably, in the mixture, the concentration of vanadium source is 0.02g / mL~0.12g / mL, such as 0.02g / mL, 0.04g / mL, 0.06g / mL, 0.07g / mL, 0.08g / mL, 0.09g / mL, 0.1g / mL or 0.12g / mL etc. If the co...

Embodiment 1

[0043] Weigh V 2 o 5 Put 20g in a 500mL flask, add a mixture of 200mL isobutanol and 50mL benzyl alcohol, then add 4.4g SiC, stir and mix evenly, reflux at 136°C for 3 hours, then cool down to below 90°C, then add dropwise at a constant speed H with a mass fraction of 85% 3 PO 4 15.5 mL and stirred, then heated to 136°C and continued to reflux for 16 hours. Cool to room temperature, then filter, wash with ethanol, obtain a sky blue precipitate after suction filtration, and dry overnight in air at 120°C to obtain a catalyst precursor. Then, the obtained catalyst precursor powder was pressed into tablets under a pressure of 20 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 430°C at a rate of 2°C / min for in-situ activation for 12 hours to obtain an activated vanadium-phosphorus-oxygen catalyst. The main active phase of the...

Embodiment 2

[0046] Weigh V 2 o 5 Put 20g in a 500mL flask, add a mixture of 200mL of isobutanol and 50mL of benzyl alcohol, then add 2.2g of SiC, stir and mix evenly, reflux at 136°C for 3 hours, then cool down to below 90°C, then add dropwise at a constant speed H with a mass fraction of 85% 3 PO 4 15.5 mL and stirred, then heated to 136°C and continued to reflux for 16 hours. Cool to room temperature, filter again, wash with ethanol and suction filter to obtain a sky blue precipitate, and dry the product in air at 120°C overnight to obtain a catalyst precursor. Then, the obtained catalyst precursor powder was pressed into tablets under a pressure of 20 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 430°C at a rate of 2°C / min for in-situ activation for 12 hours to obtain an activated vanadium-phosphorus-oxygen catalyst. The main a...

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Abstract

The invention belongs to the technical field of catalysis and mainly relates to a preparation method of an oxyvanadium phosphate catalyst and application of the oxyvanadium phosphate catalyst in maleic anhydride preparation using selective n-butane oxidation. The preparation method includes the steps of firstly, mixing a vanadium source, benzyl alcohol, C1-C8 monohydric alcohol and a heat-conduction material to obtain a mixture, and performing reaction, wherein the heat-conduction material is at least one of SiC, graphite, graphene and carbon nanotubes; secondly, mixing the reaction product obtained in the first step with a phosphorus source, heating to 100-200 DEG C, and performing reaction to obtain a oxyvanadium phosphate precursor; thirdly, calcining to obtain the oxyvanadium phosphatecatalyst. The preparation method has the advantages that the heat-conduction material is added during the preparation and can effectively achieve heat conduction to solve the problem of local overheat; the uniform and stable formation of active phase is promoted effectively, the catalyst is promoted to be heated evenly during reaction, and catalyst performance is increased.

Description

technical field [0001] The invention relates to the field of chemical catalysis, and mainly relates to a preparation method and application of a vanadium phosphorus oxygen catalyst. Background technique [0002] Maleic anhydride, also known as maleic anhydride, or maleic anhydride for short, is an economically very important intermediate product of organic chemicals and fine chemicals, and it is also the third largest acid anhydride in acid anhydride products after phthalic anhydride and acetic anhydride. It is widely used in the production of unsaturated polyester resin, γ-butyrolactone, 1,4-butanediol, tetrahydrofuran and many other chemical products, and has a wide market and strong demand. With the continuous improvement of domestic environmental requirements. For the current benzene oxidation method, the environmental pollution of raw materials and production process, as well as the status quo of cost. How to improve the production process of benzene oxidation to male...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/198B01J27/228C07D307/60
Inventor 刘瑞霞文博张瑞锐王晓晗张慧玲周志茂张锁江
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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