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Vanadyl phosphate catalyst as well as preparation method and application thereof

A technology of vanadyl phosphate catalyst and vanadium source, which is applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc. It can solve the problems of low conversion rate, low reaction yield, secondary pollution, etc., and achieve good crystallinity

Active Publication Date: 2018-07-27
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method of the present invention uses a cheap, non-toxic deep eutectic solvent to assist in the synthesis of the vanadyl phosphate catalyst, can prepare the vanadyl phosphate catalyst in an environmentally friendly manner, and can overcome the traditional reliance on noble metals to improve its performance, secondary pollution, high cost, and difficult preparation process Complicated and other disadvantages
When the catalyst is used to catalyze the reaction of n-butane selective oxidation to maleic anhydride, it improves the low yield of n-butane selective oxidation of maleic anhydride, catalyst selectivity, low conversion rate, loss of additive elements and cost in the prior art. advanced questions

Method used

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  • Vanadyl phosphate catalyst as well as preparation method and application thereof
  • Vanadyl phosphate catalyst as well as preparation method and application thereof
  • Vanadyl phosphate catalyst as well as preparation method and application thereof

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preparation example Construction

[0069] The embodiment of the present invention provides a kind of preparation method of vanadyl phosphate catalyst, it comprises the following steps:

[0070] S01: Put the vanadium source in a container, add a mixture of deep eutectic solvent: isobutanol: benzyl alcohol (volume ratio) = (0.15~0.25): (3~5): 1, and heat up to 100 ° C ~ 180 ℃ for 2 hours to 8 hours, then cooled to 30 ℃ to 80 ℃, then added phosphorus source, heated to 100 ℃ to 200 ℃ to continue the reaction for 10h to 24h, and the product was filtered, washed and dried to obtain the vanadyl phosphate precursor. The molar ratio of the phosphorus in the phosphorus source and the vanadium in the vanadium source is (0.8~1.5): 1, and the concentration of the described vanadium pentoxide in isobutanol and benzyl alcohol mixed solution is 0.02g / mL~0.12g / mL mL, the mass ratio of the vanadium source and the deep eutectic solvent is (50~10):1;

[0071] S02: Calcining the vanadyl phosphate precursor at a temperature of 350°...

Embodiment 1

[0079] Preparation of vanadyl phosphate catalyst:

[0080] (1) Weigh 10g V 2 o 5 Place in a 250mL three-necked flask, add a mixture of 1g of choline chloride-oxalic acid deep eutectic solvent, 80mL of isobutanol and 20mL of benzyl alcohol, stir and mix evenly, reflux at 135°C for 3h and then cool down to 60°C.

[0081] (2) Slowly add 7.53mL of 85% H 3 PO 4 , and continued to reflux for 16 hours at a temperature of 135° C. Filter and wash with absolute ethanol to obtain a blue precipitate, and dry it in air at 120° C. for 24 hours to obtain a vanadyl phosphate catalyst precursor powder.

[0082] (3) The obtained vanadyl phosphate catalyst precursor powder was pressed into tablets under a pressure of 15 MPa, crushed, and 20-40 mesh catalyst particles were sieved.

[0083] (4) Afterwards, the catalyst particles were activated in situ at a rate of 2°C / min to 430°C for 12 hours in an atmosphere of n-butane / oxygen / nitrogen mixed reaction gas with a volume ratio of 1.5:17:81.5 t...

Embodiment 2

[0088] Preparation of vanadyl phosphate catalyst:

[0089] (1) Weigh 10g V 2 o 5 Place in a 250mL three-necked flask, add a mixture of 1g of choline chloride-tartaric acid deep eutectic solvent, 80mL of isobutanol and 20mL of benzyl alcohol, stir and mix evenly, reflux at 135°C for 3h and then cool down to 60°C.

[0090] (2) Slowly add 7.53mL of 85% H 3 PO 4 , and continued to reflux for 16 hours at a temperature of 135° C. Filter and wash with absolute ethanol to obtain a blue-black precipitate, and dry it in air at 120° C. for 24 hours to obtain a vanadyl phosphate catalyst precursor powder.

[0091] (3) The obtained vanadyl phosphate catalyst precursor powder was pressed into tablets under a pressure of 15 MPa, crushed, and 20-40 mesh catalyst particles were sieved.

[0092] (4) Afterwards, the catalyst particles were activated in situ at a rate of 2°C / min to 430°C for 12 hours in an atmosphere of n-butane / oxygen / nitrogen mixed reaction gas with a volume ratio of 1.5:1...

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Abstract

The invention relates to a vanadyl phosphate catalyst as well as a preparation method and application thereof. The method comprises the following steps: 1) mixing a vanadium source, a choline chloride-organic carboxylic acid eutectic solvent and an alcohol, and performing a reaction, wherein the alcohol is benzyl alcohol, or a mixture of a C3-C8 monohydric alcohol and the benzyl alcohol; 2) mixingthe obtained reaction product with a phosphorus source, raising temperature until the temperature is higher than a melting point of the eutectic solvent, and continuing a reaction to obtain a vanadylphosphate precursor; and 3) performing calcination to obtain the vanadyl phosphate catalyst. The method provided by the invention uses the green cheap eutectic solvent to intensively prepare the vanadyl phosphate catalyst, and overcomes the disadvantages that a vanadyl phosphate catalyst relies on precious metals to improve performance, secondary pollution is generated, costs are high and a preparation process is complicated; and the vanadyl phosphate catalyst provided by the invention improves the difficult problems of a low yield and poor selectivity when being used for catalyzing a reaction of preparing maleic anhydride by selective oxidation of n-butane, and overcomes the disadvantages of high costs and large pollution in a conventional catalyst improving method.

Description

technical field [0001] The invention belongs to the field of chemical catalysis, and relates to a vanadyl phosphate catalyst, a preparation method and application thereof, in particular to a vanadyl phosphate catalyst, a preparation method enhanced by a deep eutectic solvent and an application thereof. Background technique [0002] Vanadyl phosphate catalyst (also known as vanadium phosphorus oxygen catalyst, referred to as VPO) is a composite metal oxide catalyst composed of V, P, and O. Due to its special structure, it can selectively oxidize butane to generate maleic anhydride. This is also the only catalyst that catalyzes this reaction. The crystal phase composition of the catalyst is very complex, and there are many crystal phases with different properties and compositions. It is reported in the literature that VOPO 4 2H 2 O, α Ⅰ -VOPO 4 、α Ⅱ -VOPO 4 , β-VOPO 4 , γ-VOPO 4 、VOHPO 4 0.5H 2 O and (VO) 2 P 2 o 7 Wait. Different crystal phases will affect the a...

Claims

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Application Information

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IPC IPC(8): B01J27/198B01J35/10C07D307/60
CPCC07D307/60B01J27/198B01J35/613B01J37/031B01J37/088B01J37/10C01B25/372B01J35/30B01J35/40B01J27/199B01J37/04C01P2004/03
Inventor 刘瑞霞贺滨张瑞锐唐红果张锁江
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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