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VOPO4 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, loss cost of additive elements, high cost, etc., and achieve crystallization good sex effect

Active Publication Date: 2018-08-03
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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  • VOPO4 catalyst as well as preparation method and application thereof
  • VOPO4 catalyst as well as preparation method and application thereof
  • VOPO4 catalyst as well as preparation method and application thereof

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preparation example Construction

[0066] The embodiment of the present invention provides a kind of preparation method of vanadyl phosphate catalyst, it comprises the following steps:

[0067] 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 to the deep eutectic solvent is (50~10):1

[0068] S02: Calcining the vanadyl phosphate precursor at a temperature of 350° C...

Embodiment 1

[0077] (1) Weigh 15g V 2 o 5 Place in a 250mL three-necked flask, add a mixture of 1.5g polyethylene glycol-thiourea deep eutectic solvent, 80mL isobutanol and 20mL benzyl alcohol, stir and mix evenly, reflux at 135°C for 3 hours and then cool to 60°C ℃.

[0078] (2) Slowly add 11.29mL 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.

[0079] (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.

[0080] (4) Afterwards, the catalyst particles were activated in situ from room temperature to 430°C at a rate of 2°C / min for 12 hours in an atmosphere of n-butane / oxygen / nitrogen reaction gas with a volume ratio of 1.5:17:81.5 to obtain phosphoric acid vanadyl cataly...

Embodiment 2

[0084] (1) Weigh 15g V 2 o 5 Place in a 250mL three-neck flask, add a mixture of 1.5g polyethylene glycol-urea deep eutectic solvent, 80mL isobutanol and 20mL benzyl alcohol, stir and mix evenly, reflux at 135°C for 3 hours and then cool down to 60°C .

[0085] (2) Slowly add 11.29mL 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.

[0086] (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.

[0087] (4) Afterwards, the catalyst particles were activated in situ from room temperature to 430° C. at a rate of 2° C. / min under a reaction gas atmosphere for 12 hours to obtain a vanadyl phosphate catalyst.

[0088] Detection:

[0089] Take by weighing vanadyl phos...

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Abstract

The invention relates to a VOPO4 catalyst as well as a preparation method and an application thereof. The method comprises the steps as follows: 1) a vanadium source, a deep-eutectic solvent and alcohol are mixed to react; 2) an obtained product is mixed with a phosphorus source, the mixture is heated to the temperature higher than the melting point of the deep-eutectic solvent to react continuously, a precursor is obtained and roasted, and the VOPO4 catalyst is obtained. The deep-eutectic solvent is any one of or a combination of at least two of urea-polyethylene glycol, urea-metal chloride,urea-choline chloride or thiourea-polyethylene glycol; the alcohol is benzyl alcohol or a mixture of C3-C8 monohydric alcohol and benzyl alcohol. The method overcomes the defects that VOPO4 catalystsdepend on precious metals to improve the performance of the VOPO4 catalysts, cause secondary pollution, are high in cost and complex to prepare and the like. The problems of low yield, poor selectivity and the like are solved and the defects of high costs and severe pollution in traditional catalyst improvement methods are overcome when the VOPO4 catalysts are applied to catalyze a reaction for preparing maleic anhydride through n-butane selective oxidation.

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] The vanadyl phosphate catalyst 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. It is also the only catalyst that can catalyze 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. (VO) 2 P 2 o 7 Wait. Different crystal phases will affect the acid strength and microscopic morphology of the VPO catalyst, which in t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/198B01J37/03B01J37/08C07D307/60
CPCB01J27/198B01J37/0018B01J37/031B01J37/08C07D307/60
Inventor 张锁江刘瑞霞张瑞锐贺滨代飞陈雪景李自航
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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