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Method for preparing rare earth-based hydrotalcite-assisted vanadium-phosphorus-oxygen catalyst

A technology of hydrotalcite and vanadium phosphorus oxide, which is applied in chemical instruments and methods, catalyst activation/preparation, physical/chemical process catalysts, etc. It can solve the problems of low butane conversion rate, high catalyst cost, low selectivity of maleic anhydride, etc. problem, to achieve the effect of improving selectivity, increasing lattice oxygen, and simplifying synthesis

Active Publication Date: 2020-09-25
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

Although these methods have improved the performance of vanadium-phosphorus-oxygen catalysts, they still have the problems of low butane conversion rate and low maleic anhydride selectivity. In addition, the addition of auxiliary agents such as dimethylsulfoxide and polyethylene glycol It will lead to an increase in the cost of the catalyst, and more importantly, the direct addition of the metal salt will produce toxic gases such as nitrogen dioxide, causing secondary pollution

Method used

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  • Method for preparing rare earth-based hydrotalcite-assisted vanadium-phosphorus-oxygen catalyst
  • Method for preparing rare earth-based hydrotalcite-assisted vanadium-phosphorus-oxygen catalyst
  • Method for preparing rare earth-based hydrotalcite-assisted vanadium-phosphorus-oxygen catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Preparation of Vanadium Phosphate Precursor

[0034] Weigh 13.5g V 2 o 5 Mix with benzyl alcohol and isobutanol, heat and reflux at 135°C for 3h under mechanical stirring, then cool down to 80°C, add 9.4mL of phosphoric acid with a mass fraction of 85wt%, raise the temperature to 135°C, and heat to reflux for 16h under continuous stirring Afterwards, the obtained product is filtered and dried to obtain a solid and dried to obtain a vanadium phosphorus oxide precursor.

[0035] Preparation of praseodymium-based hydrotalcite additive: Zn 2 Mg 1 PR 0.1 al 1 -LDO

[0036] Press Zn 2+ :Mg 2+ :Pr 3+ :Al 3+ The molar ratio is 2:1:0.1:1 to weigh Zn(NO 3 ) 2 ·6H 2 The mass of O is 11.91g, Mg(NO 3 ) 2 ·6H 2 The mass of O is 5.12g, Pr(NO 3 ) 3 ·6H 2 The mass of O is 0.87g, Al(NO 3 ) 2 9H 2 The quality of O is 7.5g, put the weighed metal salt into a 500mL three-necked flask, and then add 16.22g of urea (n urea=3.3×n(Zn 2+ +Mg 2+ +Pr 3+ +Al 3+ )) Then add 200...

Embodiment 2

[0040] Preparation of Vanadium Phosphate Precursor

[0041] Weigh 13.5g V 2 o 5 Mix with benzyl alcohol and isobutanol, heat and reflux at 135°C for 3h under mechanical stirring, then cool down to 80°C, add 9.4mL of phosphoric acid with a mass fraction of 85wt%, raise the temperature to 135°C, and heat to reflux for 16h under continuous stirring Afterwards, the obtained product is filtered and dried to obtain a solid and dried to obtain a vanadium phosphorus oxide precursor.

[0042] Preparation of Nd-based hydrotalcite additive: Zn 2 Mg 1 Nd 0.1 al 1 -LDO

[0043] Press Zn 2+ :Mg 2+ :Nd 3+ :Al 3+ The molar ratio is 2:1:0.1:1 to weigh Zn(NO 3 ) 2 ·6H 2 The mass of O is 11.91g, Mg(NO 3 ) 2 ·6H 2 The mass of O is 5.12g, Nd(NO 3 ) 3 ·6H 2 The mass of O is 0.66g, Al(NO 3 ) 2 9H 2 The quality of O is 7.5g, put the weighed metal salt into a 500mL three-necked flask, and then add 16.22g of urea (n urea=3.3×n(Zn 2+ +Mg 2+ +Al 3+ +Nd 3+ +Al 3+ )) Then add 200...

Embodiment 3

[0047] Preparation of Vanadium Phosphate Precursor

[0048] Weigh 13.5g V 2 o 5 Mix with benzyl alcohol and isobutanol, heat and reflux at 135°C for 3h under mechanical stirring, then cool down to 80°C, add 9.4mL of phosphoric acid with a mass fraction of 85wt%, raise the temperature to 135°C, and heat to reflux for 16h under continuous stirring Afterwards, the obtained product is filtered and dried to obtain a solid and dried to obtain a vanadium phosphorus oxide precursor.

[0049] Preparation of samarium-based hydrotalcite additive: Zn 2 Mg 1 SM 0.1 al 1 -LDO

[0050] Press Zn 2+ :Mg 2+ :Sm 3+ :Al 3+ The molar ratio is 2:1:0.1:1 to weigh Zn(NO 3 ) 2 ·6H 2 The mass of O is 11.91g, Mg(NO 3 ) 2 ·6H 2 The mass of O is 5.12g, Sm(NO 3 ) 3 ·6H 2 The mass of O is 0.89g, Al(NO 3 ) 2 9H 2 The quality of O is 7.5g, put the weighed metal salt into a 500mL three-necked flask, and then add 16.22g of urea (n urea=3.3×n(Zn 2+ +Mg 2+ +Sm 3+ +Al 3+ )) Then add 200mL...

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Abstract

The invention relates to a method for preparing a rare earth-based hydrotalcite-assisted vanadium-phosphorus-oxygen catalyst. The method comprises the following steps: preparing a vanadium-phosphorus-oxygen precursor; preparing a rare earth-based hydrotalcite auxiliary agent by dissolving a water-soluble inorganic zinc source, an inorganic magnesium source, an inorganic aluminum source and rare earth salt into water, adding an alkali source, carrying out heating to 65-200 DEG C for a reaction, conducting cooling, then performing aging for 6-12 hours, conducting filtering, washing and drying, and carrying out roasting at 350-550 DEG C, wherein a ratio of the total molar amount of zinc and magnesium in the inorganic zinc source, the inorganic magnesium source, the inorganic aluminum source and the rare earth salt to the total molar amount of aluminum and rare earth elements is (1-4): 1; and mixing the rare earth-based hydrotalcite auxiliary agent with the vanadium-phosphorus-oxygen precursor according to a mass ratio of (1-10): 100, carrying out heating to 300-500 DEG C, and performing roasting to obtain the vanadium phosphorus oxide catalyst.

Description

technical field [0001] The invention belongs to the field of chemical catalysis, and relates to a method for assisting a vanadium-phosphorus-oxygen catalyst with rare earth-based hydrotalcite. Background technique [0002] Maleic anhydride, referred to as maleic anhydride, is an important organic chemical raw material. So far, the selective oxidation of butane to maleic anhydride using vanadium phosphorus oxygen catalyst is the only process that has been successfully industrialized. [0003] At present, researchers have done a lot of research and attempts on catalysts used in the oxidation of n-butane to maleic anhydride. It is generally believed that the main reason for restricting the performance of vanadium-phosphorus-oxygen catalysts is that the catalysts will undergo deep oxidation during use, resulting in catalyst degradation. Reduced performance. At present, the catalytic performance of the catalyst is mainly improved by adding metal salts as auxiliary agents. For e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/198C07D307/60B01J37/00
CPCB01J27/198B01J37/0009C07D307/60
Inventor 刘瑞霞张瑞锐张慧玲谢志琦董洁代飞张锁江
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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