Method for preparing hydrotalcite-assisted vanadium-phosphorus-oxygen catalyst

A technology of vanadium phosphorus oxide and hydrotalcite, which is applied in chemical instruments and methods, catalyst activation/preparation, physical/chemical process catalysts, etc., can solve the problems of insignificant effect, achieve selectivity and conversion rate improvement, simple synthesis, low cost effect

Active Publication Date: 2020-09-25
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0004] The above-mentioned patent improves the performance of the vanadium phosphorus oxygen catalyst by adding a co-catalyst, but the effect is not significant

Method used

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  • Method for preparing hydrotalcite-assisted vanadium-phosphorus-oxygen catalyst
  • Method for preparing hydrotalcite-assisted vanadium-phosphorus-oxygen catalyst
  • Method for preparing hydrotalcite-assisted vanadium-phosphorus-oxygen catalyst

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preparation example Construction

[0017] An embodiment of the present invention provides a method for preparing a hydrotalcite-assisted vanadium-phosphorus-oxygen catalyst, which includes the following steps:

[0018] Preparation of vanadium phosphorus oxide precursor: vanadium source, benzyl alcohol and C 3 ~C 8 The monohydric alcohol is mixed to obtain a mixture, then a phosphorus source is added, the temperature is raised to 100°C to 200°C, the reaction is continued, the product is filtered and dried, and the vanadium phosphorus oxide precursor is obtained;

[0019] Preparation of hydrotalcite additive: Dissolve water-soluble inorganic zinc source, inorganic magnesium source, and inorganic aluminum source in water, add alkali source, heat to 65-200°C for reaction, age for 6-12 hours after cooling down, filter, wash, dry, and Roasting at 350-550°C to obtain the hydrotalcite additive;

[0020] The hydrotalcite additive is mixed with the vanadium phosphorus oxygen precursor according to a mass ratio of 1-10:...

Embodiment 1

[0031] Preparation of Vanadium Phosphate Precursor

[0032] 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.

[0033] Preparation of hydrotalcite additives: Zn 2 Mg 0.2 Al 1 -LDO

[0034] Molebi Zn 2+ :Mg 2+ :Al 3+ 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 1.03g, Al(NO3 ) 2 9H 2 The quality of O is 7.5g, the metal salt that weighs is put into 500mL there-necked flask, then adds 12.68g urea (n 尿素 =3.3×n(Zn 2+ +Mg 2+ +Al 3+ )) Then add 200mL of water, react at 120°C for 6h under magnetic stirring, then age for 12h, filter with suction, wash, and dry to o...

Embodiment 2

[0038] Preparation of Vanadium Phosphate Precursor

[0039] 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 85%wt, 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.

[0040] Preparation of hydrotalcite additives: Zn 2 Mg 0.5 al 1 -LDO

[0041] Molebi Zn 2+ :Mg 2+ :Al 3+ 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 2.56g, Al(NO 3 ) 2 9H 2 The quality of O is 7.5g, the metal salt that weighs is put into 500mL there-necked flask, then adds 13.87g urea (n 尿素 =3.3×n(Zn 2+ +Mg 2+ +Al 3+ )), reacted at 120°C for 6h under magnetic stirring, then aged for 12h, suction filtered, washed, and dried to obtain Zn 2 Mg 0....

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Abstract

The invention relates to a preparation method of a hydrotalcite-assisted vanadium-phosphorus-oxygen catalyst with assistance of hydrotalcite. The preparation method comprises the following steps: preparing a vanadium-phosphorus-oxygen precursor: mixing a vanadium source, benzyl alcohol and C3-C8 monohydric alcohol to obtain a mixture, adding a phosphorus source, carrying out heating to 100-200 DEGC, continuing reacting, and filtering and drying a product to obtain the vanadium-phosphorus-oxygen precursor; preparation of a hydrotalcite additive: dissolving a water-soluble inorganic zinc source, an inorganic magnesium source and an inorganic aluminum source in 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 to obtain the hydrotalcite additive; and preparation of the hydrotalcite-assisted vanadium-phosphorus-oxygen catalyst: mixing the hydrotalcite additive with the vanadium-phosphorus-oxygen precursor according to a mass ratio of (1-10): 100, carrying out heating to 300-500 DEG C, and conducting roasting to obtain the hydrotalcite-assisted vanadium-phosphorus-oxygen catalyst.

Description

technical field [0001] The invention belongs to the field of chemical catalysis, and relates to a method for preparing a vanadium-phosphorus-oxygen catalyst assisted by hydrotalcite. Background technique [0002] Maleic anhydride, referred to as maleic anhydride, also known as maleic anhydride, is an important organic chemical raw material and fine chemical product. It is currently the third largest anhydride in the world after phthalic anhydride and acetic anhydride. It is mainly used in the production of Unsaturated polyester resin, alkyd resin, used in pesticides, pharmaceuticals, coatings, inks, lubricating oil additives, textile finishing agents, food additives and surfactants, 1,4-butanediol, γ-butyrolactone, tetrahydrofuran A series of important organic chemicals and fine chemicals. [0003] Vanadium-phosphorus-oxygen catalyst is currently the most effective catalyst for the oxidation of n-butane to maleic anhydride. Its catalytic activity and selectivity are closely...

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 刘瑞霞张慧玲李英葳张永康代飞张瑞锐张锁江
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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