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Zirconium-base loaded vanadium-phosphor oxide catalyst, and its preparing and use

A technology of vanadium phosphorus oxide and catalyst, applied in physical/chemical process catalysts, chemical instruments and methods, organic chemistry, etc., can solve the problems of low conversion rate of butane and low selectivity of maleic anhydride

Inactive Publication Date: 2007-03-28
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Both butane conversion and maleic anhydride selectivity are low on such supported catalysts, such as on conventional SiO 2 The butane conversion rate of the supported VPO catalyst prepared by the aqueous phase impregnation method is about 50%, and the maleic anhydride selectivity is lower than 20% [see J.Phys.Chem.B, 101 (1997) 6895]

Method used

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  • Zirconium-base loaded vanadium-phosphor oxide catalyst, and its preparing and use

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 5.00g ZrOCl 2 ·8H 2 Dissolve O and 1.00g CTAB in water, stir to obtain a clear solution, continue to stir at 70°C for 2 hours, then slowly add 2mol / L NaOH solution dropwise to the solution, and adjust the pH to ≥ 12.00 to obtain a white sol-gel . The mixture was transferred to an autoclave and kept at 100 °C for 48 h, then cooled to room temperature naturally. The solid was filtered and washed until the pH of the filtrate was neutral. The resulting white solid was then dried at 100°C. The white solid was heated from room temperature to 550° C. at a rate of 1° C. / min in the air and roasted at this temperature for 8 hours. Thus, a zirconium-based support without phosphoric acid modification was obtained.

[0030] Weigh V 2 o 5 2.4 grams, placed in the mixed solution of isobutanol / benzyl alcohol (30ml / 30ml), after refluxing at 140°C for 6 hours, add 1.1 grams of polyethylene glycol (PEG2000) with a molecular weight of 2000, and add 6.0 grams of zirconium prepared a...

Embodiment 2

[0033] 4.00g ZrOCl 2 ·8H 2 Dissolve O and 1.00g CTAB in water, stir to obtain a clear solution, continue to stir at 70°C for 2 hours, then slowly add 2mol / L NaOH solution dropwise to the solution, and adjust the pH to ≥ 12.00 to obtain a white sol-gel . The mixture was transferred to an autoclave and kept at 100 °C for 48 h, then cooled to room temperature naturally. The solid was filtered and washed until the pH of the filtrate was neutral. The resulting white solid was then dried at 100°C and placed in 1mol / L H 3 PO 4 In the solution, add H per gram of solid sample 3 PO 4 20ml of the solution was stirred at a constant temperature of 70°C for 12h, and then the treated sample was filtered and washed until the filtrate was neutral, and then dried at 100°C. In the air at a rate of 1 ° C / min from room temperature to 550 ° C and constant temperature roasting at this temperature for 8 hours. A phosphoric acid-modified zirconium-based support is thus obtained.

[0034] We...

Embodiment 3

[0037] 4.00g ZrOCl 2 ·8H 2 Dissolve O and 1.00g CTAB in water, stir to obtain a clear solution, continue to stir at 70°C for 2 hours, then slowly add 2mol / L NaOH solution dropwise to the solution, and adjust the pH to ≥ 12.00 to obtain a white sol-gel . The mixture was transferred to an autoclave and kept at 100 °C for 48 h, then cooled to room temperature naturally. The solid was filtered and washed until the pH of the filtrate was neutral. Then the obtained white solid was dried at 100° C., raised from room temperature to 550° C. in air at a rate of 1° C. / min, and roasted at this temperature for 8 hours at a constant temperature. Put the calcined solid in 1mol / L H 3 PO 4 In the solution, add H per gram of solid sample 3 PO 4 20ml of the solution was stirred at 70°C for 12 hours, then the sample was filtered and washed until the filtrate was neutral, dried at 100°C, and then roasted under the same conditions as above to obtain a phosphoric acid-modified zirconium-based...

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Abstract

The present invention relates to a catalyst made up by using zirconium base carrier material or zirconium base carrier material modified by phosphoric acid and vanadium phosphorus oxide loaded on said carrier material. The described zirconium base carrier material is zirconium oxide, the loaded quantity of vanadium phosphorus oxide is 25-47 wt% of total mass of said catalyst, in which the atomic ratio of vanadium and phosphorus is 1.2, its specific surface area is about 21-29 sq.m / g. When it is used as catalyst for normal-butane air oxidation reaction to prepare cis-butenedioic anhydride, in the typical reaction temperature zone of 380-420deg.C its per pass conversion rate is 38-89%, the cis-butenedioic anhydride selectivity is 29-69% and maximum cis-butenedioic anhydride yield is 61.2%. Said invention also discloses the preparation method of said catalyst.

Description

technical field [0001] The invention relates to a supported vanadium phosphorus oxide catalyst and preparing maleic anhydride by catalytically oxidizing n-butane with air on the catalyst. Background technique [0002] Maleic anhydride, referred to as maleic anhydride, also known as maleic anhydride, is an important chemical raw material, which can be used in the production of unsaturated polyester resin, fumaric anhydride, lubricating oil additives, heat-resistant styrene resin and other fine chemical intermediates Body and specialty chemicals, and also raw materials for the production of high value-added fine chemicals such as 1,4-butanediol, tetrahydrofuran, γ-butyrolactone, etc., and its application range is still expanding [see Catal.Rev. - Sci. Eng., 27 (1985) 373 and Chem. Rev., 88 (1988) 50]. [0003] The early production method of maleic anhydride was to use V 2 o 5 -MoO 3 The catalyst was prepared by selective oxidation of benzene. Later, a production process r...

Claims

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Application Information

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IPC IPC(8): B01J27/198B01J21/06C07D307/60
Inventor 季伟捷冯汝明杨秀娟区泽棠陈懿
Owner NANJING UNIV
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