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Supported vanadyl pyrophosphate catalyst prepared by selective oxidation of n-butane and preparation method thereof

A vanadyl pyrophosphate catalyst and selective oxidation technology, which are applied in the directions of catalyst activation/preparation, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problems of complex preparation method, long cycle, complex catalyst preparation process, etc. The effect of improving catalytic performance, high wear resistance and longevity

Inactive Publication Date: 2014-07-30
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent CN1453071A discloses a method of pyrolysis SiO 2 As a supported VPO catalyst, it is used for the selective oxidation of n-butane, and the best catalyst prepared is 30% VPO / SiO 2 , at a reaction temperature of 400°C, the conversion of n-butane was 50.8%, the selectivity of maleic anhydride was 61.2%, and the yield of maleic anhydride was 31.1%. 2 Optimum level for supported catalysts, but less than ideal compared to bulk catalysts
[0006] Chinese patent CN1067189A discloses a method for preparing a vanadium-phosphorus-zirconium mixed oxide catalyst for the production of maleic anhydride. The prepared catalyst has high strength and high activity, but the preparation process of the catalyst is complicated and the cycle is long
[0008] VPO / TiO 2 There are not many studies on the catalyst used in the selective oxidation of n-butane. Due to the complicated preparation method of VPO catalyst, the performance of the catalyst is very poor.
[0009] In recent years, some scholars have also studied VPO / TiO 2 Catalysts, but they are used in other reactions, the application of selective oxidation of n-butane is seldom, and the preparation method adopts direct mechanical grinding and mixing

Method used

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  • Supported vanadyl pyrophosphate catalyst prepared by selective oxidation of n-butane and preparation method thereof
  • Supported vanadyl pyrophosphate catalyst prepared by selective oxidation of n-butane and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1) Weigh 5g TiO 2 Immerse in 100ml of phosphoric acid solution with a concentration of 1.0mol / L, stir in an oil bath at 70°C for 12 hours, filter, wash with distilled water three times, and dry at 110°C as a spare carrier.

[0030] 2) Weigh 0.54g V 2 o 5 Mix in isobutanol-benzyl alcohol (12ml / 12ml) mixed solvent, heat and reflux at 140°C for 6h, when the mixture turns black, add 3g of the carrier TiO treated by step 1) 2 , continue to reflux for 30min, after cooling the above mixture, slowly add 0.82g of phosphoric acid with a concentration of 85% dropwise, then rapidly raise the temperature to 140°C, and continue to reflux for 6h to form a blue precipitate, which is filtered after cooling, and the obtained solid is successively washed with isobutyl Alcohol and acetone were washed twice respectively, and the filtrate was dried in an oven at 110° C. for 12 hours to obtain the precursor of the catalyst of the present invention. The catalyst precursor is pressed into ta...

Embodiment 2

[0034] 1) Same as step 1) in Example 1.

[0035] 2) Weigh 0.80g V 2 o 5 Mix in isobutanol-benzyl alcohol (17ml / 17ml) mixed solvent, heat and reflux at 140°C for 6h, at this time the mixture turns black, then add 3g of carrier TiO treated by step 1) 2 , continue to reflux for 30min, after cooling the above mixture, slowly add 1.22g of phosphoric acid with a concentration of 85% dropwise, then rapidly raise the temperature to 140°C, and continue to reflux for 6h to form a blue precipitate. Alcohol and acetone were washed twice respectively, and the filtrate was dried in an oven at 110° C. for 12 hours to obtain the precursor of the catalyst of the present invention. The catalyst precursor is pressed into tablets, crushed, sieved, and a 40-80 mesh sample is taken for roasting.

[0036] 3) Place the catalyst precursor sample prepared in step 2) in a fluidized system fixed-bed roaster for roasting, the roasting conditions are the same as in Example 1, and the mass percentage of ...

Embodiment 3

[0039] 1) Same as step 1) in Example 1.

[0040] 2) Weigh 1.07g V 2 o 5 Mix in isobutanol-benzyl alcohol (23ml / 23ml) mixed solvent, heat and reflux at 140°C for 6h, when the mixture turns black, add 3g of the carrier TiO treated in step 1) 2 , continue to reflux for 30min, after cooling the above mixture, slowly add 1.63g of phosphoric acid with a concentration of 85% dropwise, then rapidly raise the temperature to 140°C, and continue to reflux for 6h to form a blue precipitate. Alcohol and acetone were washed twice respectively, and the filtrate was dried in an oven at 110° C. for 12 hours to obtain the precursor of the catalyst of the present invention. The catalyst precursor is pressed into tablets, crushed, sieved, and a 40-80 mesh sample is taken for roasting.

[0041] 3) Place the catalyst precursor sample prepared in step 2) in a fluidized system fixed-bed roaster for roasting, the roasting conditions are the same as in Example 1, and the mass percentage of each comp...

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Abstract

The invention discloses a supported vanadyl pyrophosphate catalyst prepared by selective oxidation of n-butane and a preparation method thereof, and relates to a maleic anhydride catalyst prepared by selective oxidation of n-butane. The catalyst contains an active ingredient and a carrier, wherein the active ingredient is (VO)2P2O7, and the carrier is TiO2 treated by a phosphoric acid solution. The preparation method comprises the steps of soaking the TiO2 into the phosphoric acid solution, stirring in an oil bath pan, filtering, washing and drying to obtain the carrier TiO2; mixing V2O5 with an isobutanol-phenylcarbinol mixed solvent, heating for refluxing to ensure that the mixed solution becomes black, then adding the carrier TiO2, refluxing continuously, cooling the mixed solution, then adding phosphoric acid, heating, refluxing continuously to generate a blue sediment, cooling, filtering, washing the obtained solid, drying the filtrate, carrying out tabletting, smashing, and screening to obtain a catalyst precursor; and putting the prepared catalyst precursor into a fixed bed roasting furnace of a mobile system, and roasting in an atmosphere of reaction gas to obtain the product.

Description

technical field [0001] The invention relates to a catalyst for producing maleic anhydride through the selective oxidation of n-butane, in particular to a supported vanadyl pyrophosphate (VO) for the selective oxidation of n-butane 2 P 2 o 7 / TiO 2 Catalyst and method for its preparation. Background technique [0002] Maleic anhydride (maleic anhydride) is a common and important organic chemical raw material, and it is the third largest anhydride in the world after acetic anhydride and phthalic anhydride. [0003] For the production of maleic anhydride by n-butane oxidation, researchers have tried many types of catalysts, and found that vanadium phosphorus composite oxide (VPO) is the most effective catalyst [US Patent US3293268 (1966)], and its main active component is coke Vanadyl phosphate, the unloaded VPO catalyst that industrial production adopts at present, but there are many problems, compared with unloaded catalyzer, supported catalyst has the following advantage...

Claims

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Application Information

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IPC IPC(8): B01J27/198B01J37/03C07D307/60
Inventor 黄传敬刘新华武华乙翁维正万惠霖
Owner XIAMEN UNIV
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