Preparation method of catalyst for producing maleic anhydride

Abstract

The invention relates to a preparation method of a catalyst for producing maleic anhydride. The preparation method mainly solves the problem that the existing catalyst has a small specific surface area and poor hydrocarbon selective oxidation reaction catalytic performances. Through preparation of VOPO4.2H2O and an intercalation reaction with an organic structure, an intercalated VOPO4 compound with an adjustable structure is obtained. Through organic alcohol reduction and roasting activation in a high-pressure synthesis kettle, the active vanadium-phosphorous oxide catalyst is obtained. The preparation method well improves the prior art and can be used for the selective oxidation of gaseous hydrocarbons to produce maleic anhydride.

Description

technical field

[0001] The invention relates to a catalyst preparation method for producing maleic anhydride. The catalyst prepared by the method is especially suitable for preparing maleic anhydride through the selective oxidation of gas-phase hydrocarbons. technical background

[0002] Maleic anhydride, referred to as maleic anhydride, that is, maleic anhydride (Maleic anhydride, MA), is an important organic chemical raw material, mainly used in the production of unsaturated polyester resin, alkyd resin, 1,4-butanediol ( BDO), γ-butyrolactone (GBL), tetrahydrofuran (THF) and other chemicals. In addition, it is also widely used in various fine chemicals.

[0003] The main method of producing maleic anhydride is gas phase oxidation. Among them, the gas phase oxidation of n-butane is one of the most important production methods of maleic anhydride.

[0004] Vanadium-phosphorus-oxygen (VPO) catalyst is by far the most effective catalyst for producing maleic anhydride from ...

Examples

Embodiment 1

[0027] Add about 0.22mol of vanadium pentoxide to 1000ml of 20wt% phosphoric acid solution, start stirring and heat the mixed solution to reflux and then reflux for 24h. After the heating and cooling are stopped, the mixed solution is filtered and washed with hot water, and then washed with acetone to obtain a filter cake Dry at 105°C for 12h to get VOPO 4 Precursor A. The resulting precursor A was added to 400ml of ethylene glycol and reacted at 50°C and 80°C for 1 hour respectively. After cooling, it was filtered and washed with acetone. The obtained filter cake was dried at 120°C for 20 hours to obtain precursor B. Precursor B and 400ml of isobutanol were placed in a small autoclave and sealed, heated to 130°C and kept for 6h, the resulting solution was cooled, filtered, washed with isobutanol and dried at 120°C for 20h to obtain a VPO precursor. The VPO precursor was heated to 415 °C for 3 h in an atmosphere of 20% air / 20% nitrogen / 10% carbon dioxide / 50% water vapor by vo...

Embodiment 2

[0031]Add about 0.22mol of vanadium pentoxide to 1000ml of 20wt% phosphoric acid solution, start stirring and heat the mixed solution to reflux and then reflux for 24h. After the heating and cooling are stopped, the mixed solution is filtered and washed with hot water, and then washed with acetone to obtain a filter cake Dry at 105°C for 12h to get VOPO 4 Precursor A. Precursor A was mixed with 300ml 1,4-butanediol and reacted at 50°C and 80°C for 1 hour respectively. After cooling, it was filtered and washed with acetone. The obtained filter cake was dried at 120°C for 20 hours to obtain precursor B. Precursor B and 400ml of isobutanol were placed in a small autoclave and sealed, heated to 130°C and kept for 6h, the resulting solution was cooled, filtered, washed with isobutanol and dried at 120°C for 20h to obtain a VPO precursor. The VPO precursor was heated to 415 °C for 3 h in an atmosphere of 20% air / 20% nitrogen / 10% carbon dioxide / 50% water vapor by volume, and finally...

Embodiment 3

[0033] Add about 0.22mol of vanadium pentoxide to 1000ml of 20wt% phosphoric acid solution, start stirring and heat the mixed solution to reflux and then reflux for 24h. After the heating and cooling are stopped, the mixed solution is filtered and washed with hot water, and then washed with acetone to obtain a filter cake Dry at 105°C for 12h to get VOPO 4 Precursor A. Precursor A was mixed with 400ml of methyl ethyl ketone and reacted at 50°C and 70°C for 1 hour respectively. After cooling, it was filtered and washed with acetone. The obtained filter cake was dried at 120°C for 20 hours to obtain precursor B. Precursor B and 400ml of isobutanol were placed in an autoclave, sealed and heated to 140°C for 6h, cooled, filtered, washed with isobutanol and dried at 120°C for 20h to obtain a VPO precursor. The VPO precursor was heated to 415 °C for 3 h in an atmosphere of 20% air / 20% nitrogen / 10% carbon dioxide / 50% water vapor by volume, and finally in an atmosphere of 40% nitroge...

technical field

[0001] The invention relates to a catalyst preparation method for producing maleic anhydride. The catalyst prepared by the method is especially suitable for preparing maleic anhydride through the selective oxidation of gas-phase hydrocarbons. technical background

[0002] Maleic anhydride, referred to as maleic anhydride, that is, maleic anhydride (Maleic anhydride, MA), is an important organic chemical raw material, mainly used in the production of unsaturated polyester resin, alkyd resin, 1,4-butanediol ( BDO), γ-butyrolactone (GBL), tetrahydrofuran (THF) and other chemicals. In addition, it is also widely used in various fine chemicals.

[0003] The main method of producing maleic anhydride is gas phase oxidation. Among them, the gas phase oxidation of n-butane is one of the most important production methods of maleic anhydride.

[0004] Vanadium-phosphorus-oxygen (VPO) catalyst is by far the most effective catalyst for producing maleic anhydride from ...

Examples

Embodiment 1

[0027] Add about 0.22mol of vanadium pentoxide to 1000ml of 20wt% phosphoric acid solution, start stirring and heat the mixed solution to reflux and then reflux for 24h. After the heating and cooling are stopped, the mixed solution is filtered and washed with hot water, and then washed with acetone to obtain a filter cake Dry at 105°C for 12h to get VOPO 4 Precursor A. The resulting precursor A was added to 400ml of ethylene glycol and reacted at 50°C and 80°C for 1 hour respectively. After cooling, it was filtered and washed with acetone. The obtained filter cake was dried at 120°C for 20 hours to obtain precursor B. Precursor B and 400ml of isobutanol were placed in a small autoclave and sealed, heated to 130°C and kept for 6h, the resulting solution was cooled, filtered, washed with isobutanol and dried at 120°C for 20h to obtain a VPO precursor. The VPO precursor was heated to 415 °C for 3 h in an atmosphere of 20% air / 20% nitrogen / 10% carbon dioxide / 50% water vapor by vo...

Embodiment 2

[0031]Add about 0.22mol of vanadium pentoxide to 1000ml of 20wt% phosphoric acid solution, start stirring and heat the mixed solution to reflux and then reflux for 24h. After the heating and cooling are stopped, the mixed solution is filtered and washed with hot water, and then washed with acetone to obtain a filter cake Dry at 105°C for 12h to get VOPO 4 Precursor A. Precursor A was mixed with 300ml 1,4-butanediol and reacted at 50°C and 80°C for 1 hour respectively. After cooling, it was filtered and washed with acetone. The obtained filter cake was dried at 120°C for 20 hours to obtain precursor B. Precursor B and 400ml of isobutanol were placed in a small autoclave and sealed, heated to 130°C and kept for 6h, the resulting solution was cooled, filtered, washed with isobutanol and dried at 120°C for 20h to obtain a VPO precursor. The VPO precursor was heated to 415 °C for 3 h in an atmosphere of 20% air / 20% nitrogen / 10% carbon dioxide / 50% water vapor by volume, and finally...

Embodiment 3

[0033] Add about 0.22mol of vanadium pentoxide to 1000ml of 20wt% phosphoric acid solution, start stirring and heat the mixed solution to reflux and then reflux for 24h. After the heating and cooling are stopped, the mixed solution is filtered and washed with hot water, and then washed with acetone to obtain a filter cake Dry at 105°C for 12h to get VOPO 4 Precursor A. Precursor A was mixed with 400ml of methyl ethyl ketone and reacted at 50°C and 70°C for 1 hour respectively. After cooling, it was filtered and washed with acetone. The obtained filter cake was dried at 120°C for 20 hours to obtain precursor B. Precursor B and 400ml of isobutanol were placed in an autoclave, sealed and heated to 140°C for 6h, cooled, filtered, washed with isobutanol and dried at 120°C for 20h to obtain a VPO precursor. The VPO precursor was heated to 415 °C for 3 h in an atmosphere of 20% air / 20% nitrogen / 10% carbon dioxide / 50% water vapor by volume, and finally in an atmosphere of 40% nitroge...