Fe-modified nano manganese oxide/MIL-125 (Ti) catalyst and preparation method thereof

Abstract

The invention belongs to the technical field of composite material preparation, and particularly relates to a Fe-modified nano manganese oxide / MIL-125 (Ti) catalyst and a preparation method thereof. The preparation method comprises the following steps: A, ultrasonically mixing MnSO4, NaClO3 and NaCl in deionized water; adding ferric trichloride hexahydrate for ultrasonic treatment; then dropwise adding concentrated sulfuric acid into the solution under the condition of ice bath stirring, and reacting in a reaction kettle; B, centrifugally washing the precipitate with absolute ethyl alcohol anddeionized water, drying, grinding, and calcining in a muffle furnace to obtain iron modified nano MnOx; C, after DMSO and C3H8O are mixed, adding 1, 3, 5-BTC and nano MnOx for ultrasonic treatment, and then dropwise adding C12H28O4Ti during stirring at the room temperature; putting the solution into a reaction kettle to react; and finally, centrifugally washing with isopropanol and water, and freeze-drying to obtain the composite catalyst. The composite catalyst provided by the invention can effectively reduce the conversion temperature of nitrogen oxides, improve the toxicity resistance andprolong the service life of the catalyst.

Description

technical field

[0001] The invention belongs to the technical field of composite material preparation, and in particular relates to an Fe-modified nano manganese oxide / MIL-125 (Ti) catalyst and a preparation method thereof. Background technique

[0002] In recent years, the problem of air pollution has become more and more serious. It has attracted great attention from government departments and the public. And set strict policy standards. Air pollutants in my country mainly come from the combustion process of fossil fuels such as coal and petroleum, so air pollutants include SO 2 , NOx, VOC, CO, PM2.5, etc. NOx is followed by dust, SO 2 Afterwards, the important emission reduction targets are largely due to the fact that NOx not only causes damage to the natural environment such as acid rain, photochemical smog, ozone layer destruction, and greenhouse effect, but also poses a threat to human health. The development of NOx control technology has a long history and can be...

Examples

Embodiment 1

[0024] Step 1: Add 0.01mol of MnSO 4 , 0.025mol of sodium chlorate NaClO 3 Dissolve 2.925g of NaCl in 50ml of deionized water, and mix well by ultrasonication for 5min; then add 0.135g of ferric chloride hexahydrate, and ultrasonicate again for 10min. Then, 8 ml of concentrated sulfuric acid was slowly dropped into the mixture under constant stirring in an ice bath to form a clear solution. After the dropwise addition was completed, it was put into a reaction kettle and reacted at 120° C. for 8 hours.

[0025] Step 2: After 8 hours, the precipitate of the solution was washed by centrifugation with absolute ethanol, and then with deionized water; and then dried in an oven at 70°C. After drying, it was put into a mortar and ground, then calcined in a muffle furnace at 400°C for 10 minutes, and then heated to 600°C at a rate of 8°C / min for 2h to obtain iron-doped modified nano-MnOx.

[0026] Step 3: Mix 42.5ml of DMSO and 15.3ml of C 3 h 8After O mixing, add 4.2 g of trimesi...

Embodiment 2

[0028] Step 1: Add 0.008mol of MnSO 4 , 0.032mol of sodium chlorate NaClO 3 Dissolve 4.69g of NaCl in 50ml of deionized water, and mix well by ultrasonication for 5min; then add 0.216g of ferric chloride hexahydrate, and ultrasonicate again for 10min. Then, 8.6 ml of concentrated sulfuric acid was slowly added dropwise with constant stirring in an ice bath to form a clear solution. After the dropwise addition was completed, it was put into a reaction kettle and reacted at 150° C. for 5 hours.

[0029] Step 2: Same as Step 2 in Example 1.

[0030] Step 3: Mix 56.7ml of DMSO and 11.5ml of C 3 h 8 After O mixing, 8.4g of trimesic acid (1,3,5-BTC) and 1.8g of modified nano-MnOx were added to the mixed solution, and the solute was evenly distributed by ultrasonication for 20min; then 1.5ml of tetraisopropyl titanic acid was added Ester (C 12 h 28 o 4 Ti), stirred at room temperature for 20 min. After stirring, the solution was transferred to a polytetrafluoroethylene linin...

Embodiment 3

[0032] Step 1: Add 0.01mol of MnSO 4 , 0.032mol of sodium chlorate NaClO 3 Dissolve 3.5g of NaCl in 50ml of deionized water, and mix well by ultrasonication for 5min; then add 0.2g of ferric chloride hexahydrate, and ultrasonicate again for 10min. Then, 9 ml of concentrated sulfuric acid was slowly added dropwise with constant stirring in an ice bath to form a clear solution. After the dripping is completed, put it into the reaction kettle and react at 140°C for 5.5h.

[0033] Step 2: Same as Step 2 in Example 1.

[0034] Step 3: Combine 50ml of DMSO and 14ml of C 3 h 8 After O mixing, add 6.3g of trimesic acid (1,3,5-BTC) and 1.5g of modified nano-MnOx into the mixed solution, and ultrasonically 20min to make the solute evenly distributed; then add 2ml of tetraisopropyl titanate (C 12 h 28 o 4 Ti), stirred at room temperature for 20 min. After stirring, the solution was transferred to a polytetrafluoroethylene lining, and reacted at 170° C. for 5 hours in a reaction ...

technical field

[0001] The invention belongs to the technical field of composite material preparation, and in particular relates to an Fe-modified nano manganese oxide / MIL-125 (Ti) catalyst and a preparation method thereof. Background technique

[0002] In recent years, the problem of air pollution has become more and more serious. It has attracted great attention from government departments and the public. And set strict policy standards. Air pollutants in my country mainly come from the combustion process of fossil fuels such as coal and petroleum, so air pollutants include SO 2 , NOx, VOC, CO, PM2.5, etc. NOx is followed by dust, SO 2 Afterwards, the important emission reduction targets are largely due to the fact that NOx not only causes damage to the natural environment such as acid rain, photochemical smog, ozone layer destruction, and greenhouse effect, but also poses a threat to human health. The development of NOx control technology has a long history and can be...

Examples

Embodiment 1

[0024] Step 1: Add 0.01mol of MnSO 4 , 0.025mol of sodium chlorate NaClO 3 Dissolve 2.925g of NaCl in 50ml of deionized water, and mix well by ultrasonication for 5min; then add 0.135g of ferric chloride hexahydrate, and ultrasonicate again for 10min. Then, 8 ml of concentrated sulfuric acid was slowly dropped into the mixture under constant stirring in an ice bath to form a clear solution. After the dropwise addition was completed, it was put into a reaction kettle and reacted at 120° C. for 8 hours.

[0025] Step 2: After 8 hours, the precipitate of the solution was washed by centrifugation with absolute ethanol, and then with deionized water; and then dried in an oven at 70°C. After drying, it was put into a mortar and ground, then calcined in a muffle furnace at 400°C for 10 minutes, and then heated to 600°C at a rate of 8°C / min for 2h to obtain iron-doped modified nano-MnOx.

[0026] Step 3: Mix 42.5ml of DMSO and 15.3ml of C 3 h 8After O mixing, add 4.2 g of trimesi...

Embodiment 2

[0028] Step 1: Add 0.008mol of MnSO 4 , 0.032mol of sodium chlorate NaClO 3 Dissolve 4.69g of NaCl in 50ml of deionized water, and mix well by ultrasonication for 5min; then add 0.216g of ferric chloride hexahydrate, and ultrasonicate again for 10min. Then, 8.6 ml of concentrated sulfuric acid was slowly added dropwise with constant stirring in an ice bath to form a clear solution. After the dropwise addition was completed, it was put into a reaction kettle and reacted at 150° C. for 5 hours.

[0029] Step 2: Same as Step 2 in Example 1.

[0030] Step 3: Mix 56.7ml of DMSO and 11.5ml of C 3 h 8 After O mixing, 8.4g of trimesic acid (1,3,5-BTC) and 1.8g of modified nano-MnOx were added to the mixed solution, and the solute was evenly distributed by ultrasonication for 20min; then 1.5ml of tetraisopropyl titanic acid was added Ester (C 12 h 28 o 4 Ti), stirred at room temperature for 20 min. After stirring, the solution was transferred to a polytetrafluoroethylene linin...

Embodiment 3

[0032] Step 1: Add 0.01mol of MnSO 4 , 0.032mol of sodium chlorate NaClO 3 Dissolve 3.5g of NaCl in 50ml of deionized water, and mix well by ultrasonication for 5min; then add 0.2g of ferric chloride hexahydrate, and ultrasonicate again for 10min. Then, 9 ml of concentrated sulfuric acid was slowly added dropwise with constant stirring in an ice bath to form a clear solution. After the dripping is completed, put it into the reaction kettle and react at 140°C for 5.5h.

[0033] Step 2: Same as Step 2 in Example 1.

[0034] Step 3: Combine 50ml of DMSO and 14ml of C 3 h 8 After O mixing, add 6.3g of trimesic acid (1,3,5-BTC) and 1.5g of modified nano-MnOx into the mixed solution, and ultrasonically 20min to make the solute evenly distributed; then add 2ml of tetraisopropyl titanate (C 12 h 28 o 4 Ti), stirred at room temperature for 20 min. After stirring, the solution was transferred to a polytetrafluoroethylene lining, and reacted at 170° C. for 5 hours in a reaction ...

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