CN108479764B - Preparation and application of manganese oxide carbon composite catalyst material applied to low-temperature electrochemical catalytic denitration - Google Patents
Preparation and application of manganese oxide carbon composite catalyst material applied to low-temperature electrochemical catalytic denitration Download PDFInfo
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Abstract
The invention discloses preparation and application of a manganese oxide carbon composite catalyst material applied to low-temperature electrochemical catalytic denitration, belongs to the field of cross catalysis chemistry and electrochemistry, and aims to solve the problems of preparation of a composite catalyst material capable of efficiently converting nitrogen oxide and application of efficient electrochemical catalytic degradation of nitrogen oxide in a low-temperature environment. Potassium permanganate is used as a manganese source, deionized water and absolute ethyl alcohol are used as mixed solvents, a manganese oxide precursor is obtained through stirring, a carbon source is added, and the Mn-containing manganese oxide is prepared through solvothermal reaction3O4a/C composite catalyst material. The preparation method has high yield at low temperature and the prepared Mn3O4the/C composite catalyst material has uniform component distribution, is a catalyst material for degrading nitrogen oxides by high-efficiency low-temperature electrochemical catalysis, and can be widely applied to the fields of industrial production of cement, steel and the like, thermal power generation, removal of nitrogen oxides in tail gas of motor vehicles and the like.
Description
Technical Field
The invention belongs to the field of catalytic chemistry and electrochemistry, and particularly relates to preparation of a composite catalyst material for efficiently converting nitrogen oxides and application of the composite catalyst material in efficient electrochemical catalytic degradation of nitrogen oxides in a low-temperature (below 200 ℃) environment.
Technical Field
With the continuous improvement of the industrial level, fossil fuels (coal, petroleum and natural gas) are continuously combusted, which causes global energy crisis and environmental pollution, wherein the atmospheric pollution seriously threatens the aspects of human health, ecological environment and the like. National NO is known during the decade from 2000 to 2010xThe emission increases by 2.1 times, NO after 2009xHas already exceeded the SO discharge2During the 'twelve-five' period, the nitrogen oxides are formally listed as the assessment indexes of energy conservation and emission reduction, and the total emission control is started.
At present, the nitrogen oxide removal method mainly comprises solid adsorption, liquid absorption and NOxStorage reduction technology (NSR), NOxSelective Catalytic Oxidation (SCO), NOxSelective non-catalytic reduction (SNCR), NOxSelective Catalytic Reduction (SCR), NOxCatalytic decomposition, and the like. Wherein the adsorption and absorption methods have poor recycling property, complex post-treatment, high operating cost and low nitrogen oxide removal efficiency. NSR is mainly applied to motor vehicle exhaust treatment, and SNCR does not need a catalyst but has high reaction temperature (>900 ℃), the reducing agent is easy to pyrolyze, and the denitration efficiency is reduced. SCO technology for converting NO into NO2And the wet method is realized for desulfurization and denitration at the same time, but the catalyst is limited in many aspects and is difficult to popularize in the industry. SCR technology is a denitration method widely applied in recent years, the reaction temperature is reduced by a lot compared with SNCR, but the catalyst in the SCR technology is possibly poisoned when contacting with other components in flue gas, and the catalytic reaction is influenced. NOxCatalytic decomposition is an ideal way to deal with NO, and the reaction is thermodynamically feasible, but the activation energy of the reaction is high, and NO catalyst suitable for the application has been found so far.
Compared with the conventional catalytic reaction, the electrochemical catalytic reaction has the function of electron migration and the function of catalyzing chemical reaction, and molecules or ions participating in the electrochemical catalytic reaction have obvious activation effect under the action of electric field force. Electrochemical catalytic decomposition of NOxAnd a reducing agent is not used, ammonia nitrogen pollution is avoided, the storage and the entry of the reducing agent into a system can be omitted, and a new idea is developed for the treatment of atmospheric pollutants.
Disclosure of Invention
The invention aims to provide a manganese oxide carbon composite catalyst material for efficiently completing electrochemical catalytic degradation of nitrogen oxides in a low-temperature environment. The preparation method has high yield and is convenient for large-scale preparation. The catalyst has the characteristics of low application temperature of less than 200 ℃, high degradation rate of nitrogen oxides and suitability for removing the nitrogen oxides in low-temperature environment.
A preparation method of a manganese oxide carbon composite catalyst material for efficiently completing electrochemical catalytic degradation of nitrogen oxides in a low-temperature environment is characterized by comprising the following steps of: the material is made of Mn3O4The composite catalyst comprises two components C, wherein the mass percentage of C in the composite catalyst material is 70-95%, and the specific steps are as follows:
(1) potassium permanganate is taken as a manganese source, dissolved in 30-50 ml of deionized water solvent, and stirred until the potassium permanganate is completely dissolved. The adding amount of the manganese source is 0.0655-0.393 mol/L.
(2) And adding an absolute ethyl alcohol solution serving as a reducing agent and a second solvent into the prepared purple black solution, and magnetically stirring at a constant speed until the purple red disappears to obtain a brown suspension. The addition amount of the absolute ethyl alcohol is 40-80 ml.
(3) Adding a carbon source into the solution prepared in the step (2), and strongly stirring until the carbon source is fully dissolved. The adding amount of the carbon source is 80-95% of the mass of the mangano-manganic oxide generated by the manganese source theory.
(4) The solution was transferred to a 200ml hydrothermal kettle with a polytetrafluoroethylene liner and subjected to solvothermal reaction in a thermostat at a certain temperature.
(5) Washing and filtering the brownish black solid prepared in the step (4) for multiple times by using ethanol and deionized water, putting the brownish black solid into an oven at 80 ℃ for air blast drying for 8 hours, and then drying the brownish black solid in vacuum for 4 hours, wherein the brown black solid can be prepared byObtaining Mn3O4a/C composite material.
The deionized water solvent in the step (1) is polyvinylpyrrolidone (PVP, K50) as an auxiliary template agent, and the addition amount of PVP is 0-0.05 g/ml.
The absolute ethyl alcohol solution in the step (2) takes Cetyl Trimethyl Ammonium Bromide (CTAB) as an auxiliary template agent,
CTAB is added in an amount of 0-100 mmol/L.
The carbon source in the step (3) is active carbon particles (30-40 meshes), active carbon powder (200 meshes), short carbon fibers (10mm) and carbon fiber powder (200 meshes).
The solvothermal reaction condition in the step (4) is that the reaction time is 2-16 h, and the reaction temperature is 120-180 ℃.
The method comprises the steps of taking potassium permanganate as a manganese source, taking deionized water and absolute ethyl alcohol as a mixed solvent, stirring to obtain a manganese oxide precursor, adding a carbon source, fully mixing, and performing solvothermal reaction to prepare the manganese-containing manganese oxide3O4the/C composite material is used as a catalyst for electrochemical catalytic degradation of nitrogen oxides. Under the action of the catalyst material, the conversion rate of nitrogen oxide is high, and the use temperature of electrochemical catalytic reaction is low (lower than 200 ℃). The method has high yield at low temperature and the prepared Mn3O4the/C composite catalyst material has uniform component distribution, is a catalyst material for degrading nitrogen oxides by high-efficiency low-temperature electrochemical catalysis, and can be widely applied to the fields of industrial production of cement, steel and the like, thermal power generation, removal of nitrogen oxides in tail gas of motor vehicles and the like.
Drawings
FIG. 1 shows Mn obtained in example 13O4The nitrogen adsorption and desorption curve of the active carbon particle composite material.
FIG. 2 shows Mn in example 13O4Scanning electron microscope photos of the/active carbon particle composite material.
FIG. 3 shows Mn in example 13O4Nitrogen oxide conversion rate curve under the action of the active carbon particle composite material.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to limit the scope of the invention:
example 1:
weighing 0.012mol of potassium permanganate, dissolving in 40ml of deionized water, and stirring until the potassium permanganate is completely dissolved; 60mL of absolute ethyl alcohol is added, the purple red color is completely disappeared by stirring, 17.39g of activated carbon particles are added, the stirring is continued for 2 hours, the obtained brown suspension containing the particles is transferred to a 200mL hydrothermal kettle with a polytetrafluoroethylene inner liner, and the hydrothermal treatment is carried out for 4 hours at a constant temperature of 160 ℃. Repeatedly centrifuging and cleaning the naturally cooled liquid with alcohol and deionized water for 3 times to obtain black brown particles, placing the black brown particles into an oven at 80 ℃ for air blast drying for 8 hours, then drying the black brown particles in vacuum for 4 hours, taking out the black brown particles, and cooling the black brown particles to room temperature to obtain Mn3O4Activated carbon particulate catalyst material. 3g of catalyst material is filled into a square tube type electrochemical catalytic reactor, two platinum electrodes with the diameter of 10 multiplied by 100mm are arranged on two sides of the square tube, the top end is a mixed simulated flue gas inlet with the diameter of 11 multiplied by 10mm, the tail end is a tail gas outlet after catalytic reaction, and the whole reactor is arranged in a vertical tube type furnace. The simulated smoke component is O222.6 percent, 500-1000 ppm of NO, and 1900sccm of total gas flow by taking nitrogen as a carrier gas. The temperature of the tubular furnace is controlled in four temperature ranges of 20 ℃, 50 ℃, 100 ℃ and 150 ℃, 0-3V voltage is applied to the platinum electrode, the gas composition before and after the reaction is detected by a flue gas component analyzer, and the conversion rate of nitrogen oxides is calculated. The result shows that the conversion rate of nitrogen oxides under the action of the catalyst at 50 ℃ and 2.5V is up to 96.8%.
Example 2:
weighing 0.012mol of potassium permanganate, dissolving in 40ml of deionized water solution containing polyvinylpyrrolidone (PVP content is 0.02g/ml), and stirring until the potassium permanganate is completely dissolved; 60mL of absolute ethyl alcohol is added, the purple red color is completely disappeared by stirring, 17.39g of activated carbon particles are added, the stirring is continued for 2 hours, the obtained brown suspension containing the particles is transferred to a 200mL hydrothermal kettle with a polytetrafluoroethylene inner liner, and the hydrothermal treatment is carried out for 4 hours at a constant temperature of 160 ℃. Repeatedly centrifuging and cleaning the naturally cooled liquid with alcohol and deionized water for 3 times to obtain black brown particles, placing the black brown particles into an oven at 80 ℃ for air blast drying for 8 hours, then drying the black brown particles in vacuum for 4 hours, taking out the black brown particles, and cooling the black brown particles to room temperature to obtain Mn3O4Activated carbon particulate catalyst material. 3g of catalyst material is filled into a square tube type electrochemical catalytic reactor, two platinum electrodes with the diameter of 10 multiplied by 100mm are arranged on two sides of the square tube, the top end is a mixed simulated flue gas inlet with the diameter of 11 multiplied by 10mm, the tail end is a tail gas outlet after catalytic reaction, and the whole reactor is arranged in a vertical tube type furnace. The simulated smoke component is O222.6 percent, 500-1000 ppm of NO, and 1900sccm of total gas flow by taking nitrogen as a carrier gas. The temperature of the tubular furnace is controlled in four temperature ranges of 20 ℃, 50 ℃, 100 ℃ and 150 ℃, 0-3V voltage is applied to the platinum electrode, the gas composition before and after the reaction is detected by a flue gas component analyzer, and the conversion rate of nitrogen oxides is calculated. The result shows that the conversion rate of nitrogen oxides under the action of the catalyst at 100 ℃ and 2.5V is up to 92.7 percent.
Example 3:
weighing 0.012mol of potassium permanganate, dissolving in 40ml of deionized water, and stirring until the potassium permanganate is completely dissolved; adding 60mL of absolute ethyl alcohol of hexadecyl trimethyl ammonium bromide (CTAB adding amount is 50mmol/L), stirring until the mauve color disappears completely, adding 17.39g of activated carbon particles, continuing stirring for 2 hours, transferring the obtained brown suspension containing the particles into a 200mL hydrothermal kettle with a polytetrafluoroethylene ethylene lining, and carrying out hydrothermal treatment at constant temperature of 160 ℃ for 4 hours. Repeatedly centrifuging and cleaning the naturally cooled liquid with alcohol and deionized water for 3 times to obtain black brown particles, placing the black brown particles into an oven at 80 ℃ for air blast drying for 8 hours, then drying the black brown particles in vacuum for 4 hours, taking out the black brown particles, and cooling the black brown particles to room temperature to obtain Mn3O4Activated carbon particulate catalyst material. 3g of catalyst material is filled into a square tube type electrochemical catalytic reactor, two platinum electrodes with the diameter of 10 multiplied by 100mm are arranged on two sides of the square tube, the top end is a mixed simulated flue gas inlet with the diameter of 11 multiplied by 10mm, the tail end is a tail gas outlet after catalytic reaction, and the whole reactor is arranged in a vertical tube type furnace. The simulated smoke component is O222.6 percent, 500-1000 ppm of NO, and 1900sccm of total gas flow by taking nitrogen as a carrier gas. The temperature of the tubular furnace is controlled in four temperature ranges of 20 ℃, 50 ℃, 100 ℃ and 150 ℃, 0-3V voltage is applied to the platinum electrode, the gas composition before and after the reaction is detected by a flue gas component analyzer, and the conversion rate of nitrogen oxides is calculated. The result shows that nitrogen is oxidized under the action of the catalyst at 100 ℃ and 2.5V voltageThe conversion of the product is up to 90.5%.
Example 4:
weighing 0.012mol of potassium permanganate, dissolving in 40ml of deionized water, and stirring until the potassium permanganate is completely dissolved; adding 60mL of absolute ethyl alcohol, stirring until the purple red color disappears completely, adding 17.39g of short carbon fibers, continuing stirring for 2 hours, transferring the obtained brown suspension containing the particles into a 200mL hydrothermal kettle with a polytetrafluoroethylene inner liner, and carrying out hydrothermal treatment at a constant temperature of 160 ℃ for 4 hours. Repeatedly centrifuging and cleaning the naturally cooled liquid with alcohol and deionized water for 3 times to obtain black brown particles, placing the black brown particles into an oven at 80 ℃ for air blast drying for 8 hours, then drying the black brown particles in vacuum for 4 hours, taking out the black brown particles, and cooling the black brown particles to room temperature to obtain Mn3O4A chopped carbon fiber catalyst material. 1.5g of catalyst material is filled into a square tube type electrochemical catalytic reactor, two platinum electrodes with the diameter of 10 multiplied by 100mm are arranged on two sides of the square tube, the top end is a mixed simulated flue gas inlet with the diameter of 11 multiplied by 10mm, the tail end is a tail gas outlet after catalytic reaction, and the whole reactor is arranged in a vertical tube type furnace. The simulated smoke component is O222.6 percent, 500-1000 ppm of NO, and 1900sccm of total gas flow by taking nitrogen as a carrier gas. The temperature of the tubular furnace is controlled in four temperature ranges of 20 ℃, 50 ℃, 100 ℃ and 150 ℃, 0-2.5V voltage is applied to the platinum electrode, the gas composition before and after the reaction is detected by a flue gas component analyzer, and the conversion rate of nitrogen oxides is calculated. The result shows that the conversion rate of nitrogen oxides under the action of the catalyst at 50 ℃ and 2V is up to 62.4%.
Example 5:
weighing 0.012mol of potassium permanganate, dissolving in 40ml of deionized water, and stirring until the potassium permanganate is completely dissolved; adding 60mL of absolute ethyl alcohol, stirring until the purple red color disappears completely, adding 8.238g of activated carbon particles, stirring for 2 hours, transferring the obtained brown suspension containing the particles into a 200mL hydrothermal kettle with a polytetrafluoroethylene ethylene lining, and carrying out hydrothermal treatment at a constant temperature of 160 ℃ for 4 hours. Repeatedly centrifuging and cleaning the naturally cooled liquid with alcohol and deionized water for 3 times to obtain black brown particles, placing the black brown particles into an oven at 80 ℃ for air blast drying for 8 hours, then drying the black brown particles in vacuum for 4 hours, taking out the black brown particles, and cooling the black brown particles to room temperature to obtain Mn3O4Activated carbon particulate catalyst material. 3g of the catalyst material was filled in a square tubeThe electrochemical catalytic reactor has two platinum electrodes of 10X 100mm on two sides of the square tube, mixed simulated fume inlet of 11X 10mm in the top and catalytic tail gas outlet in the tail, and the reactor is set inside the vertical tube furnace. The simulated smoke component is O222.6 percent, 500-1000 ppm of NO, and 1900sccm of total gas flow by taking nitrogen as a carrier gas. The temperature of the tubular furnace is controlled in four temperature ranges of 20 ℃, 50 ℃, 100 ℃ and 150 ℃, 0-5V voltage is applied to the platinum electrode, the gas composition before and after the reaction is detected by a flue gas component analyzer, and the conversion rate of nitrogen oxides is calculated. The result shows that the conversion rate of nitrogen oxides under the action of the catalyst reaches up to 84.5 percent at 100 ℃ and 4.0V.
Example 6:
weighing 0.012mol of potassium permanganate, dissolving in 40ml of deionized water, and stirring until the potassium permanganate is completely dissolved; adding 60mL of absolute ethyl alcohol, stirring until the purple red color disappears completely, adding 17.39g of activated carbon particles, continuing stirring for 2 hours, transferring the obtained brown suspension containing the particles into a 200mL hydrothermal kettle with a polytetrafluoroethylene ethylene lining, and carrying out hydrothermal treatment at a constant temperature of 120 ℃ for 4 hours. Repeatedly centrifuging and cleaning the naturally cooled liquid with alcohol and deionized water for 3 times to obtain black brown particles, placing the black brown particles into an oven at 80 ℃ for air blast drying for 8 hours, then drying the black brown particles in vacuum for 4 hours, taking out the black brown particles, and cooling the black brown particles to room temperature to obtain Mn3O4Activated carbon particulate catalyst material. 3g of catalyst material is filled into a square tube type electrochemical catalytic reactor, two platinum electrodes with the diameter of 10 multiplied by 100mm are arranged on two sides of the square tube, the top end is a mixed simulated flue gas inlet with the diameter of 11 multiplied by 10mm, the tail end is a tail gas outlet after catalytic reaction, and the whole reactor is arranged in a vertical tube type furnace. The simulated smoke component is O222.6 percent, 500-1000 ppm of NO, and 1900sccm of total gas flow by taking nitrogen as a carrier gas. The temperature of the tubular furnace is controlled in four temperature ranges of 20 ℃, 50 ℃, 100 ℃ and 150 ℃, 0-3V voltage is applied to the platinum electrode, the gas composition before and after the reaction is detected by a flue gas component analyzer, and the conversion rate of nitrogen oxides is calculated. The result shows that the conversion rate of nitrogen oxides under the action of the catalyst at 50 ℃ and 2.5V is up to 76.8 percent.
Claims (4)
1. Application toThe preparation method of the manganese oxide carbon composite catalyst material for low-temperature electrochemical catalytic denitration is characterized by comprising the following steps of: the composite catalyst material is made of Mn3O4The composite catalyst material comprises two components C, wherein the mass percentage of C in the composite catalyst material is 70-95%, and the process comprises the following steps:
(1) dissolving potassium permanganate serving as a manganese source in 30-50 ml of deionized water solvent, and stirring until the potassium permanganate is completely dissolved, wherein the addition amount of the manganese source is 0.0655-0.393 mol/L;
(2) adding an absolute ethanol solution serving as a reducing agent and a second solvent into the prepared purple black solution by taking Cetyl Trimethyl Ammonium Bromide (CTAB) as an auxiliary template agent, and magnetically stirring at a constant speed until the purple red disappears to obtain a brown suspension; the addition amount of the absolute ethyl alcohol is 40-80 ml, and the addition amount of CTAB is 0-100 mmol/L;
(3) adding a carbon source into the solution prepared in the step (2), and strongly stirring until the carbon source is fully dissolved; the adding amount of the carbon source is 80-95% of the mass of the mangano-manganic oxide generated by the manganese source theory;
(4) transferring the solution into a 200ml hydrothermal kettle with a polytetrafluoroethylene lining, and carrying out solvothermal reaction in a constant temperature box at a certain temperature;
(5) washing and filtering the brownish black solid prepared in the step (4) for multiple times by using ethanol and deionized water, putting the brownish black solid into an oven at 80 ℃ for air blast drying for 8 hours, and then drying the brownish black solid in vacuum for 4 hours to obtain Mn3O4a/C composite material.
2. The preparation method of the manganese oxide-carbon composite catalyst material applied to low-temperature electrochemical catalytic denitration according to claim 1, characterized by comprising the following steps: the deionized water solvent in the step (1) is obtained by taking polyvinylpyrrolidone (PVP) as an auxiliary template agent, dissolving 30-50 ml of deionized water with the PVP type K50, and stirring until the PVP is completely dissolved; wherein the addition amount of PVP is 0-0.05 g/ml.
3. The preparation method of the manganese oxide-carbon composite catalyst material applied to low-temperature electrochemical catalytic denitration according to claim 1, characterized by comprising the following steps: the carbon source in the step (3) is 30-40 mesh active carbon particles, 200 mesh active carbon powder, 10mm short carbon fibers and 200 mesh carbon fiber powder.
4. The preparation method of the manganese oxide-carbon composite catalyst material applied to low-temperature electrochemical catalytic denitration according to claim 1, characterized by comprising the following steps: the solvothermal reaction condition in the step (4) is that the reaction time is 2-16 h, and the reaction temperature is 120-180 ℃.
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| CN107170982A (en) * | 2017-04-14 | 2017-09-15 | 西北工业大学 | The preparation method of lithium ion battery carbon coating mangano-manganic oxide polyhedron negative material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2792622C1 (en) * | 2022-07-19 | 2023-03-22 | Федеральное государственное бюджетное учреждение науки Институт химии твердого тела Уральского отделения Российской академии наук | Method of obtaining composite mn3o4/c |
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