CN110548375A - Preparation method and application of porous manganese oxide/cerium oxide composite sulfur dioxide removal material - Google Patents
Preparation method and application of porous manganese oxide/cerium oxide composite sulfur dioxide removal material Download PDFInfo
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- CN110548375A CN110548375A CN201910849297.1A CN201910849297A CN110548375A CN 110548375 A CN110548375 A CN 110548375A CN 201910849297 A CN201910849297 A CN 201910849297A CN 110548375 A CN110548375 A CN 110548375A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/48—Sulfur compounds
- B01D53/50—Sulfur oxides
- B01D53/508—Sulfur oxides by treating the gases with solids
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
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- B01D2258/00—Sources of waste gases
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- B01D2258/012—Diesel engines and lean burn gasoline engines
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Abstract
The invention discloses a preparation method of a porous manganese oxide/cerium oxide composite sulfur dioxide removal material.
Description
The technical field is as follows:
The invention relates to the technical field of removal of sulfur dioxide in tail gas of diesel engines, in particular to a preparation method and application of a porous manganese oxide/cerium oxide composite material for removing sulfur dioxide.
background art:
The exhaust gas from diesel engines contains many harmful components, such as sulfur oxide (SO x) and nitrogen oxide (NO x), among which sulfur dioxide (SO 2) is a very harmful gas in the exhaust gas from diesel engines, and the exhaust gas is harmful to human health and causes environmental pollution.
The conventional metal oxide SO 2 removing material has the defects of slow SO 2 removing rate, low SO 2 removing capacity and the like, and cannot be effectively applied to the removal of SO 2 under the working condition of the tail gas of a diesel engine.
The invention content is as follows:
the invention aims to provide a preparation method of a porous manganese oxide/cerium oxide composite sulfur dioxide removal material aiming at the defects of the prior art, manganese oxide and cerium oxide are compounded by adopting a template method to form a porous structure, so that the manganese oxide/cerium oxide composite sulfur dioxide removal material with high active components, large specific surface area and ordered porous structure is obtained, and the performance of removing sulfur dioxide in diesel engine tail gas is improved.
The invention is realized by the following technical scheme:
a porous manganese oxide/cerium oxide composite sulfur dioxide removal material is marked as Mn 1-y Ce y O x, wherein y is the mole percentage of Ce in the sum of Mn and Ce, the y value is between 0.05 and 0.95, x refers to the number of oxygen atoms, the x value is between 1.0 and 2.0, manganese oxide and cerium oxide are compounded by adopting a template method to form a porous structure, and the preparation method comprises the following steps:
1) respectively dissolving manganese nitrate and cerium nitrate in ethanol or water to prepare a solution with the total concentration of Mn and Ce ions of 0.8-1.3mol/L and the molar percentage of Ce in the total of Mn and Ce being y;
2) Taking a molecular sieve capable of being dissolved in an alkaline solution, pretreating for 5-10 hours at 80-110 ℃ in a vacuum environment to obtain a pretreated molecular sieve, and then putting the pretreated molecular sieve into a reaction container;
3) Uniformly dripping the solution obtained in the step 1) into the pretreated molecular sieve obtained in the step 2), wherein the solid-to-liquid ratio of the pretreated molecular sieve to the solution obtained in the step 1) is 1-2g/mL, then sealing by a preservative film, performing vacuum impregnation at normal temperature for 4-6 hours after ultrasonic oscillation for 20-40min, then performing vacuum drying at 60-100 ℃ for 2-3 hours, then performing roasting at 350-450 ℃ for 3-4 hours in an oxygen atmosphere, and naturally cooling after roasting;
4) then transferring the sample to a reaction container again, uniformly dripping the solution obtained in the step 1) again, and repeating the processes of dipping, drying and roasting once;
5) After roasting, adding alkali liquor to dissolve the molecular sieve in the sample, then filtering and washing with clear water until the filtrate is neutral (pH is 7), drying the washed sample at the temperature of 100 ℃ and 120 ℃, grinding after drying, and sieving particles with the particle size of less than 100 meshes to obtain the porous manganese oxide/cerium oxide composite sulfur dioxide removal material.
Preferably, the value of y is between 0.05 and 0.35.
the molecular sieve capable of being dissolved in the alkaline solution is preferably a KIT-6 molecular sieve.
the alkali liquor in the step 5) is preferably 2mol/L NaOH solution.
The obtained porous manganese oxide/cerium oxide composite sulfur dioxide removal material is black powder, the crystal structure mainly contains a characteristic peak of manganese oxide, the total body tends to an amorphous state, the material particles are arranged orderly, and the material has rich mesoporous pore channels and a small number of macroporous pore channels, the total pore volume is between 0.38cc/g and 0.75cc/g, the specific surface area is 150m2/g～170m2between/g, the sulfur dioxide removal performance is 450mgsulfur dioxide/gSulfur dioxide removal materialAbove, the sulfur dioxide removal performance is greatly higher than that of the conventional commercially purchased manganese oxide sulfur dioxide removal material.
The invention also protects the application of the porous manganese oxide/cerium oxide composite sulfur dioxide removal material for removing sulfur dioxide in the tail gas of a diesel engine, wherein the volume concentration range of SO 2 is 100-3000ppm, and the temperature range is 200-500 ℃.
Compared with the prior art, the invention has the following advantages:
The manganese oxide/cerium oxide composite sulfur dioxide removal material prepared by the invention has a larger specific surface area and a rich pore channel structure, the specific surface area of the porous manganese oxide/cerium oxide composite sulfur dioxide removal material is between 150m 2/g and 170m 2/g, the porous manganese oxide/cerium oxide composite sulfur dioxide removal material has a plurality of three-dimensional pore channels, the pore channel structure is regular and ordered, the internal pore channels are communicated with one another, the interconnected pore channel network structures can provide a better mass transfer effect and a larger contact area for gas-solid phase reaction, and the removal reaction of SO 2 is very facilitated.
hair brushThe sulfur dioxide removal performance of the porous manganese oxide/cerium oxide composite sulfur dioxide removal material prepared by the method is 450mgSulfur dioxide/gSulfur dioxide removal materialAbove, the sulfur dioxide removal performance is greatly higher than that of the conventional commercially purchased manganese oxide sulfur dioxide removal material.
Description of the drawings:
FIG. 1 is a transmission electron microscope and a scanning electron microscope photograph of the porous manganese oxide/cerium oxide composite sulfur dioxide-removing material prepared in example 1.
FIG. 2 is an X-ray diffraction pattern of the porous manganese oxide/cerium oxide composite desulphated material prepared in examples 1-3, manganese oxide (MnO x) and cerium oxide (CeO x) prepared in comparative examples 1-2.
FIG. 3 is a graph of pore size distribution and specific surface area parameters for the porous manganese oxide/cerium oxide composite sulfur dioxide removal material prepared in examples 1-3.
FIG. 4 is a comparison graph of sulfur dioxide removal performance of the porous manganese oxide/cerium oxide composite sulfur dioxide removal material.
FIG. 5 is a graph comparing the sulfur dioxide removal performance of the porous manganese oxide/cerium oxide composite sulfur dioxide removal material obtained in example 1 with that of the sulfur dioxide removal materials of comparative examples 1-2.
the specific implementation mode is as follows:
The following is a further description of the invention and is not intended to be limiting.
example 1:
A porous manganese oxide/cerium oxide composite sulfur dioxide removal material is marked as Mn 0.85 Ce 0.15 O x, wherein 0.15 is the mole percentage of Ce in the sum of Mn and Ce, x refers to the number of oxygen atoms and ranges from 1.0 to 2.0, and the preparation method comprises the following steps:
1) Respectively dissolving manganese nitrate and cerium nitrate in ethanol to prepare a solution with the total concentration of Mn and Ce ions of 1mol/L, Ce and the molar percentage of the Mn and Ce in the total sum of Mn and Ce of 0.15;
2) taking a KIT-6 molecular sieve, pretreating for 8 hours at 100 ℃ in a vacuum environment to obtain a pretreated molecular sieve, and then taking 1g of the pretreated molecular sieve to be put into a 5ml beaker;
3) Uniformly dripping 2ml of the solution obtained in the step 1) into the pretreated 1g of molecular sieve obtained in the step 2), sealing by using a preservative film, performing ultrasonic oscillation for 30min, performing vacuum impregnation at normal temperature for 5 hours, performing vacuum drying at 70 ℃ for 2 hours, performing roasting at 400 ℃ for 4 hours under oxygen atmosphere, and naturally cooling after roasting;
4) Then transferring the sample into a 5ml beaker again, uniformly dripping 1.5ml of the solution obtained in the step 1) again, and repeating the processes of dipping, drying and roasting once;
5) And after roasting, adding 2mol/L NaOH solution to dissolve the KIT-6 molecular sieve in the sample, then filtering, washing with clear water until the pH value of filtrate is 7, drying the washed sample at 110 ℃, drying, grinding, and sieving to obtain particles with the particle size of less than 100 meshes to obtain the porous manganese oxide/cerium oxide composite sulfur dioxide removal material.
Comparative example 1:
Porous manganese oxide (MnO x, where x denotes the number of oxygen atoms, ranging from 1.0 to 2.0).
The preparation method thereof is as in example 1 except that cerium nitrate is not added in step 1).
the preparation method comprises the following steps:
1) Dissolving manganese nitrate in ethanol to prepare a solution with the total Mn concentration of 1 mol/L;
2) taking a KIT-6 molecular sieve, pretreating for 8 hours at 100 ℃ in a vacuum environment to obtain a pretreated molecular sieve, and then taking 1g of the pretreated molecular sieve to be put into a 5ml beaker;
3) Uniformly dripping 2ml of the solution obtained in the step 1) into the pretreated 1g of molecular sieve obtained in the step 2), sealing by using a preservative film, performing ultrasonic oscillation for 30min, performing vacuum impregnation at normal temperature for 5 hours, performing vacuum drying at 70 ℃ for 2 hours, performing roasting at 400 ℃ for 4 hours under oxygen atmosphere, and naturally cooling after roasting;
4) Then transferring the sample into a 5ml beaker again, uniformly dripping 1.5ml of the solution obtained in the step 1) again, and repeating the processes of dipping, drying and roasting once;
5) And after roasting, adding 2mol/L NaOH solution to dissolve the KIT-6 molecular sieve in the sample, then filtering, washing with clear water until the pH value of filtrate is 7, drying the washed sample at 110 ℃, drying, grinding, and sieving to obtain particles with the particle size of less than 100 meshes to obtain the porous manganese oxide (MnO x) sulfur dioxide removal material.
Comparative example 2:
porous cerium oxide (CeO x where x denotes the number of oxygen atoms and ranges between 1.0 and 2.0).
the preparation process is as described in example 1, except that manganese nitrate is not added in step 1).
The preparation method comprises the following steps:
1) dissolving cerous nitrate in ethanol to prepare a solution with the total concentration of Ce ions being 1 mol/L;
2) taking a KIT-6 molecular sieve, pretreating for 8 hours at 100 ℃ in a vacuum environment to obtain a pretreated molecular sieve, and then taking 1g of the pretreated molecular sieve to be put into a 5ml beaker;
3) uniformly dripping 2ml of the solution obtained in the step 1) into the pretreated 1g of molecular sieve obtained in the step 2), sealing by using a preservative film, performing ultrasonic oscillation for 30min, performing vacuum impregnation at normal temperature for 5 hours, performing vacuum drying at 70 ℃ for 2 hours, performing roasting at 400 ℃ for 4 hours under oxygen atmosphere, and naturally cooling after roasting;
4) Then transferring the sample into a 5ml beaker again, uniformly dripping 1.5ml of the solution obtained in the step 1) again, and repeating the processes of dipping, drying and roasting once;
5) And after roasting, adding 2mol/L NaOH solution to dissolve the KIT-6 molecular sieve in the sample, then filtering, washing with clear water until the pH value of filtrate is 7, drying the washed sample at 110 ℃, drying, grinding, and sieving to obtain particles with the particle size of less than 100 meshes to obtain the porous cerium oxide sulfur dioxide removal material.
Example 2:
referring to example 1, except that, in step 1), manganese nitrate and cerium nitrate were dissolved in ethanol, respectively, to prepare a solution having a total Mn and Ce ion concentration of 1mol/L, Ce in terms of mole percentage of the sum of Mn and Ce of 0.25.
example 3:
Referring to example 1, except that, in step 1), manganese nitrate and cerium nitrate were dissolved in ethanol, respectively, to prepare a solution having a total Mn and Ce ion concentration of 1mol/L, Ce in terms of mole percentage of the sum of Mn and Ce of 0.05.
detection, analysis, characterization
Detecting, analyzing and characterizing the shape, color, components, physical and chemical structure, sulfur dioxide removal performance and other parameters of the prepared porous manganese oxide/cerium oxide composite sulfur dioxide removal material;
fig. 1 is a transmission electron microscope and a scanning electron microscope photo of the porous manganese oxide/cerium oxide composite sulfur dioxide removal material prepared in example 1, and fig. 1 shows that the porous manganese oxide/cerium oxide composite sulfur dioxide removal material has a plurality of three-dimensional ordered pore channels, the structure is very regular, and the pore channels are mutually communicated, SO that a good mass transfer effect and a large contact area can be provided for gas-solid phase reaction, and the removal of SO 2 is facilitated.
FIG. 2 is an X-ray diffraction pattern of the porous manganese oxide/cerium oxide composite desulfurized dioxide material prepared in examples 1 to 3 and the porous manganese oxide (MnO x) and the porous cerium oxide (CeO x) prepared in comparative examples 1 to 2, it can be seen that the porous manganese oxide/cerium oxide composite desulfurized dioxide material mainly exhibits a characteristic peak of MnO x in the crystal structure, but the characteristic peak intensity of MnO x is continuously decreased as the Ce content is increased, and the porous manganese oxide/cerium oxide composite desulfurized dioxide material is transformed to an amorphous form.
analyzing the specific surface area and the pore size distribution of the composite sulfur dioxide removal material by using a nitrogen adsorption/desorption instrument; FIG. 3 is a graph of pore size distribution and specific surface area parameters for the porous manganese oxide/cerium oxide composite sulfur dioxide removal material prepared in examples 1-3. It can be seen that the pore size distribution of the porous manganese oxide/cerium oxide composite sulfur dioxide removal material is mainly concentrated in mesoporous channels of about 8nm and 20nm and contains a certain number of macroporous channels. With the increase of the Ce content, the specific surface area of the porous manganese oxide/cerium oxide composite material is increased to a certain extent, but the increase is not large.
a thermal balance device is used for carrying out sulfur dioxide removal performance analysis on a composite material subjected to sulfur dioxide removal, about 10mg of a porous manganese oxide/cerium oxide (Mn 0.85 Ce 0.15 O x) composite material subjected to sulfur dioxide removal is added into a thermal balance crucible, then a reaction gas chamber is sealed, oxygen and nitrogen are adjusted by a flow controller to generate a mixed gas of O 2 and N 2 with the oxygen volume concentration of 5%, the mixed gas is introduced into the reaction gas chamber of the thermal gravimetric balance at the flow rate of 40ml/min to serve as a protective gas, the temperature is kept constant for 1h after the temperature is raised to 300 ℃, the flow controller of the nitrogen, the oxygen and the sulfur dioxide is adjusted to generate a mixed gas of SO 2 component concentration of 1000ppm, a mixed gas of SO 2, O 2 and N 2 with the oxygen volume concentration of 5%, the mixed gas is introduced into the reaction chamber of the thermal gravimetric balance at the flow rate of 40ml/min, when SO 2 in the gas is absorbed by the material subjected to sulfur dioxide removal, the sample mass changes, the weight change is analyzed to calculate the performance curve of the material subjected to the removal by absorbing SO 2, and the material subjected to obtain a high-manganese oxide removal performance analysis result that the composite material subjected to the manganese oxide removal of the manganese oxide removal performance analysis, and the performance analysis of the porous manganese oxide/sulfur dioxide removal of the composite material subjected to obtain a high-sulfur dioxide removal performance analysis, and the performance analysis of the high-sulfur dioxide removal performance analysis of the composite material, and the high-removal of the manganese oxide removal material, and the high-sulfur dioxide removal performance analysis of the manganese oxide removal material, and the high.
the porous manganese oxide (MnO x) prepared in comparative example 1 and the porous cerium oxide (CeO x) prepared in comparative example 2 were also tested using this test method to obtain their sulfur dioxide removal performance and compared to the sulfur dioxide removal performance of the porous manganese oxide/cerium oxide composite material obtained in example 1. referring to FIG. 5, the results show that the reaction rate of the SO 2 removal reaction is improved by the synergy of the manganese oxide and the cerium oxide.
And (4) conclusion: the obtained porous manganese oxide/cerium oxide composite sulfur dioxide removal material is black powder, the crystal structure mainly contains a characteristic peak of manganese oxide, the total body tends to an amorphous state, the material particles are arranged orderly, and the material has rich mesoporous pore channels and a small number of macroporous pore channels, the total pore volume is between 0.38cc/g and 0.75cc/g, the specific surface area is 150m2/g～170m2between/g, the sulfur dioxide removal performance is 450mgsulfur dioxide/gSulfur dioxide removal materialAbove, the sulfur dioxide removal performance is greatly higher than that of the conventional commercially purchased manganese oxide sulfur dioxide removal material. After the manganese oxide and the cerium oxide are compounded, the manganese oxide and the cerium oxide have synergistic effect, SO is improved2The reaction rate of the removal reaction.
Claims (6)
1. A porous manganese oxide/cerium oxide composite sulfur dioxide removal material is characterized by being marked as Mn 1-y Ce y O x, wherein y is the mole percentage of Ce in the sum of Mn and Ce, the y value is between 0.05 and 0.95, x refers to the number of oxygen atoms, the x value is between 1.0 and 2.0, manganese oxide and cerium oxide are compounded by adopting a template method, and a porous structure is formed, and the preparation method comprises the following steps:
1) respectively dissolving manganese nitrate and cerium nitrate in ethanol or water to prepare a solution with the total concentration of Mn and Ce ions of 0.8-1.3mol/L and the molar percentage of Ce in the total of Mn and Ce being y;
2) Taking a molecular sieve capable of being dissolved in an alkaline solution, pretreating for 5-10 hours at 80-110 ℃ in a vacuum environment to obtain a pretreated molecular sieve, and then putting the pretreated molecular sieve into a reaction container;
3) Uniformly dripping the solution obtained in the step 1) into the pretreated molecular sieve obtained in the step 2), wherein the solid-to-liquid ratio of the pretreated molecular sieve to the solution obtained in the step 1) is 1-2g/mL, then sealing by a preservative film, performing vacuum impregnation at normal temperature for 4-6 hours after ultrasonic oscillation for 20-40min, then performing vacuum drying at 60-100 ℃ for 2-3 hours, then performing roasting at 350-450 ℃ for 3-4 hours in an oxygen atmosphere, and naturally cooling after roasting;
4) Then transferring the sample to a reaction container again, uniformly dripping the solution obtained in the step 1) again, and repeating the processes of dipping, drying and roasting once;
5) After roasting, adding alkali liquor to dissolve the molecular sieve in the sample, then filtering and washing with clear water until the filtrate is neutral, drying the washed sample at the temperature of 100 ℃ and 120 ℃, grinding after drying, and sieving particles with the particle size smaller than 100 meshes to obtain the porous manganese oxide/cerium oxide composite sulfur dioxide removal material.
2. the composite sulfur dioxide removal material of claim 1, wherein y is between 0.05 and 0.35.
3. The composite sulfur dioxide removal material of claim 1 or 2, wherein the molecular sieve capable of dissolving in an alkaline solution is a KIT-6 molecular sieve.
4. The composite sulfur dioxide removing material of claim 1 or 2, wherein the alkali solution in the step 5) is 2mol/L NaOH solution.
5. The use of the porous manganese oxide/cerium oxide composite sulfur dioxide removal material as claimed in any one of claims 1 to 4, wherein the porous manganese oxide/cerium oxide composite sulfur dioxide removal material is used for removing sulfur dioxide in diesel engine exhaust.
6. the use according to claim 5, wherein the volume concentration of SO 2 in the diesel engine exhaust gas ranges from 100-3000ppm and the temperature range is 200-500 ℃.
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