CN111282578A - Metal-doped manganese-based low-temperature denitration catalyst and preparation method thereof - Google Patents
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Abstract
The invention discloses a metal-doped manganese-based low-temperature denitration catalyst and a preparation method thereof.
Description
Technical Field
The invention relates to a metal-doped manganese-based low-temperature denitration catalyst, and belongs to the field of atmospheric pollution control.
Background
The vanadium-titanium denitration catalyst is widely applied to a Selective Catalytic Reduction (SCR) technology to remove Nitrogen Oxides (NO) of atmospheric pollutants due to the advantages of high efficiency, stability and the likex) And the environmental quality is improved. However, the vanadium-titanium catalyst has the defects of narrow active temperature window (300 ℃ - & lt 400 ℃), dangerous waste of vanadium-based waste catalyst, environmental hazard and the like. With the change of the green transformation of the power generation structure and the change of the power consumption structure, the operation of the coal-fired unit under the conditions of low load and quick variable load becomes a normal state. Under the low-load condition, the inlet flue gas temperature of the denitration reactor cannot meet the design requirement, the exit probability of the denitration facility is increased, and the hidden trouble that the NOx emission concentration exceeds the standard is increased. In other industries, such as glass furnaces, steel, coking and the like, after the flue gas is subjected to heat recovery, desulfurization and other processes, the temperature of the flue gas is generally lower than 300 ℃, the vanadium-based catalyst is difficult to operate efficiently under the temperature condition, and the flue gas is reheated, so that the flue gas temperature meets the design condition of the vanadium-titanium catalyst and a large amount of energy is consumed. Therefore, low-temperature denitration becomes the current industrial flue gas NO removal methodxIs needed.
In recent years, transition metal oxides, such as MnOxThere is a great deal of interest in having optimal low temperature SCR performance. Patent ZL201010611242.6 provides a low-temperature flue gas denitration SCR catalyst, which is composed of a carrier, manganese oxide, and a composite oxide of one or more elements of Ce, Zr, Ti, Co, Fe, and Cu. ZL201010606894.0 provides a coprecipitation method for preparing a NOx low-temperature SCR catalyst Mn-Ce-M/TiO2Wherein M represents one or more elements of Fe, Co, Cu, Cr, Zr and Al. The invention ideas of the two patents are that different metal oxides are loaded on a carrier so as to improve the denitration performance of the carrier. There are major problems: (1) the materials prepared by the two patents are metal oxide composite materials, and have the disadvantages of complex preparation, difficult adjustment of proportioning, uncontrollable uniformity and complex energy band matching, which can cause the increase of the electron recombination rate and the reduction of the material performance; (2) both of these patents support different metal oxides on different supports without taking into account the fact thatIn application, the contribution of the carrier and the catalyst to the removal rate of the organic matters is realized, and the carrier does not really participate in the reaction process, so that the preparation cost of the material is increased; (3) from the mechanism point of view, different metal oxides are compounded with the carrier, the stability and the light corrosion performance of a single material of different metal oxides determine the stability of the final material, and the metal elements do not enter the crystal lattice of the carrier, do not change the structure of the material, and do not eliminate the barrier or defect between the two materials, so that the energy transfer efficiency between the materials is reduced.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a novel denitration catalyst with a carrier participating in reaction.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a single-metal-doped manganese-based low-temperature denitration catalyst is prepared by doping a transition metal element Co in a manganese-based catalyst; the molar ratio of the element Mn to the element Co in the raw materials for preparing the low-temperature denitration catalyst is 3: 2.
The low-temperature denitration catalyst is prepared from Mn (NO)3)2As a source of Mn, with Co (NO)3)2·6H2O is a Co source and is prepared by a citric acid complexation method; the Mn (NO)3)2Middle elements Mn and Co (NO)3)2·6H2The molar ratio of the element Co in O is 3: 2.
The low-temperature denitration catalyst is prepared by the following method:
(1) taking Mn (NO)3)2、Co(NO3)2·6H2Adding citric acid into the solution to dissolve the mixture in a proper amount of deionized water, stirring, and complexing to form a complexing solution I;
(2) drying the complexing solution I, and then baking to slowly decompose the citric acid to obtain a foam-shaped catalyst composite precursor I;
(3) roasting the composite precursor I at a high temperature for a certain time to obtain a low-temperature denitration catalyst CoMnOx。
Wherein the molar ratio of the addition amount of the citric acid in the step (1) to the total metal ions in the complexing solution I is 1: 1.
In the step (1), the stirring temperature is 20-30 ℃, and the stirring time is 30-60 min; in the step (2), the drying temperature is 100-120 ℃, the drying time is 30-60 min, the baking temperature is 150-180 ℃, and the baking time is 1-3 h; in the step (3), the roasting temperature is 300-500 ℃, and the roasting time is 1-5 h.
A bimetal co-doped manganese-based low-temperature denitration catalyst is a bimetal co-doped manganese-based catalyst BaCoMnOxThe catalyst is prepared by codoping a transition metal element Co and an alkaline earth metal element Ba in a manganese-based catalyst; the molar ratio of the element Mn to the element Co in the raw materials for preparing the low-temperature denitration catalyst is 3: 2; low-temperature denitration catalyst BaCoMnOxThe loading of medium BaO was 3 wt%.
Wherein the low-temperature denitration catalyst is Mn (NO)3)2As a source of Mn, with Co (NO)3)2·6H2O and Ba (NO)3)2Respectively Co source and Ba source, and is prepared by citric acid complexation method; mn (NO)3)2Middle elements Mn and Co (NO)3)2·6H2The molar ratio of the element Co in O is 3: 2.
The bimetal co-doped manganese-based low-temperature denitration catalyst is prepared by the following method:
(1) taking Mn (NO)3)2、Co(NO3)2·6H2Adding citric acid into the solution to dissolve the mixture in a proper amount of deionized water, stirring, and complexing to form a complexing solution I;
(2) adding hydrochloric acid into the complexing solution I, adjusting pH to acidity to prevent precipitation, and adding Ba source Ba (NO)3)2Stirring for a certain time, and complexing to form a complex solution II;
(3) drying the complexing solution II, and baking to slowly decompose the citric acid to obtain a foam-shaped catalyst composite precursor II;
(4) and roasting the composite precursor II at a high temperature for a certain time to obtain the low-temperature denitration catalyst.
Wherein, the molar ratio of the addition amount of the citric acid in the step (1) to the total metal ions in the complexing solution I is 1: 1; and (3) adjusting the pH value to 4-6 in the step (2).
In the step (1) and the step (2), the stirring temperature is 20-30 ℃, and the stirring time is 30-60 min; in the step (3), the drying temperature is 100-120 ℃, the drying time is 30-60 min, the baking temperature is 150-180 ℃, and the baking time is 1-3 h; in the step (4), the roasting temperature is 300-500 ℃, and the roasting time is 1-5 h.
Compared with the prior art, the invention has the following advantages:
(1) the invention discovers that the metal doping research on the manganese-based catalyst comprises the following steps: MnO inhibition when Ba is singly dopedxCatalytic performance of Co alone promoting MnOxThe catalytic performance of (a); when Ba and Co are doped together, the performance of the catalyst is improved to the maximum extent, and good water-resistant and sulfur-resistant performance is shown.
(2) The invention adopts bimetal co-doping: a solid solution is formed after Co doping, so that the catalyst has excellent oxidation-reduction performance; ba doping provides a new NO adsorption site for the catalyst, so that a new active nitrate adsorption species is formed, and the NO adsorption performance of the catalyst is remarkably promoted.
(3) The preparation method provided by the patent is simple, the reaction condition is mild, and the physical and chemical properties of the material can be regulated and controlled by changing the loading amounts of different metals, so that the performance of the material is improved.
Drawings
FIG. 1 is a graph showing the denitration performance of different catalysts varying with temperature;
FIG. 2 shows water vapor and SO2Graph of the effect on the activity of the catalyst;
fig. 3 is a graph showing the stability of the bimetal co-doped manganese-based catalyst prepared in example 1.
Detailed Description
The present invention will be described in detail with reference to specific examples.
Example 1 BaCoMnOxPreparation of (Ba Supported 1wt% BaO) catalyst
(1) 0.5 g Mn (NO) is weighed3)2、0.6 g Co(NO3)2·6H2Adding 1.0 g of citric acid into O, dissolving in 50 mL of deionized water, stirring for 30min at the temperature of 20 ℃, and complexing to form a complexing solution I;
(2) adding 5 mL hydrochloric acid into the complexing solution I, adjusting pH to acidity of 5 to prevent precipitation, and adding 0.01g Ba source Ba (NO)3)2Stirring for 30min at the temperature of 20 ℃ to form a complex solution II after complexing;
(3) drying the complexing solution II at the temperature of 120 ℃, and baking for 3 hours at the temperature of 180 ℃ to slowly decompose citric acid to obtain a foam-shaped catalyst composite precursor II;
(4) roasting the composite precursor II at 500 ℃ for 2h to obtain the metal co-doped catalyst BaCoMnOx。
Example 23 BaCoMnOxPreparation of (Ba-supporting amount of 3wt% BaO) catalyst
(1) 0.5 g Mn (NO) is weighed3)2、0.6 g Co(NO3)2·6H2Adding 1.0 g of citric acid into O, dissolving in 50 mL of deionized water, stirring for 30min at the temperature of 20 ℃, and complexing to form a complexing solution I;
(2) adding 5 mL hydrochloric acid into the complexing solution I, adjusting pH to acidic 5 to prevent precipitation, and adding 0.04 g Ba source Ba (NO)3)2Stirring for 30min at the temperature of 20 ℃ to form a complex solution II after complexing;
(3) drying the complexing solution II at the temperature of 120 ℃, and baking for 3 hours at the temperature of 180 ℃ to slowly decompose citric acid to obtain a foam-shaped catalyst composite precursor II;
(4) roasting the composite precursor II at 500 ℃ for 2h to obtain the metal co-doped catalyst BaCoMnOx。
Denitration efficiency: 3BaCoMnOx(Ba loading of 3wt% BaO) the catalytic efficiency in 33h test time is basically over 99%, and good water and sulfur resistant performance is shown in figure 3.
Example 35 BaCoMnOxPreparation of (Ba Supported 5wt% BaO) catalyst
(1) 0.5 g Mn (NO) is weighed3)2、0.6 g Co(NO3)2·6H2Adding 1.0 g of citric acid into the solution, dissolving the solution in 50 mL of deionized water, stirring the solution for 30min at the temperature of 20 ℃, and complexing to form a complex solution I;
(2) adding 5 mL hydrochloric acid into the complexing solution I, adjusting pH to acidity of 5 to prevent precipitation, and adding 0.07 g Ba source Ba (NO)3)2Stirring for 30min at the temperature of 20 ℃ to form a complex solution II after complexing;
(3) drying the complexing solution II at the temperature of 120 ℃, and baking for 3 hours at the temperature of 180 ℃ to slowly decompose citric acid to obtain a foam-shaped catalyst composite precursor II;
(4) roasting the composite precursor II at 500 ℃ for 2h to obtain a metal co-doped catalyst BaCoMnOx。
Example 4 preparation of MnOx catalyst
(1) 0.5 g Mn (NO) is weighed3)2Adding 0.6 g of citric acid, dissolving in 50 mL of deionized water, stirring for 30min at the temperature of 20 ℃, and complexing to form a complex solution I;
(2) drying the complexing solution I at the temperature of 120 ℃, and then baking for 3 hours at the temperature of 180 ℃ to slowly decompose citric acid to obtain a foam-shaped catalyst composite precursor II;
(3) roasting the composite precursor II at 500 ℃ for 2h to obtain the metal co-doped catalyst MnOx。
Example 5 preparation of a CoMnOx catalyst
(1) 0.5 g Mn (NO) is weighed3)2，0.6 g Co(NO3)2·6H2O, adding 1.0 g of citric acid and dissolving in 50 mL of deionized waterStirring for 30min at the temperature of 20 ℃, and complexing to form a complexing solution I;
(2) drying the complexing solution I at the temperature of 120 ℃, and then baking for 3 hours at the temperature of 180 ℃ to slowly decompose citric acid to obtain a foam-shaped catalyst composite precursor II;
(3) roasting the composite precursor II at 500 ℃ for 2h to obtain a metal co-doped catalyst CoMnOx。
Example 6 preparation of a BaMnOx catalyst
(1) 0.5 g Mn (NO) is weighed3)2Adding 0.6 g of citric acid, dissolving in 50 mL of deionized water, stirring for 30min at the temperature of 20 ℃, and complexing to form a complex solution I;
(2) adding 5 mL hydrochloric acid into the complexing solution I, adjusting pH to acidity of 5 to prevent precipitation, and adding 0.01g Ba source Ba (NO)3)2Stirring for 30min at the temperature of 20 ℃ to form a complex solution II after complexing;
(3) drying the complexing solution II at the temperature of 120 ℃, and baking for 3 hours at the temperature of 180 ℃ to slowly decompose citric acid to obtain a foam-shaped catalyst composite precursor II;
(4) roasting the composite precursor II at 500 ℃ for 2h to obtain a metal co-doped catalyst BaMnOx(Ba loading was 1wt% BaO).
Example 7 preparation of a BaCoOx catalyst
(1) 0.6 g of Co (NO) is weighed3)2·6H2O, adding 0.4 g of citric acid, dissolving in 50 mL of deionized water, stirring for 30min at the temperature of 20 ℃, and complexing to form a complexing solution I;
(2) adding 5 mL hydrochloric acid into the complexing solution I, adjusting pH to acidity of 5 to prevent precipitation, and adding 0.01g Ba source Ba (NO)3)2Stirring for 30min at the temperature of 20 ℃ to form a complex solution II after complexing;
(3) drying the complexing solution II at the temperature of 120 ℃, and baking for 3 hours at the temperature of 180 ℃ to slowly decompose citric acid to obtain a foam-shaped catalyst composite precursor II;
(4) roasting the composite precursor II at 500 ℃ for 2h to obtain a metal co-doped catalyst BaCoOx(Ba loading was 1wt% BaO).
Effects of the embodiment
As shown in FIG. 1, the incorporation of metal in a manganese-based catalyst, Ba alone suppressed MnOxCatalytic performance of Co alone promoting MnOxThe catalytic performance of (a); when Ba and Co are codoped, the performance of the catalyst is improved to the maximum extent, and the loading amount of Ba is 3wt% BaO (3 BaCoMnO)x) The best catalytic performance is achieved.
As shown in FIG. 2, water vapor and SO2Although the performance of the catalyst is affected to some extent, the catalyst 3BaCoMnO is comparatively speakingx(Ba loading of 3wt% BaO) still maintained the better catalytic performance.
Claims (10)
1. A metal-doped manganese-based low-temperature denitration catalyst is characterized in that: the low-temperature denitration catalyst is prepared by doping a transition metal element Co in a manganese-based catalyst; the molar ratio of the element Mn to the element Co in the raw materials for preparing the low-temperature denitration catalyst is 3: 2.
2. The low-temperature denitration catalyst according to claim 1, characterized in that: the low-temperature denitration catalyst is Mn (NO)3)2As a source of Mn, with Co (NO)3)2·6H2O is a Co source and is prepared by a citric acid complexation method; the Mn (NO)3)2Middle elements Mn and Co (NO)3)2·6H2The molar ratio of the element Co in O is 3: 2.
3. A metal-doped manganese-based low-temperature denitration catalyst is characterized in that: the low-temperature denitration catalyst is a bimetal co-doped manganese-based catalyst BaCoMnOxThe catalyst is prepared by codoping a transition metal element Co and an alkaline earth metal element Ba in a manganese-based catalyst; preparation raw material medium element of low-temperature denitration catalystThe molar ratio of the element Mn to the element Co is 3: 2; the low-temperature denitration catalyst BaCoMnOxThe loading of medium BaO was 3 wt%.
4. The metal-doped manganese-based low-temperature denitration catalyst according to claim 3, characterized in that: the low-temperature denitration catalyst is Mn (NO)3)2As a source of Mn, with Co (NO)3)2·6H2O and Ba (NO)3)2Respectively Co source and Ba source, and is prepared by citric acid complexation method; the Mn (NO)3)2Middle elements Mn and Co (NO)3)2·6H2The molar ratio of the element Co in O is 3: 2.
5. A method for producing the low-temperature denitration catalyst of claim 1 or 2, characterized in that: the low-temperature denitration catalyst is prepared by the following method:
(1) taking Mn (NO)3)2、Co(NO3)2·6H2Adding citric acid into the solution to dissolve the mixture in a proper amount of deionized water, stirring, and complexing to form a complexing solution I;
(2) drying the complexing solution I, and then baking to slowly decompose the citric acid to obtain a foam-shaped catalyst composite precursor I;
(3) roasting the composite precursor I at a high temperature for a certain time to obtain the low-temperature denitration catalyst CoMnOx。
6. The method according to claim 5, wherein: the molar ratio of the addition amount of the citric acid in the step (1) to the total metal ions in the complexing solution I is 1: 1.
7. The method according to claim 6, wherein: in the step (1), the stirring temperature is 20-30 ℃, and the stirring time is 30-60 min; in the step (2), the drying temperature is 100-120 ℃, the drying time is 30-60 min, the baking temperature is 150-180 ℃, and the baking time is 1-3 h; in the step (3), the roasting temperature is 300-500 ℃, and the roasting time is 1-5 h.
8. The method for preparing the low-temperature denitration catalyst according to claim 3 or 4, characterized in that: the low-temperature denitration catalyst is prepared by the following method:
(1) taking Mn (NO)3)2、Co(NO3)2·6H2Adding citric acid into the solution to dissolve the mixture in a proper amount of deionized water, stirring, and complexing to form a complexing solution I;
(2) adding hydrochloric acid into the complexing solution I, adjusting pH to acidity to prevent precipitation, and adding Ba source Ba (NO)3)2Stirring for a certain time, and complexing to form a complex solution II;
(3) drying the complexing solution II, and baking to slowly decompose the citric acid to obtain a foam-shaped catalyst composite precursor II;
(4) and roasting the composite precursor II at a high temperature for a certain time to obtain the low-temperature denitration catalyst.
9. The method of claim 8, wherein: the molar ratio of the addition amount of the citric acid in the step (1) to the total metal ions in the complexing solution I is 1: 1; and (3) adjusting the pH value to 4-6 in the step (2).
10. The method of claim 9, wherein: in the step (1) and the step (2), the stirring temperature is 20-30 ℃, and the stirring time is 30-60 min; in the step (3), the drying temperature is 100-120 ℃, the drying time is 30-60 min, the baking temperature is 150-180 ℃, and the baking time is 1-3 h; in the step (4), the roasting temperature is 300-500 ℃, and the roasting time is 1-5 h.
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| CN113145126A (en) * | 2021-03-11 | 2021-07-23 | 中国科学院城市环境研究所 | Composite catalyst and preparation method and application thereof |
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