CN109453758B - A kind of denitration catalyst and preparation method thereof - Google Patents
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Abstract
本发明公开了一种脱硝催化剂及其制备方法，所述方法包括埃洛石纳米管的纯化、埃洛石纳米管的表面修饰和活性组分的负载步骤，本发明开发了一种利用沉积沉淀法和溶胶‑凝胶法联合的技术手段，制备了以介孔CeO2改性的埃洛石纳米管为载体，以钒酸镁为活性组分的催化剂，该催化剂具有较高比表面积，其能在250~450oC范围内具有高的催化活性、反应稳定性及抗SO2中毒性能强。The invention discloses a denitration catalyst and a preparation method thereof. The method includes the purification of halloysite nanotubes, the surface modification of halloysite nanotubes and the loading of active components. The combined technical means of the sol-gel method and the sol-gel method has prepared a catalyst with mesoporous CeO 2 modified halloysite nanotubes as the carrier and magnesium vanadate as the active component. The catalyst has a high specific surface area and It has high catalytic activity, reaction stability and anti-SO 2 poisoning performance in the range of 250~450 o C.
Description
Technical Field
The invention belongs to the technical field of environmental catalysis, and particularly relates to a denitration catalyst and a preparation method thereof.
Background
With the rapid development of the scientific and technological level, people can fully utilize mineral resources such as coal, petroleum, natural gas and the like to enrich and improve the living standard of the people, and simultaneously, the use of fossil fuels can generate a large amount of harmful gases, so that the people face the increasingly serious problem of environmental pollution. Among many pollutants, nitrogen oxides in tail gas discharged by coal-fired power plants and industrial boilers are one of main atmospheric pollutants in China, and the existence of the pollutants causes great harm to human health and ecological environment. Industrial removal of NO from flue gasxThe most widely used denitration technique is NH3For the selective catalytic reduction of a reducing agent to N under the action of a catalyst2And NH of water3-the SCR technology,the catalyst is the core of this technology. The most widely commercialized one is V2O5-MO3/TiO2Or V2O5-WO3/TiO2The catalyst system has high reaction activity and good water and sulfur resistance. However, the active component V of the catalyst2O5High temperature easy sublimation causing harm to environment and human, and V2O5SO under the action of2Will be oxidized to SO3And further generating NH4HSO4And (NH)4)2SO4Causing problems of equipment corrosion, catalyst active site blockage and the like. Thus, novel active ingredients were developed to replace V partially or completely2O5And a catalyst system with a wide reaction temperature window and excellent reaction activity becomes a research hotspot.
Disclosure of Invention
The invention aims to provide a denitration catalyst and a preparation method thereof, and mesoporous CeO is prepared2The catalyst has a high specific surface area, and can have high catalytic activity, reaction stability and SO resistance within the temperature range of 250-450 DEG C2The poisoning performance is strong.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method of preparing a denitration catalyst, the method comprising the steps of:
(1) purifying the halloysite nanotubes: weighing a certain amount of halloysite nanotubes, adding the halloysite nanotubes into deionized water, stirring at the speed of 700rpm for 30min at room temperature, then dropwise adding nitric acid to adjust the pH value of the solution, continuously stirring for 1h, removing impurities on the surface and in the solution, filtering and washing to be neutral, drying at 110 ℃ for 12h, and finally roasting at 500 ℃ for 5h to obtain purified halloysite nanotubes;
(2) surface modification of halloysite nanotubes: adding the purified halloysite nanotube into deionized water, adding cerium salt, urea and CTAB, stirring at room temperature for 30min, and stirring at 90 deg.C for 1Cooling to room temperature after 2h, filtering, washing, drying at 110 deg.C for 12h, and calcining at 500 deg.C for 5h to obtain mesoporous CeO2A modified halloysite nanotube;
(3) loading of active components: mixing and stirring a certain amount of vanadium acetylacetonate, magnesium acetylacetonate, acetylacetone and absolute ethyl alcohol uniformly, then adding a certain amount of mesoporous CeO2The modified halloysite nanotube is prepared by mixing the mixture at 40-60%oC, refluxing for 12-18 h under the water bath condition, and then subjecting the obtained product to 500oAnd C, roasting for 5 hours, cooling to room temperature to obtain solid powder, and finally tabletting and forming to obtain the denitration catalyst.
And (2) dropwise adding nitric acid in the step (1) to adjust the pH value of the solution to 3.9-4.2, wherein the pH value of the mixed solution is not too high or too low in the treatment process, the impurities on the surface and inside of the halloysite nanotube are not easily removed due to too high pH value, and the part of the halloysite nanotube is partially dissolved due to too low pH value to damage the structure of the halloysite nanotube.
The mass ratio of the halloysite nanotubes to the deionized water in the step (1) is 1: 5-1: 10.
In the step (2), the cerium salt is one or a mixture of cerium nitrate and cerium sulfate.
The mass ratio of the halloysite nanotubes to the deionized water after purification in the step (2) is 1: 5-1: 10, the mass ratio of the halloysite nanotubes to the cerium salt is 1: 0.1-1: 0.25, the molar ratio of urea to the cerium salt is 10:1, and the mass ratio of CTAB to the cerium salt is 1: 10-1: 20.
In the step (2), the addition amount of acetylacetone is 4 times of the sum of the molar amounts of vanadium acetylacetonate and magnesium acetylacetonate, the addition amount of anhydrous ethanol is 5 times of the sum of the molar amounts of vanadium acetylacetonate and magnesium acetylacetonate, respectively, and the molar ratio of vanadium acetylacetonate to magnesium acetylacetonate is 2: 1.
In the step (2), vanadium acetylacetonate and mesoporous CeO2The mass ratio of the modified halloysite nanotubes is 1: 100-1: 50.
The denitration catalyst prepared by the preparation method has higher specific surface area which is 200-300m2In,/g, and can be inHigh catalytic activity, reaction stability and SO resistance in the temperature range of 250-450 DEG C2The poisoning performance is strong.
Compared with the prior art, the invention has the main advantages that:
(1) on one hand, the hydroxyl on the surface of the halloysite can provide an acidic active site under certain conditions, so that the adsorption of ammonia gas can be enhanced; in addition, when the catalyst is used as a catalyst carrier, the active component can be fixed on the surface of the halloysite or in the halloysite by the nanometer tubular cavity structure of the halloysite, so that reactant molecules can penetrate through the tubular cavity to be contacted with active sites, and the catalytic selectivity is improved; on the other hand, the nano-scale tube cavity structure loaded with the catalyst has small obstruction to the migration of reactants, is beneficial to the acceleration of reaction speed, has negative charges, and can uniformly load most of active components or modification layers on halloysite, thereby overcoming the agglomeration phenomenon of the catalyst, leading the catalyst to be fully contacted with the reactants, and improving the reaction activity and the stability of the catalyst.
(2) The urea is taken as a precipitator, and the cerium dioxide is loaded on the surface of the carrier by means of deposition precipitation, SO that the specific surface area of the carrier can be increased to be beneficial to the uniform dispersion of the active components, and the SO in the reaction atmosphere can be prevented2The corrosion to the catalyst carrier and the active components in the pipe cavity is further improved, and the water resistance and the sulfur resistance of the catalyst are further improved.
(3) MgV prepared by sol-gel method2O7As an active component, on one hand, the stability of the catalyst can be improved, so that vanadium-containing species are not easy to sublimate, further the harm of the catalyst to the environment in the use process is reduced, and on the other hand, the active component can be combined with a modification layer CeO2A synergistic effect occurs to increase the reactivity of the catalyst.
(4) The catalyst is prepared by CeO2The modified halloysite nanotube is used as a carrier, and active components can be dispersed on the surface and inside a tube cavity to form a double-layer active component, so that the corrosion of the formed ammonium sulfate to the inside can be limited, and the high reaction activity and the sulfur resistance stability are kept.
Detailed Description
In order to facilitate an understanding of the present invention, the following examples are provided to further illustrate the present invention, but are not intended to limit the scope of the present invention.
Example 1
(1) Purification of halloysite nanotubes
Weighing 20g of halloysite nanotubes, adding the halloysite nanotubes into 100mL of ionized water, stirring the mixture at the speed of 700rpm for 30min at room temperature, then dropwise adding a certain amount of nitric acid into the mixture to adjust the pH value of the solution to 3.9, continuing stirring the solution for 1h to remove impurities on the surface and the inside, filtering the mixture, washing the mixture to be neutral, drying the mixture at 110 ℃ for 12h, and finally roasting the mixture at 500 ℃ for 5 h.
(2) Surface modification of halloysite nanotubes comprises adding purified halloysite nanotubes into deionized water, adding cerium nitrate and urea
And CTAB is stirred for 30min at room temperature, then transferred to 90 ℃ to be continuously stirred for 12h, and then cooled to room temperature. Filtering and washing the product, drying at 110 deg.C for 12 hr, and roasting at 500 deg.C for 5 hr to obtain mesoporous CeO2Modified halloysite nanotubes. Wherein the mass volume ratio of the halloysite nanotubes to the deionized water is 1:5, and the mass ratio of the halloysite nanotubes to the cerium nitrate is 1:0.1, the molar ratio of urea to cerium nitrate is 10:1, and the mass ratio of CTAB to cerium nitrate is 1: 10.
(3) Loading of active ingredients
Mixing and stirring a certain amount of vanadium acetylacetonate, magnesium acetylacetonate, acetylacetone and absolute ethyl alcohol, and adding a certain amount of mesoporous CeO2Modified halloysite nanotubes by mixing the mixture at 40oAnd C, refluxing for 18h under the condition of water bath. The product obtained is purified at 500oAnd C, roasting for 5 hours, cooling to room temperature to obtain solid powder, tabletting and forming the solid powder, and finally screening a 40-60-mesh sample for activity evaluation. In the preparation process, the adding amount of acetylacetone is respectively 4 times of the sum of the molar amounts of vanadium acetylacetonate and magnesium acetylacetonate, the adding amount of anhydrous ethanol is respectively 5 times of the sum of the molar amounts of vanadium acetylacetonate and magnesium acetylacetonate, and the molar ratio of vanadium acetylacetonate to magnesium acetylacetonate is2:1, vanadium acetylacetonate and mesoporous CeO2The mass ratio of the modified halloysite nanotubes is 1: 100.
Example 2
(1) Purification of halloysite nanotubes
Weighing 20g of halloysite nanotubes, adding the halloysite nanotubes into 200mL of deionized water, stirring the mixture at the speed of 700rpm for 30min at room temperature, then dropwise adding a certain amount of nitric acid into the mixture to adjust the pH value of the solution to 4.2, continuing stirring the solution for 1h to remove impurities on the surface and the inside of the solution, filtering the mixture, washing the mixture to be neutral, drying the mixture at 110 ℃ for 12h, and finally roasting the mixture at 500 ℃ for 5 h.
(2) Surface modification of halloysite nanotubes comprises adding purified halloysite nanotubes into deionized water, adding cerium sulfate and urea
And CTAB is stirred for 30min at room temperature, then transferred to 90 ℃ to be continuously stirred for 12h, and then cooled to room temperature. Filtering and washing the product, drying at 110 deg.C for 12 hr, and roasting at 500 deg.C for 5 hr to obtain mesoporous CeO2Modified halloysite nanotubes. The mass-volume ratio of the halloysite nanotubes to the deionized water is 1:10, and the mass ratio of the halloysite nanotubes to the cerium sulfate is 1:0.25, the molar ratio of urea to cerium sulfate is 10:1, and the mass ratio of CTAB to cerium sulfate is 1: 20.
(3) Loading of active ingredients
Mixing and stirring a certain amount of vanadium acetylacetonate, magnesium acetylacetonate, acetylacetone and absolute ethyl alcohol, and adding a certain amount of mesoporous CeO2Modified halloysite nanotubes, mixing the mixture at 60oAnd C, refluxing for 12 hours under the condition of water bath. The product obtained is purified at 500oAnd C, roasting for 5 hours, cooling to room temperature to obtain solid powder, tabletting and forming the solid powder, and finally screening a 40-60-mesh sample for activity evaluation. In the preparation process, the addition amount of acetylacetone is respectively 4 times of the sum of the molar amounts of vanadium acetylacetonate and magnesium acetylacetonate, the addition amount of anhydrous ethanol is respectively 5 times of the sum of the molar amounts of vanadium acetylacetonate and magnesium acetylacetonate, the molar ratio of vanadium acetylacetonate to magnesium acetylacetonate is 2:1, and vanadium acetylacetonate and mesoporous CeO are added2Modified halloysite nanoparticlesThe mass ratio of the tube was 1: 50.
Example 3
(1) Purification of halloysite nanotubes
Weighing 20g of halloysite nanotubes, adding the halloysite nanotubes into 150mL of deionized water, stirring the mixture at the speed of 700rpm for 30min at room temperature, then dropwise adding a certain amount of nitric acid into the mixture to adjust the pH value of the solution to 4, continuing stirring the solution for 1h to remove impurities on the surface and the inside, filtering the mixture, washing the mixture to be neutral, drying the mixture at 110 ℃ for 12h, and finally roasting the mixture at 500 ℃ for 5 h. In the process, the mass-to-volume ratio of the halloysite nanotubes to the deionized water is 1: 7.5.
(2) Surface modification of halloysite nanotubes comprises adding purified halloysite nanotubes into deionized water, adding cerium nitrate and urea
And CTAB is stirred for 30min at room temperature, then transferred to 90 ℃ to be continuously stirred for 12h, and then cooled to room temperature. Filtering and washing the product, drying at 110 deg.C for 12 hr, and roasting at 500 deg.C for 5 hr to obtain mesoporous CeO2Modified halloysite nanotubes. The mass ratio volume of the halloysite nanotubes to the deionized water is 1:7.5, and the mass ratio of the halloysite nanotubes to the cerium sulfate is 1: 0.18, the molar ratio of urea to cerium salt is 10:1, and the mass ratio of CTAB to cerium salt is 1: 15.
(3) Loading of active ingredients
Mixing and stirring a certain amount of vanadium acetylacetonate, magnesium acetylacetonate, acetylacetone and absolute ethyl alcohol, and adding a certain amount of mesoporous CeO2Modified halloysite nanotubes, mixing at 50oC, refluxing for 15h under the condition of water bath. The product obtained is purified at 500oAnd C, roasting for 5 hours, cooling to room temperature to obtain solid powder, tabletting and forming the solid powder, and finally screening a 40-60-mesh sample for activity evaluation. In the preparation process, the addition amount of acetylacetone is respectively 4 times of the sum of the molar amounts of vanadium acetylacetonate and magnesium acetylacetonate, the addition amount of anhydrous ethanol is respectively 5 times of the sum of the molar amounts of vanadium acetylacetonate and magnesium acetylacetonate, the molar ratio of vanadium acetylacetonate to magnesium acetylacetonate is 2:1, and vanadium acetylacetonate and mesoporous CeO are added2Modified halloysite nanoparticlesThe mass ratio of the tube was 1: 75.
The test conditions for catalyst activity were: the method is carried out in a fixed bed reactor, the dosage of the catalyst is 0.5mL, and the simulated flue gas comprises the following components: 1000ppmNH3，1000ppm NO，5% O2Ar is balance gas, the total flow is 500mL/min, and the reaction space velocity is 60,000h-1The reaction temperature is 150-500 ℃, and NO in the reaction product2The content was analyzed and determined by a flue gas analyzer KM9506
Wherein [ NO ]x]=[NO]+[NO2]
Specific test results are shown in Table 1.1
The catalyst prepared in example 1 was examined for SO on a fixed bed reactor2And H2The effect of O on catalytic activity. The composition of the reaction mixture gas is [ NH ]3]=[NO]=1000ppm，[O2]=5vol%，[SO2]=100ppm，[H2O]=10vol%, Ar is equilibrium gas, and the reaction space velocity is 60,000h-1Reaction temperature of 300 deg.CoC. The experimental results show that: in the presence of SO2And H2After O12 h, NOxThe conversion rate of (A) is slightly reduced by 1-3%, the conversion rate is still maintained to be more than 97%, the conversion rate is basically kept stable within 120 hours of experimental investigation, and when SO is used2And H2The catalytic activity was substantially restored to a level close to 100% after O removal.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (7)
1. A preparation method of a denitration catalyst is characterized by comprising the following steps: the method comprises the following steps:
(1) purifying the halloysite nanotubes: weighing a certain amount of halloysite nanotubes, adding the halloysite nanotubes into deionized water, stirring at the speed of 700rpm for 30min at room temperature, then dropwise adding nitric acid to adjust the pH value of the solution, continuously stirring for 1h, removing impurities on the surface and in the solution, filtering and washing to be neutral, drying at 110 ℃ for 12h, and finally roasting at 500 ℃ for 5h to obtain purified halloysite nanotubes;
(2) surface modification of halloysite nanotubes: adding the purified halloysite nanotube into deionized water, adding cerium salt, urea and CTAB, stirring at room temperature for 30min, continuing stirring at 90 ℃ for 12h, cooling to room temperature, filtering, washing, drying at 110 ℃ for 12h, and roasting at 500 ℃ for 5h to obtain mesoporous CeO2A modified halloysite nanotube;
(3) loading of active components: mixing and stirring a certain amount of vanadium acetylacetonate, magnesium acetylacetonate, acetylacetone and absolute ethyl alcohol uniformly, then adding a certain amount of mesoporous CeO2The modified halloysite nanotube is prepared by mixing the mixture at 40-60%oC, refluxing for 12-18 h under the water bath condition, and then subjecting the obtained product to 500oRoasting for 5 hours under C, cooling to room temperature to obtain solid powder, and finally tabletting and forming to obtain the denitration catalyst;
in the step (3), the addition amount of acetylacetone is 4 times of the sum of the molar amounts of vanadium acetylacetonate and magnesium acetylacetonate, the addition amount of anhydrous ethanol is 5 times of the sum of the molar amounts of vanadium acetylacetonate and magnesium acetylacetonate, and the molar ratio of vanadium acetylacetonate to magnesium acetylacetonate is 2: 1.
2. The method of claim 1, wherein the denitration catalyst comprises: and (2) dropwise adding nitric acid in the step (1) to adjust the pH value of the solution to 3.9-4.2.
3. The method of claim 1, wherein the denitration catalyst comprises: the mass ratio of the halloysite nanotubes to the deionized water in the step (1) is 1: 5-1: 10.
4. The method of claim 1, wherein the denitration catalyst comprises: in the step (2), the cerium salt is one or a mixture of cerium nitrate and cerium sulfate.
5. The method of claim 1, wherein the denitration catalyst comprises: the mass ratio of the halloysite nanotubes to the deionized water after purification in the step (2) is 1: 5-1: 10, the mass ratio of the halloysite nanotubes to the cerium salt is 1: 0.1-1: 0.25, the molar ratio of urea to the cerium salt is 10:1, and the mass ratio of CTAB to the cerium salt is 1: 10-1: 20.
6. The method of claim 1, wherein the denitration catalyst comprises: in the step (3), vanadium acetylacetonate and mesoporous CeO2The mass ratio of the modified halloysite nanotubes is 1: 100-1: 50.
7. A denitration catalyst produced by the production method according to any one of claims 1 to 6.
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| CN105771967A (en) * | 2016-03-30 | 2016-07-20 | 盐城工学院 | Metal oxide-vanadate/attapulgite catalyst |
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