CN107537558B - Method for preparing supported catalyst with anchored enhanced NOx removal - Google Patents
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Abstract
The invention relates to a preparation method of a carrier catalyst with anchoring enhancement and NOx removal, which is characterized in that copper and iron ions, transition metal ions and a molecular sieve react under the chemical action of ammonium carbamate at a certain temperature to ensure that the active component is uniformly loaded and dispersed, and finally, an active product formed in the combustion process has a high-efficiency selectivity effect of anchoring enhancement on NOx, so that the carrier catalyst has better NOx conversion rate. The NOx conversion rate of the carrier catalyst with the functions of anchoring, enhancing and removing NOx prepared by the invention is 96.1% at most under the working condition of B50, 82.9% at 548 ℃ C100 NOx conversion rate and 86.8% at 198 ℃ C25 NOx conversion rate, and the carrier catalyst shows higher NOx activity and low shedding rate of a coating within 198-548 ℃. Meanwhile, the preparation process is simple and convenient for industrialization.
Description
Technical Field
The invention relates to a preparation method of a carrier catalyst with the functions of anchoring, enhancing and removing NOx, belonging to the technical field of automobile emission.
Background
In order to meet emission regulations, the Urea-SCR technology has become the first line of NOx reduction technology for medium and heavy diesel engine enterprises, and the principle is that when ammonia gas generated by Urea hydrolysis and NOx in automobile exhaust pass through a carrier coated with an active coating, the NOx is rapidly reduced into nitrogen gas and water by the ammonia gas, and the ammonia gas and the NOx can perform rapid chemical reaction on an aftertreatment carrier and are inseparable from the composition of the carrier. The carrier with the active coating is composed of a carrier and a catalyst, the carrier firstly bears the coating and active components, and secondly provides a proper catalytic reaction channel without the support of the carrier, the catalyst powder can not exert the performance of the catalyst, and the cordierite honeycomb carrier has the advantages of large surface area, high pore density, thin pore wall, low thermal expansion coefficient, good thermal shock resistance and the like and shows excellent performance in the field of automobile exhaust denitration. The catalyst is used as a main active component for denitration and can only be loaded on a carrier to play a role, so that the research on how to organically combine the catalyst and the carrier to achieve the best denitration effect is a hotspot of the current research.
The invention patent CN201110275543.0 discloses a NOx selective catalytic reduction molecular sieve catalyst and a preparation method thereof. The catalyst comprises the following components: (10% to 30%) of CeO2-M + (90-70%) Fe/ZSM-5, where M is TiO2Or WO3, CeO2The mass ratio of the/M is 3: 1-1: 1; the molecular sieve ZSM-5 has a SiO2/Al2O3 ratio of 15-150. Soluble cerium salt and titanium salt or tungsten salt are used as raw materials, alkali is used as a coprecipitator, polyethylene glycol is used as a thickening agent, a molecular sieve HZSM-5 is used as a raw material, soluble ammonium salt is used as an ammonium source, and NH4/ZSM-5 is prepared by ion exchange. Soluble iron salt is used as a raw material, and Fe and ZSM-5 are prepared by ion exchange. One or more of alumina sol, silica sol or zirconium acetate is used as a binder, Fe/ZSM-5 is coated on a cordierite honeycomb ceramic carrier, and then CeO2-M is coated on the cordierite honeycomb ceramic carrier, and the cordierite honeycomb ceramic carrier is dried and roasted. The conversion rate of the catalyst in a wide active temperature window is more than 80 percent, and the high-efficiency catalytic removal of nitrogen oxides can be realized in the temperature range of 190 ℃ and 600 ℃.
The invention patent CN201110057115.0 discloses a manganese modified selective catalytic reduction catalyst for a molecular sieve type diesel engine. The catalyst adopts cordierite honeycomb ceramic as a carrier material; the main active components are Mn2+ ions entering the molecular sieve through ion exchange and manganese oxide particles; the residual non-exchanged H + and Si-Al skeleton structure in the molecular sieve are used as cocatalyst and coating matrix respectively. In the molecular sieve powder after ion exchange modification, the weight percentage of manganese element is 0.6-9.2%; in the supported catalyst composed of the cordierite honeycomb ceramic carrier and the coating after the coating is supported, the weight percentage of the coating is 5-15%. The preparation comprises the modification of the molecular sieve and the preparation of the supported catalyst.
The invention patent CN 201410643551.X discloses a manganese and zirconium bimetal modified selective catalytic reduction catalyst for a molecular sieve type diesel engine. The manganese and zirconium elements enter the molecular sieve by a liquid ion exchange-impregnation method. Based on the total weight of the modified powdery catalyst, the manganese element accounts for 4.5-7.5 wt%, and the zirconium element accounts for 4.5-15 wt%. Based on the total weight of the supported catalyst, the coating accounts for 5-15 wt%. The novel diesel vehicle SCR catalyst is prepared by adopting the nontoxic molecular sieve, the low-toxicity manganese element and the zirconium element, so that the toxicity of the catalyst to a human body is reduced; meanwhile, the high activity temperature window of the catalyst in the SCR reaction of the diesel vehicle is enlarged. The modification method improves the loading capacity, has more flexible and adjustable loading proportion and is beneficial to further optimization of the catalyst performance.
The preparation method for preparing the denitration carrier catalyst has the following problems: (1) narrow catalyst temperature window, poor selectivity, NOXThe conversion rate is low, (2) the active components are coated unevenly, and are enriched locally or the coating amount is too small; (3) the firmness of the combination of the active component coating and the carrier is low, and the coating is easy to fall off; (4) the preparation process is complicated.
Disclosure of Invention
It is an object of the present invention to provide a method for NO removal with anchoring enhancementXThe preparation method of the carrier catalyst comprises the steps of reacting copper and iron ions, transition metal ions and the molecular sieve under the chemical action of ammonium carbamate at a certain temperature to ensure that the active component is uniformly loaded and dispersed, and finally forming an active product in the combustion process, wherein the active product has a high-efficiency selectivity effect of enhancing the anchoring of NOx, so that the carrier catalyst has a better NOx conversion rate. The supported catalyst with anchored enhanced NOx removal prepared by the inventionThe highest NOx conversion rate under the working condition of B50 is 96.1%, the highest NOx conversion rate at 548 ℃ and C100 is 82.9%, the highest NOx conversion rate at 198 ℃ and C25 is 86.8%, and the NOx conversion rate at 198-548 ℃ shows higher NOx activity and low shedding rate of a coating. Meanwhile, the preparation process is simple and convenient for industrialization.
The technical scheme of the invention is realized as follows: the preparation method of the carrier catalyst with the function of anchoring and enhancing the removal of NOx is characterized by comprising the following specific steps: (1) pretreating a cordierite honeycomb carrier: soaking the carrier in 2-3.8 wt% ammonia water at room temperature for 20-60 min, taking out the cordierite ceramic carrier, repeatedly washing the carrier with deionized water until the pH value is neutral, drying the carrier, and calcining the carrier at 500 ℃ for 2-4 h; (2) preparing an anchoring enhancement mixed solution: a. dissolving 3.6-5.7 parts of ferric salt, 2.8-5.2 parts of copper salt and 1.4-2.3 parts of metal auxiliary agent in deionized water, and stirring for dissolving; b. adding 11.3-14.3 parts of molecular sieve carrier, and mixing and stirring for 2-4 h; c. adding 0.3-0.4 part of ammonium carbamate, and stirring for 1-3 hours at 45-60 ℃; c. adding a solution containing 2.1-4.7 parts of silica Sol (SiO)240 percent of content), 2.4 to 5.3 parts of alumina sol (Al)2O3The content of 40 percent), 1.9 to 6.6 parts of sodium carboxymethylcellulose aqueous solution (mass fraction of 1 percent) are mixed with a binder and stirred uniformly to obtain a mixed solution, and the mixed solution is stirred uniformly to obtain an active mixed solution containing a molecular sieve; (3) cordierite honeycomb carrier activation: and (3) placing the treated cordierite ceramic carrier in the prepared active mixed liquid containing the molecular sieve for 5-10 min, taking out the carrier, blowing away the surface residual liquid by using a sweeping gas, placing the carrier in an oven for drying at 80-105 ℃, and finally calcining at 450-530 ℃ for 2-4 h to obtain the molecular sieve cordierite honeycomb carrier catalyst.
The metal auxiliary agent in the anchoring reinforced mixed solution is one or more of La, Mn, Ni and Ce salt.
The method has the advantages that copper and iron ions, transition metal ions and the molecular sieve are reacted, so that part of mixed metal ions enter a pore channel of the molecular sieve, and the molecular sieve and the multi-component active metal component are subjected to chemical action at a certain temperature, so that the molecular sieve and the multi-component active metal component form a high-efficiency selective effect with enhanced anchoring of NOx in the calcining process, and a wider temperature window is provided; the binding agent system containing high-temperature silica sol, high-temperature alumina sol and carboxymethyl cellulose is added, so that the bonding firmness of the active component and the carrier can be enhanced, and the problems that the bonding firmness of the active component coating and the carrier is low and the coating is easy to fall off are solved; the monolithic carrier catalyst prepared by the anchoring reinforced mixed solution and the cordierite honeycomb carrier through combustion in one step effectively solves the problems that the active components of the catalyst are not uniformly coated, and are locally enriched or the coating amount is too small.
Drawings
FIG. 1 is a schematic structural diagram of a vibration test bed for testing the shedding rate of a prepared non-noble metal-containing monolithic supported catalyst.
Detailed Description
In the following description of specific examples, numerous specific details are set forth in order to provide a more thorough understanding of the present invention. It will be apparent, however, to one skilled in the art, that the present invention may be practiced without one or more of these specific details.
Example 1
(1) Cordierite honeycomb carrier pretreatment
Soaking the cordierite ceramic carrier in ammonia water with the mass fraction of 2% at room temperature, taking out after 60min, repeatedly washing with deionized water until the pH of the solution after washing shows neutrality, drying at 105 ℃, and calcining at 500 ℃ for 4 h.
(2) Preparation of anchoring reinforced mixed liquor
a. Weighing 300g of copper nitrate, 240g of ferric nitrate and 120g of cerium nitrate, and dissolving in 5300g of deionized water; b. adding 1200g of Sapo34 molecular sieve powder, and stirring for 2 hours; c. adding 21.2g of ammonium carbamate, and stirring at 60 ℃ for 1 h; 400g of silica Sol (SiO) was added240% content), 450g of alumina sol (Al)2O3The content is 40 percent), 400g of sodium carboxymethylcellulose aqueous solution (mass fraction is 1 percent) and evenly stirred to obtain mixed liquor.
(3) Cordierite honeycomb carrier activation
Placing the cordierite honeycomb carrier obtained after pretreatment in the step (1) into the molecular sieve active mixed solution prepared in the step (2)Taking out the carrier after 5min, blowing off the residual liquid on the surface by using compressed air, placing the carrier in a drying oven for drying at 80 ℃, and calcining at 450 ℃ for 4h to obtain the carrier with the functions of anchoring, enhancing and removing NOXThe supported catalyst of (1).
The molecular sieve cordierite honeycomb carrier catalyst prepared in example 1 was subjected to a coating peeling test by first weighing and then removing NO with anchoring enhancementXThe supported catalyst 3 of (a) is mounted in a jig 2 on a vibration test stand 4 and fixed by a fixing bolt 1 as shown in fig. 1. The vibration acceleration of 10g, the vibration frequency of (100 +/-5) Hz and the test time of 5h are adopted, the carrier catalyst is taken down after the experiment is finished, the mass of the carrier catalyst is weighed, and the coating falling rate is calculated to be 2.95 percent, which shows that the firmness of the combination of the active component coating and the carrier is high, and the problem that the coating is easy to fall off is solved.
The monolithic supported catalyst prepared in example 1 was subjected to engine bench tests, and the engine bench tests were performed on the monolithic supported catalyst containing non-noble metals under the experimental conditions and the test results shown in table 1.
It can be seen that the highest NOx conversion rate is 96.1% under the B50 working condition, the lowest NOx conversion rate is 82.9% under the C100 working condition, the NOx conversion rate is 86.8% under the C25 working condition at 198-548 ℃, and the high NOx activity is shown within 198-548 ℃.
Example 2
(1) Cordierite honeycomb carrier pretreatment
Soaking the cordierite ceramic carrier in ammonia water with the mass fraction of 3.8% at room temperature, taking out after 60min, repeatedly washing with deionized water until the pH of the solution after washing shows neutrality, drying at 105 ℃, and calcining at 500 ℃ for 4 h.
(2) Preparation of anchoring reinforced mixed liquor
a. Weighing 480g of copper nitrate, 400g of ferric nitrate and 150g of lanthanum nitrate, and dissolving in 5200g of deionized water; b. adding 1200g of ZSM5 molecular sieve powder, and stirring for 4 hours; c. adding 34.2g of ammonium carbamate, and stirring at 45 ℃ for 3 hours; 180g of silica Sol (SiO) were added2Content 40%), 200g of alumina sol（Al2O340 percent of the content), 550g of sodium carboxymethylcellulose aqueous solution (mass fraction of 1 percent) and uniformly stirring to obtain a mixed solution.
(3) Cordierite honeycomb carrier activation
Placing the cordierite honeycomb carrier obtained after pretreatment in the step (1) into the molecular sieve active mixed solution prepared in the step (2), taking out the carrier after 10min, blowing off the surface residual solution by using compressed air, placing the carrier into a drying oven for drying at 105 ℃, and calcining at 530 ℃ for 4h to obtain the carrier with the functions of anchoring, enhancing and removing NOXThe supported catalyst of (1).
Example 3
(1) Cordierite honeycomb carrier pretreatment
Soaking the cordierite ceramic carrier in ammonia water with the mass fraction of 2% at room temperature, taking out after 30min, repeatedly washing with deionized water until the pH of the solution after washing shows neutrality, drying at 105 ℃, and calcining at 500 ℃ for 3 h.
(2) Preparation of anchoring reinforced mixed liquor
a. Weighing 400g of copper nitrate, 400g of ferric nitrate and 180g of manganese nitrate, and dissolving in 6200g of deionized water; b. adding 1200g of Sapo34 molecular sieve powder, and stirring for 2 hours; c. 32.8g of ammonium carbamate are added and stirred for 2h at 55 ℃; 350g of silica Sol (SiO) were added2Content 40%), 300g of alumina sol (Al)2O3The content is 40 percent), 180g of sodium carboxymethylcellulose aqueous solution (mass fraction is 1 percent) and evenly stirred to obtain mixed liquor.
(3) Cordierite honeycomb carrier activation
Placing the cordierite honeycomb carrier obtained after pretreatment in the step (1) into the molecular sieve active mixed solution prepared in the step (2), taking out the carrier after 6min, blowing away the surface residual solution by using compressed air, placing the carrier into a drying oven for drying at 105 ℃, and calcining at 450 ℃ for 2h to obtain the carrier with the functions of anchoring, enhancing and removing NOXThe supported catalyst of (1).
Example 4
(1) Cordierite ceramic carrier pretreatment
Soaking the cordierite ceramic carrier in ammonia water with the mass fraction of 2% at room temperature, taking out after 30min, repeatedly washing with deionized water until the pH of the solution after washing shows neutrality, drying at 105 ℃, and calcining at 500 ℃ for 4 h.
(2) Preparation of anchoring reinforced mixed liquor
a. Weighing 440g of copper nitrate, 480g of ferric nitrate and 150g of nickel nitrate, and dissolving in 6000g of deionized water; b. adding 1200g of beta25 molecular sieve powder, and stirring for 2 h; c. adding 35.2g of ammonium carbamate, and stirring at 55 ℃ for 2 hours; 300g of silica Sol (SiO) was added2Content 40%), 300g of alumina sol (Al)2O3The content is 40 percent), 250g of sodium carboxymethylcellulose aqueous solution (mass fraction is 1 percent) and evenly stirred to obtain mixed liquor.
(3) Cordierite honeycomb carrier activation
Placing the cordierite honeycomb carrier obtained after pretreatment in the step (1) into the molecular sieve active mixed solution prepared in the step (2), taking out the carrier after 5min, blowing away the surface residual solution by using compressed air, placing the carrier into a drying oven for drying at 105 ℃, and calcining at 500 ℃ for 3h to obtain the carrier with the functions of anchoring, enhancing and removing NOXThe supported catalyst of (1).
Example 5
(1) Cordierite ceramic carrier pretreatment
Soaking the cordierite ceramic carrier in ammonia water with the mass fraction of 2% at room temperature, taking out after 30min, repeatedly washing with deionized water until the pH of the solution after washing shows neutrality, drying at 105 ℃, and calcining at 500 ℃ for 4 h.
(2) Preparation of anchoring reinforced mixed liquor
a. Weighing 400g of copper nitrate, 350g of ferric nitrate, 80g of cerium nitrate, 80g of lanthanum nitrate and 80g of manganese nitrate, and dissolving in 7000g of deionized water; b. adding 1200g of SSZ-13 molecular sieve powder, and stirring for 2 h; c. adding 31.8g of ammonium carbamate, and stirring at 60 ℃ for 2 hours; 480g of silica Sol (SiO) were added2Content 40%), 520g of alumina sol (Al)2O3The content is 40 percent), 380g of sodium carboxymethylcellulose aqueous solution (mass fraction is 1 percent) are uniformly stirred, and mixed liquor is obtained.
(3) Cordierite honeycomb carrier activation
Placing the cordierite honeycomb carrier obtained after pretreatment in the step (1) in the molecular sieve active mixed solution prepared in the step (2), and after 5minTaking out the carrier, blowing off the residual liquid on the surface by using compressed air, placing the carrier in a drying oven for drying at 105 ℃, and calcining at 530 ℃ for 2 hours to obtain the carrier with anchoring enhancement and NO removal functionsXThe supported catalyst of (1).
Claims (2)
1. The preparation method of the carrier catalyst with the function of anchoring and enhancing the removal of NOx is characterized by comprising the following specific steps: (1) pretreating a cordierite honeycomb carrier: soaking the carrier in 2-3.8 wt% ammonia water at room temperature for 20-60 min, taking out the cordierite ceramic carrier, repeatedly washing the carrier with deionized water until the pH value is neutral, drying the carrier, and calcining the carrier at 500 ℃ for 2-4 h; (2) preparing an anchoring enhancement mixed solution: a. dissolving iron salt, copper salt and metal auxiliary agent with certain mass into deionized water, and stirring for dissolving; b. adding a molecular sieve carrier, and mixing and stirring for 2-4 h; c. adding ammonium carbamate, and stirring for 1-3 h at 45-60 ℃; d. adding the binder until the mixture is uniformly stirred to obtain a mixed solution; (3) cordierite honeycomb carrier activation: placing the treated cordierite ceramic carrier in a prepared active mixed solution containing a molecular sieve for 5-10 min, taking out the carrier, blowing off surface residual liquid by using purge gas, placing the carrier in an oven for drying at 80-105 ℃, and finally calcining at 450-530 ℃ for 2-4 h to obtain the molecular sieve cordierite honeycomb carrier catalyst; 3.6-5.7 parts of iron salt, 2.8-5.2 parts of copper salt, 1.4-2.3 parts of metal auxiliary agent, 11.3-14.3 parts of molecular sieve, 0.3-0.4 part of ammonium carbamate and 9.0-14.8 parts of binder in the anchoring enhancement mixed solution;
the metal auxiliary agent in the anchoring reinforced mixed solution is one or more of La, Mn, Ni and Ce salt.
2. The method for preparing the supported catalyst with the function of anchoring and enhancing NOx removal function as claimed in claim 1, wherein the binder in the anchoring and enhancing mixed solution is a mixture of silica sol, alumina sol and sodium carboxymethyl cellulose, wherein the silica sol and SiO are 2.1-4.7 parts22.4 to 5.3 portions of alumina sol and Al with the content of 40 percent2O3The content of the sodium carboxymethyl cellulose is 40 percent, and the mass fraction of the sodium carboxymethyl cellulose aqueous solution is 1.9 to 6.6 parts.
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