CN110614101A - Catalyst for catalytic combustion of VOCs and preparation method thereof - Google Patents
Catalyst for catalytic combustion of VOCs and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a catalyst for catalyzing and combusting VOCs and a preparation method thereof, wherein cordierite honeycomb ceramics or porous metal materials are used as carriers, nano coating materials are coated on the carriers, noble metal compound transition metals are used as active components, compound rare earth oxides are used as catalyst auxiliaries, and solid solutions prepared from alkaline earth metal compounds and main group metal oxides are used as carrier modifiers; the carrier and the active components are coated by an automatic production line, the matrix binding force is strong, the active components and the carrier are high in adhesive force after high-temperature roasting, are not easy to fall off, are high in activity, good in thermal stability, good in sulfur resistance and long in service life, are a broad-spectrum VOCs oxidation catalyst, can be used for treating VOCs in industries such as spraying, printing and electronics through catalytic combustion, and are suitable for CO and RCO catalytic combustion devices.
Description
Technical Field
The invention relates to a catalyst for catalytic combustion of VOCs (volatile organic compounds) and a preparation method thereof, belonging to the field of treatment of industrial waste gas with atmospheric environmental pollution.
Background
Volatile Organic Compounds (VOCs) in industrial waste gases severely affect the atmosphereThe environment and human health, so that the pollution caused by controlling the VOCs is a main index for preventing and treating the air pollution, the discharge standard requirement of the VOCs is higher and higher, and the recovery and destruction technology is needed to treat; the treatment of VOCs in industrial waste gas is generally fully recovered and destroyed by an adsorption concentration-catalytic combustion technology for comprehensive treatment, VOCs are adsorbed by an adsorbent, then the environmental physical conditions are changed, so that the concentration of the VOCs is increased by enrichment concentration, certain chemical conditions are changed by utilizing the characteristic that the VOCs is easy to burn, and the VOCs in the waste gas is completely burnt at a lower ignition temperature by the catalytic combustion technology and decomposed into CO2And H2Non-toxic small molecules such as O; the specific principle is that practical and efficient catalytic combustion is carried out through a proper catalyst, VOCs in waste gas are completely combusted at a lower ignition temperature, a large amount of heat emitted by combustion can be recycled as system heat, and the ignition temperature, the purification efficiency and the secondary pollution degree of catalytic combustion all depend on the performance of the catalyst;
catalysts for the catalytic oxidation of VOCs are mainly classified into two types: the low-temperature activity and the thermal stability of the noble metal catalyst are superior to those of the non-noble metal catalyst, but the noble metal is expensive and the application of the noble metal is limited due to the shortage of resources; the consumption of noble metal materials is reduced under the precondition of ensuring the activity of the catalyst, noble metal and transition metal are compounded and loaded on the modified rare earth oxide, the rare earth oxide is taken as an auxiliary agent to be beneficial to the dispersion and sintering of the main active component, and further the catalytic activity is fully exerted, and compared with a single noble metal catalyst, the supported composite oxide catalyst has more superiority in the aspects of reducing the cost, catalyzing the activity and the like;
the industrial VOCs catalyst in the prior art usually adopts an integral honeycomb structure, and compared with the conventional spherical or elongated catalyst, the catalyst is large in size, complex in structure and inconvenient in uniform coating operation of active components, the traditional method generally adopts a manual coating mode for production and processing, the production efficiency is low, the strength is not high, the heat transfer effect is influenced, and the service life is short.
Disclosure of Invention
The invention aims to solve the technical problem of providing a catalyst which adopts a compounding technology with low noble metal loading, has good mass and heat transfer effect, small wind resistance, good mechanical strength, high short-time impact temperature resistance and long service life and is used for catalyzing and combusting VOCs and a preparation method thereof.
The invention relates to a catalyst for catalytic combustion of VOCs, which is characterized in that: the catalyst comprises an integral honeycomb carrier, wherein the carrier material is high-quality ceramic cordierite or porous metal, and a nano material coating is coated on the surface of the carrier to be used as a basic coating; the carrier is loaded with a mixture consisting of a main active component, a second active component, a cocatalyst, a modifier, a dispersant and an adhesive; wherein the main active component is noble metal of 0.01-0.5 g/L; based on the mass of the carrier, the second active component is 1-10% of transition metal, the cocatalyst is 1-10% of rare earth compound or metal oxide, the modifier is 0.1-5% of alkali metal or alkaline earth metal compound, the dispersant and the adhesive are 5-30% of aluminum sol or silica sol;
the carrier is a square or cylindrical honeycomb, the size of a honeycomb hole is 200-800 meshes, and the carrier is subjected to surface treatment for later use by using 1-10% dilute nitric acid and dilute hydrochloric acid solution before use;
the nano material of the basic coating is a solid solution prepared from nitrate or aluminum oxide of metal aluminum and one of metal oxides of titanium, cerium, zirconium and lanthanum under an acidic condition, and the molecular expression of the solid solution is as follows: AlX (Ti/Ce/Zr/La) yO2, wherein x: y ═ 3-7: 7-3;
the acid used in the acidic condition is citric acid or acetic acid;
the noble metal of the main active component is one or a mixture of Au, Pt, Pd, Ru and Rh;
the transition metal is one or more of Mn, Fe, Ni, Cu and Zn, the rare earth element in the rare earth compound is one of La, Ce and Pr, and the metal oxide is Al2O3ZrO or SnO2One or a mixture of several of (a); the alkali metal compound is a compound containing one or more elements of Li, Na and K; the alkaline earth metal compound is a compound of one or more elements of Mg, Ca and Ba;
the invention also relates to a preparation method of the catalyst for catalytic combustion of VOCs, which is characterized by comprising the following steps: the method comprises the following steps:
first step, honeycomb carrier pretreatment
Treating the honeycomb ceramic carrier with 1-10% of dilute nitric acid, soaking the honeycomb ceramic carrier in aluminum sol or silica sol after treatment, taking out the honeycomb ceramic carrier after full soaking, drying and roasting; wherein the drying temperature is 80-150 ℃, and the drying time is 1-5 h; the roasting temperature is 400-;
second, preparation of nano-coating solid solution
Taking Al (NO)3)3Diluting the solution and transition metal nitrate or rare earth metal nitrate with deionized water, heating and stirring under acidic condition until colloid is formed, and sintering to form solid solution AlX MyO2A composite oxide;
thirdly, preparing and loading cocatalyst coating slurry
Taking solid solution AlX MyO2Mixing and grinding the mixture with rare earth oxide for 2-6h, adding deionized water during grinding, controlling the particle size of grinding particles to be nano-scale, then mixing the grinding material with silica sol or aluminum sol, and adding a modifier with a certain molar ratio to obtain sol with dispersed cocatalyst;
the fourth step, preparation of the active component of the catalyst
Fully mixing the noble metal salt and the transition metal salt solution according to the molar ratio, adding the cocatalyst sol obtained in the second step, stirring and grinding, and uniformly dispersing to obtain slurry for later use, wherein the preparation process is completed by an automatic pulping system;
the fifth step, catalyst carrier coating
Soaking the honeycomb carrier treated in the first step in the slurry prepared in the third step in an equal volume, airing and aging after soaking saturation, putting the honeycomb carrier into a drying oven for temperature programming and drying, then transferring the honeycomb carrier into a muffle furnace for high-temperature roasting, and cooling to obtain the integral honeycomb structure catalyst, wherein the carrier is in high-strength combination with active components; wherein the temperature programming rate is 5-10 ℃/min, the drying temperature is 80-150 ℃, and the drying time is 1-5 h; the roasting temperature is 400-;
all the steps from the first step to the fifth step are prepared through an automatic coating production line, catalyst raw material proportioning addition, stirring, homogenizing, grinding, sizing and coating are automatically carried out, and the pressure, temperature, flow and weight indexes of the technological process are controlled;
in the first step, a honeycomb carrier is a 150 multiplied by 100 square cordierite honeycomb carrier, the honeycomb carrier is treated by a 5% dilute nitric acid solution, and then the honeycomb carrier is immersed in 20% aluminum sol, the drying temperature is 80 ℃, and the drying time is 2 hours; the roasting temperature is 400 ℃, and the roasting time is 4 hours;
the solid solution of the second step is made of Al (NO)3)3Powder and Ce (NO)3)3Diluting and mixing the powder with deionized water, adjusting the acid environment by adding acetic acid, and drying and sintering to form a solid solution of aluminum cerium composite oxide AlCoO2；
In the third step, 6kg of aluminum cerium composite oxide AlCeO is weighed2Powder solid solution with 0.1mol of BaSO as modifier4；
In the fourth step, the noble metal salt is 0.15g/ml Pt (NO3)25L of the solution is diluted into 10L by deionized water, and the transition metal salt solution is 100g of CuSO4；
In the fifth step, the temperature rise rate is 5 ℃/min, the drying temperature is 120 ℃, and the drying time is 2 h; the roasting temperature is 500 ℃, and the roasting time is 4 hours.
The invention relates to a catalyst for catalytic combustion of VOCs and a preparation method thereof.A compounding technology with low noble metal loading is adopted, cordierite honeycomb ceramics or porous metal materials are taken as a carrier, a nano coating material is coated on the carrier, noble metal compounding transition metal is taken as an active component, compounding rare earth oxide is taken as a catalyst auxiliary agent, and solid solution prepared from alkaline earth metal compounds and main group metal oxides is taken as a carrier modifier; the carrier and the active components are coated by an automatic production line, the binding force of a matrix is strong, the active components and the carrier are high in adhesion after high-temperature roasting, are not easy to fall off, and have high activity, good thermal stability, good sulfur resistance, long service life, good ageing resistance and good poisoning resistance; the prepared catalyst has high activity, good mass and heat transfer effects, small wind resistance, good mechanical strength, short-time impact temperature resistance of 900 ℃, minimum T90 temperature of about 200 ℃, system removal efficiency of more than 99 percent, complete conversion of VOCs into CO2 and H2O and no generation of other pollutants; the catalyst can be used for treating VOCs in industries such as spraying, printing and electronics by catalytic combustion, CO and RCO catalytic combustion devices for treating industrial VOCs, and can also be used for a large-scale diesel vehicle tail gas treatment system, and has high treatment efficiency and no secondary pollution.
Detailed Description
A catalyst for catalytic combustion of VOCs comprises a monolithic honeycomb carrier, wherein the carrier material is high-quality ceramic cordierite or porous metal, and the surface of the carrier is coated with a nano material coating as a basic coating; the carrier is loaded with a mixture consisting of a main active component, a second active component, a cocatalyst, a modifier, a dispersant and an adhesive; wherein the main active component is noble metal of 0.01-0.5 g/L; based on the mass of the carrier, the second active component is 1-10% of transition metal, the cocatalyst is 1-10% of rare earth compound or metal oxide, the modifier is 0.1-5% of alkali metal or alkaline earth metal compound, the dispersant and the adhesive are 5-30% of aluminum sol or silica sol;
the carrier is a square or cylindrical honeycomb, the size of a honeycomb hole is 200-800 meshes, and the carrier is subjected to surface treatment for later use by using 1-10% dilute nitric acid and dilute hydrochloric acid solution before use;
the nano material of the basic coating is a solid solution prepared from nitrate or aluminum oxide of metal aluminum and one of metal oxides of titanium, cerium, zirconium and lanthanum under an acidic condition, and the molecular expression of the solid solution is as follows: AlX (Ti/Ce/Zr/La) yO2, wherein x: y ═ 3-7: 7-3;
the acid used in the acidic condition is citric acid or acetic acid;
the noble metal of the main active component is one or a mixture of Au, Pt, Pd, Ru and Rh;
the transition metal is one or more of Mn, Fe, Ni, Cu and Zn, the rare earth element in the rare earth compound is one of La, Ce and Pr, and goldThe metal oxide being Al2O3ZrO or SnO2One or a mixture of several of (a); the alkali metal compound is a compound containing one or more elements of Li, Na and K; the alkaline earth metal compound is a compound of one or more elements of Mg, Ca and Ba.
1. A catalyst for catalytic combustion of VOCs comprises a monolithic honeycomb carrier, wherein the carrier material is high-quality ceramic cordierite or porous metal, and the surface of the carrier is coated with a nano material coating as a basic coating; the carrier is loaded with a mixture consisting of a main active component, a second active component, a cocatalyst, a modifier, a dispersant and an adhesive; 0.01-0.5 g/L of noble metal is loaded as a main active component of the catalyst, 1-10% of transition metal is compounded as a second active component by taking the mass of a carrier as a reference, 1-10% of rare earth compound or metal oxide is introduced as a cocatalyst, 0.1-5% of alkali metal or alkaline earth metal compound is introduced as a modifier, and 5-30% of aluminum sol or silica sol is used as a dispersing agent and an adhesive.
2. The ceramic cordierite or the porous metal material is a square or cylindrical honeycomb body, the size of a pore is 200-800 meshes, and the honeycomb body is subjected to surface treatment for later use by 1-10% of dilute nitric acid and dilute hydrochloric acid solution before use.
3. The base coating nanometer material is a solid solution formed by nitrate or aluminum oxide of metal aluminum and one of metal oxides of titanium, cerium, zirconium, lanthanum and the like, and AlX(Ti/Ce/Zr/La)yO2Wherein x is y (3-7) and (7-3).
4. The acid used for preparing the solid solution is one of citric acid or acetic acid.
5. The noble metal element is at least one of Au, Pt, Pd, Ru and Rh.
6. The transition metal element is one or more of Mn, Fe, Ni, Cu and Zn; the rare earth elements are La, Ce and Pr; the metal oxide being Al2O3ZrO or SnO2One or more of the above; the alkali metal compound is a compound containing one or more elements of Li, Na or K; the alkaline earth metal compound is a compound of one or more elements of Mg, Ca or Ba.
7. The catalyst is prepared by adopting an automatic coating production line and is used for automatically carrying out proportioning addition, stirring, homogenizing, grinding, sizing and coating of raw materials of the catalyst and controlling indexes of pressure, temperature, flow, weight and the like in the process.
8. A preparation method of a catalyst for catalytic combustion of VOCs comprises the following steps:
(1) honeycomb carrier pretreatment
Treating the honeycomb ceramic carrier with 1-10% of dilute nitric acid, soaking the honeycomb ceramic carrier in aluminum sol or silica sol after treatment, taking out the honeycomb ceramic carrier after full soaking, drying and roasting; wherein the drying temperature is 80-150 ℃, and the drying time is 1-5 h; the roasting temperature is 400-.
(2) Preparation of nano-coating solid solution
Taking Al (NO)3)3Diluting the solution and transition metal nitrate or rare earth metal nitrate with deionized water, heating and stirring under acidic condition until colloid is formed, and sintering to form solid solution AlX MyO2A composite oxide.
(3) Preparation and loading of cocatalyst coating slurry
Taking solid solution AlX MyO2Mixing and grinding the mixture with rare earth oxide for 2-6h, adding deionized water during grinding, controlling the particle size of grinding particles to be nano-scale, then mixing the grinding material with silica sol or aluminum sol, and adding a modifier with a certain molar ratio to obtain sol with dispersed cocatalyst;
(4) preparation of active component of catalyst
Fully mixing noble metal salt and transition metal salt solution according to a molar ratio, adding the cocatalyst sol obtained in the step (2), stirring and grinding, and uniformly dispersing to obtain slurry for later use, wherein the preparation process is completed by an automatic pulping system;
(5) catalyst support coating
Soaking the honeycomb carrier treated in the step (1) in the slurry prepared in the step (3) in the same volume, airing and aging after saturation, putting the honeycomb carrier into a drying oven for temperature programming and drying, then transferring the honeycomb carrier into a muffle furnace for high-temperature roasting, and cooling to obtain the monolithic honeycomb structure catalyst, wherein the carrier is in high-strength combination with the active component; wherein the temperature programming rate is 5-10 ℃/min, the drying temperature is 80-150 ℃, and the drying time is 1-5 h; the roasting temperature is 400-800 ℃, and the roasting time is 2-6 h.
The invention belongs to the field of treatment of industrial waste gas polluted by atmospheric environment, and particularly relates to a catalyst for industrial catalytic oxidation of VOCs and a preparation method thereof. The catalyst can be used for CO and RCO catalytic combustion devices for treating industrial VOCs, can also be used for a large-scale diesel vehicle tail gas treatment system, and has high treatment efficiency and no secondary pollution.
Volatile Organic Compounds (VOCs) seriously affect the atmospheric environment and human health, control of pollution caused by the VOCs becomes an important work for preventing and treating atmospheric pollution, and national governments and environmental protection departments pay high attention to the pollution control and continuously tighten the emission standards of the VOCs. The recovery and destruction technology is two main technical routes for treating VOCs in the industrial waste gas at present. The adsorption concentration-catalytic combustion technology is a fully combined recovery and destruction mode, VOCs are adsorbed by using an adsorbent, then the VOCs are enriched and concentrated by changing certain physical conditions, the concentration of the concentrated VOCs is increased, and certain chemical conditions are changed by using the characteristic that the VOCs is easy to combust, so that the VOCs are combusted and decomposed into CO2And H2O and the like.
The catalytic combustion technology is proven to be a practical and efficient VOCs purification technology, and the VOCs in the waste gas can be completely combusted at a lower ignition temperature by adopting a proper catalyst, and a large amount of heat emitted by combustion can be circularly used for providing system heat. The more efficient the catalyst, the lower the ignition temperature of VOCs, the higher the purification efficiency, and no secondary pollution. Therefore, as the core of catalytic combustion technology, the development of catalysts has attracted extensive attention of researchers at home and abroad.
The catalysts for catalytic oxidation of VOCs are mainly divided into two types: noble metal catalysts and non-noble metal catalysts. Noble metal catalysts are superior to non-noble metal catalysts in terms of low-temperature activity, thermal stability and the like, and thus are widely used in industry. However, the noble metal is expensive and the application thereof is greatly limited due to the shortage of resources. The use amount of noble metal is reduced under the condition of ensuring the activity of the catalyst, the noble metal and the transition metal are compounded and loaded on the modified rare earth oxide, the rare earth oxide is taken as an auxiliary agent to be beneficial to the dispersion and sintering of the main active component, and further the catalytic activity is fully exerted, and compared with a single noble metal catalyst, the supported composite oxide catalyst has more superiority in the aspects of reducing the cost, catalyzing the activity and the like.
The industrial VOCs catalyst adopts an integral honeycomb structure, has larger volume compared with a spherical or strip catalyst, and has higher difficulty in uniformly coating active components. At present, most of the production is still carried out by adopting a manual coating mode, and the efficiency is extremely low. Aiming at the defects, the company improves the production process of the catalyst, and provides a novel VOCs honeycomb catalyst batching, pulping, dipping and roasting integrated automatic production process. The prepared integral honeycomb catalyst has good mass and heat transfer effects, small wind resistance, good mechanical strength, short-time impact temperature resistance of 900 ℃ and long service life.
The invention overcomes the defects of the existing catalyst formula design and processing technology, provides a compounding technology with low noble metal loading capacity, and prepares the catalyst for catalyzing and oxidizing VOCs at low temperature and high efficiency. The catalyst prepared by the method has high activity, the T90 can be reduced to about 200 ℃ at the lowest, the system removal efficiency is more than 99 percent under proper process conditions, and VOCs are completely converted into CO2And H2O, no other pollutants are generated; the coating has high adhesive force, good thermal stability and good ageing resistance and poisoning resistance.
The following are specific examples of the present invention and further describe the preparation method of a catalyst for catalytic combustion of VOCs according to the present invention, but the scope of the present invention is not limited thereto.
Example 1
The preparation method of the catalyst for catalytic combustion of VOCs comprises the following steps:
(1) honeycomb carrier pretreatment
Treating a square cordierite honeycomb carrier with the specification of 150 multiplied by 100 with a 5% dilute nitric acid solution, washing the treated cordierite honeycomb carrier to be neutral by deionized water after treatment, preparing aluminum sol with the solid content of 20%, fully soaking the treated cordierite honeycomb carrier in silica sol, taking out the carrier after soaking saturation, drying the carrier at 80 ℃ for 2h, and roasting the carrier at 400 ℃ for 4h to obtain the treated honeycomb carrier for later use.
(2) Preparation of catalyst coating slurry
Measuring an appropriate amount of Al (NO)3)3Powder and Ce (NO)3)3Diluting and mixing the powder with deionized water, adding acetic acid to adjust the acid environment, stirring and heating to obtain colloid, and forming solid solution AlCoO after drying and sintering2(ii) a Mixing 6kg of aluminum cerium composite oxide AlCeO2The powder is evenly dispersed in the alumina sol, and then 0.1mol of BaSO as a modifier is added4To obtain the cocatalyst colloidal liquid.
(3) Preparation of active component of catalyst
0.15g/ml of Pt (NO3) was measured2Diluting the solution 5L with deionized water to 10L, adding 100g CuSO4And (3) fully mixing, adding the cocatalyst sol prepared in the step (2), stirring and grinding by a grinder, performing 2 cycles, and grinding the coating to a nanometer level to obtain the catalyst coating slurry.
(4) Catalyst support coating
Coating the ceramic honeycomb carrier treated in the step (2) by a coating system conveying line, conveying the slurry prepared in the step (3) to a slurry tank of the coating system, setting a program for coating, automatically operating a manipulator for soaking for 5s, turning over by 180 s, soaking for 5s again, taking out after saturation, airing and aging the honeycomb body through an air duct, putting the honeycomb body into an oven, heating to 120 ℃ at the speed of 5 ℃/min for drying for 2h, transferring to a muffle furnace for high-temperature roasting at the temperature of 500 ℃ for 4h, and cooling to obtain the high-strength integrated honeycomb structure catalyst with the carrier and the active components combined.
Example 2
The preparation method of the catalyst for catalytic combustion of VOCs comprises the following steps:
(1) honeycomb carrier pretreatment
Treating a square cordierite honeycomb carrier with the specification of 150 multiplied by 100 with a 5% dilute nitric acid solution, washing the treated cordierite honeycomb carrier to be neutral by deionized water after treatment, preparing aluminum sol with the solid content of 25%, fully soaking the treated cordierite honeycomb carrier in silica sol, taking out the carrier after the soaking saturation, drying the carrier at 80 ℃ for 2h, and roasting the carrier at 600 ℃ for 4h to obtain the treated honeycomb carrier for later use.
(2) Preparation of catalyst coating slurry
Measuring an appropriate amount of Al (NO)3)3Powder and Ce (NO)3)3Diluting and mixing the powder with deionized water, adding citric acid to adjust the acid environment, stirring and heating to obtain colloid, and forming solid solution AlCeO after drying and sintering2(ii) a Mixing 6kg of aluminum cerium composite oxide AlCeO2The powder is evenly dispersed in the alumina sol, and then 0.1mol of BaSO as a modifier is added4To obtain the cocatalyst colloidal liquid.
(3) Preparation of active component of catalyst
0.15g/ml of Pt (NO3) was measured2Solution 3L, 0.2g/ml Pd (NO3)2Diluting the solution 3L with deionized water to 12L, adding 100g CuSO4And (3) fully mixing, adding the cocatalyst sol prepared in the step (2), stirring and grinding by a grinder, performing 2 cycles, and grinding the coating to a nanometer level to obtain the catalyst coating slurry.
(4) Catalyst support coating
Coating the ceramic honeycomb carrier treated in the step (2) by a coating system conveying line, conveying the slurry prepared in the step (3) to a slurry tank of the coating system, setting a program for coating, automatically operating a manipulator for soaking for 5s, turning over by 180 s, soaking for 5s again, taking out after saturation, airing and aging the honeycomb body through an air duct, putting the honeycomb body into an oven, heating to 120 ℃ at the speed of 5 ℃/min for drying for 2h, transferring to a muffle furnace for high-temperature roasting at the temperature of 600 ℃ for 4h, and cooling to obtain the high-strength integrated honeycomb structure catalyst with the carrier and the active components combined.
Example 3
The preparation method of the catalyst for catalytic combustion of VOCs comprises the following steps:
(1) honeycomb carrier pretreatment
Treating a square cordierite honeycomb carrier with the specification of 150 multiplied by 100 with a 5% dilute nitric acid solution, washing the treated cordierite honeycomb carrier to be neutral by deionized water after treatment, preparing aluminum sol with the solid content of 20%, fully soaking the treated cordierite honeycomb carrier in silica sol, taking out the carrier after soaking saturation, drying the carrier at 80 ℃ for 4h, and roasting the carrier at 800 ℃ for 2h to obtain the treated honeycomb carrier for later use.
(2) Preparation of catalyst coating slurry
Measuring a proper amount of gamma-Al2O3Powder and La2O3Diluting and mixing the powder with deionized water, adding citric acid to adjust the acid environment, stirring and heating to obtain colloid, and forming solid solution AlLaO after drying and sintering2(ii) a Mixing AlLaO which is an aluminum-lanthanum composite oxide with the weight of 5kg2The powder is evenly dispersed in the alumina sol, and then 0.1mol of modulating agent MgSO is added4To obtain the cocatalyst colloidal liquid.
(3) Preparation of active component of catalyst
0.15g/ml of Pt (NO3) was measured22L of solution, 0.2g/ml of Pd (NO3)2Diluting 3L of the solution into 10L of the solution by using deionized water, adding 100g of MnO, fully mixing, and simultaneously adding the AlLaO prepared in the step (2)2Stirring and grinding the mixture by a grinder, and performing 2 cycles to prepare catalyst coating slurry;
(4) catalyst support coating
Coating the ceramic honeycomb carrier treated in the step (2) by a coating system conveying line, conveying the slurry prepared in the step (3) to a slurry tank of the coating system, setting a program for coating, automatically operating a mechanical arm for soaking for 5s, turning over by 180 degrees, soaking for 5s again, taking out after saturation, airing and aging the honeycomb body through an air duct, putting the honeycomb body into an oven, heating to 100 ℃ at the speed of 5 ℃/min for drying for 3h, then transferring to a muffle furnace for high-temperature roasting at the temperature of 800 ℃ for 2h, and cooling to obtain the high-strength integrated honeycomb structure catalyst with the carrier and the active component.
Example 4
The preparation method of the catalyst for catalytic combustion of VOCs comprises the following steps:
(1) honeycomb carrier pretreatment
Treating a square cordierite honeycomb carrier with the specification of 150 multiplied by 100 with a 5% diluted hydrochloric acid solution, washing the treated cordierite honeycomb carrier to be neutral by deionized water after treatment, preparing aluminum sol with the solid content of 25%, fully soaking the treated cordierite honeycomb carrier in silica sol, taking out the carrier after soaking saturation, drying the carrier at 100 ℃ for 2h, and roasting the carrier at 800 ℃ for 2h to obtain the treated honeycomb carrier for later use.
(2) Preparation of catalyst coating slurry
Measuring a proper amount of gamma-Al2O3Powder and Pr6O11Diluting and mixing the powder with deionized water, adding acetic acid to adjust the acid environment, stirring and heating to obtain a colloid, and forming a solid solution praseodymium aluminum composite oxide PrAl after drying and sintering11O9(ii) a PrAl of praseodymium-aluminum composite oxide with the weight of 5kg11O9The powder is evenly dispersed in the alumina sol, and then 0.1mol of modulating agent NaCl is added to obtain the cocatalyst colloidal fluid.
(3) Preparation of active component of catalyst
0.15g/ml of H is measured2PtCl62L of the solution, and 0.2g/ml of PdCl is measured2Diluting 3L of the solution with deionized water to 10L, adding 100g SnO2Fully mixing, and simultaneously adding the praseodymium-aluminum composite oxide PrAl prepared in the step (2)11O9Stirring and grinding the mixture by a grinder, and performing 2 cycles to prepare catalyst coating slurry;
(4) catalyst support coating
Coating the ceramic honeycomb carrier treated in the step (2) by a coating system conveying line, conveying the slurry prepared in the step (3) to a slurry tank of the coating system, setting a program for coating, automatically operating a mechanical arm for soaking for 5s, turning over by 180 s, soaking for 5s again, taking out after saturation, airing and aging the honeycomb body through an air duct, putting the honeycomb body into an oven, heating to 100 ℃ at the speed of 5 ℃/min for drying for 3h, transferring into a muffle furnace for high-temperature roasting at the temperature of 800 ℃ for 3h, and cooling to obtain the high-strength integrated honeycomb structure catalyst with the carrier and the active components combined.
Claims (9)
1. A catalyst for the catalytic combustion of VOCs, comprising: the catalyst comprises an integral honeycomb carrier, wherein the carrier material is high-quality ceramic cordierite or porous metal, and a nano material coating is coated on the surface of the carrier to be used as a basic coating; the carrier is loaded with a mixture consisting of a main active component, a second active component, a cocatalyst, a modifier, a dispersant and an adhesive; wherein the main active component is noble metal of 0.01-0.5 g/L; based on the mass of the carrier, the second active component is 1-10% of transition metal, the cocatalyst is 1-10% of rare earth compound or metal oxide, the modifier is 0.1-5% of alkali metal or alkaline earth metal compound, the dispersant and the adhesive are 5-30% of aluminum sol or silica sol.
2. The catalyst of claim 1 for the catalytic combustion of VOCs, wherein: the carrier is square or cylindrical honeycomb-shaped, the size of a honeycomb hole is 200-800 meshes, and the carrier is subjected to surface treatment for later use by using 1-10% dilute nitric acid and dilute hydrochloric acid solution before use.
3. The catalyst of claim 1 for the catalytic combustion of VOCs, wherein: the nano material of the basic coating is a solid solution prepared from nitrate or aluminum oxide of metal aluminum and one of metal oxides of titanium, cerium, zirconium and lanthanum under an acidic condition, and the molecular expression of the solid solution is as follows: AlX (Ti/Ce/Zr/La)yO2, wherein x: y is (3-7) and (7-3).
4. The catalyst of claim 1 for the catalytic combustion of VOCs, wherein: the acid used in the acidic condition is citric acid or acetic acid.
5. The catalyst of claim 1 for the catalytic combustion of VOCs, wherein: the noble metal of the main active component is one or a mixture of Au, Pt, Pd, Ru and Rh.
6. The catalyst of claim 1 for the catalytic combustion of VOCs, wherein: the transition metal is one or more of Mn, Fe, Ni, Cu and Zn, the rare earth element in the rare earth compound is one of La, Ce and Pr, and the metal oxide is Al2O3ZrO or SnO2One or a mixture of several of (a); the alkali metal compound is a compound containing one or more elements of Li, Na and K; the alkaline earth metal compound is a compound of one or more elements of Mg, Ca and Ba.
7. A method for preparing a catalyst for catalytic combustion of VOCs according to any of claims 1 to 6, comprising: the method comprises the following steps:
first step, honeycomb carrier pretreatment
Treating the honeycomb ceramic carrier with 1-10% of dilute nitric acid, soaking the honeycomb ceramic carrier in aluminum sol or silica sol after treatment, taking out the honeycomb ceramic carrier after full soaking, drying and roasting; wherein the drying temperature is 80-150 ℃, and the drying time is 1-5 h; the roasting temperature is 400-;
second, preparation of nano-coating solid solution
Taking Al (NO)3)3Diluting the solution and transition metal nitrate or rare earth metal nitrate with deionized water, heating and stirring under acidic condition until colloid is formed, and sintering to form solid solution AlX MyO2A composite oxide;
thirdly, preparing and loading cocatalyst coating slurry
Taking solid solution AlXMyO2Mixing and grinding the mixture with rare earth oxide for 2-6h, adding deionized water during grinding, controlling the particle size of grinding particles to be nano-scale, then mixing the grinding material with silica sol or aluminum sol, and adding a modifier with a certain molar ratio to obtain sol with dispersed cocatalyst;
the fourth step, preparation of the active component of the catalyst
Fully mixing the noble metal salt and the transition metal salt solution according to the molar ratio, adding the cocatalyst sol obtained in the second step, stirring and grinding, and uniformly dispersing to obtain slurry for later use, wherein the preparation process is completed by an automatic pulping system;
the fifth step, catalyst carrier coating
Soaking the honeycomb carrier treated in the first step in the slurry prepared in the third step in an equal volume, airing and aging after soaking saturation, putting the honeycomb carrier into a drying oven for temperature programming and drying, then transferring the honeycomb carrier into a muffle furnace for high-temperature roasting, and cooling to obtain the integral honeycomb structure catalyst, wherein the carrier is in high-strength combination with active components; wherein the temperature programming rate is 5-10 ℃/min, the drying temperature is 80-150 ℃, and the drying time is 1-5 h; the roasting temperature is 400-800 ℃, and the roasting time is 2-6 h.
8. The method of claim 7 for preparing a catalyst for the catalytic combustion of VOCs, wherein: all the steps from the first step to the fifth step are prepared through an automatic coating production line, catalyst raw material proportioning addition, stirring, homogenizing, grinding, sizing and coating are automatically carried out, and the pressure, temperature, flow and weight indexes of the technological process are controlled.
9. The method of claim 7 for preparing a catalyst for the catalytic combustion of VOCs, wherein: in the first step, a honeycomb carrier is a 150 multiplied by 100 square cordierite honeycomb carrier, the honeycomb carrier is treated by a 5% dilute nitric acid solution, and then the honeycomb carrier is immersed in 20% aluminum sol, the drying temperature is 80 ℃, and the drying time is 2 hours; the roasting temperature is 400 ℃, and the roasting time is 4 hours;
the solid solution of the second step is made of Al (NO)3)3Powder and Ce (NO)3)3Diluting and mixing the powder with deionized water, adjusting the acid environment by adding acetic acid, and drying and sintering to form a solid solution of aluminum cerium composite oxide AlCoO2；
In the third step, 6kg of aluminum cerium composite oxide AlCeO is weighed2Powder solid solution with 0.1mol of BaSO as modifier4；
In the fourth step, the noble metal salt is 0.15g/ml Pt (NO3)25L of the solution is diluted into 10L by deionized water, and the transition metal salt solution is 100g of CuSO4；
In the fifth step, the temperature rise rate is 5 ℃/min, the drying temperature is 120 ℃, and the drying time is 2 h; the roasting temperature is 500 ℃, and the roasting time is 4 hours.
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