Cerium basis composite oxides doped precious metal integer catalyzer and method of manufacturing the same

A technology of composite oxides and monolithic catalysts, applied in metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problems of affecting catalytic activity, complex preparation process, and reducing Catalytic activity and other issues, to achieve the effect of high effective utilization, good catalytic performance and simple preparation process

Inactive Publication Date: 2008-01-23
ZHEJIANG NORMAL UNIVERSITY
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AI-Extracted Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to aim at the Al of existing catalytic combustion monolithic catalyst 2 o 3 The process of coating preparation process is complicated and the cycle is long; additive powder, γ-Al 2 o 3 The bonding strength between the coating and the carrier is low, and it is easy to crack and fall off, which directly affects the catalytic activity. At high temperature, the added oxide additive powder is easy to combine with Al 2 o 3 The coating undergoes a solid-...
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Abstract

The invention is a ceric pyridyl compound oxide mixing with precious metal whole catalyst used for organic waste gas catalyzing burning purifying process and the preparation method, which aims to the defects of existing Pt/Ce0.68Zr0.32O2 whole catalyst preparation method with complicate preparation technique and chap on coating under high temperature, to provide a ceric pyridyl compound oxide mixing with precious metal whole catalyst with high catalyzing activity, heat stability and integration intensity and the preparation method. The catalyst comprises honeycomb ceramics carrier, addition agent and active component, wherein, the honeycomb ceramics carrier is cordierite honeycomb ceramics, the addition agent is ceric pyridyl compound oxide with the chemical formula CexM1-xO Delta, the active component is one or two of precious metal Pd and Pt. The preparation method comprises preparing soakage solution and the coating of the soakage solution on the honeycomb ceramics carrier two procedures.

Application Domain

Technology Topic

Examples

  • Experimental program(5)

Example Embodiment

[0031] Example 1
[0032] (1) Preparation of dipping solution:
[0033] a. Prepare precious metal active component precursor solution, weigh 1.159g PdCl 2 , Add 5.0mL of 1.0mol·L -1 Dissolve in dilute hydrochloric acid to form H with a concentration of 6.954g/L 2 PdCl 4 Solution
[0034] b. Weigh 3.729g Ce(NO 3 ) 3 ·6H 2 O(AR), 0.922g Zr(NO 3 ) 4 ·5H 2 O(AR), add 11.0mL of deionized water to dissolve, prepare a mixed solution of soluble cerium salt and soluble metal zirconium salt;
[0035]c. Add 3.383g of citric acid (AR) to the above solution and stir evenly;
[0036] d. Heat the above solution in a water bath at 80°C, add 1.8mL 95% ethanol dispersant; after dispersion, add 0.96g polyethylene glycol (molecular weight M=10000) nonionic surfactant; wait for surface activity After the agent is completely dissolved, take 6.954g/L of H 2 PdCl 4 4.2mL of the solution was added to the solution; the whole step was carried out under constant stirring;
[0037] e. Heat the above solution in a water bath at 80°C and stir for 5 minutes to obtain an immersion solution.
[0038] (2) Coating of dipping liquid on honeycomb ceramic carrier:
[0039] a. The cordierite honeycomb ceramic with a mass of 29.04g, a size of 48mm×24mm×40mm, and an opening rate of 31 holes/cm2 is immersed in the impregnating solution and then taken out to remove the impregnating solution remaining in the pores of the honeycomb ceramic carrier. The impregnation solution is the residual impregnation solution;
[0040] b. Let the honeycomb ceramics stand for 16 hours, then put them in an oven at 130°C and dry for 4 hours;
[0041] c. Transfer the above honeycomb ceramics into a muffle furnace and fire at 400°C for 1 hour;
[0042] d. Heat the residual immersion solution in a water bath at 80°C for 5 minutes. After the residual immersion solution is heated, immerse the honeycomb ceramic in the residual immersion solution and take it out to remove the immersion solution remaining in the pores of the honeycomb ceramic carrier;
[0043] e. Let the honeycomb ceramics stand for 16 hours, then put them in an oven at 130°C and dry for 4 hours;
[0044] f. Transfer the above honeycomb ceramics into a muffle furnace and calcinate at 400°C for 2 hours; Pd-Ce is obtained 0.8 Zr 0.2 O 2 The overall catalyst, in which the content of Pd is 0.1% of the honeycomb ceramic carrier, and Ce 0.8 Zr 0.2 O 2 The content is 6% of the honeycomb ceramic carrier.
[0045] (3) Evaluation of the catalytic performance of the catalyst:
[0046] Pd-Ce with a size of 48mm×24mm×40mm 0.8 Zr 0.2 O 2 The whole catalyst is cut into two cylinders with a diameter of 21mm×40mm in length, and then the catalysts of these two cylinders are loaded into the catalytic reactor.
[0047] The evaluation reaction was carried out in a traditional fixed-bed flow reactor, and the complete oxidation of toluene was used as a probe reaction. Toluene is brought into the fixed-bed catalytic reactor by air, and its content in air is 3.33±0.67g·m -3 , The space velocity of the reaction is 10800h -1. The concentration of toluene in the reactant and product was analyzed by the FID detector of the GC-14C (Shimadzu) gas chromatograph. The conversion rate of toluene is calculated using the following formula:
[0048] Conversion rate of toluene (%)=[(concentration of toluene in the reactant-concentration of toluene in the product)/concentration of toluene in the reactant]×100
[0049] At each temperature, when the reaction reaches a stable state, analyze the composition. The Pd-Ce 0.8 Zr 0.2 O 2 The toluene conversion rate of the monolithic catalyst is 97.4% at 210°C.

Example Embodiment

[0050] Example 2
[0051] (1) Preparation of dipping solution:
[0052] a. Prepare the precursor solution of the precious metal active component, H 2 PdCl 4 The solution was prepared according to the method in Example 1, and the concentration was 6.954g/L;
[0053] b. Weigh 2.068g Ce(NO 3 ) 3 ·6H 2 O(AR), 3.067g Zr(NO 3 ) 4 ·5H 2 O(AR), add 11.0mL of deionized water to dissolve, and prepare a mixed solution of soluble cerium salt and soluble metal zirconium salt;
[0054] c. Add 3.752g of citric acid (AR) to the above solution and stir evenly;
[0055] d. Heat the above solution in a water bath at 80°C, add 1.8mL 95% ethanol dispersant; after dispersion, add 0.96g polyethylene glycol (molecular weight M=10000) nonionic surfactant; wait for surface activity After the agent is completely dissolved, take 6.954g/L of H 2 PdCl 4 4.1 mL of solution was added to the solution; the whole step was carried out under constant stirring;
[0056] e. Heat the above solution in a water bath at 80°C and stir for 5 minutes to obtain an immersion solution.
[0057] (2) Coating of dipping liquid on honeycomb ceramic carrier:
[0058] a. Immerse the cordierite honeycomb ceramic with a mass of 28.33g, a size of 48mm×24mm×40mm, and a porosity of 31 holes/cm2 into the impregnating solution and remove the impregnating solution remaining in the pores of the honeycomb ceramic carrier. The impregnation solution is the residual impregnation solution;
[0059] b. Let the honeycomb ceramics stand for 16 hours, then put them in an oven at 130°C and dry for 4 hours;
[0060] c. Transfer the above honeycomb ceramics into a muffle furnace and fire at 400°C for 1 hour;
[0061] d. Heat the residual immersion solution in a water bath at 80°C for 5 minutes. After the residual immersion solution is heated, immerse the honeycomb ceramic in the residual immersion solution and take it out to remove the immersion solution remaining in the pores of the honeycomb ceramic carrier;
[0062] e. Let the honeycomb ceramics stand for 16 hours, then put them in an oven at 130°C and dry for 4 hours;
[0063] f. Transfer the above honeycomb ceramics into a muffle furnace and calcinate at 400°C for 2 hours; Pd-Ce is obtained 0.8 Zr 0.2 O 2 The overall catalyst, in which the content of Pd is 0.1% of the honeycomb ceramic carrier, and Ce 0.8 Zr 0.2 O 2 The content is 6% of the honeycomb ceramic carrier.
[0064] (3) Evaluation of the catalytic performance of the catalyst:
[0065] According to the method of Example 1, the Pd-Ce 0.4 Zr 0.6 O 2 The toluene conversion rate of the monolithic catalyst is 96.9% at 210°C.

Example Embodiment

[0066] Example 3
[0067] (1) Preparation of dipping solution:
[0068] a. Prepare the precursor solution of the precious metal active component, H 2 PdCl 4 The solution was prepared according to the method in Example 1, and the concentration was 6.954g/L;
[0069] b. Weigh 3.557g Ce(NO 3 ) 3 ·6H 2 O(AR), 0.879g Zr(NO 3 ) 4 ·5H 2 O(AR), add 11.0mL of deionized water to dissolve, and prepare a mixed solution of soluble cerium salt and soluble metal zirconium salt;
[0070] c. Add 3.228g of citric acid (AR) to the above solution and stir evenly;
[0071] d. Heat the above solution in a water bath at 80°C, and add 1.8 mL of 95% ethanol dispersant. After the dispersion is completed, add 0.96g polyethylene glycol (molecular weight M=10000) non-ionic surfactant; after the surfactant is completely dissolved, take 6.954g/L of H 2 PdCl 4 Add 4.0 mL of the solution to the solution; the entire step is carried out under constant stirring;
[0072] e. Heat the above solution in a water bath at 80°C and stir for 5 minutes to obtain an immersion solution.
[0073] (2) Coating of dipping liquid on honeycomb ceramic carrier:
[0074] a. Immerse the cordierite honeycomb ceramic with a mass of 27.70g, a size of 48mm×24mm×40mm, and a porosity of 31 holes/cm2 into the impregnating solution and remove the impregnating solution remaining in the pores of the honeycomb ceramic carrier. The impregnation solution is the residual impregnation solution.
[0075] b. Let the honeycomb ceramics stand for 16 hours, then put them in an oven at 130°C and dry for 4 hours;
[0076] c. Transfer the above honeycomb ceramics into a muffle furnace and fire at 400°C for 1 hour;
[0077] d. Heat the residual immersion solution in a water bath at 80°C for 5 minutes. After the residual immersion solution is heated, immerse the honeycomb ceramic in the residual immersion solution and take it out to remove the immersion solution remaining in the pores of the honeycomb ceramic carrier;
[0078] e. Let the honeycomb ceramics stand for 16 hours, then put them in an oven at 130°C and dry for 4 hours;
[0079] f. Transfer the above honeycomb ceramics into a muffle furnace and fire at 1000°C for 2 hours; then Pd-Ce fired at 1000°C is obtained 0.8 Zr 0.2 O 2 The overall catalyst, in which the content of Pd is 0.1% of the honeycomb ceramic carrier, and Ce 0.8 Zr 0.2 O 2 The content is 6% of the honeycomb ceramic carrier.
[0080] (3) Evaluation of the catalytic performance of the catalyst:
[0081] According to the method of Example 1, the Pd-Ce calcined at 1000°C 0.8 Zr 0.2 O 2 The conversion rate of toluene of the monolithic catalyst is 93.6% at 240°C.
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