CN112403490A - Sulfur-resistant catalyst, preparation method and application - Google Patents
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Abstract
The invention provides a preparation method of a sulfur-resistant catalyst, which comprises the following steps: s1, weighing SiO2And Al2O3Adding the powder into deionized water and stirring; then adding TiO2Uniformly stirring the powder and the metal compound to obtain a mixed solution; s2, adding the noble metal active component into the mixed solution, ultrasonically stirring and uniformly mixing to obtain the productTo a coating slurry; s3, completely immersing the ceramic carrier into the slurry, blowing redundant slurry in pores through airflow, drying for 10-50 min, and finally calcining at 350-1000 ℃ to obtain the sulfur-resistant catalyst. The sulfur-resistant catalyst has the advantages of strong sulfur resistance, simple preparation method and low cost.
Description
Technical Field
The invention relates to a sulfur-resistant catalyst and a preparation method thereof, belonging to the technical field of catalysts.
Background
According to the definition of the world health organization, the compound is Volatile Organic Compounds (VOCs) if the boiling point of the compound is 50 ℃ to 250 ℃ under the pressure of 101.32 kPa. They may exist in a gaseous form at normal temperature. According to the difference of the chemical structure, the method can be further divided into eight types: alkanes, aromatic hydrocarbons, alkenes, halogenated hydrocarbons, esters, aldehydes, ketones, and others. The main components of VOCs are: hydrocarbons, halogenated hydrocarbons, oxygen hydrocarbons and nitrogen hydrocarbons, which include: benzene series, organic chloride, freon series, organic ketone, amine, alcohol, ether, ester, acid and petroleum hydrocarbon compound. In recent years, with the development of industrialization, a large amount of organic waste gas is discharged, wherein waste gas in industries such as petrochemical industry, modern coal chemical industry, chemical industry (coating, ink, adhesive, pharmacy, pesticide, coking), industrial coating (whole automobile, furniture, engineering machinery, industrial coating), packaging printing (plastic, paper, metal packaging printing), oil storage and transportation and the like becomes a main source of atmospheric VOCs.
The harm of Volatile Organic Compounds (VOCs) is very obvious. When the concentration of volatile organic compounds in a room exceeds a certain concentration, people feel headache, nausea, vomiting and limb weakness in a short time; severe cases may cause convulsion, coma, and hypomnesis; volatile organic compounds harm the liver, kidneys, brain and nervous system of a person; it also contains many carcinogenic substances. Therefore, the VOCs cause serious environmental pollution, and need to be treated in an industrial production process.
At present, the common VOCs treatment technologies in industry include adsorption technology, thermal incineration technology, biotechnology, catalytic combustion technology, plasma technology, and the like. The catalytic combustion technology has high treatment efficiency and no secondary pollution, and can convert VOCs into CO at lower temperature2And H2O and other harmless substances, and has higher operation safety and high potential value for organic waste gas treatment. But because ofPart of the industrial waste gas contains H2S、SO2Sulfur-containing components such as methyl mercaptan, etc., which cause poisoning and deactivation of noble metal catalysts used in catalytic combustion technology, thereby limiting the wide application of catalytic combustion technology. Therefore, research and development of catalysts with sulfur poisoning resistance and lower cost become the key for the development of catalytic combustion technology.
Disclosure of Invention
The invention provides a sulfur-resistant catalyst and a preparation method thereof, which can effectively solve the problems.
The invention is realized by the following steps:
a preparation method of a sulfur-resistant catalyst comprises the following steps:
s1, weighing SiO2And Al2O3Adding the powder into deionized water and stirring; then adding TiO2Uniformly stirring the powder and the metal compound to obtain a mixed solution;
s2, adding a noble metal active component into the mixed solution, ultrasonically stirring, and uniformly mixing to obtain coating slurry;
s3, completely immersing the ceramic carrier into the slurry, blowing redundant slurry in pores through airflow, drying for 10-50 min, and finally calcining at 350-1000 ℃ to obtain the sulfur-resistant catalyst.
As a further improvement, the metal composite is selected from CeO2、MnO2、ZrO2One or more of Co-Mn, Ce-Zr-Mn.
As a further improvement, one or two of the noble metal active components Pt, Pd and Ru are used.
As a further improvement, the SiO2、Al2O3、TiO2The mass fractions of the metal compound and the noble metal active component in the coating slurry are respectively 0.5-30%, 0.5-40%, 3-50%, 1-20% and 0.01-1.0%.
As a further improvement, the ceramic carrier is a honeycomb ceramic carrier.
As a further improvement, after step S1, the method further includes: and S11, adding polyvinyl alcohol into the mixed solution and stirring.
As a further improvement, after step S11, the method further includes: s12, adjusting the pH value to 7-13.
As a further improvement, the time of ultrasonic stirring is 50-240 min.
A sulfur-resistant catalyst prepared by the preparation method.
An application of the sulfur-resistant catalyst in volatile organic compound treatment.
The invention has the beneficial effects that:
TiO is added into the coating of the sulfur-resistant catalytic combustion catalyst2Can improve the conversion rate and the high-temperature stability of the catalyst, and is added with CeO2、MnO2、ZrO2Metal compounds such as Co-Mn, Ce-Zr-Mn and the like can improve the catalytic activity to organic matters; simultaneously adding SiO2And Al2O3The acting force between the coating and the surface of the carrier can be enhanced, the coating can be effectively prevented from falling off and the active components can be effectively prevented from being reduced, and the cost is lower.
The invention obtains the coating by simple mixing and stirring, and then coats the coating on the surface of the carrier by dipping, and has the advantages of simple preparation process and equipment, easy operation and the like.
The catalyst prepared by the invention still has higher catalytic efficiency and good high-temperature resistance stability to the waste gases such as propane, methane and the like after vulcanization treatment.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 shows the catalyst pair propane (C) before and after sulfiding of the catalyst of example 1 of the invention3H8) Temperature-conversion ofA plot of the rate.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings of the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
In the description of the present invention, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
The invention provides a preparation method of a sulfur-resistant catalyst, which comprises the following steps:
s1, weighing SiO2And Al2O3Adding the powder into deionized water and stirring; then adding TiO2And uniformly stirring the powder and the metal compound to obtain a mixed solution. Simultaneously adding SiO2And Al2O3The powder can enhance the acting force of the coating and the surface of the carrier, effectively prevent the coating from falling off and reduce the active components, and has lower cost. Adding TiO2The conversion rate and the high-temperature stability of the catalyst can be improved.
S2, adding a noble metal active component into the mixed solution, ultrasonically stirring, and uniformly mixing to obtain coating slurry;
s3, completely immersing the ceramic carrier into the slurry, blowing redundant slurry in pores through airflow, drying for 10-50 min, and finally calcining at 350-1000 ℃ to obtain the sulfur-resistant catalyst.
As a further improvement, the metal composite is selected from CeO2、MnO2、ZrO2One or more of Co-Mn, Ce-Zr-Mn. The catalytic activity to organic substances can be improved by adding the metal compound.
As a further improvement, one or two of the noble metal active components Pt, Pd and Ru are used.
As a further improvement, the SiO2、Al2O3、TiO2The mass fractions of the metal compound and the noble metal active component in the coating slurry are respectively 0.5-30%, 0.5-40%, 3-50%, 1-20% and 0.01-1.0%.
As a further improvement, the ceramic carrier is a honeycomb ceramic carrier.
As a further improvement, after step S1, the method further includes: and S11, adding polyvinyl alcohol into the mixed solution and stirring. The addition of polyvinyl alcohol can increase the adhesive force of the coating slurry, so that the slurry can be effectively attached to the surface of the carrier, and the high-temperature resistance stability of the catalyst is improved.
As a further improvement, after step S11, the method further includes: s12, adjusting the pH value to 7-13. In the pH range, the catalytic activity and the high temperature resistance stability of the catalyst can be ensured.
As a further improvement, the ultrasonic stirring time is 50-240min, and in the range, the sufficient and uniform stirring can be ensured, large particles in the coating slurry can be prevented, the coating can be effectively prevented from falling off and the active components can be effectively reduced, and the catalytic activity and the high-temperature resistance stability of the catalyst can be enhanced.
A sulfur-resistant catalyst prepared by the preparation method.
An application of the sulfur-resistant catalyst in volatile organic compound treatment.
Example 1
The preparation method of this example includes the following steps:
A. weighing 15 percent of SiO according to mass fraction2、10％Al2O3、30％TiO23% Co-Mn, 2% Ce-Zr, 0.04% Pt powder;
B. mixing SiO2And Al of2O3Adding the powder into deionized water and stirring;
C. then adding TiO2Stirring Co-Mn and Ce-Zr powder, and then adding 2mL of polyvinyl alcohol for stirring; adjusting the pH value to 8;
D. finally, adding Pt into the solution, ultrasonically stirring in an ultrasonic device for 100min, and fully and uniformly mixing to obtain coating slurry;
E. completely immersing a honeycomb ceramic carrier with the diameter of 100mm multiplied by 50mm into the prepared slurry, blowing redundant slurry in pores through air flow, drying in microwave for 40min, and finally calcining at 600 ℃ in air atmosphere to obtain the sulfur-resistant catalyst.
The prepared catalyst is placed at 50ppm SO2And (5) carrying out vulcanization treatment for 240h under the atmosphere to obtain the vulcanized catalyst. The method for testing the catalytic combustion activity of the pre-sulfided (fresh) and post-sulfided catalysts was as follows: in a fixed bed reactor, the catalyst was placed in a reaction tube and 5000ppm of propane (C) was introduced3H8) And 20% of O2+N2Mixed gas with space velocity of 12000h-1The reaction tail gas is analyzed by a gas chromatograph, the conversion rate at different temperatures is recorded, and the experimental result is shown in figure 1. As can be seen from FIG. 1, the catalyst had passed through a reactor containing 50ppm SO2The catalytic activity of the catalyst after the gas vulcanization treatment is not obviously reduced, but is slightly improved, which shows that the catalyst has good sulfur resistance.
Example 2
The preparation method of this example includes the following steps:
A. weighing 10% SiO by mass fraction2、15％Al2O3、30％TiO23% of Co-Mn, 2% of Ce-Zr and 0.04% of Pt powderGrinding;
B. mixing SiO2And Al2O3Adding the powder into deionized water and stirring;
C. then adding TiO2Stirring Co-Mn and Ce-Zr powder, and then adding 2mL of polyvinyl alcohol for stirring; adjusting the pH value to 9;
D. finally, adding Pt into the solution, ultrasonically stirring in an ultrasonic device for 120min, and fully and uniformly mixing to obtain coating slurry;
E. completely immersing a honeycomb ceramic carrier with the diameter of 100mm multiplied by 50mm into the prepared slurry, blowing redundant slurry in pores through air flow, drying in microwave for 30min, and finally calcining at 800 ℃ in air atmosphere to obtain the sulfur-resistant catalyst.
Example 3
The preparation method of this example includes the following steps:
A. weighing 10% SiO by mass fraction2、10％Al2O3、35％TiO23% Co-Mn, 2% Ce-Zr, 0.04% Pt powder;
B. mixing SiO2And Al2O3Adding the powder into deionized water and stirring;
C. then adding TiO2Stirring Co-Mn and Ce-Zr powder, and then adding 2mL of polyvinyl alcohol for stirring; adjusting the pH value to 10;
D. finally, adding Pt into the solution, ultrasonically stirring in an ultrasonic device for 160min, and fully and uniformly mixing to obtain coating slurry;
E. completely immersing a honeycomb ceramic carrier with the diameter of 100mm multiplied by 50mm into the prepared slurry, blowing redundant slurry in pores through air flow, drying for 50min in microwave, and finally calcining at 500 ℃ in air atmosphere to obtain the sulfur-resistant catalyst.
Example 4
The preparation method of this example includes the following steps:
A. weighing 10% SiO by mass fraction2、10％Al2O3、30％TiO25% Co-Mn, 5% Ce-Zr, 0.04% Pt powder;
B. mixing SiO2And Al2O3Adding the powder into deionized water and stirring;
C. then adding TiO2Stirring Co-Mn and Ce-Zr powder, and then adding 2mL of polyvinyl alcohol for stirring; adjusting the pH value to 9;
D. finally, adding Pt into the solution, ultrasonically stirring in an ultrasonic device for 200min, and fully and uniformly mixing to obtain coating slurry;
E. completely immersing a honeycomb ceramic carrier with the diameter of 100mm multiplied by 50mm into the prepared slurry, blowing redundant slurry in pores through air flow, drying in microwave for 40min, and finally calcining at 600 ℃ in air atmosphere to obtain the sulfur-resistant catalyst.
Comparative example 1
Without addition of TiO2The other operations are basically the same as in example 1.
Comparative example 2
The operation was substantially the same as in example 1 except that Co-Mn and Ce-Zr powders were not added.
Comparative example 3
Without addition of SiO2The other operations are basically the same as in example 1.
In order to evaluate the effect of each catalyst on the treatment of sulfur-containing organic exhaust gas, the catalyst was subjected to experimental evaluation.
The catalysts prepared in examples 1-4 and comparative examples 1-3 above were mixed at 50ppm SO2And (3) testing the catalytic combustion activity of the vulcanized catalyst after the vulcanization treatment for 240 hours in the atmosphere, and testing in a fixed bed reactor: the catalyst was placed in a reaction tube and 5000ppm of propane (C) was introduced3H8) And 20% of O2+N2Mixed gas with space velocity of 12000h-1The reaction tail gas was analyzed by gas chromatograph, and the results are shown in table 1 when the conversion rates at different temperatures were recorded.
TABLE 1 purification treatment effect of catalyst on exhaust gas
| Catalyst and process for preparing same | T50(temperature at which conversion is 50%) | T90(temperature at 90% conversion) |
| Example 1 | 285℃ | 394℃ |
| Example 2 | 289℃ | 397℃ |
| Example 3 | 287℃ | 399℃ |
| Example 4 | 280℃ | 389℃ |
| Comparative example 1 | 360℃ | 485℃ |
| Comparative example 2 | 320℃ | 443℃ |
| Comparative example 3 | 315℃ | 437℃ |
Watch with watch1, T in examples 1 to 450And T90Is obviously lower than comparative examples 1 to 3, which shows that the catalysts prepared in examples 1 to 4 have higher catalytic efficiency and good high-temperature stability.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a sulfur-resistant catalyst is characterized by comprising the following steps:
s1, weighing SiO2And Al2O3Adding the powder into deionized water and stirring; then adding TiO2Uniformly stirring the powder and the metal compound to obtain a mixed solution;
s2, adding a noble metal active component into the mixed solution, ultrasonically stirring, and uniformly mixing to obtain coating slurry;
s3, completely immersing the ceramic carrier into the slurry, blowing redundant slurry in pores through airflow, drying for 10-50 min, and finally calcining at 350-1000 ℃ to obtain the sulfur-resistant catalyst.
2. The method for preparing a sulfur-resistant catalyst according to claim 1, wherein the metal composite is selected from CeO2、MnO2、ZrO2One or more of Co-Mn, Ce-Zr-Mn.
3. The method of claim 1, wherein the noble metal active component is one or two of Pt, Pd, and Ru.
4. The method of preparing a sulfur-resistant catalyst according to claim 1, wherein the SiO is2、Al2O3、TiO2The mass fractions of the metal compound and the noble metal active component in the coating slurry are respectively 0.5-30%, 0.5-40%, 3-50%, 1-20% and 0.01-1.0%.
5. The method of preparing a sulfur-resistant catalyst according to claim 1, wherein the ceramic support is a honeycomb ceramic support.
6. The method for preparing a sulfur-resistant catalyst according to claim 1, further comprising, after step S1: and S11, adding polyvinyl alcohol into the mixed solution and stirring.
7. The method for preparing a sulfur-resistant catalyst according to claim 6, further comprising, after step S11: s12, adjusting the pH value to 7-13.
8. The method for preparing the sulfur-resistant catalyst according to claim 1, wherein the time of the ultrasonic stirring is 50 to 240 min.
9. A sulfur-resistant catalyst prepared by the preparation method according to any one of claims 1 to 8.
10. Use of a sulfur-resistant catalyst according to claim 9 in the treatment of volatile organic compounds.
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