CN112958086A - Sandwich-type catalyst for propane catalytic combustion and preparation method thereof - Google Patents
Sandwich-type catalyst for propane catalytic combustion and preparation method thereof Download PDFInfo
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/005—Spinels
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/58—Platinum group metals with alkali- or alkaline earth metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/63—Platinum group metals with rare earths or actinides
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J33/00—Protection of catalysts, e.g. by coating
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
- F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
- F23G7/00—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals
- F23G7/06—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases
- F23G7/07—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases in which combustion takes place in the presence of catalytic material
Abstract
The invention relates to a catalyst for propane catalytic combustion and a preparation method thereof, wherein the catalyst is prepared from gamma-Al2O3As carrier, by step-by-step loading method on Al2O3Surface construction of MgAl2O4After the spinel layer is loaded with Pd-Pt, a rare earth oxide protective layer is introduced on the surface of the spinel layer, so that a sandwich configuration is realized. The catalyst has simple preparation method, and can be used for catalytic oxidation of water<10% of propane waste gas has better deep oxidation activity and hydrothermal stability, realizes the high-efficiency purification of propane waste gas, and has wide application prospect in industrial end propane waste gas purification.
Description
Technical Field
The invention belongs to the technical field of catalysts, and particularly relates to a propane catalytic combustion catalyst with hydrothermal stability and high activity and a preparation method thereof.
Background
The volatile organic waste gas is one of air pollution sources and seriously threatens the life health of human beings. Propane is a common low-carbon alkane, is the most common volatile organic pollutants (VOCs), is a byproduct of natural gas treatment and crude oil refining processes, is also a tail gas emission of gasoline vehicles, and can generate a large amount of propane waste gas particularly in the large industries of propylene preparation through propane dehydrogenation, acrylic acid preparation through propane oxidation and the like. Therefore, the solution to the decontamination of propane becomes a difficult point and hot point.
The catalytic combustion technology is a relatively high-efficiency and reliable organic waste gas purification technology, and can catalytically oxidize organic waste gas into pollution-free CO under the action of a catalyst2And H2O, has the advantages of low operation temperature, high purification efficiency, wide application range, safety and reliability. However, compared with common aromatic hydrocarbons and oxygen-containing organic matters, propane has a simple molecular structure, but has higher catalytic combustion difficulty, higher ignition temperature and complete combustion temperature, and more practically, propane waste gas is often accompanied by a large amount of water vapor components (more than 5%), the traditional Pd and Pt catalysts are easy to sinter under high temperature conditions, are easy to collapse under high water vapor conditions, are easy to deactivate under severe reaction conditions, and have great challenges in constructing a hydrothermally stable catalyst.
Disclosure of Invention
In order to overcome the defect of hydrothermal stability of the existing low-carbon alkane catalytic combustion, the invention provides a catalyst for propane catalytic combustion and a preparation method thereof, and the catalyst is used in the propane catalytic combustion reaction and has better low-temperature catalytic activity and stability of resisting the condition of less than 10% of water vapor.
Aiming at the purposes, the 'sandwich' type catalyst for propane catalytic combustion is Mg modified gamma-Al2O3The carrier is loaded with Pd-Pt active components, and then a rare earth metal oxide protective layer is introduced on the surface of the carrier; the Mg modified gamma-Al2O3Medium, Mg and gamma-Al2O3The mass ratio of (A) to (B) is 0.03-0.10: 1; modification of gamma-Al with Mg2O3The load capacity of the Pd-Pt active component is 1-5% by 100% by mass, and the mass ratio of Pd to Pt is 1: 4-4: 1; mg modified gamma-Al loaded with Pd-Pt active component2O3The weight of the rare earth metal is 100 percent, and the loading amount of the rare earth metal is 3 to 10 percent.
The Mg modified gamma-Al2O3Is the surface formation of MgAl2O4gamma-Al of spinel layer2O3(ii) a The Mg modified gamma-Al2O3Of these, Mg and γ -Al are preferable2O3The mass ratio of (A) to (B) is 0.05-0.06: 1; modification of gamma-Al with Mg2O3The mass of the Pd-Pt active component is 100%, preferably, the load capacity of the Pd-Pt active component is 2% -3%, and the mass ratio of Pd to Pt is 1: 1-2: 1; mg modified gamma-Al loaded with Pd-Pt active component2O3The amount of (b) is 100%, and the preferable amount of the rare earth metal is 5 to 6%.
The rare earth metal oxide is any one of Ce, Zr, La and Y.
The preparation method of the sandwich-type catalyst comprises the following steps:
step 1: dissolving magnesium salt in deionized water, adjusting the pH value to 1-4 by using acid, and then adding gamma-Al2O3Stirring for 1-4 h, rotary evaporation drying, transferring to an oven for complete drying at 80-120 ℃, grinding the obtained dried solid, and roasting at 800-1200 ℃ for 2-4 h to obtain Mg modified gamma-Al2O3Is marked as Mg/Al2O3；
Step 2: adding Mg/Al to an aqueous solution containing a palladium precursor and a platinum precursor2O3Stirring for 1-2 h, rotary evaporation drying, transferring to an oven for complete drying at 80-120 ℃, grinding the obtained dried solid, roasting at 400-600 ℃ for 2-4 h to obtain Pd-Pt loaded Mg/Al2O3Is marked as Pd-Pt/Mg/Al2O3；
And step 3: adding Pd-Pt/Mg/Al into aqueous solution of rare earth metal nitrate2O3Stirring for 1-4 h, rotary evaporation drying, transferring to an oven for complete drying at 80-120 ℃, grinding the obtained dried solid, roasting at 400-600 ℃ for 2-4 h to obtain Pd-Pt/Mg/Al with a rare earth metal oxide protective layer formed on the surface2O3I.e., a "sandwich" type catalyst.
The magnesium salt is magnesium nitrate, the palladium precursor is palladium nitrate, the platinum precursor is platinum nitrate, and the rare earth metal nitrate is any one of nitrate of Ce, Zr, La and Y.
In the step 1, preferably, the obtained solid is roasted at 950-1050 ℃ for 2-4 h after being ground.
In the step 2, the obtained solid is preferably roasted for 2-4 hours at 500-550 ℃ after being ground.
In the step 3, the rare earth metal nitrate is preferably any one of cerium nitrate, zirconium nitrate, lanthanum nitrate and yttrium nitrate.
In the step 3, the obtained solid is preferably roasted for 2-4 hours at 500-550 ℃ after being ground.
The invention has the following beneficial effects:
the spinel-based Al-O, Mg-O composite material has the characteristics of strong Al-O, Mg-O ionic bond, firm structure, stable chemical property and good thermal stability when used as a carrier2O3The surface is constructed with layered spinel to prevent Pd-Pt from sintering at high temperature; a rare earth oxide protective layer is constructed on the surface of the catalyst, so that the surface collapse and inactivation of the catalyst under the condition of high temperature and water vapor are prevented, and a sandwich-type catalyst is constructed. The catalyst has simple preparation method, has high-efficiency deep catalytic oxidation effect on propane, is used for the catalytic combustion reaction of propane containing water vapor, has stable hydrothermal performance, realizes the high-efficiency purification of propane waste gas, and is suitable for industrial productionHas wide application prospect in the purification of the alkane waste gas.
Drawings
FIG. 1 shows the activity of the catalysts of comparative example 1 and examples 1 to 4 for the catalytic combustion of propane.
FIG. 2 shows the stability of the catalysts of comparative example 1 and examples 1-4 to catalytic combustion of propane.
FIG. 3 shows the activity of the catalysts of comparative example 1 and examples 1 to 4 on catalytic combustion of propane after hydrothermal aging.
FIG. 4 is a stability evaluation of the catalyst of example 1 for catalytic combustion of propane.
Detailed Description
The invention will be further described in detail with reference to the following figures and examples, but the scope of the invention is not limited to these examples.
Comparative example 1
Step 1: weighing 1.05g Mg (NO)3)2·6H2Adding water to dilute the solution to 10mL, and adjusting the pH value to 2.03 by using HNO 3; 1.9g of commercially available gamma-Al are weighed out2O3Adding into the solution, stirring for 1h, rotary evaporating at 70 deg.C in water bath for drying, drying in oven at 100 deg.C for 8h, grinding the obtained solid, transferring to muffle furnace, heating at 5 deg.C/min, and roasting at 1000 deg.C for 2h to obtain Mg/Al2O3；
Step 2: 0.3mL of Pd (NO) was measured3)2(Pd content 0.1g/mL), 0.2mL Pt (NO)3)2(Pt content 0.1g/mL) solution, adding water to dilute to 10 mL; weighing 1.95g of Mg/Al prepared in the step a2O3Adding into the solution, stirring for 1h, rotary evaporating at 70 deg.C in water bath for drying, drying in oven at 100 deg.C for 8h, grinding the obtained solid, transferring to muffle furnace, heating at 5 deg.C/min, and roasting at 500 deg.C for 2h to obtain Pd-Pt/Mg/Al2O3A catalyst.
Example 1
Step 1: same as comparative example 1, step 1.
Step 2: same as comparative example 1, step 2.
And step 3: 0.31g of Ce (NO) is weighed3)3·6H2Adding water to dilute the solution to 10 mL; weighing the P prepared in the step bd-Pt/Mg/Al2O3Adding a catalyst into the solution, stirring for 1h, then rotationally evaporating and drying the catalyst in 70 ℃ water bath, transferring the dried catalyst to an oven for drying for 8h at 100 ℃, grinding the obtained solid, transferring the ground solid to a muffle furnace, heating at 5 ℃/min, roasting at 500 ℃ for 2h to obtain CeO with the surface formed2Pd-Pt/Mg/Al of protective layer2O3I.e. "sandwich" type catalysts, denoted Ce/Pd-Pt/Mg/Al2O3。
Example 2
Step 1: same as comparative example 1, step 1.
Step 2: same as comparative example 1, step 2.
And step 3: 0.47g of Zr (NO) was weighed3)4·5H2Adding water to dilute the solution to 10 mL; weighing the Pd-Pt/Mg/Al prepared in the step b2O3Adding a catalyst into the solution, stirring for 1h, then rotationally evaporating and drying the catalyst in 70 ℃ water bath, transferring the catalyst to an oven for drying for 8h at 100 ℃, grinding the obtained solid, transferring the solid to a muffle furnace, heating at 5 ℃/min, roasting at 500 ℃ for 2h to obtain ZrO formed on the surface2Pd-Pt/Mg/Al of protective layer2O3I.e. "sandwich" type catalysts, noted Zr/Pd-Pt/Mg/Al2O3。
Example 3
Step 1: same as comparative example 1, step 1.
Step 2: same as comparative example 1, step 2.
And step 3: 0.31g La (NO) was weighed out3)3·6H2Adding water to dilute the solution to 10 mL; weighing the Pd-Pt/Mg/Al prepared in the step b2O3Adding a catalyst into the solution, stirring for 1h, then rotationally evaporating and drying the solution in a water bath at 70 ℃, transferring the solution to an oven at 100 ℃ for drying for 8h, grinding the obtained solid, transferring the ground solid to a muffle furnace, heating at 5 ℃/min, roasting at 500 ℃ for 2h to obtain the La formed on the surface2O3Pd-Pt/Mg/Al of protective layer2O3I.e. "sandwich" type catalysts, noted La/Pd-Pt/Mg/Al2O3。
Example 4
Step 1: same as comparative example 1, step 1.
Step 2: same as comparative example 1, step 2.
And step 3: weigh 0.43g Y (NO)3)3·6H2Adding water to dilute the solution to 10 mL; weighing the Pd-Pt/Mg/Al prepared in the step b2O3Adding the catalyst into the solution, stirring for 1h, performing rotary evaporation drying in 70 ℃ water bath, drying in an oven at 100 ℃ for 8h, grinding the obtained solid, transferring to a muffle furnace, heating at 5 ℃/min, and roasting at 500 ℃ for 2h to obtain the product with the surface formed with Y2O3Pd-Pt/Mg/Al of protective layer2O3I.e. "sandwich" type catalysts, denoted as Y/Pd-Pt/Mg/Al2O3。
The performance of the propane combustion for catalysis of the catalysts prepared in comparative example 1 and examples 1 to 4 was evaluated by using a fixed bed reactor (phi 8mm x 400mm), and the reaction gas composition was: sieving a catalyst with 40-60 meshes by using 5 per mill propane, 5 percent oxygen, 10 percent water vapor and the balance nitrogen, wherein the dosage is 150mg, the total gas flow is 250mL/min, and the evaluation airspeed is 100000 mL.h-1·g-1The evaluation temperature range is 200-500 ℃. The reaction tail gas is detected and analyzed by gas chromatography, and the catalytic activity and stability are determined by the conversion rate of propane. The results are shown in FIGS. 1-2. FIG. 1 shows that the catalyst of comparative example 1 has better catalytic activity, and the catalysts of examples 1-4 have activity slightly weaker than that of comparative example 1 due to the fact that rare earth oxide is introduced to cover part of active centers; the test result of FIG. 2 shows that after 60 hours of operation, the stability of the catalysts of examples 1-4 is obviously improved, especially the catalyst of example 1 has obvious activity attenuation phenomenon compared with the catalyst of comparative example 1.
And further evaluating the hydrothermal stability of the catalyst for propane catalytic combustion, wherein before evaluation, the catalyst is aged for 10 hours in a fixed bed reactor at 750 ℃ under the condition of 10% of water gas, and then is naturally cooled and dried to evaluate the performance. The test result of FIG. 3 shows that after aging, the catalysts in comparative example 1 and examples 1-4 have certain attenuation in activity, but the catalyst in comparative example 1 has larger attenuation, and the hydrothermal stability of examples 1-4 is higher. The catalyst of example 1 was used repeatedly 5 times to evaluate its stability. The test result of FIG. 4 shows that the catalyst of example 1 has extremely high reusability after 5 times of repeated use, which indicates that the catalyst has stable performance.
The test results show that the catalyst has good deep oxidation activity and hydrothermal stability when used for catalytic oxidation of propane waste gas with water content of less than 10%, and has good application prospect in propane catalytic combustion.
Claims (10)
1. A catalyst of the "sandwich" type for the catalytic combustion of propane, characterized in that: the catalyst is Mg modified gamma-Al2O3The carrier is loaded with Pd-Pt active components, and then a rare earth metal oxide protective layer is introduced on the surface of the carrier; the Mg modified gamma-Al2O3Medium, Mg and gamma-Al2O3The mass ratio of (A) to (B) is 0.03-0.10: 1; modification of gamma-Al with Mg2O3The load capacity of the Pd-Pt active component is 1-5% by 100% by mass, and the mass ratio of Pd to Pt is 1: 4-4: 1; mg modified gamma-Al loaded with Pd-Pt active component2O3The weight of the rare earth metal is 100 percent, and the loading amount of the rare earth metal is 3 to 10 percent.
2. "sandwich" type catalyst for propane catalytic combustion according to claim 1, characterized in that: the Mg modified gamma-Al2O3Medium, Mg and gamma-Al2O3The mass ratio of (A) to (B) is 0.05-0.06: 1; modification of gamma-Al with Mg2O3The load capacity of the Pd-Pt active component is 2-3% by 100% by mass, and the mass ratio of Pd to Pt is 1: 1-2: 1; mg modified gamma-Al loaded with Pd-Pt active component2O3The weight of the rare earth metal is 100 percent, and the loading amount of the rare earth metal is 5 to 6 percent.
3. "sandwich" -type catalyst for propane catalytic combustion according to claim 1 or 2, characterized in that: the Mg modified gamma-Al2O3Is the surface formation of MgAl2O4gamma-Al of spinel layer2O3。
4. "sandwich" -type catalyst for propane catalytic combustion according to claim 1 or 2, characterized in that: the rare earth metal oxide is any one of Ce, Zr, La and Y.
5. A process for the preparation of the "sandwich" type catalyst according to claim 1, characterized in that: the method comprises the following steps:
step 1: dissolving magnesium salt in deionized water, adjusting the pH value to 1-4 by using acid, and then adding gamma-Al2O3Stirring for 1-4 h, rotary evaporation drying, transferring to an oven for complete drying at 80-120 ℃, grinding the obtained dried solid, and roasting at 800-1200 ℃ for 2-4 h to obtain Mg modified gamma-Al2O3Is marked as Mg/Al2O3；
Step 2: adding Mg/Al to an aqueous solution containing a palladium precursor and a platinum precursor2O3Stirring for 1-2 h, rotary evaporation drying, transferring to an oven for complete drying at 80-120 ℃, grinding the obtained dried solid, roasting at 400-600 ℃ for 2-4 h to obtain Pd-Pt loaded Mg/Al2O3Is marked as Pd-Pt/Mg/Al2O3；
And step 3: adding Pd-Pt/Mg/Al into aqueous solution of rare earth metal nitrate2O3Stirring for 1-4 h, rotary evaporation drying, transferring to an oven for complete drying at 80-120 ℃, grinding the obtained dried solid, roasting at 400-600 ℃ for 2-4 h to obtain Pd-Pt/Mg/Al with a rare earth metal oxide protective layer formed on the surface2O3I.e., a "sandwich" type catalyst.
6. The process for the preparation of a catalyst of the "sandwich" type according to claim 5, characterized in that: the magnesium salt is magnesium nitrate, the palladium precursor is palladium nitrate, the platinum precursor is platinum nitrate, and the rare earth metal nitrate is any one of nitrate of Ce, Zr, La and Y.
7. The process for the preparation of a catalyst of the "sandwich" type according to claim 5, characterized in that: in the step 1, the obtained solid is roasted for 2-4 hours at 950-1050 ℃ after being ground.
8. The process for the preparation of a catalyst of the "sandwich" type according to claim 5, characterized in that: in the step 2, the obtained solid is roasted for 2-4 hours at 500-550 ℃ after being ground.
9. The "sandwich" type catalyst according to claim 5, characterized in that: in the step 3, the rare earth metal nitrate is any one of cerium nitrate, zirconium nitrate, lanthanum nitrate and yttrium nitrate.
10. The process for the preparation of a catalyst of the "sandwich" type according to claim 5, characterized in that: in the step 3, the obtained solid is roasted for 2-4 hours at 500-550 ℃ after being ground.
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| CN114950420A (en) * | 2022-06-16 | 2022-08-30 | 昆明理工大学 | Liquid nitrogen washing tail gas oxidation purification catalyst with hydrothermal stability resistance |
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