CN109647420B - Calcium-doped lanthanum perovskite cobaltite type oxide for thermal catalytic oxidation of toluene and preparation method and application thereof - Google Patents
Calcium-doped lanthanum perovskite cobaltite type oxide for thermal catalytic oxidation of toluene and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a calcium-doped lanthanum perovskite type oxide for thermal catalytic oxidation of toluene, which is prepared by the following steps: using lanthanum salt, cobalt salt and calcium salt as raw materials, citric acid as a complexing agent and ethanol-water mixed solution as a solvent, obtaining a calcium-doped perovskite precursor by a sol-gel method, and then calcining, tabletting, crushing and screening to obtain a perovskite catalyst for thermally catalyzing and oxidizing toluene; the calcium-doped lanthanum perovskite cobaltate catalyst for thermally catalyzing and oxidizing the toluene prepared by the invention is granular, can effectively catalyze and oxidize high-concentration toluene and is used for removing high-concentration (>1000mL/m3) The toluene removal rate can reach 100 percent; the catalyst has the advantages of low cost, high catalytic activity, strong water resistance, good thermal stability, no secondary pollution and the like, and is suitable for purifying high-concentration toluene waste gas in industrial waste gas.
Description
The technical field is as follows:
the invention relates to a calcium-doped lanthanum perovskite cobaltite type oxide for thermally catalyzing and oxidizing toluene, and a preparation method and application thereof.
Background art:
at present, with the rapid development of the industry in China, the problem of air pollution is increasingly serious, and the industrial waste gas treatment technology is more and more widely concerned. Toluene (C)6H5CH3) Is an important raw material in the field of organic chemical production, and can be widely used as a solvent and a high-octane gasoline additive. Toluene is a typical volatile organic compound (VO)Cs) has acute toxicity, reproductive toxicity, mutagenicity, etc., and its direct discharge can cause serious harm to human health and environment.
The thermal catalytic oxidation method is an effective method for industrially treating high-concentration toluene at present, and has the advantages of low catalytic temperature, high activity, small environmental pollution and the like. The catalyst is the core of the thermal catalytic oxidation technology. Conventional catalysts include noble metal catalysts and metal oxide catalysts. The noble metal catalyst has good initial catalytic activity, but has the defects of high price, easy poisoning, easy sintering at high temperature and the like. Although the transition metal oxide catalyst is inexpensive, the catalytic activity is often poor. Therefore, the development of efficient and cheap catalysts has become one of the important researches for the thermal catalytic oxidation of toluene. Perovskite type oxide belongs to composite oxide, because the composition is various, stable in structure, low cost and advantage such as being friendly to the environment, receive more and more attention in the aspect of pollutant control.
The invention content is as follows:
the invention aims to provide a calcium-doped lanthanum perovskite cobaltate oxide for thermally catalyzing and oxidizing toluene, which has high catalytic activity, good thermal stability, strong water resistance and low cost, is synthesized by adopting an improved sol-gel method, optimizes the structure, further improves the catalytic activity, improves the catalytic performance and the water resistance, and is suitable for the thermal catalytic oxidation treatment of the industrial toluene waste gas with medium and high concentration.
The invention is realized by the following technical scheme:
a calcium-doped lanthanum perovskite type oxide for thermally catalyzing and oxidizing toluene is prepared by the following steps: using lanthanum salt, cobalt salt and calcium salt as raw materials, citric acid as a complexing agent and ethanol-water mixed solution as a solvent, obtaining a calcium-doped perovskite precursor by a sol-gel method, and then calcining, tabletting, crushing and screening to obtain a perovskite catalyst for thermally catalyzing and oxidizing toluene; the method specifically comprises the following steps:
1) adding lanthanum salt, cobalt salt, calcium salt and citric acid into the ethanol-water mixed solution, and stirring at room temperature for 2-3h to obtain sol, wherein the molar ratio of the lanthanum salt to the cobalt salt to the calcium salt is 1-x:1: x, wherein x is more than 0 and less than or equal to 0.4; the molar ratio of the sum of metal cations such as lanthanum ions, cobalt ions, calcium ions and the like to the citric acid is 1: 1.0-1.5;
2) continuously stirring the sol obtained in the step 1) for 5-6h at 80-85 ℃, and drying in a vacuum drying oven at 85-95 ℃ for 20-24h to obtain dry gel which is a calcium-doped perovskite precursor;
3) calcining the xerogel obtained in the step 2) at the temperature of 400-720 ℃ for 3-5 hours, then calcining at the temperature of 680-720 ℃ for 4-6 hours, tabletting, crushing, screening out 35-60-mesh lanthanum cobaltate particles in a grading way, and then calcining in a muffle furnace at the temperature of 400 ℃ for 3 hours to obtain the calcium-doped lanthanum perovskite oxide for thermally catalyzing and oxidizing toluene.
Preferably, the lanthanum salt is La (NO)3)3·6H2O, the cobalt salt is Co (NO)3)2·6H2O, the calcium salt is Ca (NO)3)2·4H2O。
Preferably, the value of x is 0.01 to 0.15, and most preferably, the value of x is 0.1.
Preferably, the volume ratio of the ethanol to the water in the ethanol-water mixed solution is 1: 1-2.
The invention also protects the application of the calcium-doped lanthanum perovskite cobaltite oxide for the thermal catalytic oxidation of toluene in the aspect of catalytic oxidation of toluene.
The invention has the following beneficial effects: the calcium-doped lanthanum perovskite cobaltate catalyst La for thermally catalyzing and oxidizing toluene prepared by the invention1-xCaxCoO3(0<x is less than or equal to 0.4) is granular, has excellent catalytic activity on toluene, wherein La0.9Ca0.1CoO3The nanoparticles had a toluene concentration of 1000ppm and a space velocity of 30000cm3 g-1h-1Under the condition that the temperature of the toluene for complete oxidation is 215 ℃, the reaction product only contains CO2And H2O, no other secondary pollution byproducts are generated, in addition, the catalyst catalyzes toluene for 24 hours at 250 ℃ without deactivation, which shows that the catalyst has good thermal stability, and in addition, the activity is not reduced under the condition of 5000ppm of water vapor, which shows that the catalyst has excellent water resistance. The catalyst hasLow cost, high catalytic activity, strong water resistance, good thermal stability, no secondary pollution and the like, and is suitable for the purification treatment of high-concentration toluene waste gas in industrial waste gas.
Description of the drawings:
FIG. 1 is an X-ray diffraction pattern of calcium doped lanthanum perovskite type oxide for the thermal catalytic oxidation of toluene prepared in examples 1-5;
FIG. 2 is a graph showing the evaluation of the catalytic activity of calcium-doped lanthanum perovskite type oxide for the thermal catalytic oxidation of toluene prepared in examples 1 to 5;
FIG. 3 is a graph showing the water resistance and stability evaluation of the calcium-doped lanthanum perovskite cobaltate-type oxide for the thermal catalytic oxidation of toluene prepared in example 2 as a catalyst;
wherein, example 1 is the abbreviation of embodiment 1, example 2 is the abbreviation of embodiment 2, example 3 is the abbreviation of embodiment 3, example 4 is the abbreviation of embodiment 4, and example 5 is the abbreviation of embodiment 5.
The specific implementation mode is as follows:
the following is a further description of the invention and is not intended to be limiting.
Example 1:
1) 30mL of ethanol was measured, added to 30mL of ultrapure water, stirred well, and then 4.331g (0.01mol) of La (NO) was added3)3·6H2O，2.911g(0.01mol)Co(NO3)2·6H2O and 4.62g of citric acid, and stirring the mixture at room temperature for 3 hours to obtain sol.
2) The sol is continuously stirred for 6 hours under the condition of oil bath at the temperature of 80 ℃, and is dried for 24 hours in a vacuum drying oven at the temperature of 90 ℃ to obtain xerogel.
3) And placing the obtained dried gel in a muffle furnace to be calcined for 4 hours at 400 ℃, calcining for 5 hours at 700 ℃, tabletting, crushing, selecting 35-60 meshes of lanthanum cobaltite by a grading sieve, placing in the muffle furnace to be calcined for 3 hours at 400 ℃, and obtaining a sample 1.
The compound sample 1 was subjected to an identification analysis, and its XRD (XRD, an abbreviation for X-ray diffraction) pattern (shown in fig. 1) was consistent with that of standard card (PDF), which indicated that pure phase lanthanum perovskite cobaltate was synthesized. A sample of 0.1g of this complex was taken1 as a catalyst, the gas flow rate is 100mL/min, the corresponding space velocity is 30000 mL/(g.h), and the toluene concentration is 1000mL/m3Under the conditions of normal pressure and 225 ℃, the toluene removal rate is 8.7 percent. The results of the activity evaluation are shown in FIG. 2.
Example 2
1) 30mL of ethanol was measured, added to 30mL of ultrapure water, stirred well, and then 3.897g (0.009mol) of La (NO) was added3)3·6H2O，0.236g Ca(NO3)2·4H2O(0.001mol)，2.911g(0.01mol)Co(NO3)2·6H2O (lanthanum nitrate, cobalt nitrate and calcium nitrate in a molar ratio of 0.9:1:0.1) and 4.62g of citric acid were stirred at room temperature for 3 hours to obtain a sol.
2) The sol is continuously stirred for 6 hours under the condition of oil bath at the temperature of 80 ℃, and is dried for 24 hours in a vacuum drying oven at the temperature of 90 ℃ to obtain xerogel.
3) And placing the obtained dried gel in a muffle furnace to be calcined for 4 hours at 400 ℃, calcining for 5 hours at 700 ℃, tabletting, crushing, selecting 35-60-mesh lanthanum cobaltate by a grading sieve, placing in the muffle furnace to be calcined for 3 hours at 400 ℃, and obtaining a sample 2.
The sample 2 was identified and analyzed, and its XRD spectrum was similar to that of lanthanum cobaltate, and its diffraction peak was shifted toward high angle, indicating that calcium entered the lanthanum perovskite structure, as shown in fig. 1. Taking 0.1g of the compound sample 2 as a catalyst, wherein the gas flow rate is 100mL/min, the corresponding space velocity is 30000 mL/(g.h), and the toluene concentration is 1000mL/m3Under the conditions of normal pressure and 225 ℃, the toluene removal rate is 100 percent. The results of the activity evaluation are shown in FIG. 2. The water resistance and stability of the catalyst are evaluated in fig. 3. The catalyst catalyzes toluene for 24 hours at 250 ℃ without inactivation, which indicates that the catalyst has good thermal stability, and in addition, the activity is not reduced under the condition of 5000ppm of water vapor, which indicates that the catalyst has excellent water resistance.
Example 3
1) 30mL of ethanol was measured, added to 30mL of ultrapure water, stirred well, and then 3.464g (0.008mol) of La (NO) was added3)3·6H2O，0.472g Ca(NO3)2·4H2O(0.002mol)，2.911g(0.01mol)Co(NO3)2·6H2O (lanthanum nitrate, cobalt nitrate and calcium nitrate in a molar ratio of 0.8:1:0.2) and 4.62g of citric acid were stirred at room temperature for 3 hours to obtain a sol.
2) The sol obtained is continuously stirred for 6h under the condition of oil bath at the temperature of 80 ℃, and is dried for 24h in a vacuum drying oven at the temperature of 90 ℃. A xerogel is obtained.
3) And placing the obtained dried gel in a muffle furnace to be calcined for 4 hours at 400 ℃, calcining for 5 hours at 700 ℃, tabletting, crushing, selecting 35-60 meshes of lanthanum cobaltite by a grading sieve, placing in the muffle furnace to be calcined for 3 hours at 400 ℃, and obtaining a sample 3.
The sample 3 was identified and analyzed, and its XRD spectrum was similar to that of lanthanum cobaltate, and its diffraction peak was shifted toward high angle, indicating that calcium entered the lanthanum perovskite structure, as shown in fig. 1. As shown in fig. 1. A0.1 g compound sample 1 is taken as a catalyst, the gas flow rate is 100mL/min, the corresponding space velocity is 30000 mL/(g.h), the toluene concentration is 1000mL/m3, and the toluene removal rate is 41% under the conditions of normal pressure and 225 ℃. The results of the activity evaluation are shown in FIG. 2. The catalyst catalyzes toluene for 24 hours at 250 ℃ without inactivation, which indicates that the catalyst has good thermal stability, and in addition, the activity is not reduced under the condition of 5000ppm of water vapor, which indicates that the catalyst has excellent water resistance.
Example 4
1) 30mL of ethanol was measured, added to 30mL of ultrapure water, stirred well, and then 3.031g (0.007mol) of La (NO) was added3)3·6H2O，0.708g(0.003mol)Ca(NO3)2·4H2O，2.911g(0.01mol)Co(NO3)2·6H2O (lanthanum nitrate, cobalt nitrate and calcium nitrate in a molar ratio of 0.7:1:0.3) and 4.62g of citric acid were stirred at room temperature for 3 hours to obtain a sol.
2) The sol obtained is continuously stirred for 6h under the condition of oil bath at the temperature of 80 ℃, and is dried for 24h in a vacuum drying oven at the temperature of 90 ℃. A xerogel is obtained.
3) And placing the obtained dried gel in a muffle furnace to be calcined for 4 hours at 400 ℃, calcining for 5 hours at 700 ℃, tabletting, crushing, selecting 35-60 meshes of lanthanum cobaltite by a grading sieve, placing in the muffle furnace to be calcined for 3 hours at 400 ℃, and obtaining a sample 4.
The sample 4 was identified and analyzed, and its XRD spectrum was similar to that of lanthanum cobaltate, and its diffraction peak was shifted toward high angle, indicating that calcium entered the lanthanum perovskite structure, as shown in fig. 1. As shown in fig. 1. Taking 0.1g of the compound sample 1 as a catalyst, wherein the gas flow rate is 100mL/min, the corresponding space velocity is 30000 mL/(g.h), and the toluene concentration is 1000mL/m3Under the conditions of normal pressure and 225 ℃, the toluene removal rate is 29 percent. The results of the activity evaluation are shown in FIG. 2. The catalyst catalyzes toluene for 24 hours at 250 ℃ without inactivation, which indicates that the catalyst has good thermal stability, and in addition, the activity is not reduced under the condition of 5000ppm of water vapor, which indicates that the catalyst has excellent water resistance.
Example 5
1) 30mL of ethanol was measured, added to 30mL of ultrapure water, stirred well, and then 2.598g (0.006mol) of La (NO) was added3)3·6H2O，0.944g Ca(NO3)2·4H2O(0.004mol)，2.911g(0.01mol)Co(NO3)2·6H2O (lanthanum nitrate, cobalt nitrate and calcium nitrate in a molar ratio of 0.6:1:0.4) and 4.62g of citric acid were stirred at room temperature for 3 hours to obtain a sol.
2) The sol obtained is continuously stirred for 6h under the condition of oil bath at the temperature of 80 ℃, and is dried for 24h in a vacuum drying oven at the temperature of 90 ℃. A xerogel is obtained.
3) And placing the obtained dried gel in a muffle furnace to be calcined for 4 hours at 400 ℃, calcining for 5 hours at 700 ℃, tabletting, crushing, selecting 35-60 meshes of lanthanum cobaltite by a grading sieve, placing in the muffle furnace to be calcined for 3 hours at 400 ℃, and obtaining a sample 5.
The sample 5 was identified and analyzed, and its XRD spectrum was similar to that of lanthanum cobaltate, and its diffraction peak was shifted toward high angle, indicating that calcium entered the lanthanum perovskite structure, as shown in fig. 1. As shown in fig. 1. Taking 0.1g of the compound sample 1 as a catalyst, wherein the gas flow rate is 100mL/min, the corresponding space velocity is 30000 mL/(g.h), and the toluene concentration is 1000mL/m3Under the conditions of normal pressure and 225 DEG CThe toluene removal rate was 25%. The results of the activity evaluation are shown in FIG. 2. The catalyst catalyzes toluene for 24 hours at 250 ℃ without inactivation, which indicates that the catalyst has good thermal stability, and in addition, the activity is not reduced under the condition of 5000ppm of water vapor, which indicates that the catalyst has excellent water resistance.
Claims (3)
1. The application of calcium-doped lanthanum perovskite cobaltate oxide in the aspect of catalytic oxidation of toluene is characterized in that the concentration of the toluene is 1000mL/m3And the space velocity is 30000cm3g-1h-1Under the condition of (1), calcium is doped with lanthanum perovskite type oxide La of cobaltite0.9Ca0.1CoO3The temperature for the complete oxidation of the catalytic oxidation toluene is 225 ℃, and the reaction product only contains CO2And H2O; calcium-doped lanthanum perovskite type oxide La0.9Ca0.1CoO3The preparation method comprises the following steps: 1) adding lanthanum salt, cobalt salt, calcium salt and citric acid into the ethanol-water mixed solution, and stirring at room temperature for 2-3h to obtain sol, wherein the molar ratio of the lanthanum salt to the cobalt salt to the calcium salt is 1-x:1: x, and the value of x is 0.1; the molar ratio of the sum of the metal cations to the citric acid is 1: 1.0-1.5;
2) continuously stirring the sol obtained in the step 1) for 5-6h at the temperature of 80-85 ℃, and drying in a vacuum drying oven at the temperature of 85-95 ℃ for 20-24h to obtain xerogel;
3) calcining the xerogel obtained in the step 2) at the temperature of 400-720 ℃ for 3-5 hours, then calcining at the temperature of 680-720 ℃ for 4-6 hours, tabletting, crushing, screening out 35-60-mesh lanthanum cobaltate particles in a grading way, and then calcining in a muffle furnace at the temperature of 400 ℃ for 3 hours to obtain the calcium-doped lanthanum perovskite oxide for thermally catalyzing and oxidizing toluene.
2. The use of the calcium-doped lanthanum perovskite cobaltite-type oxide for the catalytic oxidation of toluene as claimed in claim 1, wherein the lanthanum salt is La (NO)3)3·9H2O, the cobalt salt is Co (NO)3)2·6H2O, the calcium salt is Ca (NO)3)2·4H2O。
3. The use of the calcium-doped lanthanum perovskite cobaltate oxide in the catalytic oxidation of toluene according to claim 1, wherein the volume ratio of ethanol to water in the ethanol-water mixed solution is 1: 1-2.
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