CN107597104B - Oxide supported Pt catalyst with core-shell structure and preparation method and application thereof - Google Patents
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Abstract
A nuclear shell structure oxide supported Pt catalyst and a preparation method and application thereof belong to the technical field of environmental catalysis and atmospheric pollution control. The catalyst is prepared from SiO with a core-shell structure2@TiO2Is used as a carrier, and Pt is used as an active component. It is characterized by that it is a spherical SiO2As a core, SiO2The surface of the inner core is coated with TiO2，SiO2@TiO2The generation of the core-shell structure obviously improves the selective reduction of NO by hydrogen on the Pt catalystxThe catalyst has good low-temperature denitration performance. The preparation process is simple, and NO can be realized at low temperaturexThe method has high efficiency removal and wide application prospect.
Description
Technical Field
The invention relates to a core-shell structure oxide supported Pt catalyst, a preparation method thereof and a method for selectively catalyzing and reducing NO by utilizing the catalyst under the condition of oxygen enrichmentx. Is suitable for NO in the smoke of mobile sources such as diesel vehicles and the like and fixed sources such as industrial boilers, smelting plants and the likexBelonging to the technical field of environmental catalysis and atmospheric pollution control.
Background
With the growing consumption of energy and the rapid increase in the amount of motor vehicles kept, the consumption of large amounts of fossil fuels leads to the emission of NO into the atmospherexRapid increase of NOxNot only can cause the problems of acid rain, haze and other ecological environments, but also seriously harms the health of people. Thus, how to effectively eliminate NOxIs a hot spot of research in the fields of atmospheric pollution control and environmental catalysis at present. NH (NH)3Selective catalytic reduction technique (NH)3SCR) NO emission already at thermal power plantsxIs widely applied to the control of the motor. However, when ammonia is used as a reducing agent, the conventional vanadium tungsten titanium catalyst cannot effectively remove NO discharged by motor vehicles and industrial boilers because the temperature window is in a high-temperature region (300-x(ii) a In addition, NH is also limited by ammonia slip and the like3-the use of SCR. In recent years, hydrogen has been used to selectively reduce NOx(H2SCR) has attracted high interest to researchers. When hydrogen is used as the reducing agent, NOxThe reduction temperature is greatly reduced, and excessive hydrogen and oxygen are combusted to generate water, so that secondary pollution is avoided.
Currently used for the selective reduction of NO by hydrogenxThe catalysts are mostly noble metals, and have the problems of narrow temperature window and NOxThe conversion of (a) is to be improved and the noble metal is expensive. Therefore, development of H having a low noble metal content and a high activity2SCR denitration catalyst capable of satisfying NO emission of lean-burn gasoline vehicles and diesel vehiclesxCan also be applied to the emission of NO from fixed sources such as industrial boilers and the likexThe low-temperature catalytic removal has important significance and application prospect.
The invention prepares NO at low temperaturexThe catalyst has excellent performance in catalyzing and removing the oxide load Pt catalyst with the core-shell structure.
Disclosure of Invention
The invention aims to provide a method for preparing NO by selective catalytic reduction of hydrogen with simple preparation methodxAn oxide supported Pt catalyst with a high activity and a core-shell structure and a preparation method thereof. Considering that the interaction between the active component and the carrier has obvious influence on the catalytic performance of the catalyst, the invention synthesizes SiO with a core-shell structure2@TiO2Oxide, by SiO2With TiO2The mutual action and the synergistic effect between the core-shell structure carrier and the noble metal Pt develop a method for selectively catalyzing and reducing NO by hydrogenxThe denitration catalyst has good activity.
The purpose of the invention is realized by the following technical scheme:
the catalyst composition is expressed as Pt/SiO2@TiO2In which the SiO is spherical2As a core, SiO2The surface of the inner core is coated with TiO2Wherein the outer shell is TiO2With SiO core2The molar ratio of (A) to (B) is 0.1 to 0.2, the mass of Pt is in proportion to SiO2@TiO2The mass ratio is 0.5-1%.
The invention provides a preparation method of an oxide supported Pt catalyst with a core-shell structure, which is characterized by comprising the following steps: the method sequentially comprises the following steps:
(1) stirring and mixing ethanol, ammonia water and deionized water to obtain a mixed solution, adding tetraethyl orthosilicate into the mixed solution, heating to 50-70 ℃, and refluxing in a water bath for 2-4 hours. Cooling to room temperature, centrifuging the reaction solution, drying at 120 deg.C to 12EAfter 24 hours, spherical SiO was obtained2；
(2) Ultrasonically mixing ethanol and tetrabutyl titanate to obtain a mixed solution, and carrying out step (1) to obtain the spherical SiO2Adding into the mixed solution, stirring, and performing ultrasonic treatment for 30min to obtain mixed solution A; stirring and mixing ethanol and deionized water, and marking as a solution B;
(3) dropwise adding the solution B obtained in the step (2) into the mixed solution A, continuously stirring and reacting for 8-12h after dropwise adding is finished, centrifugally separating the solution, drying for 12-24 h at 120 ℃, and then roasting for 4-8 h at 500 ℃ in a muffle furnace to obtain the SiO with the core-shell structure2@TiO2；
(4) Taking the SiO obtained in the step (3)2@TiO2Grinding the mixture into powder, adding 0.01-0.02mol/L chloroplatinic acid or platinum nitrate solution, and then stirring for 2-4 hours until the mixture is in a slurry state;
(5) drying the slurry-like solid obtained in the step (4) at 120 ℃ for 12-24 hours, and then calcining the dried slurry-like solid in a muffle furnace at 450-550 ℃ for 4-8 hours to obtain Pt/SiO2@TiO2A catalyst.
The invention also provides the application of the oxide supported Pt catalyst with the core-shell structure in selective reduction of NO by hydrogenxThe method is characterized in that the application method comprises the following steps:
(1) loading a core-shell structure oxide supported Pt catalyst in a fixed bed reactor, and controlling the reaction temperature to be 75-250 ℃;
(2) hydrogen is used as a reducing agent, the total flow of the gas is controlled to be 200-400 ml/min, and the space velocity is controlled to be 43,000-86,000 h-1。
Compared with the prior art, the invention has the following advantages and prominent effects: by using SiO with core-shell structure2@TiO2As a carrier of the active component Pt, the catalyst greatly improves the selective reduction of NO to hydrogen by the synergistic catalytic action between Pt and the oxide with the core-shell structurexThe catalyst has excellent low-temperature denitration performance although the noble metal loading is low.
Drawings
FIG. 1 is a 0.5% Pt/SiO2Scanning electron micrographs of the catalyst
FIG. 2 is a 0.5% Pt/SiO2@TiO2Scanning electron micrographs of (Ti: Si ═ 1:5) catalyst
Detailed Description
The technical scheme of the invention is further explained by combining the embodiment as follows: the mass percentage concentration of ammonia in the following examples is 25%.
Example 1: 0.5% Pt/SiO2@TiO2Preparation of (Ti: Si ═ 1:5) catalyst
a) Taking 145mL of ethanol, 95mL of ammonia water and 20mL of deionized water, stirring and mixing to obtain a mixed solution, then adding 50mmol of tetraethyl orthosilicate into the mixed solution, heating to 50 ℃, refluxing in a water bath for 2 hours, cooling to room temperature, then carrying out centrifugal filtration on the reaction solution, drying for 24 hours at 120 ℃ to obtain spherical SiO2；
b) Ultrasonically mixing 250mL of ethanol and 10mmol of tetrabutyl titanate to obtain a mixed solution, and subjecting the spherical SiO obtained in the step (a)2Adding into the mixed solution, stirring, and performing ultrasonic treatment for 30min to obtain mixed solution A; 50mL of ethanol was mixed with 250mL of deionized water with stirring and was designated as solution B.
c) And (c) dropwise adding the solution B obtained in the step (B) into the mixed solution A, and continuously stirring for reacting for 12 hours after the dropwise adding is finished. Centrifugally separating the solution, drying at 120 ℃ for 12 hours, and then roasting in a muffle furnace at 500 ℃ for 6 hours to obtain SiO with a core-shell structure2@TiO2。
d) Taking the SiO obtained in the step (c)2@TiO2Ground to a powder, and 4.87mL of a 0.02mol/L chloroplatinic acid solution was added, followed by stirring for 2 hours until the mixture was in a slurry state.
e) Drying the slurry solid obtained in the step (d) at 120 ℃ for 12 hours, and then calcining the dried slurry solid in a muffle furnace at 500 ℃ for 4 hours to obtain 0.5% Pt/SiO2@TiO2(Ti: Si ═ 1:5) catalyst.
Example 2: 0.5% Pt/SiO2@TiO2Preparation of (Ti: Si ═ 1:7.5) catalyst
a) Taking 145mL of ethanol, 95mL of ammonia water and 20mL of deionized water, stirring and mixing to obtain a mixed solution, then adding 50mmol of tetraethyl orthosilicate into the mixed solution, heating to 70 ℃, refluxing in a water bath for 4 hours, cooling to room temperature, then carrying out centrifugal filtration on the reaction solution, and drying for 12 hours at 120 ℃ to obtain spherical SiO2；
b) Ultrasonically mixing 200mL of ethanol and 6.67mmol of tetrabutyl titanate to obtain a mixed solution, and mixing the spherical SiO obtained in the step (a)2Adding into the mixed solution, stirring, and performing ultrasonic treatment for 30min to obtain mixed solution A; stirring and mixing 50mL of ethanol and 200mL of deionized water, and marking as a solution B;
c) and (c) dropwise adding the solution B obtained in the step (B) into the mixed solution A, and continuously stirring for reacting for 8 hours after the dropwise adding is finished. Centrifugally separating the solution, drying the solution for 24 hours at 120 ℃, and then roasting the solution for 4 hours in a muffle furnace at 500 ℃ to prepare SiO with a core-shell structure2@TiO2；
d) Taking the SiO obtained in the step (c)2@TiO2Grinding the mixture into powder, adding 4.54mL of 0.02mol/L chloroplatinic acid solution, and stirring the mixture for 2 hours until the mixture is in a slurry state;
e) drying the slurry-like solid obtained in the step (d) at 120 ℃ for 24 hours, and then calcining the dried slurry-like solid in a muffle furnace at 450 ℃ for 8 hours to obtain 0.5% Pt/SiO2@TiO2(Ti: Si ═ 1:7.5) catalyst.
Example 3: 0.5% Pt/SiO2@TiO2Preparation of (Ti: Si ═ 1:10) catalyst
a) Taking 145mL of ethanol, 95mL of ammonia water and 20mL of deionized water, stirring and mixing to obtain a mixed solution, then adding 50mmol of tetraethyl orthosilicate into the mixed solution, heating to 60 ℃, refluxing in a water bath for 3 hours, cooling to room temperature, then carrying out centrifugal filtration on the reaction solution, drying for 12 hours at 120 ℃ to obtain spherical SiO2；
b) Ultrasonically mixing 180mL of ethanol and 5.0mmol of tetrabutyl titanate to obtain a mixed solution, and mixing the spherical SiO obtained in the step (a)2Adding into the mixed solution, stirring, and performing ultrasonic treatment for 30min to obtain mixed solution A; stirring and mixing 50mL of ethanol and 250mL of deionized water, and marking as a solution B;
c) and (c) dropwise adding the solution B obtained in the step (B) into the mixed solution A, and continuously stirring for reacting for 10 hours after the dropwise adding is finished. Centrifugally separating the solution, drying at 120 ℃ for 12 hours, and then roasting in a muffle furnace at 500 ℃ for 8 hours to obtain SiO with a core-shell structure2@TiO2；
d) Taking the SiO obtained in the step (c)2@TiO2Grinding the mixture into powder, adding 8.72mL of 0.01mol/L platinum nitrate solution, and then stirring the mixture for 3 hours until the mixture is in a slurry state;
e) drying the slurry-like solid obtained in the step (d) at 120 ℃ for 18 hours, and then placing the dried slurry-like solid in a muffle furnace to calcine the dried slurry-like solid at 500 ℃ for 6 hours to obtain 0.5% Pt/SiO2@TiO2(Ti: Si ═ 1:10) catalyst.
Example 4: 1% Pt/SiO2@TiO2Preparation of (Ti: Si ═ 1:10) catalyst
a) Taking 145mL of ethanol, 95mL of ammonia water and 20mL of deionized water, stirring and mixing to obtain a mixed solution, then adding 50mmol of tetraethyl orthosilicate into the mixed solution, heating to 50 ℃, refluxing in a water bath for 4 hours, cooling to room temperature, then carrying out centrifugal filtration on the reaction solution, drying for 24 hours at 120 ℃ to obtain spherical SiO2；
b) Ultrasonically mixing 180mL of ethanol and 5.0mmol of tetrabutyl titanate to obtain a mixed solution, and mixing the spherical SiO obtained in the step (a)2Adding into the mixed solution, stirring, and performing ultrasonic treatment for 30min to obtain mixed solution A; stirring and mixing 50mL of ethanol and 250mL of deionized water, and marking as a solution B;
c) and (c) dropwise adding the solution B obtained in the step (B) into the mixed solution A, and continuously stirring for reacting for 8 hours after the dropwise adding is finished. Centrifugally separating the solution, drying the solution for 24 hours at 120 ℃, and then roasting the solution for 6 hours in a muffle furnace at 500 ℃ to prepare SiO with a core-shell structure2@TiO2；
d) Taking the SiO obtained in the step (c)2@TiO2Grinding the mixture into powder, adding 8.72mL of 0.02mol/L platinum nitrate solution, and then stirring the mixture for 2 hours until the mixture is in a slurry state;
e) subjecting the slurry solid obtained in step (d) to a temperature of 120 deg.CDrying for 24 hours under the condition, then placing the mixture into a muffle furnace to calcine for 4 hours at the temperature of 550 ℃ to prepare 1 percent Pt/SiO2@TiO2(Ti: Si ═ 1:10) catalyst.
Example 5 (reference): 0.5% Pt/SiO2Preparation of the catalyst
a) And (3) stirring and mixing 145mL of ethanol, 95mL of ammonia water and 20mL of deionized water to obtain a mixed solution, then adding 50mmol of tetraethyl orthosilicate into the mixed solution, heating to 50 ℃, and refluxing in a water bath for 2 hours. Cooling to room temperature, centrifuging and filtering the reaction solution, and drying at 120 ℃ for 24 hours to obtain spherical SiO2；
b) Taking the spherical SiO obtained in the step (a)2Grinding the mixture into powder, adding 7.69mL of 0.01mol/L chloroplatinic acid solution, and stirring the mixture for 2 hours until the mixture is in a slurry state;
c) drying the slurry solid obtained in the step (b) at 120 ℃ for 12 hours, and then calcining the dried slurry solid in a muffle furnace at 500 ℃ for 4 hours to obtain 0.5% Pt/SiO2A catalyst.
Example 6: the catalyst was prepared in the same manner as in example 1, with 0.2g of catalyst being loaded in a fixed bed reactor, the reaction gas composition being 0.2% NO, 1% H2，5％O2The flow rate of the reaction gas is 200ml/min, and the space velocity is 43,000h-1. The activity evaluation temperature range is 75-250 ℃, and the conversion rate of the catalyst for reducing the nitrogen oxide at different temperatures is shown in table 1.
Example 7: the catalyst was prepared in the same manner as in example 2, by loading 0.2g of the catalyst in a fixed bed reactor with a reaction gas composition of 0.2% NO, 1% H2，5％O2The flow rate of the reaction gas is 200ml/min, and the space velocity is 43,000h-1. The activity evaluation temperature range is 75-250 ℃, and the conversion rate of the catalyst for reducing the nitrogen oxide at different temperatures is shown in table 1.
Example 8: the catalyst was prepared in the same manner as in example 3, with 0.2g of catalyst loaded in a fixed bed reactor, the reaction gas composition being 0.2% NO, 1% H2，5％O2The flow rate of the reaction gas is 200ml/min, and the space velocity is 43,000h-1. Activity ofThe evaluation temperature range is 75-250 ℃, and the conversion rate of the catalyst for reducing the nitrogen oxides at different temperatures is shown in table 1.
Example 9: the catalyst was prepared in the same manner as in example 4, by loading 0.2g of the catalyst in a fixed bed reactor with a reaction gas composition of 0.2% NO, 1% H2，5％O2The flow rate of the reaction gas is 200ml/min, and the space velocity is 43,000h-1. The activity evaluation temperature range is 75-250 ℃, and the conversion rate of the catalyst for reducing the nitrogen oxide at different temperatures is shown in table 1.
TABLE 1 evaluation results of the activity of oxide-supported Pt catalyst having core-shell structure and reference catalyst
Claims (1)
1. Core-shell structure oxide supported Pt catalyst for selective reduction of NO by hydrogenxCharacterized in that the catalyst is expressed as Pt/SiO2@TiO2In which the SiO is spherical2As a core, SiO2The surface of the inner core is coated with TiO2Wherein the outer shell is TiO2With SiO core2The molar ratio of (A) to (B) is 0.1 to 0.2, the mass of Pt is in proportion to SiO2@TiO2The mass ratio is 0.5-1%;
the preparation method sequentially comprises the following steps:
(1) stirring and mixing ethanol, ammonia water and deionized water to obtain a mixed solution, adding tetraethyl orthosilicate into the mixed solution, heating to 50-70 ℃, and refluxing in a water bath for 2-4 hours; cooling to room temperature, then carrying out centrifugal filtration on the reaction solution, and drying for 12-24 hours at 120 ℃ to obtain spherical SiO2；
(2) Ultrasonically mixing ethanol and tetrabutyl titanate to obtain a mixed solution, and carrying out step (1) to obtain the spherical SiO2Adding into the mixed solution, stirring, and performing ultrasonic treatment for 30min to obtain mixed solution A; stirring and mixing ethanol and deionized water, and marking as a solution B;
(3) dropwise adding the solution B obtained in the step (2) into the mixed solution A, and continuously stirring the solution BPerforming centrifugal separation on the solution for 8-12 hours, drying the solution for 12-24 hours at the temperature of 120 ℃, and then roasting the solution for 4-8 hours in a muffle furnace at the temperature of 500 ℃ to prepare SiO with a core-shell structure2@TiO2；
(4) Taking the SiO obtained in the step (3)2@TiO2Grinding the mixture into powder, adding 0.01-0.02mol/L chloroplatinic acid or platinum nitrate solution, and then stirring for 2-4 hours until the mixture is in a slurry state;
(5) drying the slurry-like solid obtained in the step (4) at 120 ℃ for 12-24 hours, and then calcining the dried slurry-like solid in a muffle furnace at 450-550 ℃ for 4-8 hours to obtain Pt/SiO2@TiO2A catalyst;
the application comprises the following steps:
(1) mixing Pt with SiO2@TiO2Loading a catalyst in a fixed bed reactor, and controlling the reaction temperature to be 75-250 ℃;
(2) hydrogen is used as a reducing agent, the total flow of the gas is controlled to be 200-400 mL/min, and the space velocity is controlled to be 43,000-86,000 h-1。
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