CN114345333A - Preparation method of automobile exhaust purification catalyst with controllable precious metal content and obtained product - Google Patents
Preparation method of automobile exhaust purification catalyst with controllable precious metal content and obtained product Download PDFInfo
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Abstract
The invention discloses a preparation method of an automobile exhaust purification catalyst with controllable precious metal content and an obtained product. The method has the advantages of simple process and low cost, the active noble metal content on the surface of the obtained catalyst is controllable, the particle size is small, the dispersibility is good, the application range of the catalyst carrier is wide, and the problems of poor noble metal dispersibility, low utilization rate and the like existing in methods such as dipping preparation and the like are effectively avoided.
Description
Technical Field
The invention relates to a preparation method of an automobile exhaust purification catalyst with controllable precious metal content and an obtained product, and belongs to the technical field of preparation of automobile exhaust purification catalysts.
Background
With the rapid development of economic society, the automobile keeping quantity in China is continuously improved in recent years, and Nitrogen Oxide (NO) discharged from tail gas x ) And pollutants such as hydrocarbon (CH), carbon monoxide (CO) and Particulate Matters (PM) are increasing day by day, so that the problems of atmospheric pollution such as acid rain, haze, photochemical smog, increased ozone concentration and the like are increasing day by day, the ecological environment is seriously damaged, and the health of human is damaged. Therefore, the purification and elimination of automobile exhaust pollutants are important problems to be solved urgently in the work of air pollution prevention and control.
Catalytic purification is the most effective automobile exhaust pollution control technology recognized at present, and mainly comprises a three-way catalytic converter (TWC) for gasoline vehicles, a diesel vehicle oxidation catalyst (DOC) for diesel vehicles and passive NO x Adsorption (PNA), Ammonia Slip Catalyst (ASC), catalytic particle trap (CDPF), and the like. The core of the above technology is catalytic materials, and most of these catalytic materials are supported catalysts using noble metals as active components. However, the preparation of the noble metal-supported catalyst usually adopts an impregnation method, and the obtained catalyst has poor noble metal dispersibility, is easy to agglomerate, and has larger particle size, so that the utilization rate of the noble metal is lower. Therefore, the development of a catalyst preparation method which can uniformly disperse the noble metal on the surface of the catalyst carrier material, keep the noble metal in a smaller particle size and is not easy to agglomerate has important significance for the preparation and application of the automobile exhaust catalyst and can generate certain positive influence on the development of the field of air pollution control.
CN103223347B discloses a method for synthesizing a silica supported nickel platinum catalyst by ultrasonic spray pyrolysis, which requires that a carrier is vaporized and decomposed into liquid drops, and then the liquid drops are contacted with atomized noble metal vapor to react, so that the dispersion is not uniform enough, and the liquid drops formed by carrier vaporization easily embed active sites such as noble metals in the inner covering active sites, resulting in the reduction of catalyst activity.
Disclosure of Invention
Aiming at the problems of poor dispersity, easy agglomeration, low utilization rate and the like of precious metal components of the automobile exhaust purification catalyst, the invention provides a preparation method of the automobile exhaust purification catalyst with controllable precious metal content.
The specific technical scheme of the invention is as follows:
a preparation method of an automobile exhaust purification catalyst with controllable precious metal content comprises the following steps:
(1) mixing a noble metal precursor with a solvent to prepare a precursor solution;
(2) atomizing the precursor solution by using an ultrasonic atomizer, and spraying the obtained spray onto a catalyst carrier;
(3) after spraying is finished, treating the catalyst carrier under the protection of atmosphere to decompose the noble metal precursor in situ on the surface of the catalyst carrier;
(4) after the precursor is decomposed, the catalyst carrier is roasted under the protection of atmosphere to obtain the automobile exhaust purification catalyst with controllable noble metal content.
Further, in the step (1), the precious metal is one or more of platinum, palladium and rhodium, the precursor of platinum includes one or more of platinum nitrate, platinum chloride, chloroplatinic acid, platinum tetraammine nitrate, potassium hexachloroplatinate and platinum tetraammine hydroxide, the precursor of palladium includes one or more of palladium nitrate, palladium sulfate, palladium chloride, palladium acetate, ammonium tetrachloropalladate, ammonium hexachloropalladate, tetraammine palladium chloride, potassium tetrachloropalladate, potassium hexachloropalladate, tetraaminopalladium nitrate and palladium acetylacetonate, and the precursor of rhodium includes one or more of rhodium nitrate, rhodium chloride, rhodium sulfate, ammonium hexachlororhodium and rhodium acetylacetonate.
Further, the solvent is water or/and ethanol.
Further, the concentration of the precursor solution is 0.001-1 mol/L, preferably 0.001-0.2 mol/L.
Further, the catalyst carrier is one or a composite oxide of alumina, cerium oxide, zirconium oxide, cerium-zirconium solid solution, yttrium zirconium oxide, lanthanum oxide, copper oxide, iron oxide and barium oxide, or the catalyst carrier is ZSM-5, Beta, SSZ-13 or SAPO-34. After a series of screens, the catalyst support is preferably alumina or SSZ-13 molecular sieve.
Further, in the step (2), the spraying frequency is 1-5 Hz, the spraying temperature is 120-200 ℃, and the spraying time is 20-600 min, preferably 1-2 h.
Further, in the step (2), the catalyst carrier is placed into a tube furnace, the temperature of the tube furnace is maintained at 120-.
Further, in the step (3), the catalyst carrier is treated under air or nitrogen atmosphere, and the gas flow rate is 50-70 mL/min. The treatment temperature is 250-550 ℃, and the treatment time is 2-4h, so that the noble metal precursor is decomposed in situ on the surface of the catalyst carrier.
Further, in the step (4), the catalyst carrier is calcined in the air or nitrogen atmosphere, and the gas flow rate is 90-110 mL/min. The roasting temperature is 400-800 ℃, and the roasting time is 4-6 h.
Further, after the step (4), for the catalyst to be reduced, a step of reducing in a hydrogen atmosphere is also included, that is, after the catalyst carrier is calcined under the atmosphere protection, the catalyst carrier is reduced in the hydrogen atmosphere to obtain the automobile exhaust purification catalyst with controllable precious metal content. The hydrogen atmosphere is filled with mixed gas of hydrogen and nitrogen, wherein the volume content of the hydrogen is 8-12%, the flow rate of the mixed gas is 90-120mL/min, and the reduction temperature range is 300-oC。
In a specific embodiment of the present invention, a method for preparing a specific catalyst for purifying automobile exhaust with controllable precious metal content is provided, which comprises the following steps:
(1) putting a catalyst carrier into a porcelain boat of a tube furnace, dissolving a noble metal precursor into a solvent to obtain a precursor solution with a certain concentration, setting the tube furnace at a certain temperature, setting an ultrasonic sprayer at a certain spraying frequency and time, and spraying the precursor solution generated by the ultrasonic sprayer into the tube furnace filled with the catalyst carrier;
(2) after spraying is finished, raising the temperature of the tubular furnace to a certain temperature and introducing atmosphere to decompose the precursor solution in situ on the surface of the carrier material;
(3) after the precursor solution is decomposed, continuously roasting at a certain temperature and in an atmosphere to prepare the catalyst.
Furthermore, the automobile exhaust purification catalyst with controllable noble metal content obtained by the method is also within the protection range of the invention, and compared with the catalyst obtained by the traditional impregnation method, the catalyst obtained by the invention has the advantages of good noble metal dispersibility, difficult agglomeration, small size and better catalytic performance.
The invention has the following beneficial effects:
1. the prepared noble metal precursor solution is sprayed into a mist shape through an ultrasonic sprayer, and the fine liquid drops are directly loaded on the surface of the catalyst carrier in the tubular furnace, so that the dispersion of the solution on the surface of the carrier material is greatly improved.
2. The catalyst carrier material provided by the invention does not need atomization and other treatments, and can directly load noble metal in situ to prepare the automobile exhaust purification catalyst with high-dispersion active sites. The invention is suitable for catalyst carrier materials such as various oxides, molecular sieves and the like, has wide application range, and the preparation and the roasting of the catalyst are carried out in the same device without transfer, which is equivalent to the step roasting and then reducing, thereby improving the stability of the noble metal on the surface of the catalyst.
Detailed Description
The technical solution of the present invention will be described in detail with reference to the following specific examples, but the scope of the present invention is not limited to the following specific examples.
Example 1
A preparation method of an automobile exhaust purification catalyst comprises the following steps:
1. weigh 10 g of CeO2-Al2O3The catalyst carrier material is put into a porcelain boat of a tube furnace, and the temperature of the tube furnace is set to be 200oC。
2. Dissolving chloroplatinic acid into absolute ethyl alcohol to prepare 0.0133 mol/L precursor solution, adding 50mL of the precursor solution into an ultrasonic atomizer, adjusting the frequency of the atomizer to be 1 Hz, spraying the obtained spray into a tubular furnace, and ultrasonically spraying for 1 h;
3. after the ultrasonic spraying is finished, the temperature of the tube furnace is raised to 350 ℃ in the air atmosphereoC, controlling the air flow rate in the tube furnace to be 60mL/min, and preserving the heat for 2h to enable the chloroplatinic acid to be dropped on the CeO2-Al2O3Surface decomposition;
4. then the tube furnace is heated to 500 DEGoC, in N2Roasting for 4H under the atmosphere, controlling the nitrogen flow rate to be 100mL/min, and finally introducing 10% H2/N2At 500oContinuing roasting for 3 hours under C, wherein the flow rate of the mixed gas is 100mL/min, and reducing to obtain Pt/CeO2-Al2O3A catalyst.
Example 2
Pt/CeO was prepared according to the method of example 12-Al2O3A catalyst, except that: in the step 2, the concentration of the precursor solution is 0.133 mol/L.
The noble metal particle size, noble metal loading, noble metal dispersion, and ammonia oxidation activity of the catalysts obtained in examples 1 and 2 were measured by a high angle annular dark field transmission electron microscope (HAADF), noble metal loading was measured by inductively coupled plasma emission spectroscopy, and noble metal dispersion was measured by CO titration.
The ammoxidation activity is tested by adopting simulated tail gas, and the simulated tail gas comprises the following components: 300 ppm NH3、8 vol.% O2、10 vol.% H2O and balance gas are He. Introducing the simulated tail gas into a reactor containing 50 mg of catalyst, and keeping the reaction temperature at 30-600 DEGoC, the gas flow rate is 100mL/min.
The performance results of the catalysts obtained in examples 1 and 2 are shown in table 1 below:
as can be seen from Table 1, the 1.3 wt% Pt loading is Pt/CeO2-Al2O3The activity of the catalyst is better than that of Pt/CeO loaded at 0.13 wt percent2-Al2O3The catalytic activity of (3).
Example 3
1. Weighing 10 g of Na-SSZ-13 molecular sieve into a porcelain boat of a tube furnace, wherein the temperature of the tube furnace is set to be 150oC. Dissolving palladium chloride into absolute ethyl alcohol to prepare 0.0019 mol/L precursor solution, adding 600mL of the precursor solution into an ultrasonic atomizer, adjusting the frequency of the atomizer to be 2 Hz, spraying the obtained spray into a tubular furnace, and ultrasonically spraying for 1.5 h;
2. after the ultrasonic spraying is finished, the temperature of the tube furnace is raised to 500 ℃ in the air atmosphereoC, controlling the air flow rate in the tube furnace to be 60mL/min, and preserving the heat for 3 hours to enable palladium chloride liquid drops to be decomposed on the surface of the Na-SSZ-13 molecular sieve;
3. then the tube furnace is heated to 600 DEGoC, in N2Roasting for 4 hours in the atmosphere, and controlling the nitrogen flow rate to be 100mL/min to prepare the Pd-SSZ-13 molecular sieve catalyst.
The catalyst obtained in example 3 was tested for noble metal particle size, noble metal loading, noble metal dispersion, and passive nitrogen oxide adsorption performance of the catalyst, while control catalyst 1 and control catalyst 2 were used as controls.
Control catalyst 1 was prepared by impregnation, as follows:
1. weighing 10 g of Na-SSZ-13 molecular sieve in a small beaker, dropwise adding 0.2 mol/L palladium chloride aqueous solution which is equal to the volume of the molecular sieve pores, and ultrasonically dispersing for 5 min;
2. mixing the molecular sieve with palladium chloride at 40 deg.coC, stirring and evaporating in a water bath, and performing isovolumetric impregnation;
3. placing the mixture of the molecular sieve and the palladium chloride obtained by impregnation in a tubular furnace, and heating to 600 DEGoC, in N2Roasting for 4 hours in the atmosphere, and controlling the nitrogen flow rate to be 100mL/min to prepare the Pd-SSZ-13 molecular sieve catalyst.
Control catalyst 2 was prepared as follows:
1. weighing 10 g of Na-SSZ-13 molecular sieve into a porcelain boat of a tube furnace, wherein the temperature of the tube furnace is set to be 150oC. Dissolving palladium chloride into absolute ethyl alcohol to prepare a precursor solution of 0.0019 mol/L, adding 6000mL of the precursor solution into an ultrasonic atomizer, adjusting the frequency of the atomizer to be 2 Hz, spraying the obtained spray into a tubular furnace, and ultrasonically spraying for 1.5 h;
2. after the ultrasonic spraying is finished, the temperature of the tube furnace is raised to 500 ℃ in the air atmosphereoC, controlling the air flow rate in the tube furnace to be 100mL/min, and preserving the heat for 3 hours to enable palladium chloride liquid drops to be decomposed on the surface of the Na-SSZ-13 molecular sieve;
3. then the tube furnace is heated to 600 DEGoC, in N2Roasting for 4 hours in the atmosphere, and controlling the nitrogen flow rate to be 60mL/min to prepare the Pd-SSZ-13 molecular sieve catalyst.
The size of the noble metal particles is measured by a high-angle annular dark field transmission electron microscope (HAADF), the noble metal loading is measured by inductively coupled plasma emission spectroscopy, and the noble metal dispersion is measured by CO titration.
Passive nitrogen oxide adsorption performance adopts simulation tail gas to test, and the simulation tail gas composition is: 200 ppm NO, 14 vol.% O2And the balance gas is He. Introducing the simulated tail gas into a reactor containing 120 mg of catalyst, and keeping the reaction temperature at 30-600 DEGoC, the gas flow rate is 300 mL/min.
The results of the experiment are shown in table 2 below:
from the results in the table, it can be seen that, under the condition of the same Pd loading, the catalyst obtained by the ultrasonic spray pyrolysis method of the present invention has smaller noble metal particle size, higher dispersity, better catalytic performance and better passive nitrogen oxide adsorption performance compared with the catalyst obtained by the impregnation method. And a product with better performance can be obtained by controlling the flow rate of the atmosphere.
Example 4
1. Weigh 10 g Ce0.22Pr0.7Nd0.7Zr0.57Y0.7O0.2Placing the composite oxide into a porcelain boat of a tube furnace, wherein the temperature of the tube furnace is set to be 120oDissolving chloroplatinic acid into absolute ethyl alcohol to prepare 0.0082 mol/L precursor solution, adding 60mL of the precursor solution into an ultrasonic atomizer, adjusting the frequency of the atomizer to be 2 Hz, spraying the obtained spray into a tube furnace, and ultrasonically spraying for 2 hours;
2. after the ultrasonic spraying is finished, the temperature of the tube furnace is raised to 350 ℃ in the air atmosphereoC, controlling the air flow rate in the tube furnace to be 60mL/min, and preserving the heat for 3 h to enable the chloroplatinic acid to be dropped on the Ce0.22Pr0.7Nd0.7Zr0.57Y0.7O0.2Surface decomposition;
3. then the tube furnace is heated to 600 DEGoC, in N2Roasting for 4H under the atmosphere, controlling the nitrogen flow rate in the tubular furnace to be 100mL/min, and finally introducing 10% H with the flow rate of 100mL/min2/N2At 300, inoReduction preparation under C to obtain Pt-Ce0.22Pr0.7Nd0.7Zr0.57Y0.7O0.2A catalyst.
The catalyst obtained in example 4 was tested for precious metal particle size, precious metal loading, precious metal dispersion and dynamic oxygen storage performance (DOSC) and three-way performance (TWC) of the catalyst, while being compared to a catalyst prepared according to the method disclosed in CN 103223347B. The preparation method of the control catalyst was: the carrier is selected from Ce (NO) with a certain concentration3)3、Pr(NO3)3、Nd(NO3)3、Zr(NO3)4、Y(NO3)3Mixing salt solution, heating and vaporizing the salt solution, feeding the salt solution into a pyrolysis reactor under the drive of carrier gas, simultaneously contacting the generated oxide with Pt liquid drops, and preparing Pt-Ce with the same Pt content0.22Pr0.7Nd0.7Zr0.57Y0.7O0.2A catalyst.
The size of the noble metal particles is measured by a high-angle annular dark field transmission electron microscope (HAADF), the noble metal loading is measured by inductively coupled plasma emission spectroscopy, and the noble metal dispersion is measured by CO titration.
The dynamic oxygen storage performance (DOSC) is tested by adopting simulated tail gas under the following test conditions: introducing the simulated tail gas into a reactor containing 50 mg of catalyst, and keeping the reaction temperature at 200-500 DEG CoAnd C, the gas flow rate is 50 mL/min, and the pulse test switching frequency is 0.05 Hz. The simulated tail gas composition is shown in table 3 below:
the three-way performance (TWC) is tested by adopting simulated tail gas, and the test conditions are as follows: the simulated tail gas is introduced into a reactor containing 100 mg of catalyst, and the reaction temperature is kept at 100-oC, the gas flow rate is 300 mL/min. The simulated tail gas composition is shown in table 4 below:
the results of the experiments are shown in tables 5-7 below:
as can be seen from the results in the table, the Pt-Ce prepared by the method of the invention0.22Pr0.7Nd0.7Zr0.57Y0.7O0.2The dynamic oxygen storage capacity and the three-way catalytic performance are both superior to those of the contrast catalyst.
Example 5
1. Weigh 10 g of CeO2The carrier material is put into a porcelain boat of a tube furnace, and the temperature of the tube furnace is set to be 200oC. Dissolving platinum tetraammine nitrate into absolute ethyl alcohol to prepare 0.0082 mol/L precursor solution, adding 60mL of the precursor solution into an ultrasonic atomizer, adjusting the frequency of the atomizer to be 1 Hz, spraying the obtained spray into a tube furnace, and ultrasonically spraying for 1 h;
2. after the ultrasonic spraying is finished, the temperature of the tube furnace is raised to 550 ℃ in the air atmosphereoC, controlling the air flow rate in the tube furnace to be 60mL/min, and preserving the heat for 2h to ensure that the platinum tetraammine nitrate is in CeO2Surface decomposition;
3. the tube furnace was then warmed to 750 deg.foC, in N2Roasting for 4H under the atmosphere, controlling the nitrogen flow rate in the tubular furnace to be 100mL/min, and finally introducing 10% H with the flow rate of 100mL/min2/N2At 300, inoReducing under C to obtain Pt/CeO2A catalyst.
The catalyst obtained in example 5 was tested for precious metal particle size, precious metal loading, precious metal dispersion, and catalytic soot combustion activity of the catalyst, while control catalysts 1 and 2 were used as controls.
Control catalyst 1 was prepared as follows: the carrier is selected from Ce (NO) with a certain concentration3)3Precursor salt solution, first Ce (NO)3)3Heating and vaporizing salt solution, and introducing the vaporized salt solution into a pyrolysis reactor through carrier gas to obtain CeO2The liquid drops are contacted with the Pt liquid drops in the reactor to prepare Pt/CeO with the same Pt loading capacity2。
Control catalyst 2 was prepared as follows:
1. weigh 10 g of CeO2The carrier material is put into a porcelain boat of a tube furnace, and the temperature of the tube furnace is set to be 200oC. Dissolving platinum tetraammine nitrate into absolute ethyl alcohol to prepare 0.0082 mol/L precursor solution, adding 60mL of the precursor solution into an ultrasonic atomizer, adjusting the frequency of the atomizer to be 1 Hz, spraying the obtained spray into a tube furnace, and ultrasonically spraying for 1 h;
2. after the ultrasonic spraying is finished, the temperature of the tube furnace is raised to 750 DEGoC, in N2Roasting for 4H under the atmosphere, controlling the nitrogen flow rate in the tubular furnace to be 100mL/min, and finally introducing 10% H with the flow rate of 100mL/min2/N2At 300, inoReducing under C to obtain Pt/CeO2A catalyst.
The size of the noble metal particles is measured by a high-angle annular dark field transmission electron microscope (HAADF), the noble metal loading is measured by inductively coupled plasma emission spectroscopy, and the noble metal dispersion is measured by CO titration.
The test conditions for the catalytic soot combustion activity are as follows: 45 mg of catalyst and 5 mg of soot were mixed and 5vol.% O was introduced at a rate of 100mL/min2and/He, performing soot combustion activity test.
The results of the experiments are shown in tables 8-9.
As can be seen from the results in the table, the Pt/CeO prepared by the invention2Has higher activity (T)90 oC = 396) and carbon dioxide selectivity, which shows that the catalyst obtained by the method of the invention has more excellent catalytic performance.
The foregoing has shown and described the principles, broad features and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed.
Claims (10)
1. A preparation method of an automobile exhaust purification catalyst with controllable precious metal content is characterized by comprising the following steps:
(1) mixing a noble metal precursor with a solvent to prepare a precursor solution;
(2) atomizing the precursor solution by using an ultrasonic atomizer, and spraying the obtained spray onto a catalyst carrier;
(3) after spraying is finished, treating the catalyst carrier under the protection of atmosphere to decompose the noble metal precursor in situ on the surface of the catalyst carrier;
(4) after the precursor is decomposed, the catalyst carrier is roasted under the protection of atmosphere to obtain the automobile exhaust purification catalyst with controllable noble metal content.
2. The method of claim 1, wherein: in the step (4), after the catalyst carrier is roasted under the protection of atmosphere, the method also comprises the step of reducing the catalyst carrier under the hydrogen atmosphere to obtain the final automobile exhaust purification catalyst with controllable noble metal content, wherein the mixed gas of hydrogen and nitrogen is introduced into the hydrogen atmosphere, the volume content of the hydrogen is 8-12%, the flow rate of the mixed gas is 90-120mL/min, and the reduction temperature range is 300-oC。
3. The method according to claim 1 or 2, characterized in that: in the step (1), the precious metal is one or more of platinum, palladium and rhodium, the precursor of platinum comprises one or more of platinum nitrate, platinum chloride, chloroplatinic acid, platinum tetraammine nitrate, potassium hexachloroplatinate and platinum tetraammine hydroxide, the precursor of palladium comprises one or more of palladium nitrate, palladium sulfate, palladium chloride, palladium acetate, ammonium tetrachloropalladate, ammonium hexachloropalladate, palladium tetraammine chloride, potassium tetrachloropalladate, potassium hexachloropalladate, palladium tetraaminonitrate and palladium acetylacetonate, and the precursor of rhodium comprises one or more of rhodium nitrate, rhodium chloride, rhodium sulfate, ammonium hexachlororhodate and rhodium acetylacetonate.
4. The method according to claim 1 or 2, characterized in that: the solvent is water or/and ethanol.
5. The method according to claim 1 or 2, characterized in that: the catalyst carrier is one or a composite oxide of alumina, cerium oxide, zirconium oxide, cerium-zirconium solid solution, yttrium zirconium oxide, lanthanum oxide, copper oxide, iron oxide and barium oxide, or ZSM-5, Beta, SSZ-13 or SAPO-34.
6. The method of claim 1, wherein: in the step (1), the concentration of the precursor solution is 0.001-1 mol/L.
7. The method of claim 1, wherein: in the step (2), the spraying frequency is 1-5 Hz, and the spraying temperature is 120-oC, spraying for 20-600 min; preferably, the catalyst support is placed in a tube furnace and then the spray is sprayed onto the catalyst support.
8. The method of claim 1, wherein: in the step (3), the treatment is carried out for 2-4h at the temperature of 250-550 ℃; in the step (4), the roasting temperature is 400-.
9. The method according to claim 1 or 8, wherein: in the step (3), the treatment is carried out in the air or nitrogen atmosphere, and the gas flow rate is 50-70 mL/min; in the step (4), roasting is carried out in the air or nitrogen atmosphere, and the gas flow rate is 90-110 mL/min.
10. The product of the method for preparing the catalyst for purifying automobile exhaust gas with controllable noble metal content according to claim 1.
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