CN114471543A - Method for preparing platinum-based noble metal catalyst by wet process - Google Patents
Method for preparing platinum-based noble metal catalyst by wet process Download PDFInfo
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- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
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Abstract
A method for preparing a platinum-based noble metal catalyst by a wet method belongs to the field of heterogeneous catalysis, and provides a preparation method of a green and environment-friendly high-activity platinum-based catalyst suitable for industrialization. The method is used for overcoming the defects of complex steps, more control conditions and low utilization rate of platinum atoms of the existing commercial platinum-based catalyst in the existing synthetic method. The method adopts a simple hydrothermal method to synthesize precursor material from the carrier powder of the precursor, and the precursor material is calcined in various gases by a tubular furnace and finally ground, granulated and the like to obtain the Pt-based catalyst material with high activity. The material can reach 100% carbon monoxide oxidation efficiency under the standard carbon monoxide oxidation condition at the low temperature of 90 ℃. The synthesis method adopts a simple hydrothermal method for synthesis, adopts an excessively complex noble metal synthesis route, improves the utilization efficiency of raw materials, reduces the synthesis cost, has a simple synthesis process, is a green and simple wet synthesis route, and is suitable for industrial large-scale production.
Description
Technical Field
The invention belongs to the field of heterogeneous catalysis, and provides a preparation method of a green and environment-friendly platinum-based catalyst, which is suitable for industrialization.
Background
Heterogeneous catalytic reactions, which have been an important research topic for many years, have many potential applications, in particular in air purification, respiratory protection and pollution control devices, in industry and in the field of industrial applicationsThe device for automobile exhaust has wide application. The catalysts used for CO oxidation are mostly noble metal catalysts and some transition metal catalysts. CoOX、MnOXThe transition metal has better selectivity and lower cost, and the development of the catalyst without noble metal can not only reduce the unit cost, but also meet the emission regulation target. Small particles and higher specific surface area catalysts can also compete with noble metals. But the utilization rate is low, the activity is far lower than that of a noble metal catalyst, and the catalyst cannot be widely applied.
Smaller noble metal nanoparticles generally have higher activity at lower temperatures, however, catalysts have temperatures as high as 750 ℃ under some special conditions, resulting in sintering of the noble metal into larger particles, losing the original high activity. In addition, the catalyst is easy to cause poisoning of water and sulfur, and even carbonate species formed on the surface of the catalyst prevent further reaction of the catalyst. However, many noble metal catalysts reported now solve the above problems, and monatomic catalysts, in which all metal atoms are exposed on a usable support, have been extensively studied and utilized. For the catalytic reaction, the problems of expensive noble metal, insufficient supply, difficulty in finding a suitable substitute and the like can be solved. The electronic properties of the isolated monatomic metal are significantly different from the active sites in the bulk material and nanoparticles, potentially allowing for the efficient use of more noble metal elements.
Although noble metals have many disadvantages, noble metal catalysts have been used most widely due to the continuous development of research and development in recent years. Surface-supported isolated atoms in monatomic catalysts typically have a variety of defects. To maximize the number of catalyst active sites available, the noble metal may be dispersed on a monoatomic or sub-nanoclustered support. The activity and stability of the supported metal catalyst are closely related to the oxidation state and the local coordination structure of the catalytic metal active site, and the interaction with the carrier is influenced. Isolated noble metal monoatomic species can be stabilized by strong covalent metal-support interactions (CMSI) or Electronic Metal Support Interactions (EMSI) independent of support defects, creating highly supported and thermally stable catalysts by trapping already deposited monoatomic species or noble metal oxide vapor units that evaporate from nanoparticles during high temperature calcination, and can even be extended to non-reducible metal oxide supports.
Noble metal catalysts can be used not only for reduction, hydrogenolysis, hydrocarbon oxidation, isomerization and cyclization reactions, but also for oxidation reactions. In particular, Pt-based catalysts are the most studied and used noble metal catalysts in CO oxidation. Research on the problem of CO oxidation by a Pt catalyst has been carried out as early as 70 years in the 20 th century, and research shows that the catalyst loaded with Pt for CO oxidation is easy to sinter under a high-temperature condition, and experiments show that the reaction rate of CO shows that the reaction is not easy to occur at a low CO concentration and a higher CO concentration, and because the lower CO concentration is not beneficial to the occurrence of the CO oxidation reaction, the too high concentration is easy to cover the surface absorbing oxygen, so that the CO oxidation is hindered. The CO oxidation is divided into two steps, the first step is an E-R mechanism, the second step is chemical adsorption of oxygen, the excessive CO concentration prevents the process from going on, and the surface exposed atom surface area is seriously reduced under the condition of high temperature (800 ℃) of air, which shows that the catalyst is easy to sinter under the high temperature condition, so that the catalytic activity of the catalyst is reduced, and the apparent activation energy is higher.
Pt-based multi-phase catalysts are also key catalysts in many important industrial chemical processes, but their atom utilization is low due to the use of only surface active site atoms. Thus, a highly dispersible noble metal Pt catalyst is synthesized, Pt is anchored on the surface of the carrier in isolated single atom form, the catalyst has extremely high atom utilization rate, and CO oxidation and CO H are carried out2PROX in (2) shows excellent stability and high activity. The chemical reaction principle of the monoatomic Pt with positive charge in the catalyst is greatly different from that of a single Au atom or a cation on the same carrier, the monoatomic Au is inactive, but the electron of the Pt atom can be transferred to the surface of the carrier, so that the monoatomic Pt has enough 5d empty orbitals, which is beneficial to reducing CO adsorption energy and CO oxidation activation energy barrier, and the catalytic activity of the catalyst is improved. The monatomic Pt catalyst is not limited to acting on CO oxidation, and in addition, by a charge transfer mechanismThe stable single atom on the actual oxide carrier is also suitable for other noble metal systems through further extension, and the carrier oxide also has diversity. The discovery of such platinum catalysts not only demonstrates the concept of heterogeneous catalysis, but also has great potential for reducing the high cost of industrial precious metal catalysts.
Disclosure of Invention
The invention aims to solve the defects of complex steps, more control conditions, toxic and harmful synthetic raw materials and low utilization rate of noble metal atoms in the conventional synthetic method. Provides a preparation method of a green and environment-friendly platinum-based catalyst suitable for industrialization. The method adopts a hydrothermal method to synthesize a precursor suspension, and finally adopts a physical method to granulate to obtain the platinum-based catalyst after the steps of washing, drying, calcining and the like.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for preparing a platinum-based noble metal catalyst by a wet method is characterized by comprising the following steps:
step 1, mixing 10mg/ml chloroplatinic acid aqueous solution and P25 titanium dioxide, adding distilled water, and then carrying out hydrothermal reaction to obtain yellow suspended slurry. Wherein 3-4 ml of chloroplatinic acid aqueous solution of 10mg/ml, 1.1-1.3 g of P25, 90-110 ml of distilled water, 75-85 ℃ of hydrothermal reaction conditions and 2-4 hours of hydrothermal reaction duration are added.
And 2, centrifuging the suspension obtained in the step 1 by using a centrifugal machine, removing clear liquid, adding distilled water, and re-dispersing the precipitate for washing. The washing step is repeated for a plurality of times, precipitates are removed, and the precipitate is freeze-dried by a freeze dryer and then ground into fine powder P.
And 3, calcining the solid powder P obtained in the step 2 in a tubular furnace, and naturally cooling to obtain solid powder O after the calcination is finished. Wherein the calcining temperature range of the tubular furnace is 200-800 ℃, the calcining time is 2-6 h, and the heating rate is 4-6 ℃/min.
And 4, putting the solid powder O obtained in the step 3 into a die with the diameter of 10mm, and pressurizing the die filled with the powder by using a tablet machine to obtain a flaky material.
And 5, grinding the flaky material obtained in the step 4 on a 40-60-mesh sieve by using a quartz pestle, and sieving particles which do not conform to the size by using the sieve to obtain the high-activity platinum-based catalyst material.
The invention has the following advantages:
1. the method adopts a hydrothermal method to synthesize a precursor suspension, and finally adopts a physical method to granulate to obtain the platinum-based catalyst after the steps of washing, drying, calcining and the like. The method solves the problem of complex conventional synthesis route of the catalyst, simultaneously solves the waste of the commercial noble metal catalyst in the synthesis process, and greatly improves the atom utilization rate of the noble metal.
2. The method is a route for preparing the high-activity platinum-based catalyst suitable for heterogeneous catalysis by a wet method, and the wet method is adopted in the synthesis process. The reaction conditions are milder, the complexity is lower, and the large-scale industrial production is easier to realize.
3. The material synthesized by the experiment has high atomic dispersibility, effectively improves the utilization rate of noble metal and effectively reduces the cost of the catalyst.
4. The experiment can achieve very excellent catalytic effect under the CO oxidation condition, and the catalyst particles can completely oxidize all CO gas in the atmosphere at 90 ℃.
Drawings
FIG. 1 is an XRD pattern for the preparation of a platinum-based catalyst (three methods)
FIG. 2 is a graph showing the activity curves of the preparation of a platinum-based catalyst (three methods) under carbon monoxide oxidation conditions
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Example 1
After 3.45ml of a 10mg/ml chloroplatinic acid aqueous solution and 1.3g of P25 titanium dioxide were mixed in a certain proportion, 100ml of distilled water was added, followed by hydrothermal reaction at 80 ℃ for 3 hours to obtain a yellow suspension slurry. Centrifuging the suspension with a centrifuge, removing the clear solution, adding distilled water, and re-dispersing the precipitate for washing. After the washing step was repeated three times, the precipitate was lyophilized with a lyophilizer and then ground into a solid powder P. And calcining the solid powder P in a tubular furnace, wherein the calcining condition is 350 ℃, the calcining time is 3h, and the heating rate is 5 ℃/min. And naturally cooling after calcination to obtain solid powder O, taking 100mg of the solid powder O obtained in the previous step, putting the solid powder O into a die with the diameter of 10mm, and pressurizing the die with the powder by using a tablet press for 50 s. A sheet-like material is obtained. And grinding the obtained flaky material on a 40-60-mesh sieve by using a quartz pestle, and sieving particles which do not conform to the size by using the sieve to obtain the high-activity platinum-based catalyst material A.
XRD phase analysis is carried out on the material A, as shown in figure 1, the prepared sample has signals of titanium dioxide anatase phase and rutile phase, 80mg of catalyst particles and 400mg of quartz sand particles with 40-60 meshes are uniformly mixed and then are placed in a fixed bed reactor to test conditions: the gas volume ratio is 1% carbon monoxide, 1% oxygen and 98% nitrogen atmosphere. The fixed bed reactor was heated and the catalyst was able to completely oxidize the carbon monoxide in the reactor at 90 c as shown in figure 2.
Example 2
After 3.18ml of a 10mg/ml chloroplatinic acid aqueous solution and 1.2g of P25 titanium dioxide were mixed in a certain proportion, 105ml of distilled water was added, followed by hydrothermal reaction at 85 ℃ for 3 hours to obtain a yellow suspension slurry. Centrifuging the suspension with a centrifuge, removing the clear solution, adding distilled water, and re-dispersing the precipitate for washing. After the washing step was repeated three times, the precipitate was lyophilized with a lyophilizer and then ground into a solid powder P. And calcining the solid powder P in a tubular furnace, wherein the calcining condition is 450 ℃, the calcining time is 5h, and the heating rate is 5 ℃/min. And naturally cooling after calcination to obtain solid powder O, taking 100mg of the solid powder O obtained in the previous step, putting the solid powder O into a die with the diameter of 10mm, and pressurizing the die with the powder by using a tablet press for 80 s. A sheet-like material is obtained. And grinding the obtained flaky material on a 40-60-mesh sieve by using a quartz pestle, and sieving particles which do not conform to the size by using the sieve to obtain the high-activity platinum-based catalyst material B.
XRD phase analysis is carried out on the material B, as shown in figure 1, the prepared sample has signals of titanium dioxide anatase phase and rutile phase, 80mg of catalyst particles and 400mg of quartz sand particles of 40-60 meshes are uniformly mixed and then are placed in a fixed bed reactor, and the test conditions are that the gas volume ratio is 1% of carbon monoxide, 1% of oxygen and 98% of nitrogen atmosphere. Heating a fixed bed reactor, as shown in figure 2, the catalyst was able to completely oxidize the carbon monoxide in the reactor at 150 ℃.
Example 3
After 3.18ml of a 10% chloroplatinic acid aqueous solution and 1.2g of P25 titanium dioxide were mixed in proportion, 110ml of distilled water was added, followed by hydrothermal reaction at 75 ℃ for 2.5 hours to obtain a yellow suspension slurry. Centrifuging the suspension with a centrifuge, removing the clear solution, adding distilled water, and re-dispersing the precipitate for washing. After the washing step was repeated three times, the precipitate was lyophilized with a lyophilizer and then ground into a solid powder P. And calcining the solid powder P in a tubular furnace under the calcining condition of 550 ℃, the calcining time of 6h and the heating rate of 5 ℃/min. And naturally cooling after calcination to obtain solid powder O, taking 100mg of the solid powder O obtained in the previous step, putting the solid powder O into a die with the diameter of 10mm, and pressurizing the die with the powder by using a tablet press for 60 s. And obtaining the sheet material. The obtained flaky material was ground with a quartz pestle on a 40-60 mesh screen, and particles not conforming to the size were sieved out with the mesh screen to obtain a highly active platinum-based catalyst material C.
XRD phase analysis is carried out on the material C, as shown in figure 1, the prepared sample has signals of titanium dioxide anatase phase and rutile phase, 80mg of catalyst particles and 400mg of quartz sand particles of 40-60 meshes are uniformly mixed and then are placed in a fixed bed reactor, and the test conditions are that the gas volume ratio is 1% of carbon monoxide, 1% of oxygen and 98% of nitrogen atmosphere. Heating a fixed bed reactor, as shown in figure 2, the catalyst was able to completely oxidize the carbon monoxide in the reactor at 120 ℃.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.
Claims (4)
1. A method for preparing a platinum-based noble metal catalyst by a wet method is characterized by comprising the following steps:
step 1, mixing 10mg/ml chloroplatinic acid aqueous solution and P25 titanium dioxide, adding distilled water, and then carrying out hydrothermal reaction to obtain yellow suspended slurry; wherein 3-4 ml of 10mg/ml chloroplatinic acid aqueous solution is added, 1.1-1.3 g of P25 is added, the volume of the added distilled water is 90-110 ml, the hydrothermal reaction condition is 75-85 ℃, and the duration of the hydrothermal reaction is 2-4 hours;
step 2, centrifuging the suspension obtained in the step 1 by using a centrifugal machine, removing clear liquid, adding distilled water to re-disperse the precipitate for washing; repeating the washing step for several times, removing precipitate, lyophilizing with a lyophilizer, and grinding into fine powder P;
step 3, calcining the solid powder P obtained in the step 2 in a tubular furnace, and naturally cooling to obtain solid powder O after the calcining is finished; wherein the calcining temperature range of the tubular furnace is 200-800 ℃, the calcining time is 2-6 h, and the heating rate is 4-6 ℃/min;
step 4, putting the solid powder O obtained in the step 3 into a die with the diameter of 10mm, and pressurizing the die filled with the powder by using a tablet machine to obtain a sheet material;
and 5, grinding the flaky material obtained in the step 4 on a 40-60-mesh sieve by using a quartz pestle, and sieving particles which do not conform to the size by using the sieve to obtain the high-activity platinum-based catalyst material.
2. The method for preparing a platinum-based noble metal catalyst by a wet process according to claim 1, wherein the washing is repeated 2 to 4 times in the step 2.
3. The method for preparing the platinum-based noble metal catalyst according to claim 1, wherein in the step 4, the amount of the powder added to the grinding tool is 60-160 mg at a time, and the pressing time is 30-240 s.
4. The method for preparing the platinum-based noble metal catalyst by the wet process according to claim 1, wherein in the step 5, the size of the sieved particles is 40-60 meshes.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108671907A (en) * | 2018-05-16 | 2018-10-19 | 浙江大学城市学院 | A kind of platinum/titanium oxide nanoflower composite material and preparation method and application |
| CN109433192A (en) * | 2018-12-07 | 2019-03-08 | 东北大学 | A kind of noble metal single atomic dispersion type cleaning catalyst and preparation method thereof |
| CN112044435A (en) * | 2020-09-15 | 2020-12-08 | 复旦大学 | Pt-W catalyst for preparing 1, 3-propylene glycol by selective hydrogenolysis of glycerol and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108671907A (en) * | 2018-05-16 | 2018-10-19 | 浙江大学城市学院 | A kind of platinum/titanium oxide nanoflower composite material and preparation method and application |
| CN109433192A (en) * | 2018-12-07 | 2019-03-08 | 东北大学 | A kind of noble metal single atomic dispersion type cleaning catalyst and preparation method thereof |
| CN112044435A (en) * | 2020-09-15 | 2020-12-08 | 复旦大学 | Pt-W catalyst for preparing 1, 3-propylene glycol by selective hydrogenolysis of glycerol and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| LAN ZHANG等: "High active platinum clusters on titanium dioxide supports toward carbon monoxide oxidation", 《APPLIED CATALYSIS B: ENVIRONMENTAL》, pages 118629 * |
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