CN111185221A - PdAg alloy supported Ti-SBA-15 catalyst and preparation method and application thereof - Google Patents
PdAg alloy supported Ti-SBA-15 catalyst and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the field of environmental catalysis, and discloses a PdAg alloy supported Ti-SBA-15 catalyst, and a preparation method and application thereof. The catalyst is prepared by dissolving a surfactant P123 in hydrochloric acid, and stirring at 30-150 ℃ to obtain a solution; dropwise adding ethyl orthosilicate and a Ti source into the solution, stirring at 30-150 ℃, then aging the obtained suspension A at 40-150 ℃, carrying out suction filtration, washing, drying, and roasting at 500-550 ℃ to obtain a Ti-SBA-15 carrier; dissolving Pd precursor, Ag precursor and Ti-SBA-15 carrier in ultrapure water, stirring at room temperature to obtain suspension B, adding NaBH4Stirring the solution, filtering, washing and drying to obtain the product. The total load of Pd and Ag in the catalyst of the invention0.1-10 wt%, and shows good low ignition temperature, high performance and high stability in the catalytic combustion process of VOCs.
Description
Technical Field
The invention belongs to the technical field of environmental catalysis, and particularly relates to a PdAg alloy supported Ti-SBA-15 catalyst, and a preparation method and application thereof.
Background
In recent years, with the rapid development of national industrialization and urbanization, the amount of Volatile Organic Compounds (VOCs) produced has also increased dramatically. And the release of VOCs has certain influence to human health and environment, and some VOCs can induce the ash haze, produce photochemistry smog and then cause the decline of air quality. Generally, the control measures for VOCs are divided into two major components, recycling and destruction technologies. Catalytic combustion is one of VOCs destruction technologies, and is concerned by scholars at home and abroad due to high-efficiency catalytic performance and economic feasibility. However, the catalyst for catalytic combustion of VOCs generally has the disadvantages of high ignition temperature, high application cost, poor stability and the like. Therefore, the catalyst which has low ignition temperature, high efficiency, stability, economy and feasibility is prepared, and has very important research significance and social benefit.
The noble metal Pd catalyst is widely used for catalytic combustion of VOCs due to the advantages of high-efficiency VOCs catalytic performance, low ignition temperature and high temperature resistance. However, in the noble metal supported catalyst, only the noble metal exposed on the surface of the carrier can participate in the catalytic reaction, while the existing noble metal supported catalyst synthesis method mainly comprises the methods of impregnation reduction, impregnation calcination and the like, and the reduced noble metal particles are generally from several nanometers to dozens of nanometers, so that the defects of high noble metal loading, low utilization rate and the like are caused, and the cost of the catalyst is increased to a great extent. In addition, the problems of low catalytic activity, low selectivity, poor stability and the like of the single metal catalyst still exist in a plurality of catalytic systems. Therefore, in order to improve the catalytic performance of the noble metal catalyst and reduce the loading amount of the noble metal, researchers at home and abroad mainly improve the utilization rate of the noble metal nanoparticles by reducing the size of the noble metal particles. The method has the advantages that the Pd atom electron cloud density is increased by introducing Ag with lower price into noble metal Pd, the adsorption performance and activation energy of Pd on VOCs are further promoted, the activity, selectivity and stability of the catalyst on the reaction are effectively improved, and the cost of the catalyst is reduced. However, the traditional preparation method of the bimetallic catalyst needs to add a stabilizer, a polymer ligand and the like, and the preparation process is relatively complex. Therefore, how to prepare the alloy supported mesoporous molecular sieve catalytic material with high efficiency, stability and low cost is a problem to be solved urgently.
Disclosure of Invention
In order to solve the defects of the prior art, the invention mainly aims to provide a PdAg alloy supported Ti-SBA-15 catalyst.
The invention also aims to provide a preparation method of the PdAg alloy supported Ti-SBA-15 catalyst. The method adopts a solvent reduction method to highly disperse PdAg alloy on ordered mesoporous Ti-SBA-15, reduces the use amount of Pd by introducing Ag, and effectively improves the high activity and high stability of the Pd catalyst.
The invention further aims to provide application of the PdAg alloy supported Ti-SBA-15 catalyst.
The purpose of the invention is realized by the following technical scheme:
a PdAg alloy supported Ti-SBA-15 catalyst is prepared by dissolving a surfactant polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer with a molecular formula of PEO-PPO-PEO, which is abbreviated as P123 in a hydrochloric acid solution, and stirring the solution I at 30-150 ℃ to obtain a solution; dropwise adding ethyl orthosilicate and a Ti source into the solution, stirring II at 30-150 ℃, then aging the obtained suspension A at 40-150 ℃, carrying out suction filtration, washing and drying, heating to 500-550 ℃, and roasting to obtain a Ti-SBA-15 carrier; dissolving a Pd precursor, an Ag precursor and a Ti-SBA-15 carrier in ultrapure water, stirring the solution III at room temperature to obtain a suspension B, and then adding NaBH into the suspension B4Stirring the solution IV, and then sequentially carrying out suction filtration, washing and drying to obtain the solution IV; the total load of Pd and Ag in the catalyst is 0.1-10 wt%.
Preferably, the concentration of the hydrochloric acid solution is 0.01-1.0 mol/L; the mass ratio of the P123 to the hydrochloric acid solution is (10-1): 1.
preferably, the Ti source is an organic titanium source or an inorganic titanium source.
More preferably, the organic titanium source is titanium isopropoxide, tetraethyl titanate or tetrabutyl titanate, and the inorganic titanium source is titanium tetrachloride, titanium trichloride or titanyl sulfate.
Preferably, the molar ratio of Si in the ethyl orthosilicate to Ti in the Ti source is (50-500): 1; the volume ratio of the ethyl orthosilicate to the Ti source to the solution is (10-150): 1: (200-3000).
Preferably, the stirring time of the stirring I is 2-24 h; the stirring time of the stirring II is 24-72 hours; the stirring time of the stirring III is 2-24 h; the stirring IV is carried out for 15-120 min; the rate of temperature rise is 1-5 ℃/min.
Preferably, the Pd precursor is palladium chloride, palladium nitrate or palladium acetate; the Ag precursor is silver nitrate, silver acetate or silver acetylacetonate.
Preferably, the mass ratio of the Pd precursor to the Ag precursor to the Ti-SBA-15 carrier to the ultrapure water is (1-50): 1: (200-10000): (200000 to 6000000); the mole ratio of the Pd precursor to the Ag precursor is (1-50): 1; the suspension B and NaBH4The volume ratio of the solution is (10-300): 1; the total mole of the Pd precursor and the Ag precursor is equal to that of NaBH4The molar ratio of the solution is 1: (1-50).
The preparation method of the PdAg alloy supported Ti-SBA-15 catalyst comprises the following specific steps:
s1, dissolving a surfactant P123 in a hydrochloric acid solution, and stirring for 2-24 hours at 30-150 ℃ to obtain a solution A;
s2, dropwise adding ethyl orthosilicate and a Ti source into the solution A, and stirring at 30-150 ℃ to obtain a suspension B; then, aging the suspension B at 40-150 ℃ for 24-72 h, carrying out suction filtration, washing, drying, and roasting at 500-550 ℃ for 4-8 h to obtain a Ti-SBA-15 carrier;
s3, dissolving the Pd precursor, the Ag precursor and the Ti-SBA-15 carrier in ultrapure water, stirring at room temperature to obtain a suspension C, and then adding NaBH into the suspension C4Stirring the solution, and then sequentially carrying out suction filtration, washing and drying to obtain the PdAg alloy supported Ti-SBA-15 catalyst.
The PdAg alloy supported Ti-SBA-15 catalyst is applied to the field of catalytic purification of VOCs.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention uses the porous material with ordered mesoporous pore canalsThe specific surface area Ti-SBA-15 is used as a carrier, sodium borohydride is used as a reducing agent, and Pd is added2+、Ag+The catalyst is reduced into PdAg alloy nano particles and highly dispersed on the ordered mesoporous Ti-SBA-15, so that the high activity and high thermal stability of the low-load PdAg alloy catalyst in the catalytic combustion process of VOCs are realized, and the problems of easy agglomeration, complex preparation, low activity, poor stability and the like of the traditional bimetallic catalyst are solved.
2. The PdAg alloy loaded Ti-SBA-15 has the advantages of small particle size of an active component PdAg, high dispersion degree and low load capacity.
3. The PdAg alloy-loaded Ti-SBA-15 catalyst prepared by the invention has the advantages of low ignition temperature, high catalytic activity, good stability and the like on typical difficultly-degraded macromolecular cyclohexane VOCs.
4. The preparation method has the advantages of simple preparation process and low cost.
Drawings
FIG. 1 is a graph of the catalytic combustion performance of PdAg alloy supported Ti-SBA-15 catalyst of example 1 and Pd supported Ti-SBA-15 catalyst of comparative example 1 on cyclohexane for the same metal loading.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Example 1
1. 8.01g of a polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer (molecular formula: PEO-PPO-PEO, abbreviated as P123) was dissolved in 300ml of a hydrochloric acid solution (concentration: 0.1mol/L), and stirred at 40 ℃ for 2 hours to obtain a solution A.
2. Adding 15mL of Tetraethoxysilane (TEOS) into the solution A dropwise, then adding 115 mu L of tetrabutyl titanate dropwise (the molar ratio of Si in TEOS to Ti in tetrabutyl titanate is 200), and stirring for 24h at 40 ℃ to obtain a suspension B; and transferring the suspension B into a reaction kettle, aging at 80 ℃ for 24h, then carrying out suction filtration, washing, drying, roasting at 500 ℃ for 6h (the heating rate is 2 ℃/min), and naturally cooling to room temperature to obtain the Ti-SBA-15 carrier.
3. 0.0049gPd (NO)3)2、0.0004gAgNO30.5g of the Ti-SBA-15 carrier obtained in the step S2 was dissolved in 300mL of ultrapure water, stirred at room temperature for 4 hours to obtain a suspension C, and 1178. mu. of LNaBH was added to the suspension C4And continuously stirring the solution (with the concentration of 0.1mol/L) for 15min, and then sequentially performing suction filtration, washing and drying to obtain the PdAg alloy supported Ti-SBA-15 catalyst (PdAg/Ti-SBA-15), wherein the Pd loading is 0.45 wt% and the Ag loading is 0.05 wt%.
FIG. 1 is a graph of catalytic combustion performance of PdAg alloy supported Ti-SBA-15 catalyst of the same metal loading in this example and Pd supported Ti-SBA-15 catalyst of comparative example 1 on cyclohexane. The catalyst obtained in the example is used for performance detection: cyclohexane is respectively used as catalytic oxidation objects, the initial concentration of the cyclohexane is respectively 40 +/-1 ppm, the gas flow is 3000ml/h, and the using amount of the catalyst is 50 mg. As can be seen from the catalytic combustion performance curve of the PdAg alloy-supported Ti-SBA-15 catalyst on gas-phase cyclohexane in FIG. 1, under the condition of simple heating, PdAg/Ti-SBA-15 has strong degradation and mineralization capacity on cyclohexane, the ignition temperature on cyclohexane is 180 ℃, and the temperature T on cyclohexane is 180 DEG C100276 deg.C (square in the figure). The degradation effect on cyclohexane is similar to that of Pd/Ti-SBA-15 (round dots in the figure), but the introduction of silver reduces the using amount of Pd and the catalytic effect is improved. In addition, the carrier with high specific surface area of Ti-SBA-15 can inhibit the agglomeration problem of PdAg particles.
Comparative example 1
1. A certain amount of Pd precursor (mass ratio of Pd/polyvinylpyrrolidone is 1: 1.2) was added to 120mL of deionized water, and stirred for 6 hours.
2. Dispersing a proper amount of 0.3g of Ti-SBA-15 in 20mL of methanol, and then adding the solution into the mixed solution (the theoretical Pd loading is 0.5%); vigorously stirred for 3h, 0.05g NaBH dissolved in deionized water4Dripping into the above mixed solution, stirring for 1h, vacuum filtering, washing, drying, heating to 500 deg.C at 2 deg.C/min, calcining for 3h, and naturally cooling to room temperatureTo obtain a Pd-supported Ti-SBA-15 catalyst (Pd/Ti-SBA-15), wherein the supported amount of Pd is 0.5 wt%.
Example 2
1. 8.01g of P123 was dissolved in 300ml of a hydrochloric acid solution (concentration: 0.1mol/L), and the solution was stirred at 40 ℃ for 2 hours to obtain a solution A.
2. Dropwise adding 15mL of TEOS into the solution A, then dropwise adding a certain amount of tetrabutyl titanate (the molar ratio of Si in the TEOS to Ti in the tetrabutyl titanate is 200), and stirring for 24h at 40 ℃ to obtain a suspension B; and transferring the suspension B into a reaction kettle, aging at 80 ℃ for 24h, then carrying out suction filtration, washing, drying, roasting at 500 ℃ for 6h (the heating rate is 2 ℃/min), and naturally cooling to room temperature to obtain the Ti-SBA-15 carrier.
3. 0.0043gPd (NO)3)2、0.0008gAgNO30.5g of the Ti-SBA-15 carrier obtained in the step S2 was dissolved in 300mL of ultrapure water, stirred at room temperature for 4 hours to obtain a suspension C, and 1175. mu. of NaBH was added to the suspension C4And continuously stirring the solution (with the concentration of 0.1mol/L) for 15min, and then sequentially performing suction filtration, washing and drying to obtain the PdAg alloy supported Ti-SBA-15 catalyst (PdAg/Ti-SBA-15), wherein the Pd loading is 0.4 wt% and the Ag loading is 0.1 wt%.
Example 3
1. 8.01g of P123 was dissolved in 300ml of a hydrochloric acid solution (concentration: 0.1mol/L), and the solution was stirred at 40 ℃ for 2 hours to obtain a solution A.
2. Dropwise adding 15mL of TEOS into the solution A, then dropwise adding a certain amount of tetrabutyl titanate (the molar ratio of Si in the TEOS to Ti in the tetrabutyl titanate is 200: 1), and stirring for 24h at 40 ℃ to obtain a suspension B; and transferring the suspension B into a reaction kettle, aging at 80 ℃ for 24h, then carrying out suction filtration, washing, drying, roasting at 500 ℃ for 6h (the heating rate is 2 ℃/min), and naturally cooling to room temperature to obtain the Ti-SBA-15 carrier.
3. 0.0032gPd (NO)3)2、0.0016gAgNO30.5g of the Ti-SBA-15 carrier obtained in the step S2 was dissolved in 300mL of ultrapure water, stirred at room temperature for 4 hours to obtain a suspension C, and 1171. mu. of LNaBH was added to the suspension C4The solution (concentration 0.1mol/L) is stirred for 15min and then sequentially stirredAnd carrying out suction filtration, washing and drying to obtain the PdAg alloy supported Ti-SBA-15 catalyst (PdAg/Ti-SBA-15), wherein the Pd loading is 0.3 wt%, and the Ag loading is 0.2 wt%.
Example 4
1. 8.01g of P123 was dissolved in 300ml of a hydrochloric acid solution (concentration: 0.1mol/L), and the solution was stirred at 40 ℃ for 2 hours to obtain a solution A.
2. Dropwise adding 15mL of TEOS into the solution A, then dropwise adding a certain amount of tetrabutyl titanate (the molar ratio of Si in the TEOS to Ti in the tetrabutyl titanate is 200), and stirring for 24h at 40 ℃ to obtain a suspension B; and transferring the suspension B into a reaction kettle, aging at 80 ℃ for 24h, then carrying out suction filtration, washing, drying, roasting at 500 ℃ for 6h (the heating rate is 2 ℃/min), and naturally cooling to room temperature to obtain the Ti-SBA-15 carrier.
3. Mixing 0.0027gPd (NO)3)2、0.0020gAgNO30.5g of the Ti-SBA-15 carrier obtained in the step S2 is dissolved in 300mL of ultrapure water, stirred at room temperature for 4 hours to obtain a suspension C, and 1169 mu of LNaBH is added into the suspension C4And continuously stirring the solution (with the concentration of 0.1mol/L) for 15min, and then sequentially performing suction filtration, washing and drying to obtain the PdAg alloy supported Ti-SBA-15 catalyst (PdAg/Ti-SBA-15), wherein the Pd loading is 0.25 wt% and the Ag loading is 0.25 wt%.
Example 5
1. 8.01g of P123 was dissolved in 300ml of a hydrochloric acid solution (concentration: 0.1mol/L), and the solution was stirred at 40 ℃ for 2 hours to obtain a solution A.
2. Dropwise adding 15mL of TEOS into the solution A, then dropwise adding a certain amount of tetrabutyl titanate (the molar ratio of Si in the TEOS to Ti in the tetrabutyl titanate is 200), and stirring for 24h at 40 ℃ to obtain a suspension B; and transferring the suspension B into a reaction kettle, aging at 80 ℃ for 24h, then carrying out suction filtration, washing, drying, roasting at 500 ℃ for 6h (the heating rate is 2 ℃/min), and naturally cooling to room temperature to obtain the Ti-SBA-15 carrier.
3. Adding 0.0011gPd (NO)3)2、0.0032gAgNO30.5g of the Ti-SBA-15 carrier obtained in the step S2 is dissolved in 300mL of ultrapure water, stirred at room temperature for 4 hours to obtain a suspension C, and 1166 mu of LNaBH is added into the suspension C4And continuously stirring the solution (with the concentration of 0.1mol/L) for 15min, and then sequentially performing suction filtration, washing and drying to obtain the PdAg alloy supported Ti-SBA-15 catalyst (PdAg/Ti-SBA-15), wherein the Pd loading is 0.1 wt% and the Ag loading is 0.4 wt%.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A PdAg alloy supported Ti-SBA-15 catalyst is characterized in that a surfactant polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer with a molecular formula of PEO-PPO-PEO, which is abbreviated as P123 is dissolved in a hydrochloric acid solution, and the solution is obtained by stirring I at 30-150 ℃; dropwise adding ethyl orthosilicate and a Ti source into the solution, stirring II at 30-150 ℃, then aging the obtained suspension A at 40-150 ℃, carrying out suction filtration, washing and drying, heating to 500-550 ℃, and roasting to obtain a Ti-SBA-15 carrier; dissolving a Pd precursor, an Ag precursor and a Ti-SBA-15 carrier in ultrapure water, stirring the solution III at room temperature to obtain a suspension B, and then adding NaBH into the suspension B4Stirring the solution IV, and then sequentially carrying out suction filtration, washing and drying to obtain the solution IV; the total load of Pd and Ag in the catalyst is 0.1-10 wt%.
2. The PdAg alloy supported Ti-SBA-15 catalyst according to claim 1, wherein the concentration of the hydrochloric acid solution is 0.01 to 1.0 mol/L; the mass ratio of the P123 to the hydrochloric acid solution is (10-1): 1.
3. the PdAg alloy-supported Ti-SBA-15 catalyst of claim 1, wherein the Ti source is an organic or inorganic titanium source.
4. The PdAG alloy-supported Ti-SBA-15 catalyst of claim 3, wherein the organic titanium source is titanium isopropoxide, tetraethyl titanate or tetrabutyl titanate and the inorganic titanium source is titanium tetrachloride, titanium trichloride or titanyl sulfate.
5. The PdAg alloy-supported Ti-SBA-15 catalyst according to claim 1, wherein the molar ratio of Si in the tetraethoxysilane to Ti in the Ti source is (50 to 500): 1; the volume ratio of the ethyl orthosilicate to the Ti source to the solution is (10-150): 1: (200-3000).
6. The PdAg alloy supported Ti-SBA-15 catalyst as claimed in claim 1, wherein the stirring I time is 2 to 24 hours; the stirring time of the stirring II is 24-72 hours; the stirring time of the stirring III is 2-24 h; the stirring IV is carried out for 15-120 min; the rate of temperature rise is 1-5 ℃/min.
7. The PdAg alloy-supported Ti-SBA-15 catalyst according to claim 1, wherein the Pd precursor is palladium chloride, palladium nitrate or palladium acetate; the Ag precursor is silver nitrate, silver acetate or silver acetylacetonate.
8. The PdAg alloy-supported Ti-SBA-15 catalyst according to claim 1, wherein the mass ratio of the Pd precursor to the Ag precursor to the Ti-SBA-15 carrier to the ultrapure water is (1-50): 1: (200-10000): (200000 to 6000000); the mole ratio of the Pd precursor to the Ag precursor is (1-50): 1; the suspension B and NaBH4The volume ratio of the solution is (10-300): 1; the total mole of the Pd precursor and the Ag precursor is equal to that of NaBH4The molar ratio of the solution is 1: (1-50).
9. The preparation method of the PdAg alloy supported Ti-SBA-15 catalyst according to any one of claims 1 to 8, comprising the following specific steps:
s1, dissolving a surfactant P123 in a hydrochloric acid solution, and stirring for 2-24 hours at 30-150 ℃ to obtain a solution A;
s2, dropwise adding ethyl orthosilicate and a Ti source into the solution A, and stirring at 30-150 ℃ to obtain a suspension B; then, aging the suspension B at 40-150 ℃ for 24-72 h, carrying out suction filtration, washing, drying, and roasting at 500-550 ℃ for 4-8 h to obtain a Ti-SBA-15 carrier;
s3, dissolving the Pd precursor, the Ag precursor and the Ti-SBA-15 carrier in ultrapure water, stirring at room temperature to obtain a suspension C, and then adding NaBH into the suspension C4Stirring the solution, and then sequentially carrying out suction filtration, washing and drying to obtain the PdAg alloy supported Ti-SBA-15 catalyst.
10. The use of the PdAg alloy-supported Ti-SBA-15 catalyst according to any one of claims 1 to 8 in the field of catalytic purification of VOCs.
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| CN117718042A (en) * | 2024-02-09 | 2024-03-19 | 北京理工大学 | Pd(OH) 2 Diatomite catalyst and preparation method and application thereof |
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| CN110560147A (en) * | 2019-07-31 | 2019-12-13 | 广东工业大学 | Sub-nano Pd particle loaded Ti-SBA-15 catalyst, and preparation method and application thereof |
| CN110681397A (en) * | 2019-09-03 | 2020-01-14 | 广东工业大学 | Silver palladium/ferric oxide catalyst and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110560147A (en) * | 2019-07-31 | 2019-12-13 | 广东工业大学 | Sub-nano Pd particle loaded Ti-SBA-15 catalyst, and preparation method and application thereof |
| CN110681397A (en) * | 2019-09-03 | 2020-01-14 | 广东工业大学 | Silver palladium/ferric oxide catalyst and preparation method and application thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117718042A (en) * | 2024-02-09 | 2024-03-19 | 北京理工大学 | Pd(OH) 2 Diatomite catalyst and preparation method and application thereof |
| CN117718042B (en) * | 2024-02-09 | 2024-05-28 | 北京理工大学 | Pd(OH)2Diatomite catalyst and preparation method and application thereof |
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