CN111921541A - Platinum-iron alloy catalyst, preparation method thereof and application thereof in catalytic oxidation of VOCs (volatile organic compounds) - Google Patents
Platinum-iron alloy catalyst, preparation method thereof and application thereof in catalytic oxidation of VOCs (volatile organic compounds) Download PDFInfo
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Abstract
The invention discloses a platinum-iron alloy catalyst, a preparation method thereof and application thereof in catalytic oxidation of VOCs. The preparation method comprises the steps of mixing a platinum source and an iron source by a liquid phase method, adding the mixture to the surface of a carbonaceous reducing agent, volatilizing to remove a solvent, applying ultrashort current pulse to the precursor mixture under a protective atmosphere to carry out reduction reaction, and rapidly quenching to room temperature after the reduction reaction is finished to obtain platinum-iron alloy nanoparticles; mixing the platinum-iron alloy nanoparticles with activated alumina sol, demulsifying and precipitating, centrifugally separating, and drying in vacuum to obtain the catalyst. The catalyst has high iron-platinum ratio and low cost, is used for the catalytic oxidation of VOCs, and has the characteristics of high low-temperature catalytic activity, good stability in long-term use and the like.
Description
Technical Field
The invention relates to a catalytic material, in particular to a platinum-iron alloy catalyst, and particularly relates to an active alumina-supported platinum-iron alloy catalyst, a method for preparing the platinum-iron alloy catalyst by a carbothermic reduction impact method and application of the platinum-iron alloy catalyst in catalytic oxidation of VOCs (volatile organic compounds), belonging to the technical field of catalysis.
Background
Volatile Organic Compounds (VOCs) are compounds that are ubiquitous in the atmosphere and have a polluting property, and generally refer to organic compounds that have a high saturated vapor pressure, a low boiling point, a small molecular weight, and are volatile at room temperature under normal atmospheric conditions. Volatile organic compounds are further classified according to their chemical structure and can be roughly classified into eight types: alkanes, aromatic hydrocarbons, alkenes, halocarbons, esters, aldehydes, ketones, and others. In outdoor open environment, a large amount of VOCs can be brought into the atmosphere by industrial waste gas, automobile tail gas and the like generated by fuel combustion, transportation and industrial production, and in a room, coal and natural gas required by life of people are combusted, and indoor decoration materials, wooden furniture and cleaning agents are used as emission sources of the VOCs.
There are many methods for reducing the concentration of VOCs in the environment, such as catalytic oxidation, catalytic cracking, biofiltration, condensation and adsorption, where catalytic oxidation is receiving increasing attention due to its high efficiency and wide applicability. The catalytic oxidation is an oxidation reaction which takes a metal material or an alloy such as Pt, Pd, Ni, Fe, etc. as a catalyst and takes air, oxygen, ozone, etc. as an oxidant under certain pressure and temperature conditions. Under the action of catalyst, the hydrocarbon in the organic waste gas is quickly oxidized into water and carbon dioxide under the condition of low temperature, so as to achieve the purpose of treatment. However, the catalyst is easy to be poisoned in the catalytic process, and how to find a catalyst which has long service life and is not easy to be poisoned is particularly important on the premise of reducing the catalytic temperature.
Generally, the catalyst is classified into a supported noble metal catalyst and an unsupported noble metal oxide catalyst according to the active components of the catalyst. Noble metal catalysts exhibit good activity and stability for catalytic oxidation of VOCs, but their expensive cost and susceptibility to deactivation limit their commercial application. Compared with noble metal oxide catalysts, non-noble metal oxide catalysts are lower in cost and have certain antitoxic capability, but the efficiency is lower, so that the energy consumption is higher.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides a catalyst formed by platinum-iron alloy nanoparticles loaded on an active aluminum trioxide carrier, the catalyst has the characteristics of high iron-platinum proportion, low cost, high low-temperature catalytic activity, good long-term use stability and the like, is used for catalytic oxidation of VOCs, can realize complete catalytic oxidation of VOCs at low temperature, particularly has a catalytic oxidation conversion rate of over 99 percent on toluene which is difficult to oxidize, almost all oxidation products are water and carbon dioxide, and the catalytic oxidation reaction is thorough.
The second purpose of the invention is to provide a simple, rapid and low-cost method for preparing the platinum-iron alloy catalyst.
The third purpose of the invention is to provide the application of the platinum-iron alloy catalyst in catalyzing the oxidation of VOCs, and the platinum-iron alloy catalyst has the advantages of high activity, good stability in long-term use, complete catalytic oxidation reaction and the like at a lower temperature.
In order to achieve the technical purpose, the invention provides a preparation method of a platinum-iron alloy catalyst, which comprises the following steps:
1) mixing a platinum source and an iron source by a liquid phase method, adding the mixture to the surface of a carbonaceous reducing agent, and volatilizing to remove a solvent to obtain a precursor mixture;
2) under the protective atmosphere, applying ultrashort current pulses to the precursor mixture to perform a reduction reaction, and rapidly quenching to room temperature after the reduction reaction is completed to obtain platinum-iron alloy nanoparticles;
3) mixing the platinum-iron alloy nanoparticles with activated alumina sol, demulsifying and precipitating, centrifugally separating, and drying in vacuum to obtain the catalyst.
Preferably, the platinum source is a readily soluble platinum-containing compound, mainly a platinum salt, such as at least one of platinum acetylacetonate, platinum chlorate and platinum chloride.
As a preferred scheme, the iron source is an iron-containing compound which is easy to dissolve, mainly iron salt, and commonly at least one of ferric acetylacetonate, ferric chloride and ferrous chloride.
As a preferable scheme, the molar ratio of iron to platinum in the iron source and the platinum source is 1-3: 1, preferably 2-3: 1; most preferably 3: 1. Generally speaking, the catalytic activity of the pure platinum catalyst is relatively high, but the cost is correspondingly high, and the pure platinum has poor anti-toxicity performance, but the alloying of iron and platinum can reduce the cost of the platinum catalyst and improve the stability of the platinum catalyst by the alloying of iron and platinum. In the prior art, the catalytic performance of the platinum alloy obtained by doping transition metal in platinum is obviously reduced compared with that of pure platinum, and the platinum-iron alloy obtained by the method of the invention is doped with iron with high proportion, so that still higher catalytic activity can be obtained, such as PtFe prepared according to the iron-platinum ratio of 3:13The type alloy catalyst can completely catalyze and oxidize the toluene at 255 ℃ to convert the toluene into water and carbon dioxide, does not generate other waste gas, and can keep the toluene conversion rate over 99 percent for a long time, which is unexpected and fully highlights the advantages of the platinum-iron alloy catalyst prepared by the method.
Preferably, the mass ratio of the total mass of the platinum source and the iron source to the carbonaceous reducing agent is 1: 1-5.
As a preferred scheme, the ultra-short current pulse duration is 30-70 ms, and the current intensity is 3-5A; further preferably, the ultra-short current pulse duration is 50-60 ms, the current intensity is 4A-5A, and the severe carbothermic reduction reaction can be rapidly initiated under the preferable reaction conditions, so that the platinum-iron alloy is favorably generated.
As a preferred scheme, the proportion of the platinum-iron alloy nanoparticles to the activated alumina sol is measured by the mass percentage of the platinum-iron alloy nanoparticles to the activated alumina being 2-10% and 90-98%.
Preferably, the platinum source and the iron source are mixed in liquid phase by using an ethanol solvent as a medium.
As a preferred scheme, the demulsification process comprises the following steps: under the condition of stirring, tetrahydrofuran is dripped into the mixed solution of the platinum-iron alloy nano particles and the activated alumina sol.
As a preferable scheme, in the centrifugation process, the rotating speed is 8000-11000 rpm, and the centrifugation time is 10-15 min.
As a preferable scheme, in the vacuum drying process, the drying temperature is 40-60 ℃, and the drying time is more than 12 hours.
The invention also provides a platinum-iron alloy catalyst which is prepared by the preparation method.
As a preferable scheme, the platinum-iron alloy catalyst is formed by dispersing platinum-iron alloy nano particles on the surface of active aluminum oxide.
The invention also provides an application of the platinum-iron alloy catalyst, which is used as a VOCs catalytic oxidation catalyst.
The platinum-iron alloy catalyst is used in the catalytic oxidation process of VOCs, the catalyst is used as a stationary phase to participate in the reaction, and the dosage can be determined according to actual requirements. For example, in illustrative examples of the invention: the dosage of the platinum-iron alloy catalyst is 30mg, toluene is taken as a model VOC, the reaction gas is 1000ppm toluene, and the volume fraction O is 20 percent2，N2As equilibrium gas, the reaction space velocity is 12000h respectively-1～36000h-1。
Compared with the prior art, the technical scheme of the invention has the following beneficial technical effects:
compared with the existing platinum catalyst, the platinum iron alloy catalyst provided by the invention has the advantages that the cost can be obviously reduced due to the introduction of high-proportion iron, and the surface electronic structure of platinum metal is improved by using transition metal iron, so that the toxicity resistance of the platinum metal is improved, and the stability of the platinum metal is improved.
The platinum-iron alloy catalyst provided by the invention has excellent low-temperature VOCs catalytic oxidation performance and reaction stability, and can maintain high catalytic activity for a long time.
The platinum-iron alloy catalyst has simple preparation process and low carrier price, and can realize large-scale industrial use.
Drawings
FIG. 1 shows the preparation of PtFe in example 13TEM images of type platinum-iron alloy catalysts;
FIG. 2 shows the preparation of PtFe in example 13P-toluene catalyzed oxygen of type platinum-iron alloy catalystA chemical effect graph;
FIG. 3 is the preparation of PtFe in example 13A test chart of the catalytic oxidation stability of the type platinum-iron alloy catalyst to toluene;
FIG. 4 shows the preparation of PtFe in example 22The effect graph of the type platinum-iron alloy catalyst on the catalytic oxidation of toluene;
FIG. 5 shows the effect of PtFe type Pt-Fe alloy catalyst prepared in example 3 on the catalytic oxidation of toluene;
FIG. 6 preparation of PtFe in example 43The type platinum-iron alloy catalyst has catalytic oxidation effect on toluene.
Detailed Description
The following examples are intended to further illustrate the present disclosure, but not to limit the scope of the claims.
Example 1
0.125mmol of platinum acetylacetonate and 0.375mmol of iron acetylacetonate were placed in a beaker containing 15ml of anhydrous ethanol, and the mixed solution was dropwise added by syringe onto a microtest (0.05ml of cm) containing carbon black-2) And after the absolute ethyl alcohol is completely volatilized, putting the absolute ethyl alcohol into an argon atmosphere glove box for operation. Applying a high-intensity instantaneous current (5A, 55ms) to the miniature experiment table by using a direct current power supply in a glove box, wherein a bright light appears at the moment, which indicates that the experiment is successful, and preparing the PtFe3-type C platinum-iron alloy catalyst. Then, the PtFe obtained above is reacted with a catalyst3Mixing the catalyst and active alumina sol, and dropwise adding Tetrahydrofuran (THF) under magnetic stirring to demulsify PtFe3The catalyst is deposited on the surface of active alumina, centrifuged for 15min at 10000rpm, and then dried in vacuum for 12h at 50 ℃ to obtain the final catalyst.
For PtFe prepared in example 13The type platinum-iron alloy catalyst is used for VOCs catalytic oxidation activity experiments, and reactants and products of toluene catalytic oxidation are detected and quantitatively analyzed by an online gas chromatograph equipped with an FID detector by taking toluene as a model VOC. Wherein the space velocity is 12000h-1The reaction conditions were as follows: the mass of the catalyst is 0.03g, and the mass of the quartz sand is 1 g; reaction gas: 1000ppm toluene + 20% O2The balance gas is N2The flow rate was 160 ml/min. The space velocity is 24000h-1The reaction conditions were as follows: the mass of the catalyst is 0.03g, and the mass of the quartz sand is 0.72 g; reaction gas: 1000ppm toluene + 20% O2The balance gas is N2Flow rate 240 ml/min. The space velocity is 36000h-1The reaction conditions were as follows: the mass of the catalyst is 0.03g, and the mass of the quartz sand is 0.47 g; reaction gas: 1000ppm toluene + 20% O2The balance gas is N2Flow rate 240 ml/min.
PtFe prepared in example 13The reaction activity curve of the type platinum-iron alloy catalyst under different airspeeds is shown in figure 2, and the catalyst can reach 99 percent of toluene conversion rate at 255 ℃ under three airspeeds.
For PtFe prepared in example 13The type platinum-iron alloy catalyst is used for VOCs catalytic oxidation experiment stability test experiment, toluene is used as a model VOC, and the reaction conditions are as follows: the mass of the catalyst is 0.03g, and the mass of the quartz sand is 1 g; reaction gas: 1000ppm toluene + 20% O2The balance gas is N2The flow rate is 160 ml/min; reaction temperature: 255 ℃. As shown in figure 3, the catalyst can continuously test at 255 ℃ for 72h, the catalyst can always maintain the conversion rate of the toluene to be more than 99%, and the catalytic oxidation products are almost all water and carbon dioxide, and no other waste gas is generated.
Example 2
0.125mmol of platinum acetylacetonate and 0.25mmol of iron acetylacetonate were placed in a beaker containing 15ml of anhydrous ethanol, and the mixed solution was dropwise added to a carbon black-containing microtest (0.05ml of cm)-2) And after the absolute ethyl alcohol is completely volatilized, putting the absolute ethyl alcohol into an argon atmosphere glove box for operation. Applying a high-intensity instantaneous current (5A, 55ms) to the miniature experiment table by using a direct current power supply in a glove box, wherein a bright light appears at the moment, which indicates that the experiment is successful, and preparing the PtFe2Type platinum-iron alloy catalyst. Then, the PtFe obtained above is reacted with a catalyst2Mixing the catalyst and active alumina sol, and dropwise adding Tetrahydrofuran (THF) under magnetic stirring to demulsify PtFe2The catalyst is deposited on the surface of active alumina, centrifuged for 15min at 10000rpm, and then dried in vacuum for 12h at 50 ℃ to obtain the final catalyst.
For PtFe prepared in example 22Type platinum iron alloyThe gold catalyst was subjected to a VOCs catalytic oxidation activity test, and the reactants and products of toluene catalytic oxidation were detected and quantitatively analyzed by an on-line gas chromatograph equipped with an FID detector, using toluene as a model VOC. The reaction conditions are as follows: space velocity of 12000h-10.03g of catalyst mass and 1g of quartz sand; reaction gas: 1000ppm toluene + 20% O2The balance gas is N2The flow rate was 160 ml/min. Almost all of the catalytic oxidation products are water and carbon dioxide, and no other waste gas is generated.
Example 3
0.25mmol of platinum acetylacetonate and 0.25mmol of iron acetylacetonate were placed in a beaker containing 20ml of anhydrous ethanol, and the mixed solution was dropwise added to a mini-laboratory bench (0.05ml of cm) containing carbon black by means of a syringe-2) And after the absolute ethyl alcohol is completely volatilized, putting the absolute ethyl alcohol into an argon atmosphere glove box for operation. In a glove box, a direct current power supply is used for applying a high-intensity instantaneous current (5A, 55ms) to the miniature experiment table, and at the moment, a bright light appears, which indicates that the experiment is successful, so that the PtFe type platinum-iron alloy catalyst is prepared. Then, the PtFe catalyst obtained above is mixed with activated alumina sol, Tetrahydrofuran (THF) is added dropwise under magnetic stirring to perform emulsion breaking, so that the PtFe catalyst is deposited on the surface of the activated alumina, the mixture is centrifuged at 10000rpm for 15min, and then the mixture is dried in vacuum at 50 ℃ for 12h to obtain the final catalyst.
The PtFe-type platinum-iron alloy catalyst prepared in example 3 was subjected to a VOCs catalytic oxidation activity test, and reactants and products of catalytic oxidation of toluene were detected and quantitatively analyzed by an on-line gas chromatograph equipped with an FID detector using toluene as a model VOC. The reaction conditions are as follows: space velocity of 12000h-10.03g of catalyst mass and 1g of quartz sand; reaction gas: 1000ppm toluene + 20% O2The balance gas is N2The flow rate was 160 ml/min. Almost all of the catalytic oxidation products are water and carbon dioxide, and no other waste gas is generated.
Example 4
0.125mmol of platinum acetylacetonate and 0.375mmol of iron acetylacetonate were placed in a beaker containing 15ml of anhydrous ethanol, and the mixed solution was dropwise added by syringe onto a microtest (0.05ml of cm) containing carbon black-2) And after the absolute ethyl alcohol is completely volatilized, putting the absolute ethyl alcohol into an argon atmosphere glove box for operation. In the glove box, a direct current power supply is used for applying a high-intensity instantaneous current (3A, 35ms) to the miniature experiment table, and a brighter light appears at the moment, which indicates that the experiment is successful, so that the PtFe is prepared3Type platinum-iron alloy catalyst. Then, the PtFe obtained above is reacted with a catalyst3Mixing the catalyst and active alumina sol, and dropwise adding Tetrahydrofuran (THF) under magnetic stirring to demulsify PtFe3The catalyst is deposited on the surface of active alumina, centrifuged for 15min at 10000rpm, and then dried in vacuum for 12h at 50 ℃ to obtain the final catalyst.
PtFe prepared in example 43The type platinum-iron alloy catalyst is used for VOCs catalytic oxidation activity experiments, and reactants and products of toluene catalytic oxidation are detected and quantitatively analyzed by an online gas chromatograph equipped with an FID detector by taking toluene as a model VOC. Wherein the space velocity is 12000h-1The reaction conditions were as follows: the mass of the catalyst is 0.03g, and the mass of the quartz sand is 1 g; reaction gas: 1000ppm toluene + 20% O2The balance gas is N2The flow rate was 160 ml/min. As can be seen from the figure, PtFe prepared in example 43The catalytic performance of the type platinum-iron alloy is reduced compared with that of the example 1, and probably because the adding current and the adding time are low, the alloying step is incomplete, and the catalytic effect is reduced.
Claims (10)
1. A preparation method of a platinum-iron alloy catalyst is characterized by comprising the following steps: the method comprises the following steps:
1) mixing a platinum source and an iron source by a liquid phase method, adding the mixture to the surface of a carbonaceous reducing agent, and volatilizing to remove a solvent to obtain a precursor mixture;
2) under the protective atmosphere, applying ultrashort current pulses to the precursor mixture to perform a reduction reaction, and rapidly quenching to room temperature after the reduction reaction is completed to obtain platinum-iron alloy nanoparticles;
3) mixing the platinum-iron alloy nanoparticles with activated alumina sol, demulsifying and precipitating, centrifugally separating, and drying in vacuum to obtain the catalyst.
2. The method for preparing a platinum-iron alloy catalyst according to claim 1, wherein:
the platinum source is at least one of platinum acetylacetonate, platinum chlorate and platinum chloride;
the iron source is at least one of ferric acetylacetonate, ferric chloride and ferrous chloride.
3. The method for preparing a platinum-iron alloy catalyst according to claim 1 or 2, wherein: the molar ratio of iron to platinum in the iron source and the platinum source is 1-3: 1.
4. The method for preparing a platinum-iron alloy catalyst according to claim 1, wherein: the mass ratio of the total mass of the platinum source and the iron source to the carbonaceous reducing agent is 1: 1-5.
5. The method for preparing a platinum-iron alloy catalyst according to claim 1, wherein: the ultra-short current pulse duration is 30-70 ms, and the current intensity is 3A-5A.
6. The method for preparing a platinum-iron alloy catalyst according to claim 5, wherein: the ultra-short current pulse duration is 50-60 ms, and the current intensity is 4A-5A.
7. The method for preparing a platinum-iron alloy catalyst according to claim 1, wherein: the proportion of the platinum-iron alloy nanoparticles to the activated alumina sol is measured by the mass percentage of the platinum-iron alloy nanoparticles to the activated alumina being 2-10% and 90-98%.
8. A platinum-iron alloy catalyst, characterized by: the preparation method of any one of claims 1 to 7.
9. A platinum-iron alloy catalyst according to claim 8, wherein: is formed by dispersing and loading platinum-iron alloy nano particles on the surface of active aluminum oxide.
10. Use of a platinum-iron alloy catalyst according to claim 8 or 9, wherein: the catalyst is applied as a catalytic oxidation catalyst for VOCs.
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| CN114289032A (en) * | 2021-11-18 | 2022-04-08 | 江苏大学 | Preparation method and application of tungsten oxide loaded platinum-iron nano alloy catalyst |
| CN114471555A (en) * | 2022-01-27 | 2022-05-13 | 中自环保科技股份有限公司 | Low-temperature high-efficiency bimetallic synergetic catalytic purification catalyst for VOCs and preparation method thereof |
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| CN114289032A (en) * | 2021-11-18 | 2022-04-08 | 江苏大学 | Preparation method and application of tungsten oxide loaded platinum-iron nano alloy catalyst |
| CN114289032B (en) * | 2021-11-18 | 2024-03-19 | 江苏大学 | Preparation method and application of tungsten oxide loaded platinum-iron nano alloy catalyst |
| CN114471555A (en) * | 2022-01-27 | 2022-05-13 | 中自环保科技股份有限公司 | Low-temperature high-efficiency bimetallic synergetic catalytic purification catalyst for VOCs and preparation method thereof |
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