CN103223347A - Method for synthesis of silica loaded nickel-platinum catalyst by ultrasonic spray pyrolysis - Google Patents
Method for synthesis of silica loaded nickel-platinum catalyst by ultrasonic spray pyrolysis Download PDFInfo
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- CN103223347A CN103223347A CN2013101307686A CN201310130768A CN103223347A CN 103223347 A CN103223347 A CN 103223347A CN 2013101307686 A CN2013101307686 A CN 2013101307686A CN 201310130768 A CN201310130768 A CN 201310130768A CN 103223347 A CN103223347 A CN 103223347A
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Abstract
The invention relates to a method for synthesis of a silica loaded nickel-platinum catalyst by ultrasonic spray pyrolysis. The method includes: step 1. preparing a nickel-platinum-containing soluble compound solution; step 2. atomizing the nickel-platinum-containing soluble compound solution; step 3. vaporizing silicon tetrachloride; step 4. bringing the atomized nickel-platinum liquid drops and silicon tetrachloride vapor to undergo a pyrolytic reaction so as to generate nanoscale silica, simultaneously making the active nickel-platinum-containing soluble compound form catalyst particles under high temperature and loading them on the nano-silica; and step 5. collecting and drying the catalyst. The method provided in the invention solves the problems that a silica carrier is expensive and the loading process is complex, has a simple synthesis process, and the obtained nano-silica loaded nickel-platinum catalyst has high activity and good dispersity.
Description
Technical field
The invention belongs to catalyst preparation technical field, be specifically related to the method for ultrasonic atomization pyrolysismethod synthetic silica nickel-loaded platinum catalyst.
Background technology
Nanometer grade silica has huge specific area, and proper pore structure distributes, and excellent mechanical intensity and chemical inertness is arranged, the carrier of useful as catalysts.Silicon dioxide carried nickel platinum metal catalyst can be used for multiple reactions such as catalytic hydrogenation, dehydrogenation, hydrocracking.
The preparation of silicon dioxide carried active metal catalyst, at present infusion processes that adopt are about to carrier silica and are immersed in fully contact in the solution that contains active component more, again through filtration, dry, roasting and activation, make catalyst.Catalyst prepared, the active component of load mainly is distributed in carrier surface, is evenly distributed, and the utilization rate height is fit to noble metal catalysts such as preparation Ni, Pt very much.Directly make carrier with the nano silicon of moulding, though saved complicated technologies such as carrier moulding, preliminary treatment, nanometer grade silica is as high-end nanometer product, and price is relatively costly.
The ultrasonic atomization pyrolysismethod is with ultrasonic wave solution to be sprayed, and with another kind of material pyrolytic reaction takes place at high temperature.Because hyperacoustic vibrating dispersion effect, the particle diameter of ejection solution is about 5 μ m, with the high-temperature gas reaction, can synthesize that concentration class is little, good dispersion, nano material that specific area is high.Utilize the principle of the silicon dioxide carried metallic nickel of ultrasonic atomization pyrolysismethod synthesis of nano, platinum to be, to contain the soluble compound solution sonic oscillation ejection of active metal nickel, platinum, with the silica presoma pyrolytic reaction takes place at high temperature, the silicon dioxide carried nickel platinum catalyst of synthesis of nano.Adopt polysilicon refuse silicon tetrachloride (SiCl in the reaction
4) substitute the presoma that traditional ethyl orthosilicate (TEOS) is made silica, can reduce cost and realize the utilization again of resource.Adopt the method for the silicon dioxide carried nickel platinum catalyst of ultrasonic atomization pyrolysismethod synthesis of nano, not relevant at present patent and research report both at home and abroad.
Summary of the invention
In order to overcome the defective of above-mentioned prior art, urge shortcomings such as carrier costs an arm and a leg, carrier complex forming technology at the nano silicon that infusion process exists, the object of the present invention is to provide a kind of method of ultrasonic atomization pyrolysismethod synthetic silica nickel-loaded platinum catalyst, solved that silica supports costs an arm and a leg, the load process complicated problems, it is simple to have synthesis technique, the nano silicon nickel-loaded platinum catalyst activity height that obtains, good dispersion.
To achieve these goals, technical scheme of the present invention is:
The method of ultrasonic atomization pyrolysismethod synthetic silica nickel-loaded platinum catalyst may further comprise the steps:
The preparation of the soluble compound solution of step 1, nickel metal platinum: reactive metal adopts nickel, platinum or the combination of both arbitrary proportions, and the preparation mass concentration is the soluble compound solution of 0.2～2% nickel metal platinum;
The atomizing of the soluble compound solution of step 2, nickel metal platinum: adopt power 200W, transducer frequency is the ultrasonic ultrasonic delay line memory of 1.7MHz, atomization rates is 0.4mL/min, and it is that the droplet of 5 μ m sprays into pyrolysis reactor that the soluble compound solution mist of nickel metal platinum is changed into average grain diameter;
The vaporization of step 3, silicon tetrachloride: adopt silicon tetrachloride as by-product of polysilicon to make raw material, silicon tetrachloride carries out purifying through distillation equipment earlier, silicon tetrachloride is heated to more than 60 ℃ vaporizes then, and taken out of by carrier gas;
Metallic nickel platinum drop and silicon tetrachloride steam generation pyrolytic reaction after step 4, the atomizing: the nickel platinum drop after silicon tetrachloride steam and the atomizing is sprayed into pyrolysis reactor, the mol ratio of silicon tetrachloride gas and nickel platinum drop is 1:10～1:50, under 200～500 ℃ of temperature, react, silicon tetrachloride gas and micron-sized drop generation hydrolysis, generate nanometer grade silica, residual moisture is by evaporate to dryness in the drop, and the soluble compound that contains active nickel platinum simultaneously at high temperature forms catalyst granules and loads on the nano silicon.
The collection of step 5, catalyst is with dry: nano silicon nickel-loaded platinum catalyst powder deposition takes out powder and at 200 ℃ of following dry 2h, obtains product in gatherer.
Advantage of the present invention:
(1) adopt the ultrasonic atomization pyrolysismethod, a step is realized the preparation of nanometer silicon dioxide and the load of active component, and technology is simple, the catalyst activity height, the good dispersion that obtain.
What (2) the silica presoma adopted is silicon tetrachloride as by-product of polysilicon, replaces ethyl orthosilicate commonly used, realizes the utilization again of resource when reducing cost.
(3) can obtain the catalyst of different catalytic efficiencies by changing the soluble chemical component solution concentration of nickeliferous platinum.
The specific embodiment
Below in conjunction with embodiment the present invention is done detailed description.
Embodiment one
The method of ultrasonic atomization pyrolysismethod synthetic silica nickel-loaded platinum catalyst specifically comprises following step:
Step 1, contain the preparation of the soluble compound solution of reactive metal: with Ni (OH)
2Be dissolved in the hydrochloric acid solution of 0.4mol/L, form NiCl
2Solution guarantees that the mass fraction of nickel is 1%.
Step 2, NiCl
2The atomizing of solution: adopt power 200W, transducer frequency is the ultrasonic ultrasonic delay line memory of 1.7MHz, and atomization rates is 0.4mL/min, with NiCl
2It is that the droplet of 5 μ m sprays into pyrolysis reactor that solution mist changes into average grain diameter.
The vaporization of step 3, silicon tetrachloride: adopt silicon tetrachloride as by-product of polysilicon to make raw material, silicon tetrachloride is vaporized through entering evaporimeter after the distillation equipment purifying, and silicon tetrachloride sample introduction speed is 0.2mL/min.
Step 4, NiCl
2Drop and silicon tetrachloride steam generation pyrolytic reaction: silicon tetrachloride steam and NiCl
2Drop is sprayed into pyrolysis reactor, and the mol ratio of silicon tetrachloride gas and nickel platinum drop is 1:10～1:50, reacts at 300 ℃, silicon tetrachloride gas and micron-sized drop generation hydrolysis, generate nanometer grade silica, in the drop residual moisture by evaporate to dryness, NiCl
2At high temperature forming the Ni catalyst granules loads on the nano silicon.
The collection of step 5, catalyst is with dry: nano silicon supported ni catalyst powder deposition takes out powder and at 200 ℃ of following dry 2h, obtains product in gatherer.
This catalyst is tested sign, and the BET specific area is 245m
2/ g, total pore volume is 0.18mL/g, the XRF data result shows that the mass percent of nickel/silica is 22%.
Embodiment two
The method of ultrasonic atomization pyrolysismethod synthetic silica nickel-loaded platinum catalyst specifically comprises following step:
Step 1, contain the preparation of the soluble compound solution of reactive metal: with chloroplatinic acid (H
2PtCl
6) be dissolved in the pure water, guarantee that the mass fraction of platinum is 1%.
Step 2, H
2PtCl
6The atomizing of solution: adopt power 200W, transducer frequency is the ultrasonic ultrasonic delay line memory of 1.7MHz, and atomization rates is 0.4mL/min, with H
2PtCl
6It is that the droplet of 5 μ m sprays into pyrolysis reactor that solution mist changes into average grain diameter.
The vaporization of step 3, silicon tetrachloride: adopt silicon tetrachloride as by-product of polysilicon to make raw material, silicon tetrachloride is vaporized through entering evaporimeter after the distillation equipment purifying, and silicon tetrachloride sample introduction speed is 0.2mL/min.
Step 4, H
2PtCl
6Drop and silicon tetrachloride steam generation pyrolytic reaction: silicon tetrachloride steam and H
2PtCl
6Drop is sprayed into pyrolysis reactor, and the mol ratio of silicon tetrachloride gas and nickel platinum drop is 1:10～1:50, reacts at 300 ℃.Silicon tetrachloride gas and micron-sized drop generation hydrolysis generate nanometer grade silica, in the drop residual moisture by evaporate to dryness, H
2PtCl
6At high temperature forming the Pt catalyst granules loads on the nano silicon.
The collection of step 5, catalyst is with dry: nano silicon loaded Pt catalyst powder deposition takes out powder and at 200 ℃ of following dry 2h, obtains product in gatherer.
This catalyst is tested sign: the BET specific area is 275m
2/ g, total pore volume is 0.37mL/g, the mass percent that XRF records platinum/silica is 24%.
Embodiment three
The method of ultrasonic atomization pyrolysismethod synthetic silica nickel-loaded platinum catalyst specifically comprises following step:
Step 1, contain the preparation of the soluble compound solution of reactive metal: preparation Ni mass fraction is 0.5% NiCl
2Solution and Pt mass fraction are 0.5% H
2PtCl
6Solution.
Step 2, contain the atomizing of Ni/Pt active component mixed liquor: adopt power 200W, transducer frequency is the ultrasonic ultrasonic delay line memory of 1.7MHz, atomization rates is 0.4mL/min, and it is that the droplet of 5 μ m sprays into pyrolysis reactor that the Ni/Pt living solution is atomized into average grain diameter.
The vaporization of step 3, silicon tetrachloride: adopt silicon tetrachloride as by-product of polysilicon to make raw material, silicon tetrachloride is vaporized through entering evaporimeter after the distillation equipment purifying, and silicon tetrachloride sample introduction speed is 0.2mL/min.
Step 4, Ni/Pt living solution drop and silicon tetrachloride steam generation pyrolytic reaction: silicon tetrachloride steam and Ni/Pt living solution drop are sprayed into pyrolysis reactor, the mol ratio of silicon tetrachloride gas and nickel platinum drop is 1:10～1:50, react at 300 ℃, silicon tetrachloride gas and micron-sized drop generation hydrolysis, generate nanometer grade silica, residual moisture is by evaporate to dryness in the drop, NiCl
2/ H
2PtCl
6At high temperature forming the nickel Pt catalyst granule loads on the nano silicon.
The collection of step 5, catalyst is with dry: nano silicon nickel-loaded platinum catalyst powder deposition takes out powder and at 200 ℃ of following dry 2h, obtains product in gatherer.
This catalyst is tested sign: the BET specific area is 230m
2/ g, total pore volume is 0.53mL/g.
Claims (4)
1. the method for ultrasonic atomization pyrolysismethod synthetic silica nickel-loaded platinum catalyst is characterized in that, may further comprise the steps:
The preparation of the soluble compound solution of step 1, nickel metal platinum: reactive metal adopts nickel, platinum or the combination of both arbitrary proportions, and the preparation mass concentration is the soluble compound solution of 0.2～2% nickel metal platinum;
The atomizing of the soluble compound solution of step 2, nickel metal platinum: adopt power 200W, transducer frequency is the ultrasonic ultrasonic delay line memory of 1.7MHz, atomization rates is 0.4mL/min, and it is that the droplet of 5 μ m sprays into pyrolysis reactor that the soluble compound solution mist of nickel metal platinum is changed into average grain diameter;
The vaporization of step 3, silicon tetrachloride: adopt silicon tetrachloride as by-product of polysilicon to make raw material, silicon tetrachloride carries out purifying through distillation equipment earlier, silicon tetrachloride is heated to more than 60 ℃ vaporizes then, and taken out of by carrier gas;
Metallic nickel platinum drop and silicon tetrachloride steam generation pyrolytic reaction after step 4, the atomizing: the nickel platinum drop after silicon tetrachloride steam and the atomizing is sprayed into pyrolysis reactor, the mol ratio of silicon tetrachloride gas and nickel platinum drop is 1:10～1:50, under 200～500 ℃ of temperature, react, silicon tetrachloride gas and micron-sized drop generation hydrolysis, generate nanometer grade silica, residual moisture is by evaporate to dryness in the drop, and the soluble compound that contains active nickel platinum simultaneously at high temperature forms catalyst granules and loads on the nano silicon;
The collection of step 5, catalyst is with dry: nano silicon nickel-loaded platinum catalyst powder deposition takes out powder and at 200 ℃ of following dry 2h, obtains product in gatherer.
2. the method for ultrasonic atomization pyrolysismethod synthetic silica nickel-loaded platinum catalyst according to claim 1 is characterized in that, may further comprise the steps: step 1, contain the preparation of the soluble compound solution of reactive metal: with Ni (OH)
2Be dissolved in the hydrochloric acid solution of 0.4mol/L, form NiCl
2Solution guarantees that the mass fraction of nickel is 1%;
Step 2, NiCl
2The atomizing of solution: adopt power 200W, transducer frequency is the ultrasonic ultrasonic delay line memory of 1.7MHz, and atomization rates is 0.4mL/min, with NiCl
2It is that the droplet of 5 μ m sprays into pyrolysis reactor that solution mist changes into average grain diameter;
The vaporization of step 3, silicon tetrachloride: adopt silicon tetrachloride as by-product of polysilicon to make raw material, silicon tetrachloride is vaporized through entering evaporimeter after the distillation equipment purifying, and silicon tetrachloride sample introduction speed is 0.2mL/min;
Step 4, NiCl
2Drop and silicon tetrachloride steam generation pyrolytic reaction: silicon tetrachloride steam and NiCl
2Drop is sprayed into pyrolysis reactor, and the mol ratio of silicon tetrachloride gas and nickel platinum drop is 1:10～1:50, reacts at 300 ℃, silicon tetrachloride gas and micron-sized drop generation hydrolysis, generate nanometer grade silica, in the drop residual moisture by evaporate to dryness, NiCl
2At high temperature forming the Ni catalyst granules loads on the nano silicon;
The collection of step 5, catalyst is with dry: nano silicon supported ni catalyst powder deposition takes out powder and at 200 ℃ of following dry 2h, obtains product in gatherer.
3. the method for ultrasonic atomization pyrolysismethod synthetic silica nickel-loaded platinum catalyst according to claim 1 is characterized in that, step 1, contains the preparation of the soluble compound solution of reactive metal: with chloroplatinic acid (H
2PtCl
6) be dissolved in the pure water, guarantee that the mass fraction of platinum is 1%;
Step 2, H
2PtCl
6The atomizing of solution: adopt power 200W, transducer frequency is the ultrasonic ultrasonic delay line memory of 1.7MHz, and atomization rates is 0.4mL/min, with H
2PtCl
6It is that the droplet of 5 μ m sprays into pyrolysis reactor that solution mist changes into average grain diameter;
The vaporization of step 3, silicon tetrachloride: adopt silicon tetrachloride as by-product of polysilicon to make raw material, silicon tetrachloride is vaporized through entering evaporimeter after the distillation equipment purifying, and silicon tetrachloride sample introduction speed is 0.2mL/min;
Step 4, H
2PtCl
6Drop and silicon tetrachloride steam generation pyrolytic reaction: silicon tetrachloride steam and H
2PtCl
6Drop is sprayed into pyrolysis reactor, and the mol ratio of silicon tetrachloride gas and nickel platinum drop is 1:10～1:50, reacts at 300 ℃.Silicon tetrachloride gas and micron-sized drop generation hydrolysis generate nanometer grade silica, in the drop residual moisture by evaporate to dryness, H
2PtCl
6At high temperature forming the Pt catalyst granules loads on the nano silicon;
The collection of step 5, catalyst is with dry: nano silicon loaded Pt catalyst powder deposition takes out powder and at 200 ℃ of following dry 2h, obtains product in gatherer.
4. the method for ultrasonic atomization pyrolysismethod synthetic silica nickel-loaded platinum catalyst according to claim 1 is characterized in that, step 1, contains the preparation of the soluble compound solution of reactive metal: preparation Ni mass fraction is 0.5% NiCl
2Solution and Pt mass fraction are 0.5% H
2PtCl
6Solution;
Step 2, contain the atomizing of Ni/Pt active component mixed liquor: adopt power 200W, transducer frequency is the ultrasonic ultrasonic delay line memory of 1.7MHz, atomization rates is 0.4mL/min, and it is that the droplet of 5 μ m sprays into pyrolysis reactor that the Ni/Pt living solution is atomized into average grain diameter;
The vaporization of step 3, silicon tetrachloride: adopt silicon tetrachloride as by-product of polysilicon to make raw material, silicon tetrachloride is vaporized through entering evaporimeter after the distillation equipment purifying, and silicon tetrachloride sample introduction speed is 0.2mL/min;
Step 4, Ni/Pt living solution drop and silicon tetrachloride steam generation pyrolytic reaction: silicon tetrachloride steam and Ni/Pt living solution drop are sprayed into pyrolysis reactor, the mol ratio of silicon tetrachloride gas and nickel platinum drop is 1:10～1:50, react at 300 ℃, silicon tetrachloride gas and micron-sized drop generation hydrolysis, generate nanometer grade silica, residual moisture is by evaporate to dryness in the drop, NiCl
2/ H
2PtCl
6At high temperature forming the nickel Pt catalyst granule loads on the nano silicon;
The collection of step 5, catalyst is with dry: nano silicon nickel-loaded platinum catalyst powder deposition takes out powder and at 200 ℃ of following dry 2h, obtains product in gatherer.
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Cited By (6)
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| CN103464220A (en) * | 2013-09-13 | 2013-12-25 | 太原理工大学 | Method for modifying catalyst through ultrasonic atomization |
| CN106964409A (en) * | 2017-03-31 | 2017-07-21 | 合肥悦兰信息技术有限公司 | Liquid catalyst agent carrier by matrix of nano silicon |
| CN109590028A (en) * | 2018-11-28 | 2019-04-09 | 浙江工商大学 | A method of nm-class catalyst is prepared using ultrasonic atomizatio plasma reaction |
| CN111359673A (en) * | 2020-03-26 | 2020-07-03 | 安徽元琛环保科技股份有限公司 | MnO2PPS composite material and preparation method and application thereof |
| CN114345333A (en) * | 2022-01-14 | 2022-04-15 | 济南大学 | Preparation method of automobile exhaust purification catalyst with controllable precious metal content and obtained product |
| CN114425055A (en) * | 2020-10-15 | 2022-05-03 | 武汉工程大学 | Silicon dioxide loaded multi-metal nano-particles, preparation method and antibacterial application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103464220A (en) * | 2013-09-13 | 2013-12-25 | 太原理工大学 | Method for modifying catalyst through ultrasonic atomization |
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| CN114345333A (en) * | 2022-01-14 | 2022-04-15 | 济南大学 | Preparation method of automobile exhaust purification catalyst with controllable precious metal content and obtained product |
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