CN103223347B - 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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- CN103223347B CN103223347B CN201310130768.6A CN201310130768A CN103223347B CN 103223347 B CN103223347 B CN 103223347B CN 201310130768 A CN201310130768 A CN 201310130768A CN 103223347 B CN103223347 B CN 103223347B
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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, suitable pore size distribution$, and has good mechanical strength and chemical inertness, can be used as the carrier of catalyst.Silicon dioxide carried nickel platinum metal catalyst can be used for the multiple reactions such as catalytic hydrogenation, dehydrogenation, hydrocracking.
The preparation of silicon dioxide carried active metal catalyst, adopts infusion process at present, fully contacts by the solution that carrier silicas is immersed in containing active component, then through filtering, dry, roasting and activation, obtained catalyst.Catalyst prepared by infusion process, the active component of load is mainly distributed in carrier surface, is evenly distributed, and utilization rate is high, is applicable to very much the noble metal catalysts such as preparation Ni, Pt.Directly make carrier with shaping nano silicon, although eliminate the complicated technologies such as carrier is shaping, pretreatment, nanometer grade silica is as high-end nanometer product, and price is relatively costly.
Ultrasonic atomization pyrolysismethod is sprayed by solution with ultrasonic wave, at high temperature pyrolytic reaction occurs with another kind of material.Due to hyperacoustic vibrating dispersion effect, the particle diameter of ejection solution is about 5 μm, reacts, can synthesize the nano material that concentration class is little, good dispersion, specific area are high with high-temperature gas.Utilize ultrasonic atomization pyrolysismethod synthesis of nano silica supported metal nickel, the principle of platinum is, by the soluble compound solution sonic oscillation ejection containing active metal nickel, platinum, at high temperature pyrolytic reaction is there is, the silicon dioxide carried nickel platinum catalyst of synthesis of nano with silica precursor.Polysilicon refuse silicon tetrachloride (SiCl is adopted in reaction
4) substitute traditional ethyl orthosilicate (TEOS) and make the presoma of silica, can reduce costs and realize the recycling of resource.Adopt the method for the silicon dioxide carried nickel platinum catalyst of ultrasonic atomization pyrolysismethod synthesis of nano, there is no Patents and research report at present both at home and abroad.
Summary of the invention
In order to overcome the defect of above-mentioned prior art, the nano silicon existed for infusion process urges the shortcomings such as carrier is expensive, carrier complex forming technology, the object of the present invention is to provide a kind of method of ultrasonic atomization pyrolysismethod synthetic silica nickel-loaded platinum catalyst, solve the problem that silica supports is expensive, load process is complicated, there is synthesis technique simple, the nano silicon nickel-loaded platinum catalyst activity obtained is high, 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, comprises the following steps:
The preparation of the soluble compound solution of step one, nickel metal platinum: active metal adopts the combination of nickel, platinum or both arbitrary proportions, preparation mass concentration is the soluble compound solution of the nickel metal platinum of 0.2 ~ 2%;
The atomization 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 the soluble compound solution mist of nickel metal platinum being changed into average grain diameter is that the droplet of 5 μm sprays into pyrolysis reactor;
The vaporization of step 3, silicon tetrachloride: adopt silicon tetrachloride as by-product of polysilicon to make raw material, silicon tetrachloride first carries out purifying through distillation equipment, then silicon tetrachloride is heated to more than 60 DEG C and vaporizes, and taken out of by carrier gas;
Metallic nickel platinum drop after step 4, atomization and silicon tetrachloride steam generation pyrolytic reaction: silicon tetrachloride steam and the nickel platinum drop after being atomized are injected into pyrolysis reactor, the mol ratio of silicon tetrachloride gas and nickel platinum drop is 1:10 ~ 1:50, react at 200 ~ 500 DEG C of temperature, silicon tetrachloride gas and micron-sized drop generation hydrolysis, generate nanometer grade silica, in drop, residual moisture is by evaporate to dryness, and the soluble compound simultaneously containing active nickel platinum at high temperature forms supporting catalyst particles on nano silicon.
The collection of step 5, catalyst is with dry: nano silicon nickel-loaded platinum catalyst powder deposition in collector, take out powder and at 200 DEG C dry 2h, obtain product.
Advantage of the present invention:
(1) adopt ultrasonic atomization pyrolysismethod, a step realizes the preparation of nanometer silicon dioxide and the load of active component, and technique is simple, and the catalyst activity obtained is high, good dispersion.
(2) what silica precursor adopted is silicon tetrachloride as by-product of polysilicon, replaces conventional ethyl orthosilicate, realizes the recycling of resource while reducing costs.
(3) by changing the soluble chemical component solution concentration of nickeliferous platinum, the catalyst of different catalytic efficiency is obtained.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in detail.
Embodiment one
The method of ultrasonic atomization pyrolysismethod synthetic silica nickel-loaded platinum catalyst, specifically comprises following step:
Step one, preparation containing the soluble compound solution of active metal: by Ni (OH)
2be dissolved in the hydrochloric acid solution of 0.4mol/L, form NiCl
2solution, ensures that the mass fraction of nickel is 1%.
Step 2, NiCl
2the atomization of solution: adopt power 200W, transducer frequency is the ultrasonic ultrasonic delay line memory of 1.7MHz, and atomization rates is 0.4mL/min, by NiCl
2it is that the droplet of 5 μm 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 enters evaporimeter and vaporizes after 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 injected into pyrolysis reactor, and the mol ratio of silicon tetrachloride gas and nickel platinum drop is 1:10 ~ 1:50, reacts at 300 DEG C, silicon tetrachloride gas and micron-sized drop generation hydrolysis, generate nanometer grade silica, in drop, residual moisture is by evaporate to dryness, NiCl
2at high temperature form Ni supporting catalyst particles on nano silicon.
The collection of step 5, catalyst is with dry: nano silicon supported ni catalyst powder deposition in collector, take out powder and at 200 DEG C dry 2h, obtain product.
Carry out test to this catalyst to characterize, BET specific surface area is 245m
2/ g, total pore volume is the mass percent of 0.18mL/g, XRF data result display nickel/silica is 22%.
Embodiment two
The method of ultrasonic atomization pyrolysismethod synthetic silica nickel-loaded platinum catalyst, specifically comprises following step:
Step one, preparation containing the soluble compound solution of active metal: by chloroplatinic acid (H
2ptCl
6) be dissolved in pure water, ensure that the mass fraction of platinum is 1%.
Step 2, H
2ptCl
6the atomization of solution: adopt power 200W, transducer frequency is the ultrasonic ultrasonic delay line memory of 1.7MHz, and atomization rates is 0.4mL/min, by H
2ptCl
6it is that the droplet of 5 μm 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 enters evaporimeter and vaporizes after 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 injected into pyrolysis reactor, and the mol ratio of silicon tetrachloride gas and nickel platinum drop is 1:10 ~ 1:50, reacts at 300 DEG C.Silicon tetrachloride gas and micron-sized drop generation hydrolysis, generate nanometer grade silica, in drop, residual moisture is by evaporate to dryness, H
2ptCl
6at high temperature form Pt supporting catalyst particles on nano silicon.
The collection of step 5, catalyst is with dry: nano silicon loaded Pt catalyst powder deposition in collector, take out powder and at 200 DEG C dry 2h, obtain product.
Carry out test to this catalyst to characterize: BET specific surface area is 275m
2/ g, total pore volume is the mass percent that 0.37mL/g, XRF record platinum/silica is 24%.
Embodiment three
The method of ultrasonic atomization pyrolysismethod synthetic silica nickel-loaded platinum catalyst, specifically comprises following step:
Step one, preparation containing the soluble compound solution of active metal: preparation Ni mass fraction is the NiCl of 0.5%
2solution and Pt mass fraction are the H of 0.5%
2ptCl
6solution.
Step 2, atomization containing 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 Ni/Pt living solution being atomized into average grain diameter is that the droplet of 5 μm sprays into pyrolysis reactor.
The vaporization of step 3, silicon tetrachloride: adopt silicon tetrachloride as by-product of polysilicon to make raw material, silicon tetrachloride enters evaporimeter and vaporizes after 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 injected into pyrolysis reactor, the mol ratio of silicon tetrachloride gas and nickel platinum drop is 1:10 ~ 1:50, react at 300 DEG C, silicon tetrachloride gas and micron-sized drop generation hydrolysis, generate nanometer grade silica, in drop, residual moisture is by evaporate to dryness, NiCl
2/ H
2ptCl
6at high temperature form the load of nickel Pt catalyst granule on nano silicon.
The collection of step 5, catalyst is with dry: nano silicon nickel-loaded platinum catalyst powder deposition in collector, take out powder and at 200 DEG C dry 2h, obtain product.
Carry out test to this catalyst to characterize: BET specific surface 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, comprise the following steps:
The preparation of the soluble compound solution of step one, nickel metal platinum: active metal adopts the combination of nickel, platinum or both arbitrary proportions, preparation mass concentration is the soluble compound solution of the nickel metal platinum of 0.2 ~ 2%;
The atomization 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 the soluble compound solution mist of nickel metal platinum being changed into average grain diameter is that the droplet of 5 μm sprays into pyrolysis reactor;
The vaporization of step 3, silicon tetrachloride: adopt silicon tetrachloride as by-product of polysilicon to make raw material, silicon tetrachloride first carries out purifying through distillation equipment, then silicon tetrachloride is heated to more than 60 DEG C and vaporizes, and taken out of by carrier gas;
Metallic nickel platinum drop after step 4, atomization and silicon tetrachloride steam generation pyrolytic reaction: silicon tetrachloride steam and the nickel platinum drop after being atomized are injected into pyrolysis reactor, the mol ratio of silicon tetrachloride gas and nickel platinum drop is 1:10 ~ 1:50, react at 200 ~ 500 DEG C of temperature, silicon tetrachloride gas and micron-sized drop generation hydrolysis, generate nanometer grade silica, in drop, residual moisture is by evaporate to dryness, and the soluble compound simultaneously containing active nickel platinum at high temperature forms supporting catalyst particles on nano silicon;
The collection of step 5, catalyst is with dry: nano silicon nickel-loaded platinum catalyst powder deposition in collector, take out powder and at 200 DEG C dry 2h, obtain product.
2. the method for ultrasonic atomization pyrolysismethod synthetic silica nickel-loaded platinum catalyst according to claim 1, is characterized in that, comprise the following steps: step one, preparation containing the soluble compound solution of active metal: by Ni (OH)
2be dissolved in the hydrochloric acid solution of 0.4mol/L, form NiCl
2solution, ensures that the mass fraction of nickel is 1%;
Step 2, NiCl
2the atomization of solution: adopt power 200W, transducer frequency is the ultrasonic ultrasonic delay line memory of 1.7MHz, and atomization rates is 0.4mL/min, by NiCl
2it is that the droplet of 5 μm 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 enters evaporimeter and vaporizes after 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 injected into pyrolysis reactor, and the mol ratio of silicon tetrachloride gas and nickel platinum drop is 1:10 ~ 1:50, reacts at 300 DEG C, silicon tetrachloride gas and micron-sized drop generation hydrolysis, generate nanometer grade silica, in drop, residual moisture is by evaporate to dryness, NiCl
2at high temperature form Ni supporting catalyst particles on nano silicon;
The collection of step 5, catalyst is with dry: nano silicon supported ni catalyst powder deposition in collector, take out powder and at 200 DEG C dry 2h, obtain product.
3. the method for ultrasonic atomization pyrolysismethod synthetic silica nickel-loaded platinum catalyst according to claim 1, is characterized in that, step one, preparation containing the soluble compound solution of active metal: by chloroplatinic acid (H
2ptCl
6) be dissolved in pure water, ensure that the mass fraction of platinum is 1%;
Step 2, H
2ptCl
6the atomization of solution: adopt power 200W, transducer frequency is the ultrasonic ultrasonic delay line memory of 1.7MHz, and atomization rates is 0.4mL/min, by H
2ptCl
6it is that the droplet of 5 μm 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 enters evaporimeter and vaporizes after 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 injected into pyrolysis reactor, and the mol ratio of silicon tetrachloride gas and nickel platinum drop is 1:10 ~ 1:50, reacts at 300 DEG C, silicon tetrachloride gas and micron-sized drop generation hydrolysis, generate nanometer grade silica, in drop, residual moisture is by evaporate to dryness, H
2ptCl
6at high temperature form Pt supporting catalyst particles on nano silicon;
The collection of step 5, catalyst is with dry: nano silicon loaded Pt catalyst powder deposition in collector, take out powder and at 200 DEG C dry 2h, obtain product.
4. the method for ultrasonic atomization pyrolysismethod synthetic silica nickel-loaded platinum catalyst according to claim 1, is characterized in that, step one, preparation containing the soluble compound solution of active metal: preparation Ni mass fraction is the NiCl of 0.5%
2solution and Pt mass fraction are the H of 0.5%
2ptCl
6solution;
Step 2, atomization containing 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 Ni/Pt living solution being atomized into average grain diameter is that the droplet of 5 μm sprays into pyrolysis reactor;
The vaporization of step 3, silicon tetrachloride: adopt silicon tetrachloride as by-product of polysilicon to make raw material, silicon tetrachloride enters evaporimeter and vaporizes after 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 injected into pyrolysis reactor, the mol ratio of silicon tetrachloride gas and nickel platinum drop is 1:10 ~ 1:50, react at 300 DEG C, silicon tetrachloride gas and micron-sized drop generation hydrolysis, generate nanometer grade silica, in drop, residual moisture is by evaporate to dryness, NiCl
2/ H
2ptCl
6at high temperature form the load of nickel Pt catalyst granule on nano silicon;
The collection of step 5, catalyst is with dry: nano silicon nickel-loaded platinum catalyst powder deposition in collector, take out powder and at 200 DEG C dry 2h, obtain product.
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| CN103464220B (en) * | 2013-09-13 | 2015-01-14 | 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 |
| CN114425055B (en) * | 2020-10-15 | 2024-04-19 | 武汉工程大学 | Silica supported multi-metal nano-particle, preparation method and antibacterial 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 |
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| CN1320557A (en) * | 2000-03-28 | 2001-11-07 | 德古萨股份公司 | Doped titanium dioxide |
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| DE19650500A1 (en) * | 1996-12-05 | 1998-06-10 | Degussa | Doped, pyrogenic oxides |
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|---|---|---|---|---|
| CN1040932A (en) * | 1988-09-08 | 1990-04-04 | 清华大学 | Ultrasonic atomizing preparation of superfine powder |
| CN1320557A (en) * | 2000-03-28 | 2001-11-07 | 德古萨股份公司 | Doped titanium dioxide |
Non-Patent Citations (2)
| Title |
|---|
| "MAGNETIC PROPERTIES OF Ni-Pt/SiO2 NANOAGGREGATES SYNTHESISED BY RADIOLYSIS";N.Keghouche等;《Proceedings of Ⅻ International Symposium on Small Particles and Inorganic Clusters》;20040901;摘要 * |
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