CN105214685A - A kind of platinum cobalt alloy structured catalysis material for brine electrolysis and preparation method thereof - Google Patents
A kind of platinum cobalt alloy structured catalysis material for brine electrolysis and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of platinum cobalt alloy structured catalysis material for brine electrolysis, described brine electrolysis catalysis material is made up of catalytic activity thing and carrier, described catalytic activity thing is platinum cobalt alloy structure, described carrier is ultrafine carbon fiber, does is the load capacity of catalytic activity thing 2-20 on described carrier? wt%.The present invention is a kind of platinum cobalt alloy structure/ultrafine carbon fiber hybrid material, and this hybrid material adopts in-situ method to prepare platinum cobalt alloy.The present invention in order to improve its catalytic activity while reduction platinum catalyst content, and described carrier have selected ultrafine carbon fiber.Catalysis material of the present invention has high-ratio surface sum porosity, be conducive to diffusion and the desorbing gas of electrolyte, the characteristic of platinum cobalt alloy makes this material have higher hydrogen evolution activity, simultaneously without the need to loading on electrode, directly can be used as working electrode and carrying out electro-catalysis hydrogen manufacturing.
Description
Technical field
The present invention relates to a kind of brine electrolysis catalysis material, particularly a kind of platinum cobalt alloy structured catalysis material for brine electrolysis and preparation method thereof.
Background technology
Current, Hydrogen Energy cleanliness without any pollution, and efficiently, renewable, be acknowledged as following most potential energy carrier.Water electrolysis hydrogen production is a kind of one of efficient, clean and the most promising method preparing hydrogen.For water electrolysis hydrogen production, how to improve the activity of electrode catalytic materials, reduce overpotential of hydrogen evolution, and improve emphasis and the key that the stability of electrode material and durability are electro-catalysis area researches.In recent years, the bimetallic catalyst of alloy structure is more and more for the correlative study of water electrolysis hydrogen production, the utilization rate of metal can not only be improved, reduce catalyst cost, and catalytic performance be improved due to the electronic effect that has between two kinds of metals and cooperative effect.As everyone knows, Pt and 3d transition metal (Ni, Fe, Co etc.) is prepared into alloy structure, and this nanometer electrical catalyst demonstrates good catalytic activity and stability in electrocatalytic reaction.
Carbon nano-fiber (CNF) is by the curling fibrous nano material with carbon element of Multi-layer graphite sheet, due to characteristics such as its good mechanical property, light weight and high electric conductivity, be potentially applied to the fields such as hydrogen storage material, high-capacity electrode material, high-performance composite materials, fuel cell.As novel material with carbon element, CNF, owing to having the series of advantages such as large, the unique surface texture of acid-alkali-corrosive-resisting, specific area, has a wide range of applications at catalytic field.
So far, platinum cobalt alloy structure is used for electro-catalysis hydrogen preparation field and still there is more problem, the stability that first 3d transition metal is poor in acid solution, reduces the catalytic efficiency of catalyst; It two is stability and recyclability problems of electrode.Stability and the cyclicity of the electro catalytic electrode prepared by current various method are often poor, and therefore good conductive substrates supported catalyst is vital for electro-catalysis.Therefore, how designing and prepare the water electrolysis hydrogen production catalysis material with high catalytic activity and good stability is current problem demanding prompt solution.
Summary of the invention
The object of the invention is to the above-mentioned shortcoming solving prior art existence, a kind of platinum cobalt alloy structured catalysis material for brine electrolysis is provided.
The present invention also provides the preparation method of described platinum cobalt alloy structured catalysis material.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of platinum cobalt alloy structured catalysis material for brine electrolysis, described brine electrolysis catalysis material is made up of catalytic activity thing and carrier, described catalytic activity thing is platinum cobalt alloy structure, and described carrier is ultrafine carbon fiber, and on described carrier, the load capacity of catalytic activity thing is 2-20wt%.The present invention is a kind of platinum cobalt alloy structure/ultrafine carbon fiber hybrid material, and this hybrid material adopts in-situ method to prepare platinum cobalt alloy.First ultrafine carbon fiber presoma is configured to spinning solution, then the presoma of platinum and cobalt is dissolved in spinning solution.Utilize electrostatic spinning technique to be prepared into ultrafine carbon fiber spinning solution, then utilize tube furnace to carry out carbonization to ultrafine carbon fiber, in carbonisation, form platinum cobalt alloy structure/ultrafine carbon fiber hybrid material.
The present invention in order to improve its catalytic activity while reduction platinum catalyst content, and described carrier have selected ultrafine carbon fiber.Catalysis material of the present invention has high-ratio surface sum porosity, be conducive to diffusion and the desorbing gas of electrolyte, the characteristic of platinum cobalt alloy makes this material have higher hydrogen evolution activity, simultaneously without the need to loading on electrode, directly can be used as working electrode and carrying out electro-catalysis hydrogen manufacturing.
As preferably, described platinum cobalt alloy structure is platinum cobalt alloy nanoparticles, and its particle size is 5-20nm.Described platinum cobalt alloy structure is coated by thin carbon layer, and carbon thin layer is not herein carrier, is in the preparation process of alloy, the thin layer that the surface that a small amount of carbon is coated on alloy is formed, as shown in the carbonlayer in Fig. 2 f upper right illustration.
As preferably, the fineness of described ultrafine carbon fiber is 50-1000nm.
A kind of preparation method of the described platinum cobalt alloy structured catalysis material for brine electrolysis, the method comprises the steps: 1) by ultrafine carbon fiber presoma N, dinethylformamide is made into the spinning solution that mass concentration is 5-15%, the presoma of platinum cobalt alloy is dissolved in spinning solution, then adopts method of electrostatic spinning to be prepared into ultrafine carbon fiber spinning solution; 2) ultrafine carbon fiber is incubated pre-oxidation 3 hours after being at room temperature warming up to 200-300 DEG C; then continue to heat up under inert gas shielding and vacuum state; 800-1200 DEG C is warming up in 2 hours; insulation carbonization 5-12 hour; finally under inert gas shielding, be cooled to room temperature, obtain platinum cobalt alloy structured catalysis material.Described inert gas can select conventional protective gas, as argon gas etc.
As preferably, in step 1), controlling spinning voltage during electrostatic spinning is 8-20kV, and receiving system is 10-20cm to the distance of spinning syringe needle, and solution flow rate is 0.2mL/h.
As preferably, in step 1), described ultrafine carbon fiber presoma is one or more in polyacrylonitrile, polymine, polyvinyl alcohol.
As preferably, in step 1), in platinum cobalt alloy, the presoma of platinum is one or both in chloroplatinic acid, acetylacetone,2,4-pentanedione platinum.
As preferably, in step 1), in platinum cobalt alloy, the presoma of cobalt is one or more in cobalt nitrate, cobalt chloride, cobaltous sulfate, cobalt carbonate.
As preferably, step 2) in, described heating rate is 5 DEG C/min.
An application for the described platinum cobalt alloy structured catalysis material for brine electrolysis, specifically: described platinum cobalt alloy structured catalysis material is as the catalyst of the cathode catalysis liberation of hydrogen of brine electrolysis.Brine electrolysis catalysis material prepared by the present invention has higher catalytic hydrogen evolution effect.
The invention has the beneficial effects as follows:
(1) utilize the electronic effect that has between alloy structure two kinds of metals and cooperative effect that catalytic performance is improved, catalyst cost can be reduced simultaneously;
(2) the brine electrolysis catalysis material prepared by has high-ratio surface sum porosity, is conducive to diffusion and the desorbing gas of electrolyte;
(3) utilize confinement and the induced growth effect of graphite linings in one dimension material with carbon element, regulation and control nano-interface structure, can improve electro catalytic activity further;
(4) ultrafine carbon fiber can available protecting platinum cobalt alloy from the erosion of electrolyte, give the good stability of hybrid material and durability;
(5) brine electrolysis catalysis material is without the need to loading on electrode, directly can be used as electrode and carry out electro-catalysis hydrogen manufacturing.
Accompanying drawing explanation
Fig. 1 is the microscopic appearance of platinum of the present invention cobalt alloy/ultrafine carbon fiber (PtCo/CNFs) hybrid material.(a-c): the field emission scanning electron microscope photo of PtCo/CNFs, Pt/CNFs and Co/CNFs; (d, e) PtCo/CNFs transmission electron microscope photo, illustration is respectively the corresponding domain size distribution of platinum cobalt alloy nanoparticles and is coated on the high-resolution-ration transmission electric-lens photo of platinum cobalt alloy of ultrafine carbon fiber inside; The energy spectrogram of (f): PtCo/CNFs;
The electro catalytic activity of Fig. 2 brine electrolysis catalysis material of the present invention.(a, b): CNFs, Co/CNFs, Pt/CNFs, business Pt/C (20wt%) and PtCo/CNFs is at 0.5MH
2sO
4in polarization curve and corresponding Tafel slope (load capacity of catalyst is 212 μ gcm
-2, sweep speed is 2mV/s), in a, illustration produces the photo of hydrogen gas bubbles on its surface when 50mV operates for overlaying on PtCo/CNFs catalyst on glass-carbon electrode (GCE); (c): the energy Qwest curve that Co/CNFs, Pt/CNFs and PtCo/CNFs test under open-circuit voltage; The polarization curve of (d) PtCo/CNFs and business Pt/C (20wt%) before and after 1000 loop tests, illustration is the Cyclic voltamogram curve of PtCo/CNFs before and after loop test; E (catalyst loadings is 1mg/cm to () PtCo/CNFs film
2) time current response curve (j-t) when constant voltage-0.3V, illustration is that PtCo/CNFs catalyst proceeds to the 6 little pictures producing hydrogen gas bubbles constantly in test, and enlarged drawing refers to place shown in broken circle; Corresponding high-resolution-ration transmission electric-lens photo in transmission electron microscope photo after (f) PtCo/CNFs stability test and illustration.
Detailed description of the invention
Below by specific embodiment, technical scheme of the present invention is described in further detail.In the present invention, if not refer in particular to, the raw material adopted and equipment etc. all can be buied from market or this area is conventional.Method in following embodiment, if no special instructions, is the conventional method of this area.
Embodiment 1:
Get 0.15g chloroplatinic acid and 0.1g cobalt chloride and join N containing 3g polyacrylonitrile, in dinethylformamide solution (wherein the mass concentration of polyacrylonitrile is 12%), then method of electrostatic spinning is adopted to carry out spinning to this spinning solution, control spinning voltage is 15kV, receiving system is 15cm(and receiving range to the distance of spinning syringe needle is 15cm), solution flow rate is 0.2mL/h, namely obtains ultrafine carbon fiber.
Be placed in corundum boat by regular for the cutting of 500mg ultrafine carbon fiber, be then transferred to the heating position in tube furnace, be warming up to 230 DEG C with 5 DEG C/min first in atmosphere and maintain 3 hours.Open argon gas after 30 minutes, temperature is continued to heat up with 5 DEG C/min; After 2 hours, tube furnace temperature rises to 1000 DEG C, is incubated 8 hours; finally under argon shield, be cooled to room temperature; obtain platinum cobalt alloy/ultrafine carbon fiber hybrid material, this material is the platinum cobalt alloy structured catalysis material of the present invention for brine electrolysis, and microscopic appearance is shown in Fig. 1.Using this material directly as electrode, in 0.5M sulfuric acid solution, test its electrocatalytic hydrogen evolution active, the data obtained as shown in Figure 2.
By the brine electrolysis catalysis material with platinum cobalt alloy structure that the method obtains; electronic effect between alloy structure two kinds of metals and cooperative effect make catalytic performance improve; and ultrafine carbon fiber can available protecting platinum cobalt alloy from the erosion of electrolyte, give the good stability of hybrid material and durability.
Embodiment 2:
Get 0.15g acetylacetone,2,4-pentanedione platinum and 0.1g cobalt carbonate and join N containing 1g polymine, in dinethylformamide solution (wherein the mass concentration of polymine is 8%), then method of electrostatic spinning is adopted to carry out spinning to this spinning solution, control spinning voltage is 8kV, receiving system is 10cm(and receiving range to the distance of spinning syringe needle is 10cm), solution flow rate is 0.2mL/h, namely obtains ultrafine carbon fiber.
Be placed in corundum boat by regular for the cutting of 500mg ultrafine carbon fiber, be then transferred to the heating position in tube furnace, be warming up to 200 DEG C with 5 DEG C/min first in atmosphere and maintain 3 hours.Open argon gas after 30 minutes, temperature is continued to heat up with 5 DEG C/min; After 2 hours, tube furnace temperature rises to 800 DEG C, is incubated 12 hours, finally under argon shield, is cooled to room temperature, obtain platinum cobalt alloy/ultrafine carbon fiber hybrid material, and this material is the platinum cobalt alloy structured catalysis material of the present invention for brine electrolysis.
Embodiment 3:
Get 0.3g chloroplatinic acid and 0.2g cobalt carbonate and join N containing 5g polyvinyl alcohol, in dinethylformamide solution (wherein the mass concentration of polyvinyl alcohol is 12%), then method of electrostatic spinning is adopted to carry out spinning to this spinning solution, control spinning voltage is 20kV, receiving system is 20cm(and receiving range to the distance of spinning syringe needle is 20cm), solution flow rate is 0.2mL/h, namely obtains ultrafine carbon fiber.
Be placed in corundum boat by regular for the cutting of 500mg ultrafine carbon fiber, be then transferred to the heating position in tube furnace, be warming up to 300 DEG C with 5 DEG C/min first in atmosphere and maintain 3 hours.Open argon gas after 30 minutes, temperature is continued to heat up with 5 DEG C/min; After 2 hours, tube furnace temperature rises to 1200 DEG C, is incubated 5 hours, finally under argon shield, is cooled to room temperature, obtain platinum cobalt alloy/ultrafine carbon fiber hybrid material, and this material is the platinum cobalt alloy structured catalysis material of the present invention for brine electrolysis.
With reference to the method for specific embodiment, the present invention can adjust raw material, technological parameter etc. according to the scope of claim, prepares multiple material.Above-described embodiment is one of the present invention preferably scheme, not does any pro forma restriction to the present invention, also has other variant and remodeling under the prerequisite not exceeding the technical scheme described in claim.
Claims (10)
1. the platinum cobalt alloy structured catalysis material for brine electrolysis, it is characterized in that: described brine electrolysis catalysis material is made up of catalytic activity thing and carrier, described catalytic activity thing is platinum cobalt alloy structure, described carrier is ultrafine carbon fiber, and on described carrier, the load capacity of catalytic activity thing is 2-20wt%.
2. platinum cobalt alloy structured catalysis material according to claim 1, is characterized in that: described platinum cobalt alloy structure is platinum cobalt alloy nanoparticles, and its particle size is 5-20nm.
3. platinum cobalt alloy structured catalysis material according to claim 1 and 2, is characterized in that: the fineness of described ultrafine carbon fiber is 50-1000nm.
4., as claimed in claim 1 for the preparation method of the platinum cobalt alloy structured catalysis material of brine electrolysis, it is characterized in that, the method comprises the steps:
1) ultrafine carbon fiber presoma DMF is made into the spinning solution that mass concentration is 5-15%, the presoma of platinum cobalt alloy is dissolved in spinning solution, then adopt method of electrostatic spinning to be prepared into ultrafine carbon fiber spinning solution;
2) ultrafine carbon fiber is incubated pre-oxidation 3 hours after being at room temperature warming up to 200-300 DEG C; then continue to heat up under inert gas shielding and vacuum state; 800-1200 DEG C is warming up in 2 hours; insulation carbonization 5-12 hour; finally under inert gas shielding, be cooled to room temperature, obtain platinum cobalt alloy structured catalysis material.
5. preparation method according to claim 4, is characterized in that: in step 1), and controlling spinning voltage during electrostatic spinning is 8-20kV, and receiving system is 10-20cm to the distance of spinning syringe needle, and solution flow rate is 0.2mL/h.
6. preparation method according to claim 4, is characterized in that: in step 1), and described ultrafine carbon fiber presoma is one or more in polyacrylonitrile, polymine, polyvinyl alcohol.
7. preparation method according to claim 4, is characterized in that: in step 1), and in platinum cobalt alloy, the presoma of platinum is one or both in chloroplatinic acid, acetylacetone,2,4-pentanedione platinum.
8. preparation method according to claim 4, is characterized in that: in step 1), and in platinum cobalt alloy, the presoma of cobalt is one or more in cobalt nitrate, cobalt chloride, cobaltous sulfate, cobalt carbonate.
9. preparation method according to claim 4, is characterized in that: step 2) in, described heating rate is 5 DEG C/min.
10., as claimed in claim 1 for the application of the platinum cobalt alloy structured catalysis material of brine electrolysis, it is characterized in that: described platinum cobalt alloy structured catalysis material is as the catalyst of the cathode catalysis liberation of hydrogen of brine electrolysis.
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