CN106824238A - For the bifunctional catalyst nanoscale Ni of electrolysis water2P CoP double-metal phosphides - Google Patents

For the bifunctional catalyst nanoscale Ni of electrolysis water2P CoP double-metal phosphides Download PDF

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CN106824238A
CN106824238A CN201710017249.7A CN201710017249A CN106824238A CN 106824238 A CN106824238 A CN 106824238A CN 201710017249 A CN201710017249 A CN 201710017249A CN 106824238 A CN106824238 A CN 106824238A
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CN106824238B (en
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梁鑫
郑冰霞
陈标华
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Beijing University of Chemical Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/14—Phosphorus; Compounds thereof
    • B01J27/185—Phosphorus; Compounds thereof with iron group metals or platinum group metals
    • B01J27/1853—Phosphorus; Compounds thereof with iron group metals or platinum group metals with iron, cobalt or nickel
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/02—Hydrogen or oxygen
    • C25B1/04—Hydrogen or oxygen by electrolysis of water
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
    • C25B11/069—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of at least one single element and at least one compound; consisting of two or more compounds
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

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  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)

Abstract

The invention provides a kind of bifunctional catalyst nanoscale Ni for electrolysis water2P CoP double-metal phosphides, the catalyst does not only have excellent electrolysis water oxygen evolution activity, and also shows excellent activity in the test of electrolysis water liberation of hydrogen.4 8h are reacted at a temperature of utilizing 180 DEG C of hydro-thermal method 130 DEG C in the reactor for have polytetrafluoroethyllining lining, nickel cobalt organic/inorganic composite material is obtained.The nickel cobalt organic/inorganic composite material that will be obtained after drying is with NaH2PO2It is placed in tube furnace together, the two is separated with silica wool, under Ar protections, reacts 2 5h at 300 DEG C 350 DEG C and just obtain product, the product utilization deionized water that will be obtained after phosphatization obtains nanoscale Ni with absolute ethyl alcohol cross washing 5 times, centrifugation2The granular size of P CoP double-metal phosphides is 10 20nm.Obtained material is used for catalytic electrolysis elutriation hydrogen with electrolysis elutriation oxygen, the catalyst is than single Ni2P、CoP、Ni2Electricity of the P+CoP according to a certain ratio obtained by mechanical mixture urges the activity of agent will to get well, and possesses good application prospect.

Description

For the bifunctional catalyst nanoscale Ni of electrolysis water2P-CoP double-metal phosphides
Technical field
The present invention relates to a kind of nickel cobalt double-metal phosphide Ni2P-CoP elctro-catalysts, the synthetic method of the catalyst and its In the difunctional application that electrolysis water liberation of hydrogen is catalyzed with electrolysis elutriation oxygen.
Background technology
Transition metal phosphide is the elctro-catalyst of a kind of very important electrolysis water liberation of hydrogen and analysis oxygen.Transition metal phosphatization It is thing nano material rich reserves, cheap, and according to reporting that this kind of elctro-catalyst has activity well.Bimetallic phosphatization Thing has more excellent performance than monometallic phosphide, and this is due to intermetallic synergy, so it is expensive to become replacement The ideal material of metal elctro-catalyst.
The pattern of transition metal phosphide, size, composition have significant impact to its electro catalytic activity, are first closed in the present invention Into the organic-inorganic composition material containing nickel cobalt element, be then obtained by phosphating reaction have excellent electrolysis water liberation of hydrogen with Analyse the bifunctional electrocatalyst Ni of the catalysis activity of oxygen2P-CoP.The catalyst is than single Ni2P、CoP、Ni2P+CoP is according to one Surely the electricity obtained by proportioning mechanical mixture urges the activity of agent will to get well.Tian Tian, Lunhong Ai, Jing Jiang (RSC Adv., 2015,5,10290-10295) organic-inorganic metal framework material by the use of nickel is reported as presoma by phosphatization Ni is synthesized2P, the catalyst has good electrolysis water hydrogen evolution activity.Shaofang Fu, Yuehe (ACS EnergyLett.2016,1,792-796) the nickel cobalt bimetallic with non-uniform topographical with size has been synthesized using hard mould agent method Phosphide, and the catalyst illustrates excellent electro catalytic activity in electrolysis water oxygen evolution reaction.In conventional report, metal phosphorus Compound is all as the electrolysis water catalyst of simple function, i.e., for being electrolysed elutriation oxygen or for electrolysis water liberation of hydrogen, and this hair Ni in bright2P-CoP is used not only for electrolysis water liberation of hydrogen, and can be used in being electrolysed elutriation oxygen.
The content of the invention
It is an object of the invention to provide a kind of bifunctional catalyst Ni nanoparticle for electrolysis water2P-CoP bimetallic phosphorus Compound.The composite organic-inorganic material of the nickel cobalt of solvent structure ball top shape is utilized in dynamic kettle, then in tube furnace Protected using Ar, NaH2PO2Nickel cobalt composite organic-inorganic material phosphatization is obtained granular nickel cobalt bimetallic phosphorus as phosphorus source Compound Ni2P-CoP, and the nickel cobalt metal phosphide for preparing can have excellent in electrolysis water liberation of hydrogen is with two reactions of analysis oxygen Electro catalytic activity.
Above-mentioned purpose of the invention is obtained by the following technical programs：
For the bifunctional catalyst nanoscale Ni of electrolysis water2The synthetic method of P-CoP double-metal phosphides, its feature exists In first with solvent structure nickel cobalt composite organic-inorganic material, NaH2PO2As phosphorus source reduction, entered phosphorus in tube furnace Change reaction to be made, comprise the steps of：
Step 1：By four water cobalt acetates, nickel acetylacetonate, terephthalic acid (TPA), polyvinylpyrrolidone, four kinds of materials of the above Mass ratio be 5:5:1:8, water is dissolved in in the mixed solution of DMF, mixed solution reclaimed water is with N, N- bis- The volume ratio of NMF is 3:5.Magnetic agitation obtains well mixed solution, and above-mentioned solution is transferred to equipped with polytetrafluoro In the dynamic response kettle of ethene liner；
Step 2：By dynamic response kettle good seal, 6-8h is reacted at a temperature of 130 DEG C -170 DEG C, obtain nickel cobalt it is organic-nothing Machine composite, by product with deionized water with being done in DMF cross washing, centrifugation, 60 DEG C of baking ovens It is dry.
Step 3：The nickel cobalt composite organic-inorganic material that will be obtained after drying is with NaH2PO2It is placed in tube furnace together, The mass ratio of the two is 1:5, both are separated using silica wool, reacting 2-4h under Ar protections, at 300 DEG C -350 DEG C just obtains Product, the product utilization deionized water that will be obtained after phosphatization in absolute ethyl alcohol cross washing, centrifugation, 60 DEG C of baking ovens with being done It is dry.
Further, described preparation method, must be intersected with water when washed product with DMF Washing 3 to 5 times.Centrifugation can obtain product under 6000r/min-8000r/min.
Further：In the product after washing phosphatization must with absolute ethyl alcohol with deionized water cross washing 5 times, and Being centrifuged under the conditions of 8000r/min-10000r/min can just obtain product.
The synthetic technology process is simple that the present invention is used, the product morphology for arriving of reaction is uniform, and size is small, has in ethanol There is good dispersiveness.To benzene, dioctyl phthalate is acting as part.Polyvinylpyrrolidone is surfactant, can make product The pattern of formation rule, will not form big reunion.NaH2PO2As phosphorus source, reducibility gas H is produced at high temperature3P, by nickel Cobalt composite organic-inorganic material is reduced to nanoscale Ni2P-CoP double-metal phosphides.Under Ar protections, have nickel cobalt under high temperature Organo-functional group in machine-inorganic composite materials is changed into carbon, in can increasing the electric conductivity of elctro-catalyst and not making product There is oxide impurity.
Brief description of the drawings
Fig. 1 is the TEM figures of the nickel cobalt composite organic-inorganic material obtained by embodiment.
Fig. 2 is the SEM figures of the nickel cobalt composite organic-inorganic material obtained by embodiment.
Fig. 3 is the FT-IR collection of illustrative plates of the nickel cobalt composite organic-inorganic material obtained by embodiment.
Fig. 4 is the nanoscale Ni obtained by implementation2The TEM figures of P-CoP double-metal phosphides.
Fig. 5 is the nanoscale Ni obtained by implementation2The XRD spectrum of P-CoP double-metal phosphides.
Fig. 6 is the nanoscale Ni obtained by implementation2The LSV collection of illustrative plates of the electrolysis water liberation of hydrogen of P-CoP double-metal phosphides.
Fig. 7 is the nanoscale Ni obtained by implementation2The Tafel collection of illustrative plates of the electrolysis water liberation of hydrogen of P-CoP double-metal phosphides.
Fig. 8 is the nanoscale Ni obtained by implementation2The LSV collection of illustrative plates of the electrolysis elutriation oxygen of P-CoP double-metal phosphides
Fig. 9 is the nanoscale Ni obtained by implementation2The Tafel collection of illustrative plates of the electrolysis elutriation oxygen of P-CoP double-metal phosphides
Specific embodiment
Product prepared by the present invention, its microscopic appearance is determined by transmission electron microscope (TEM), the surface topography of material by SEM (SEM) is determined, and metal ion is surveyed with the coordination situation of part by Fourier infrared absorption spectrum (FT-IR) Fixed, the crystal structure of material is determined by X-ray diffractometer (XRD), and the catalysis activity of electrolysis water liberation of hydrogen and analysis oxygen is in Shanghai morning China Measured on electrochemical workstation.
Embodiment
(1) by 100mg nickel acetylacetonates, the water cobalt acetates of 100mg tetra-, 400mg polyvinylpyrrolidones (Mw=30000), 50mg terephthalic acid (TPA)s are put into 80mL water with (volume ratio V1 in the mixed solution of N,N-dimethylformamide:V2=3:5), magnetic force Stirring 20min, is well mixed；Above-mentioned solution is transferred in the dynamic response kettle equipped with polytetrafluoroethyllining lining.
(2) by dynamic response kettle good seal, 6h is reacted at a temperature of 150 DEG C, obtains nickel cobalt composite organic-inorganic material, Question response is cooled to room temperature, by product deionized water with DMF cross washing 3 times, 7400r/min from 24h is dried in the heart, 60 DEG C of baking ovens, yellowish powdered nickel cobalt composite organic-inorganic material is obtained.
(3) the nickel cobalt composite organic-inorganic material that will be obtained after drying is with NaH2PO2It is placed in tube furnace together, NaH2PO2It is 5 with the mass ratio of nickel cobalt composite organic-inorganic material:1, the two is separated using silica wool, under Ar protections, from room Heated up at 20 DEG C of temperature, heating rate is 2 DEG C/min, 3h is reacted at 350 DEG C and just obtains product.The product utilization that will be obtained after phosphatization Deionized water obtains receiving for black with drying 12h in absolute ethyl alcohol cross washing 5 times, 8500r/min centrifugations 6min, 60 DEG C of baking ovens Meter level Ni2P-CoP double-metal phosphides.
The activity rating method of elctro-catalyst：Electrolysis water liberation of hydrogen is with oxygen evolution reaction
Electro catalytic activity is determined using CHI660e types electrochemical workstation.Electrolysis water Hydrogen Evolution Performance test electrolyte be 0.5M H2SO4.In order to ensure the H in electrolyte2Content is in saturation state, is needed during test constantly to electrolyte In be passed through the H of high-purity2.Test uses three-electrode system, i.e. working electrode, reference electrode and to electrode.Working electrode Be glass carbon rotation electrode, calomel electrode be reference electrode, be to electrode with carbon-point.In electrolysis elutriation oxygen performance evaluation, use It is also CHI660e type electrochemical workstations, electrolyte is 0.1M KOH；Test is also working electrode, reference electrode and to electrode The three-electrode system of composition, equally with calomel electrode as reference electrode, but uses Pt to electrode.In order to ensure electrolysis O in liquid2Content is in saturation state, will be constantly to the O that high-purity is passed through in electrolyte in test process2.The system of working electrode It is standby：Take the nanoscale Ni of 5mg2P-CoP double-metal phosphides, 2mg electrically conductive graphites add 1mL absolute ethyl alcohols, the 5wt% of 25 μ L Nafion, ultrasound about 30min obtains well mixed solution.The catalyst solution for measuring 10 μ L with liquid-transfering gun is uniformly dripped to On rotary glass carbon electrode, treat that it is spontaneously dried, effective work area of working electrode is 0.196cm2.It is anti-in electrolysis water liberation of hydrogen Active testing is answered, linear volt-ampere curve (during LSV), sweep limits is -0.3V--0.6V, and sweep speed is 5mV/s, experiment Obtain in 10mA/cm2When overpotential be 121mV, and the material Tafel slopes be 56mV/dev；It is anti-in electrolysis elutriation oxygen Active testing is answered, when surveying LSV curves, sweep limits is 0.2V -0.8V, and sweep speed is 5mV/s, and experiment is obtained in 10mA/ cm2When overpotential be 320mV, and the material Tafel slopes be 69mV/dev.

Claims (3)

1. the bifunctional catalyst nanoscale Ni of electrolysis water is used for2The synthetic method of P-CoP double-metal phosphides, it is characterised in that Comprise the steps of：
Step 1：By four water cobalt acetates, nickel acetylacetonate, terephthalic acid (TPA), polyvinylpyrrolidone, four kinds of matter of material of the above Amount is than being 5:5:1:8, water is dissolved in in the mixed solution of DMF, mixed solution reclaimed water is with N, N- dimethyl The volume ratio of formamide is 3:5；Magnetic agitation obtains well mixed solution, and above-mentioned solution is transferred to equipped with polytetrafluoroethylene (PTFE) In the dynamic response kettle of liner；
Step 2：By dynamic response kettle good seal, 6-8h is reacted at a temperature of 130 DEG C -170 DEG C, obtain nickel cobalt organic and inorganic and answer Condensation material, by product deionized water with being dried in DMF cross washing, centrifugation, 60 DEG C of baking ovens；
Step 3：The nickel cobalt composite organic-inorganic material that will be obtained after drying is with NaH2PO2It is placed in tube furnace together, the two Mass ratio be 1:5, both are separated using silica wool, react 2-4h under Ar protections, at 300 DEG C -350 DEG C and just produced Thing, the product utilization deionized water that will be obtained after phosphatization in absolute ethyl alcohol cross washing, centrifugation, 60 DEG C of baking ovens with being dried.
2. synthetic method according to claim 1, it is characterised in that water must be used in step 2 when washed product With DMF cross washing 3 to 5 times, centrifugation can obtain product under 6000r/min-8000r/min.
3. synthetic method according to claim 1, it is characterised in that certain in the product after washing phosphatization in step 3 With absolute ethyl alcohol with deionized water cross washing 5 times, and it is centrifuged under the conditions of 8000r/min-10000r/min and can be just obtained Product.
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CN107252700A (en) * 2017-06-26 2017-10-17 中国石油大学(华东) A kind of catalytic center equally distributed many metal phosphide nano tube catalysts and low temperature preparation method
CN107416785A (en) * 2017-07-20 2017-12-01 中北大学 Flower-shaped CoP3/Ni2The preparation method and application of P nano hybrids
CN107723735A (en) * 2017-09-27 2018-02-23 中国科学院长春应用化学研究所 A kind of nano metal simple substance and its modified oxide transient metal sulfide array catalyst and its preparation method and application
CN107737604A (en) * 2017-11-21 2018-02-27 宁波科邦华诚技术转移服务有限公司 A kind of preparation method of nano level metal phosphide composite photo-catalyst
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CN108383093A (en) * 2018-05-11 2018-08-10 西北师范大学 A kind of preparation and application of double-metal phosphide carbon nano tube compound material
CN109055975A (en) * 2018-08-01 2018-12-21 北京工业大学 One kind preparing porous Ni based on two-dimensional metallic organic backbone template2The method of P/C electrode
CN109395752A (en) * 2018-06-20 2019-03-01 长沙理工大学 A kind of self-supporting double-metal phosphide Ni2P-Cu3P composite material and preparation method
CN109621995A (en) * 2018-12-28 2019-04-16 华北电力大学（保定） A kind of phosphatization cobalt nanowire electrolysis aquatic products hydrogen catalyst and preparation method thereof
CN109626346A (en) * 2019-02-01 2019-04-16 广西民族大学 A kind of core-shell structure CoP-Ni2The preparation method of P nanometer rods
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CN109999861A (en) * 2019-03-06 2019-07-12 江苏大学 A kind of nickel cobalt double-metal phosphide elctro-catalyst and its synthetic method and application
CN110026215A (en) * 2018-05-30 2019-07-19 南方科技大学 Three-dimensional porous nano catalyst and preparation method thereof
CN110038602A (en) * 2019-04-30 2019-07-23 哈尔滨工业大学 A kind of preparation method and applications of double-metal phosphide
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CN110182775A (en) * 2019-06-17 2019-08-30 贵阳学院 Using metal organic frame as the preparation method of the bimetallic phosphorus compound of template and obtained bimetallic phosphorus compound and its application
CN110280316A (en) * 2019-07-11 2019-09-27 广东工业大学 A kind of metal phosphide and its preparation method and application based on MOF gel
CN110639565A (en) * 2018-06-27 2020-01-03 北京印刷学院 Carbon-bimetal phosphide composite material and preparation method thereof
CN111111716A (en) * 2020-01-19 2020-05-08 西北师范大学 Preparation and application of nickel-cobalt double-metal phosphide guided by MOF
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CN109999861A (en) * 2019-03-06 2019-07-12 江苏大学 A kind of nickel cobalt double-metal phosphide elctro-catalyst and its synthetic method and application
CN110038602A (en) * 2019-04-30 2019-07-23 哈尔滨工业大学 A kind of preparation method and applications of double-metal phosphide
CN110152708A (en) * 2019-05-27 2019-08-23 安徽理工大学 A kind of hollow open-celled structure Ferrious material phosphide and preparation method thereof, application
CN110152708B (en) * 2019-05-27 2022-02-11 安徽理工大学 Hollow open-pore structure iron series metal phosphide and preparation method and application thereof
CN110182775A (en) * 2019-06-17 2019-08-30 贵阳学院 Using metal organic frame as the preparation method of the bimetallic phosphorus compound of template and obtained bimetallic phosphorus compound and its application
CN110280316A (en) * 2019-07-11 2019-09-27 广东工业大学 A kind of metal phosphide and its preparation method and application based on MOF gel
CN111111716A (en) * 2020-01-19 2020-05-08 西北师范大学 Preparation and application of nickel-cobalt double-metal phosphide guided by MOF
CN111111716B (en) * 2020-01-19 2022-10-18 西北师范大学 Preparation and application of nickel-cobalt double-metal phosphide guided by MOF
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CN111468150A (en) * 2020-05-26 2020-07-31 陕西科技大学 Fullerene nanorod/transition metal phosphide electrocatalyst and preparation method thereof
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CN113699536B (en) * 2021-07-26 2022-12-23 安徽理工大学 Metal phosphide electrocatalyst based on MOF derivation, preparation method and application
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