CN107497444A - A kind of preparation method of nickel vanadium dual metal hydroxide nano chip arrays water oxidation catalyst - Google Patents

A kind of preparation method of nickel vanadium dual metal hydroxide nano chip arrays water oxidation catalyst Download PDF

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CN107497444A
CN107497444A CN201710613610.2A CN201710613610A CN107497444A CN 107497444 A CN107497444 A CN 107497444A CN 201710613610 A CN201710613610 A CN 201710613610A CN 107497444 A CN107497444 A CN 107497444A
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nickel
reaction
chip arrays
foam
product
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黄剑锋
刘倩倩
冯亮亮
曹丽云
吴建鹏
杨丹
何元元
席乔
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Shaanxi University of Science and Technology
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    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/847—Vanadium, niobium or tantalum or polonium
    • B01J23/8472—Vanadium
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    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
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    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
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    • B01J35/33—Electric or magnetic properties
    • 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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08—Heat treatment
    • B01J37/10—Heat treatment in the presence of water, e.g. steam
    • 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
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    • C25B1/02—Hydrogen or oxygen
    • C25B1/04—Hydrogen or oxygen by electrolysis of water
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    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
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    • C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
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Abstract

A kind of preparation method of nickel vanadium dual metal hydroxide nano chip arrays water oxidation catalyst, nickel foam is immersed in pure acetone solution and is cleaned by ultrasonic, nickel foam is immersed in hydrochloric acid be cleaned by ultrasonic again, finally replaced respectively with ethanol with deionized water and rinsed well, the nickel foam after finally vacuum drying is handled；By NiCl2·6H2O、VCl3With Co (NH2)2It is added to simultaneously in deionized water and obtains settled solution A；Nickel foam is put into reaction liner, sealed after solution A is poured into reaction liner again, then liner is loaded in outer kettle after fixing and be placed in homogeneous reaction instrument, room temperature is naturally cooled to after carrying out hydro-thermal reaction, then the foam nickel product cooled down after reaction is taken out, product is collected by washing to wash after alternating cleans up with alcohol, product vacuum is dried to obtain NiV LDH nano-chip arrays.Product chemistry composition prepared by the present invention is homogeneous, and purity is high, and pattern is uniform, and excellent chemical property can be shown when it is as electrolysis water electrode material.

Description

A kind of preparation of nickel vanadium dual metal hydroxide nano chip arrays water oxidation catalyst Method
Technical field
The invention belongs to field of inorganic material preparing technology, is related to photoelectric semiconductor material and prepares and apply, and in particular to a kind of nickel The preparation method of vanadium dual metal hydroxide nano chip arrays water oxidation catalyst.
Background technology
Electrocatalytic decomposition water technology is one of effective way of hydrogen and oxygen production, is one and develops sustainable clean energy resource most Potential technology.During water decomposition, water oxygen is the ratedeterming step in water splitting processes, restricts the whole of water-splitting Process, thus seek the emphasis that a kind of elctro-catalyst of efficient-decomposition water is numerous researcher's concerns at present.Hydrotalcite is also known as Layered double hydroxide (1ayered double hydroxides, LDHs), is a kind of anion type laminated compound, Because it has unique two-dimentional veneer structure, a composition adjustability, interlayer ion interchangeability, the features such as memory effect, as Water oxidation reaction catalyst is more and more paid close attention to by researcher.
It has recently been demonstrated that the structure of the material based on nickel can effectively improve OER performance, meanwhile, vanadium Valence state flexibly (+3 ,+4 ,+5), there is good reactivity, can be effective in addition, catalyst is combined with conductive substrates Ground promotes electric charge transmission, and can significantly strengthen its catalytic activity and stability.
At present, the nickel-vanadium layer shape double-metal hydroxide prepared by the methods of hydro-thermal method, coprecipitation proposed both at home and abroad Pattern include：Lamella accordion, graininess etc..Chinese invention issued patents the 201610060321.Xth disclose a kind of nickel The preparation method of vanadium hydrotalcite/carbon composite, is made using coprecipitation, its complex steps, requires high to atmosphere etc., technology Difficulty is big.Nickel-Based Layered Double Hydroxide From Guest Vanadium Oxide Ni V-LDH are prepared using coprecipitation in Anions.Hae Woong Park et al., its product skewness, and prepare Complex process.The preparation of nickel vanadium hydrotalcite and its carbon composite and electrochemical capacitance performance study, Chu little Yan is using co-precipitation legal system It is standby go out different nickel vanadium ions than nickel vanadium hydrotalcite, but its preparation technology is complicated, and product morphology is irregular.
The content of the invention
It is an object of the invention to provide a kind of simple to operate, reaction condition is gentle, takes short, the product purity of preparation The preparation method of the nickel vanadium dual metal hydroxide nano chip arrays water oxidation catalyst of height, pattern and size uniformity, it is prepared Material be effectively improved stability of the vanadium-based materials in alkali lye, so as to effectively improve electrolysis elutriation oxygen performance.
To reach above-mentioned purpose, the technical solution adopted by the present invention is：
1) 2 × 5cm nickel foam is immersed in pure acetone solution and is cleaned by ultrasonic, nickel foam is immersed in 2~4mol/L again Hydrochloric acid in be cleaned by ultrasonic, finally replaced respectively with ethanol with deionized water and rinsed well, finally vacuum drying obtain processing after Nickel foam；
2) (2~4) are pressed:(0.5~2):The mol ratio of (5~7) takes NiCl26H2O、VCl3With Co (NH2)2Add simultaneously The concentration for making nickel source into deionized water is (0.05~0.2) mol/L, and magnetic agitation obtains settled solution A at room temperature；
3) nickel foam for handling step 1) well is put into reaction liner, then is sealed after solution A is poured into reaction liner, Reaction-filling ratio should be controlled 20~80%, then by liner be loaded in outer kettle it is fixed after be placed in homogeneous reaction instrument, then Hydro-thermal reaction is carried out at 90~150 DEG C；
4) hydro-thermal reaction terminates, and reactor is naturally cooled into room temperature, then takes the foam nickel product cooled down after reaction Go out, collect product by washing to wash after alternating cleans up with alcohol, product vacuum is dried to obtain NiV-LDH nano-chip arrays.
The ultrasonic cleaning time of the step 1) is 5~15min.
The vacuum drying of the step 1) is 10~14h of vacuum drying at 25~35 DEG C.
The vacuum drying of the step 4) is 10~14h of vacuum drying at 25~35 DEG C.
Beneficial effect：
(1) because the present invention using a step hydro-thermal reaction directly synthesizes final product, thus there is low synthesis temperature Degree, simple synthesis path, it is not necessary to large scale equipment and harsh reaction condition, raw material is cheap and easy to get, and cost is low, and yield is high, It is environmentally friendly without post-processing, it can be adapted to mass produce.
(2) NiV-LDH nanometer lengths of a film prepared by this method form the nano-chip arrays of rule in foam nickel base, Its nanometer sheet thickness is about 15~25nm.This nano-chip arrays are very beneficial for freeing in and out for ion, while also have very much Beneficial to fully contacting for electrolyte and NiV-LDH nano-chip arrays, its chemical property can be then greatly enhanced.
(3) the product chemistry composition that prepared by this method is homogeneous, and purity is high, and pattern is uniform, and it is as electrolysis water electrode material When can show excellent chemical property, in 10mA/cm-2Current density under, its overpotential is about 206mV, and Under 0.35V voltage, 5h stability can be at least kept.
Brief description of the drawings
Fig. 1 is the X-ray diffraction of the NiV-LDH nano-chip arrays being grown in nickel foam prepared by the embodiment of the present invention 3 (XRD) collection of illustrative plates；
Fig. 2 is the ESEM of the NiV-LDH nano-chip arrays being grown in nickel foam prepared by the embodiment of the present invention 3 (SEM) photo.
Fig. 3 is the linear scan volt of the NiV-LDH nano-chip arrays being grown in nickel foam prepared by the embodiment of the present invention 3 Pacify (LSV) performance test figure.
Embodiment
Below in conjunction with the accompanying drawings and specific embodiment is described in further detail to the present invention.
Embodiment 1：
1) 2 × 5cm nickel foam is immersed in pure acetone solution and is cleaned by ultrasonic 10min, then nickel foam is immersed in 2mol/ It is cleaned by ultrasonic in L hydrochloric acid, is finally replaced respectively with ethanol with deionized water and rinsed well, is finally dried in vacuo at 25 DEG C 10h handled after nickel foam；
2) 2 are pressed：0.5：5 mol ratio takes NiCl2·6H2O、VCl3With Co (NH2)2Being added to simultaneously in deionized water makes nickel The concentration in source is 0.1mol/L, and magnetic agitation obtains settled solution A at room temperature；
3) nickel foam for handling step 1) well is put into reaction liner, then is sealed after solution A is poured into reaction liner, Reaction-filling ratio should be controlled 20%, then by liner loaded on being placed in after being fixed in outer kettle in homogeneous reaction instrument, then 90 Hydro-thermal reaction is carried out at DEG C；
4) hydro-thermal reaction terminates, and reactor is naturally cooled into room temperature, then takes the foam nickel product cooled down after reaction Go out, collect product by washing to wash after alternating cleans up with alcohol, product is dried in vacuo into 14h at 25 DEG C obtains NiV-LDH Nano-chip arrays.
Embodiment 2：
1) 2 × 5cm nickel foam is immersed in pure acetone solution and is cleaned by ultrasonic 10min, then nickel foam is immersed in 3mol/ It is cleaned by ultrasonic in L hydrochloric acid, is finally replaced respectively with ethanol with deionized water and rinsed well, is finally dried in vacuo at 25 DEG C 12h handled after nickel foam；
2) 2.5 are pressed：1：5.5 mol ratio takes NiCl2·6H2O、VCl3With Co (NH2)2Being added to simultaneously in deionized water makes The concentration of nickel source is 0.15mol/L, and magnetic agitation obtains settled solution A at room temperature；
3) nickel foam for handling step 1) well is put into reaction liner, then is sealed after solution A is poured into reaction liner, Reaction-filling ratio should be controlled 50%, then by liner loaded on being placed in after being fixed in outer kettle in homogeneous reaction instrument, then 110 Hydro-thermal reaction is carried out at DEG C；
4) hydro-thermal reaction terminates, and reactor is naturally cooled into room temperature, then takes the foam nickel product cooled down after reaction Go out, collect product by washing to wash after alternating cleans up with alcohol, product is dried in vacuo into 12h at 30 DEG C obtains NiV-LDH Nano-chip arrays.
Embodiment 3：
1) 2 × 5cm nickel foam is immersed in pure acetone solution and is cleaned by ultrasonic 10min, then nickel foam is immersed in 3mol/ It is cleaned by ultrasonic in L hydrochloric acid, is finally replaced respectively with ethanol with deionized water and rinsed well, is finally dried in vacuo at 25 DEG C 12h handled after nickel foam；
2) 3 are pressed：1.5：6 mol ratio takes NiCl2·6H2O、VCl3With Co (NH2)2Being added to simultaneously in deionized water makes nickel The concentration in source is 0.2mol/L, and magnetic agitation obtains settled solution A at room temperature；
3) nickel foam for handling step 1) well is put into reaction liner, then is sealed after solution A is poured into reaction liner, Reaction-filling ratio should be controlled 60%, then by liner loaded on being placed in after being fixed in outer kettle in homogeneous reaction instrument, then 130 Hydro-thermal reaction is carried out at DEG C；
4) hydro-thermal reaction terminates, and reactor is naturally cooled into room temperature, then takes the foam nickel product cooled down after reaction Go out, collect product by washing to wash after alternating cleans up with alcohol, product is dried in vacuo into 12h at 30 DEG C obtains NiV-LDH Nano-chip arrays.
NiV-LDH nano-chip arrays manufactured in the present embodiment, as can be seen from Figure 1 length has gone up material in nickel foam, and And the sample angle of diffraction be 9.5 °, 21.7 °, 35.2 ° occur respectively (003), (006), (009) crystal face diffraction maximum, It is the nickel vanadium dual metal hydroxide with hydrotalcite structure to illustrate product.
It is to be grown in nano-chip arrays in nickel foam from the pattern of Fig. 2 SEM it can be seen from the figure thats samples, and nanometer sheet Thickness be about 20nm.
From Fig. 3 linear sweep voltammetry it can be seen from the figure that, the sample is 10mA/cm in current density2When, it excessively electric Gesture is 206mV, is 100mA/cm in current density2When, its overpotential is 440mV.With good electro-catalysis oxygen evolution activity.
Embodiment 4：
1) 2 × 5cm nickel foam is immersed in pure acetone solution and is cleaned by ultrasonic 15min, then nickel foam is immersed in 4mol/ It is cleaned by ultrasonic in L hydrochloric acid, is finally replaced respectively with ethanol with deionized water and rinsed well, is finally dried in vacuo at 35 DEG C 14h handled after nickel foam；
2) 3.5 are pressed：2：6.5 mol ratio takes NiCl2·6H2O、VCl3With Co (NH2)2Being added to simultaneously in deionized water makes The concentration of nickel source is 0.05mol/L, and magnetic agitation obtains settled solution A at room temperature；
3) nickel foam for handling step 1) well is put into reaction liner, then is sealed after solution A is poured into reaction liner, Reaction-filling ratio should be controlled 80%, then by liner loaded on being placed in after being fixed in outer kettle in homogeneous reaction instrument, then 150 Hydro-thermal reaction is carried out at DEG C；
4) hydro-thermal reaction terminates, and reactor is naturally cooled into room temperature, then takes the foam nickel product cooled down after reaction Go out, collect product by washing to wash after alternating cleans up with alcohol, product is dried in vacuo into 12h at 30 DEG C obtains NiV-LDH Nano-chip arrays.
Embodiment 5：
1) 2 × 5cm nickel foam is immersed in pure acetone solution and is cleaned by ultrasonic 5min, then nickel foam is immersed in It is cleaned by ultrasonic in 2.5mol/L hydrochloric acid, is finally replaced respectively with ethanol with deionized water and rinsed well, it is finally true at 30 DEG C Sky dries the nickel foam after 13h is handled；
2) 4 are pressed：2：7 mol ratio takes NiCl2·6H2O、VCl3With Co (NH2)2Being added to simultaneously in deionized water makes nickel source Concentration be 0.13mol/L, magnetic agitation obtains settled solution A at room temperature；
3) nickel foam for handling step 1) well is put into reaction liner, then is sealed after solution A is poured into reaction liner, Reaction-filling ratio should be controlled 40%, then by liner loaded on being placed in after being fixed in outer kettle in homogeneous reaction instrument, then 100 Hydro-thermal reaction is carried out at DEG C；
4) hydro-thermal reaction terminates, and reactor is naturally cooled into room temperature, then takes the foam nickel product cooled down after reaction Go out, collect product by washing to wash after alternating cleans up with alcohol, product is dried in vacuo into 10h at 35 DEG C obtains NiV-LDH Nano-chip arrays.
Embodiment 6：
1) 2 × 5cm nickel foam is immersed in pure acetone solution and is cleaned by ultrasonic 12min, then nickel foam is immersed in It is cleaned by ultrasonic in 3.5mol/L hydrochloric acid, is finally replaced respectively with ethanol with deionized water and rinsed well, it is finally true at 32 DEG C Sky dries the nickel foam after 11h is handled；
2) 3 are pressed：1.5：6 mol ratio takes NiCl2·6H2O、VCl3With Co (NH2)2Being added to simultaneously in deionized water makes nickel The concentration in source is 0.18mol/L, and magnetic agitation obtains settled solution A at room temperature；
3) nickel foam for handling step 1) well is put into reaction liner, then is sealed after solution A is poured into reaction liner, Reaction-filling ratio should be controlled 70%, then by liner loaded on being placed in after being fixed in outer kettle in homogeneous reaction instrument, then 120 Hydro-thermal reaction is carried out at DEG C；
4) hydro-thermal reaction terminates, and reactor is naturally cooled into room temperature, then takes the foam nickel product cooled down after reaction Go out, collect product by washing to wash after alternating cleans up with alcohol, product is dried in vacuo into 11h at 32 DEG C obtains NiV-LDH Nano-chip arrays.

Claims (4)

  1. A kind of 1. preparation method of nickel vanadium dual metal hydroxide nano chip arrays water oxidation catalyst, it is characterised in that including with Lower step：
    1) 2 × 5cm nickel foam is immersed into ultrasonic cleaning in pure acetone solution, nickel foam is immersed in 2~4mol/L salt again It is cleaned by ultrasonic in acid, is finally replaced respectively with ethanol with deionized water and rinsed well, the bubble after finally vacuum drying is handled Foam nickel；
    2) (2~4) are pressed:(0.5~2):The mol ratio of (5~7) takes NiCl2·6H2O、VCl3With Co (NH2)2It is added to simultaneously The concentration for making nickel source in ionized water is (0.05~0.2) mol/L, and magnetic agitation obtains settled solution A at room temperature；
    3) nickel foam for handling step 1) well is put into reaction liner, then is sealed after solution A is poured into reaction liner, reaction Packing ratio control is 20~80%, then by liner loaded on being placed in after being fixed in outer kettle in homogeneous reaction instrument, then 90~150 Hydro-thermal reaction is carried out at DEG C；
    4) hydro-thermal reaction terminates, and reactor is naturally cooled into room temperature, then takes out the foam nickel product cooled down after reaction, warp Cross washing and alcohol is washed after alternately cleaning up and collects product, product vacuum is dried to obtain NiV-LDH nano-chip arrays.
  2. 2. the preparation method of nickel vanadium dual metal hydroxide nano chip arrays water oxidation catalyst according to claim 1, It is characterized in that：The ultrasonic cleaning time of the step 1) is 5~15min.
  3. 3. the preparation method of nickel vanadium dual metal hydroxide nano chip arrays water oxidation catalyst according to claim 1, It is characterized in that：The vacuum drying of the step 1) is 10~14h of vacuum drying at 25~35 DEG C.
  4. 4. the preparation method of nickel vanadium dual metal hydroxide nano chip arrays water oxidation catalyst according to claim 1, It is characterized in that：The vacuum drying of the step 4) is 10~14h of vacuum drying at 25~35 DEG C.
CN201710613610.2A 2017-07-25 2017-07-25 A kind of preparation method of nickel vanadium dual metal hydroxide nano chip arrays water oxidation catalyst Pending CN107497444A (en)

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CN111013618A (en) * 2019-12-26 2020-04-17 景德镇陶瓷大学 Phosphorus-doped cobalt-iron-vanadium trimetal catalyst and preparation method thereof
CN111097423A (en) * 2020-01-13 2020-05-05 哈尔滨工业大学 Nickel-based layered double-metal hydroxide nanosheet and room-temperature rapid green preparation method and application thereof
CN112877729A (en) * 2021-01-14 2021-06-01 辽宁大学 NiMn-LDH nanosheet loaded on foamed nickel, preparation method thereof and application of NiMn-LDH nanosheet in electrocatalytic oxidation of benzylamine
CN113481535A (en) * 2021-06-18 2021-10-08 常州工学院 Iron-nickel-vanadium double metal hydroxide and preparation method and application thereof

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CN110560065B (en) * 2019-08-23 2022-08-05 万华化学集团股份有限公司 Metal carrier supported catalyst, preparation method and application thereof in preparation of m-xylylenediamine
CN110777393A (en) * 2019-11-05 2020-02-11 陕西科技大学 Nickel-vanadium double metal hydroxide electrode for wide-range full-hydrolysis and preparation method and application thereof
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Application publication date: 20171222