CN109201038A - A kind of V2O3/VO2Composite electrocatalyst and preparation method thereof - Google Patents

A kind of V2O3/VO2Composite electrocatalyst and preparation method thereof Download PDF

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CN109201038A
CN109201038A CN201811272287.8A CN201811272287A CN109201038A CN 109201038 A CN109201038 A CN 109201038A CN 201811272287 A CN201811272287 A CN 201811272287A CN 109201038 A CN109201038 A CN 109201038A
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nac
reaction
solution
composite electrocatalyst
preparation
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CN109201038B (en
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黄剑锋
徐瑞
冯亮亮
曹丽云
张宁
王琳琳
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Shaanxi University of Science and 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/20—Vanadium, niobium or tantalum
    • B01J23/22—Vanadium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
    • C01B3/042—Decomposition of water
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/02—Processes for making hydrogen or synthesis gas
    • C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
    • C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/10—Catalysts for performing the hydrogen forming reactions
    • C01B2203/1041—Composition of the catalyst
    • 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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  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Combustion & Propulsion (AREA)
  • Inorganic Chemistry (AREA)
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  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The present invention provides a kind of V2O3/VO2Composite electrocatalyst is prepared by following methods: by NH4VO3Aqueous solution, with the aqueous solution of N-acetyl-L-cysteine (NAC), according to NH4VO3: the molar ratio of NAC is (1 ~ 4): after (3 ~ 7) mix and are uniformly dispersed, 170 ~ 220 DEG C of progress hydro-thermal reactions obtain V2O3/VO2Composite electrocatalyst.This method directly synthesizes final product using a step hydro-thermal reaction, has low synthesis temperature, and simple process is easy to operate, and raw material is cheap and easy to get, at low cost, and yield is high, is not necessarily to post-processing, environmentally friendly, can be suitble to be mass produced；Product chemistry composition is uniform, and purity is high, pattern is uniform, and the water-splitting that can be applied in electro-catalysis field produces hydrogen elctro-catalyst.

Description

A kind of V2O3/VO2Composite electrocatalyst and preparation method thereof
Technical field
Water-splitting of the present invention produces hydrogen elctro-catalyst technical field, and in particular to a kind of V2O3/VO2Composite electrocatalyst and its Preparation method.
Background technique
Vanadium is typical multivalent state element, and there are various various forms of oxides.A variety of oxidation state of vanadium oxygen system and Coordination polyhedrom property allows it to insertion organic group or metal ion, and the characteristic with thermal induced phase transition.Common vanadium oxygen Compound, such as V2O5, VO2, V2O3, due to special property and potential application of force, so that they are in industry, ceramics, the neck such as energy Domain occupies an important position.
Powder body material is VO2And V2O3A kind of main material of material, it can not only be used to prepare ceramic material, can also To be used to prepare thin-film material, polymer composite and as catalyst material.
Currently, about VO2And V2O3The report of elctro-catalyst is very limited, and this patent passes through simple one step hydro thermal method A kind of V is directly synthesized2O3/VO2Composite electrocatalyst.
Summary of the invention
The present invention is in view of the above shortcomings of the prior art, it is therefore intended that proposes a kind of V2O3/VO2The system of composite electrocatalyst Preparation Method, this method is easy to operate, and reaction condition is mild, the V of preparation2O3/VO2Pattern is uniform.To achieve the goals above, originally Invention uses following technical scheme.
(1) NH is weighed4VO3With N-acetyl-L-cysteine (NAC), molar ratio is (1 ~ 4): (3 ~ 7), it is dissolved in 10 respectively ~ In 20ml deionized water, the concentration that the concentration in vanadium source is (0.02 ~ 0.04) mol/L, NAC at this time is (0.06 ~ 0.7) mol/L, 10 ~ 30min of magnetic agitation at room temperature obtains clear solution；
(2) two kinds of clear solutions in (1) are mixed, 40 ~ 60min of magnetic agitation, obtains clear mixed solution at room temperature；
(3) the clarification mixed solution in (2) is poured into 50ml reaction kettle, is sealed, hydro-thermal reaction is carried out in baking oven, setting is anti- Answering temperature is 170 ~ 220 DEG C, and the reaction time is 18 ~ 28h；
(4) after reaction, to reaction kettle cooled to room temperature, solution is filtered, then uses ethyl alcohol and deionized water It is respectively washed 3 times, finally will be dried in vacuo 5 ~ 10h at 40 ~ 70 DEG C of black powder obtained to get V is arrived2O3/VO2Powder.
Beneficial effect of the invention are as follows:
(1) this method is since it using a step hydro-thermal reaction directly synthesizes final product, thus has low synthesis temperature, Simple process is easy to operate, and raw material is cheap and easy to get, at low cost, and yield is high, is not necessarily to post-processing, environmentally friendly, can be suitble to big Large-scale production；
(2) the product chemistry composition of this method preparation is uniform, purity is high, and pattern is uniform；
(3) V of this method preparation2O3/VO2Powder can be applied to the water-splitting in electro-catalysis field and produce hydrogen elctro-catalyst.
Detailed description of the invention:
Fig. 1 is V prepared by the embodiment of the present invention 32O3/VO2X-ray diffraction (XRD) map of powder；
Fig. 2 is V prepared by the embodiment of the present invention 32O3/VO2Scanning electron microscope (SEM) photo of powder；
Fig. 3 is V prepared by the embodiment of the present invention 32O3/VO2Linear sweep voltammetry (LSV) performance test figure of powder.
Specific embodiment:
With reference to the accompanying drawing and embodiment invention is further described in detail:
Embodiment 1:
(1) NH is weighed4VO3With N-acetyl-L-cysteine (NAC), molar ratio 1:3 is dissolved in respectively in 10ml deionized water, The concentration in vanadium source is 0.02mol/L at this time, and the concentration of NAC is 0.06mol/L, and magnetic agitation 10min, is clarified at room temperature Solution；
(2) two kinds of clear solutions in (1) are mixed, magnetic agitation 40min, obtains clear mixed solution at room temperature；
(3) the clarification mixed solution in (2) is poured into 50ml reaction kettle, is sealed, hydro-thermal reaction is carried out in baking oven, setting is anti- Answering temperature is 170 DEG C, reaction time 28h；
(4) after reaction, to reaction kettle cooled to room temperature, solution is filtered, then uses ethyl alcohol and deionized water It is respectively washed 3 times, finally will be dried in vacuo 10h at 40 DEG C of black powder obtained to get V is arrived2O3/VO2Powder.
Embodiment 2:
(1) NH is weighed4VO3And NAC, molar ratio 4:9 are dissolved in respectively in 15ml deionized water, the concentration in vanadium source is at this time The concentration of 0.267mol/L, NAC are 0.06mol/L, and magnetic agitation 20min, obtains clear solution at room temperature；
(2) two kinds of clear solutions in (1) are mixed, magnetic agitation 50min, obtains clear mixed solution at room temperature；
(3) the clarification mixed solution in (2) is poured into 50ml reaction kettle, is sealed, hydro-thermal reaction is carried out in baking oven, setting is anti- Answering temperature is 220 DEG C, reaction time 20h；
(4) after reaction, to reaction kettle cooled to room temperature, solution is filtered, then uses ethyl alcohol and deionized water It is respectively washed 3 times, finally will be dried in vacuo 8h at 60 DEG C of black powder obtained to get V is arrived2O3/VO2Powder.
Embodiment 3:
(1) NH is weighed4VO3And NAC, molar ratio 3:5 are dissolved in respectively in 15ml deionized water, the concentration in vanadium source is at this time The concentration of 0.04mol/L, NAC are 0.067mol/L, and magnetic agitation 20min, obtains clear solution at room temperature；
(2) two kinds of clear solutions in (1) are mixed, magnetic agitation 50min, obtains clear mixed solution at room temperature；
(3) the clarification mixed solution in (2) is poured into 50ml reaction kettle, is sealed, hydro-thermal reaction is carried out in baking oven, setting is anti- Answering temperature is 220 DEG C, reaction time 20h；
(4) after reaction, to reaction kettle cooled to room temperature, solution is filtered, then uses ethyl alcohol and deionized water It is respectively washed 3 times, finally will be dried in vacuo 8h at 60 DEG C of black powder obtained to get V is arrived2O3/VO2Powder.
Fig. 1 is V manufactured in the present embodiment2O3/VO2X-ray diffraction (XRD) map of powder.Fig. 1 shows, system of the present invention The XRD characteristic peak of standby product respectively with V2O3And VO2Characteristic peak it is corresponding, illustrate that the present invention is prepared for V2O3/VO2Mixing Material.
Fig. 2 is V manufactured in the present embodiment2O3/VO2Scanning electron microscope (SEM) photo of powder.Fig. 2 shows prepared by the present invention V2O3/VO2Powder has well-regulated nano bar-shape pattern.
Fig. 3 is V manufactured in the present embodiment2O3/VO2Linear sweep voltammetry (LSV) performance test figure of powder.Fig. 3 shows, The sample is 10mA/cm in current density2When, its overpotential is 453mV, has good electrocatalytic hydrogen evolution activity.
Embodiment 4:
(1) NH is weighed4VO3With N-acetyl-L-cysteine (NAC), molar ratio 4:7 is dissolved in respectively in 20ml deionized water, The concentration in vanadium source is 0.04mol/L at this time, and the concentration of NAC is 0.07mol/L, and magnetic agitation 30min, is clarified at room temperature Solution；
(2) two kinds of clear solutions in (1) are mixed, magnetic agitation 60min, obtains clear mixed solution at room temperature；
(3) the clarification mixed solution in (2) is poured into 50ml reaction kettle, is sealed, hydro-thermal reaction is carried out in baking oven, setting is anti- Answering temperature is 200 DEG C, reaction time 20h；
(4) after reaction, to reaction kettle cooled to room temperature, solution is filtered, then uses ethyl alcohol and deionized water It is respectively washed 3 times, finally will be dried in vacuo 6h at 60 DEG C of black powder obtained to get V is arrived2O3/VO2Powder.

Claims (4)

1. a kind of V2O3/VO2The preparation method of composite electrocatalyst, which comprises the following steps:
By NH4VO3Aqueous solution, with the aqueous solution of N-acetyl-L-cysteine NAC, according to NH4VO3: the molar ratio of NAC be (1 ~ 4): after (3 ~ 7) mix and are uniformly dispersed, 170 ~ 220 DEG C of progress hydro-thermal reactions obtain V2O3/VO2Composite electrocatalyst.
2. a kind of V according to claim 12O3/VO2The preparation method of composite electrocatalyst, which is characterized in that hydro-thermal is anti- The reaction temperature answered is 170 ~ 220 DEG C, and the reaction time is 18 ~ 28h.
3. a kind of V according to claim 12O3/VO2The preparation method of composite electrocatalyst, which is characterized in that specific step Suddenly include:
1) by NH4VO3And NAC is dissolved in respectively in 10 ~ 20ml deionized water, 10 ~ 30min of magnetic agitation, obtains at room temperature NH4VO3Solution and NAC solution；
2) by the NH in 1)4VO3Solution and NAC solution are (1 ~ 4) by the molar ratio of solute: (3 ~ 7) mix, and are dissolved in 10 respectively In ~ 20ml deionized water, the concentration in vanadium source is 0.02 ~ 0.04mol/L at this time, and the concentration of NAC is 0.06 ~ 0.7mol/L, in room Lower 40 ~ the 60min of magnetic agitation of temperature, obtains clear mixed solution；
3) 2) the clarification mixed solution in is poured into 50ml reaction kettle, is sealed, hydro-thermal reaction, setting reaction are carried out in baking oven Temperature is 170 ~ 220 DEG C, and the reaction time is 18 ~ 28h；
4) after reaction, to reaction kettle cooled to room temperature, solution is filtered, then uses ethyl alcohol and deionization moisture Qing Xi not be 3 times, finally will at 40 ~ 70 DEG C of black powder obtained be dried in vacuo 5 ~ 10h to get arrive V2O3/VO2Powder.
4. a kind of V of any one of claim 1 ~ 3 the method preparation2O3/VO2Composite electrocatalyst.
CN201811272287.8A 2018-10-30 2018-10-30 V-shaped groove2O3/VO2Composite electrocatalyst and method of making Active CN109201038B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109772366A (en) * 2019-03-18 2019-05-21 陕西科技大学 A kind of preparation method of cuprous sulfide/vanadium trioxide as full PH elctro-catalyst
CN110560078A (en) * 2019-09-30 2019-12-13 陕西科技大学 v-shaped groove2O3Preparation method of @ Ni difunctional composite electrocatalyst
CN112811467A (en) * 2021-01-18 2021-05-18 陕西科技大学 V-shaped groove2O3Method for preparing nanoparticles

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008011198A2 (en) * 2006-01-18 2008-01-24 Vanderbilt University Method of preparing vanadium dioxide nanoparticles
CN102910675A (en) * 2011-08-05 2013-02-06 中国科学院大连化学物理研究所 Preparation of VO2 nanosheet material and applications thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008011198A2 (en) * 2006-01-18 2008-01-24 Vanderbilt University Method of preparing vanadium dioxide nanoparticles
CN102910675A (en) * 2011-08-05 2013-02-06 中国科学院大连化学物理研究所 Preparation of VO2 nanosheet material and applications thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109772366A (en) * 2019-03-18 2019-05-21 陕西科技大学 A kind of preparation method of cuprous sulfide/vanadium trioxide as full PH elctro-catalyst
CN110560078A (en) * 2019-09-30 2019-12-13 陕西科技大学 v-shaped groove2O3Preparation method of @ Ni difunctional composite electrocatalyst
CN112811467A (en) * 2021-01-18 2021-05-18 陕西科技大学 V-shaped groove2O3Method for preparing nanoparticles

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