CN109052340A - A kind of preparation method of selenium/selenizing vanadium compound phase material - Google Patents
A kind of preparation method of selenium/selenizing vanadium compound phase material Download PDFInfo
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- CN109052340A CN109052340A CN201811176597.XA CN201811176597A CN109052340A CN 109052340 A CN109052340 A CN 109052340A CN 201811176597 A CN201811176597 A CN 201811176597A CN 109052340 A CN109052340 A CN 109052340A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/02—Elemental selenium or tellurium
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- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/02—Preparation of oxygen
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- 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
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The present invention discloses a kind of preparation method of selenium/selenizing vanadium compound phase material, be in molar ratio (2~6): 1 weighs selenium source and vanadium source, in the solution for being dissolved deionized water and dehydrated alcohol composition, magnetic agitation sufficiently dissolves, Morphological control agent is added in mixed liquor, reaction kettle is sealed, reaction 18~for 24 hours is placed in baking oven at 200~220 DEG C, the product for obtaining black is centrifuged repeatedly several times with ultrapure water and dehydrated alcohol respectively, vacuum drying, obtain selenium/selenizing vanadium composite material, using simple process, short preparation period and the easily controlled solvent-thermal method of reaction, design for composite material elctro-catalyst provides thinking；The selenium of preparation/selenizing vanadium composite material has bigger surface area relative to selenizing vanadium, improves selenium/selenizing vanadium composite material catalytic activity.
Description
Technical field
The invention belongs to electro-catalysis energy and material preparation fields, and in particular to a kind of system of selenium/selenizing vanadium compound phase material
Preparation Method.
Background technique
In recent years, with the fast development of grapheme material, other two-dimensional materials also have been to be concerned by more and more people with
Research.Two-dimensional material usually shows unique electricity, optics and magnetic property, itself has unique structural advantage, this
New approaches are provided to explore novel electro-catalytic agent and energy storage material, have guided new direction.Due to two-dimentional Transition Metal Sulfur
Compounds of group (TMDs) unique physicochemical properties, so that the research for TMDs is also gradually taken seriously, and metal selenizing
Object, especially two-dimensional layer metal selenide are becoming the new hot spot of investigation of materials, have attracted that numerous researchers' is extensive
It pays close attention to and competitively studies.
Ultra-thin two chalcogenide of transition metal (TMDs) has formula M X2See that file 1 is recorded, wherein M is transition metal
Element (M=Ti, V, Ta, Mo, Re, W), X are chalcogen atom (X=S, Se, Te).TMDs is as next-generation New type atom grade
Thin device becomes at present since the peculiar property being not present in its bulk counterpart becomes active in a recent study
One of two-dimensional layer material most with prospects.MX2Crystal structure be by the strongly covalent X-M-X key of interlayer and weak interlayer
XX interaction and formed.In all two-dimensional TM Ds, transition metal element is usually Mo or W, chalcogen
Atom is S or Se, and the two-dimensional TM Ds formed has excellent electricity, optics, magnetics and chemical property, thus by many
Researcher is of interest to see that file 2 is recorded, however these two-dimensional TMs Ds is usually nonmetallic state, thus its electric conductivity is owed
It is good.In recent years, the two-dimensional TM Ds catalyst of metallic state includes CoS2、Ni3S2、Co9S8、VS2Deng gradually developing, wherein especially with
VS2With preferably electrocatalysis characteristic, thus two dimension VS2Nano material gradually become for evolving hydrogen reaction (HER) efficient and
Cheap elctro-catalyst is shown in that file 3 is recorded.
Selenium element and element sulphur belong to the Group VIA of the periodic table of elements, outermost electron number having the same, i.e. metallic selenium
Compound and sulfide have certain similitude in the chemically, see that file 4 is recorded.However, selenium element is in element sulphur
Different cycles in the periodic table of elements, thus there are many differences: 1) selenium element than element sulphur have stronger metallicity, in turn
Has superior electric conductivity；2) selenium atom has bigger atomic radius than sulphur atom；3) selenium atom has more than sulphur atom
Small ionization energy.Based on the above property, can initial guess, compared to metal sulfide, metal selenide and selenides compound phase
Certain peculiar properties can be shown in electrocatalytic hydrogen evolution field.
[1]Chia X,Ambrosi A,Lazar P,et al.Electrocatalysis of layered Group
5metallic transition metal dichalcogenides(MX2, M=V, Nb, and Ta；X=S, Se, and Te)
[J].Journal of Materials Chemistry A,2016,4(37):14241.
[2]Falmbigl M,Fiedler A,Atkins R E,et al.Suppressing a Charge Density
Wave by Changing Dimensionality in the Ferecrystalline Compounds([SnSe]1.15)1
(VSe2) n with n=1,2,3,4. [J] .Nano Letters, 2015,15 (2): 943.
[3]Yan M,Pan X,Wang P,et al.Field-Effect Tuned Adsorption Dynamics of
VSe2Nanosheets for Enhanced Hydrogen Evolution Reaction[J].Nano Letters,2017,
17(7):4109.
[4]Xu K,Chen P,Li X,et al.Ultrathin nanosheets of vanadium
diselenide:a metallic two-dimensional material with ferromagnetic charge-
density-wave behavior[J].Angewandte Chemie International Edition,2013,52(40):
10477。
Summary of the invention
Present invention aims at proposing that a kind of preparation process is simple, preparation condition is mild, at low cost, short preparation period, work
The easily controlled selenium of skill process/selenizing vanadium compound phase material preparation method, compound phase material surface area obtained is bigger, improves
Selenium/selenizing vanadium composite material catalytic activity.
To achieve the goals above, the present invention uses following technical scheme.
A kind of preparation method of selenium/selenizing vanadium compound phase material, includes the following steps:
1) be in molar ratio (2~6): 1 weigh selenium source and vanadium source, and being dissolved in 35mL volume ratio is (3~4): 1 goes
In the solution of ionized water and dehydrated alcohol composition, magnetic agitation sufficiently dissolves, and obtains mixed liquor；
2) the resulting mixed liquor in step 1) is transferred in autoclave of the 50mL with poly- polyparaphenylene liner, with
Added in backward reaction kettle the hexa of 0.038~0.059g, the lauryl sodium sulfate of 0.226~0.324g,
The NN- dimethylformamide Morphological control agent of the polyvinylpyrrolidone and 0.056~0.087g of 0.023~0.035g, will be anti-
It answers kettle to seal, is placed in baking oven at 200~220 DEG C reaction 18~for 24 hours；
3) to which after reaction, after cooled to room temperature, the product for obtaining black uses ultrapure water and dehydrated alcohol respectively
It is centrifuged repeatedly several times, obtains sample；
4) finally, gained sample is dried in vacuo, selenium/selenizing vanadium composite material is obtained.
Further, the selenium source in the step 1) is one of selenourea, selenium powder, selenium dioxide, sodium selenide or a variety of.
Further, the vanadium source in the step 2) is one of vanadic anhydride, ammonium metavanadate, vanadium chloride or a variety of.
Further, the magnetic agitation time is 30min in the step 1).
Further, black product obtained in the step 3) carries out being centrifuged repeatedly 3 with ultrapure water and dehydrated alcohol respectively
It is secondary to obtain sample.
Further, gained sample is dried in vacuo at 50~120 DEG C in the step 4), obtains selenium/selenizing vanadium composite wood
Material.
Selenium/selenizing vanadium the composite material prepared by the above method produces hydrogen for electro-catalysis, compared to the prior art, this
Inventing has technical effect beneficial below:
1) selenium of the invention/selenizing vanadium method for synthesizing composite material uses simple process, short preparation period and reaction and holds
Manageable solvent-thermal method, the design for composite material elctro-catalyst provide thinking；
2) selenium/selenizing vanadium composite material prepared in the present invention has bigger surface area, has relative to selenizing vanadium
Conducive to coming into full contact with for electrolyte and electrode catalyst active material surface, so that it is living to improve the catalysis of selenium/selenizing vanadium composite material
Property；
3) selenium/selenizing vanadium composite material of this method preparation can be applied to the full pH value of the water-splitting in electro-catalysis field and produce hydrogen
Produce oxygen electrode.
Detailed description of the invention
Fig. 1 is that the embodiment of the present invention 1 prepares selenium/selenizing vanadium compound phase XRD diagram
Fig. 2 is that the embodiment of the present invention 2 prepares selenium/selenizing vanadium compound phase SEM figure
Fig. 3 is that the embodiment of the present invention 3 prepares selenium/selenizing vanadium compound phase linear sweep voltammetry curve performance figure
Specific embodiment
Present invention is further described in detail combined with specific embodiments below, but not as a limitation of the invention.
Embodiment 1:
1) selenium dioxide and vanadic anhydride are weighed for 5:1 in molar ratio, i.e., both quality be respectively 554.79mg and
182.00mg is dissolved in the solution of deionized water and dehydrated alcohol composition that volume ratio is 3:1 (total 35mL), and magnetic force stirs
30min is mixed, mixed liquor is obtained；
2) the resulting mixed liquor in step 1) is transferred in autoclave of the 50mL with poly- polyparaphenylene liner, with
The polyethylene pyrrole of the hexa of 0.038g, the lauryl sodium sulfate of 0.324g, 0.023g are added in backward reaction kettle
The NN- dimethylformamide Morphological control agent of pyrrolidone and 0.087g, reaction kettle is sealed, and is placed in baking oven at 220 DEG C anti-
Answer 18h；
3) to after reaction, after cooled to room temperature, obtain the product of black, ultrapure water and dehydrated alcohol are used respectively
Be centrifuged repeatedly 3 times；
4) finally, gained sample is dried in vacuo at 50 DEG C, selenium/selenizing vanadium composite material is obtained.
The selenium prepared in the present embodiment/selenizing vanadium compound phase VSe in XRD spectra can be observed by Fig. 12With the diffraction of Se
Peak (JCPDS Card No.89-1641 and JCPDS Card No.73-0465).
Embodiment 2:
1) sodium selenide and ammonium metavanadate are weighed for 3:1 in molar ratio, i.e., both quality be respectively 374.82mg and
116.99mg is dissolved in the solution of deionized water and dehydrated alcohol composition that volume ratio is 4:1 (total 35mL), and magnetic force stirs
30min is mixed, mixed liquor is obtained；
2) the resulting mixed liquor in step 1) is transferred in autoclave of the 50mL with poly- polyparaphenylene liner, with
The polyethylene pyrrole of the hexa of 0.059g, the lauryl sodium sulfate of 0.226g, 0.035g are added in backward reaction kettle
The NN- dimethylformamide Morphological control agent of pyrrolidone and 0.056g, reaction kettle is sealed, and is placed in baking oven at 200 DEG C anti-
It should for 24 hours；
3) to after reaction, after cooled to room temperature, obtain the product of black, ultrapure water and dehydrated alcohol are used respectively
Be centrifuged repeatedly 3 times；
4) finally, gained sample is dried in vacuo at 120 DEG C, selenium/selenizing vanadium composite material is obtained.
The selenium prepared in the present embodiment/selenizing vanadium compound phase microscopic appearance figure can be observed by Fig. 2, there is big surface
Product, so that electrolyte and electrode catalyst active material surface come into full contact with.
Embodiment 3:
1) selenium powder and vanadium chloride being weighed for 4:1 in molar ratio, i.e., both quality is respectively 315.84mg and 157.30mg,
It is dissolved in the solution of deionized water and dehydrated alcohol composition that volume ratio is 3:1 (total 35mL), magnetic agitation 30min,
Obtain mixed liquor；
2) the resulting mixed liquor in step 1) is transferred in autoclave of the 50mL with poly- polyparaphenylene liner, with
The polyethylene pyrrole of the hexa of 0.048g, the lauryl sodium sulfate of 0.275g, 0.029g are added in backward reaction kettle
The NN- dimethylformamide Morphological control agent of pyrrolidone and 0.072g, reaction kettle is sealed, and is placed in baking oven at 210 DEG C anti-
Answer 21h；
3) to after reaction, after cooled to room temperature, obtain the product of black, ultrapure water and dehydrated alcohol are used respectively
Be centrifuged repeatedly 3 times；
4) finally, gained sample is dried in vacuo at 90 DEG C, selenium/selenizing vanadium composite material is obtained.
Selenium/selenizing vanadium compound phase linear sweep voltammetry curve performance the figure prepared in the present embodiment can be obtained by Fig. 3, from
It can be seen that the material has good electrocatalysis characteristic in figure.
Embodiment 4:
1) selenium powder and vanadic anhydride are weighed for 6:1 in molar ratio, i.e., both quality be respectively 473.76mg and
182.00mg is dissolved in the solution of deionized water and dehydrated alcohol composition that volume ratio is 4:1 (total 35mL), and magnetic force stirs
30min is mixed, mixed liquor is obtained；
2) the resulting mixed liquor in step 1) is transferred in autoclave of the 50mL with poly- polyparaphenylene liner, with
The polyethylene pyrrole of the hexa of 0.040g, the lauryl sodium sulfate of 0.296g, 0.026g are added in backward reaction kettle
The NN- dimethylformamide Morphological control agent of pyrrolidone and 0.083g, reaction kettle is sealed, and is placed in baking oven at 220 DEG C anti-
Answer 19h；
3) to after reaction, after cooled to room temperature, obtain the product of black, ultrapure water and dehydrated alcohol are used respectively
Be centrifuged repeatedly 3 times；
4) finally, gained sample is dried in vacuo at 100 DEG C, selenium/selenizing vanadium composite material is obtained.
Embodiment 5:
1) selenium powder and vanadium chloride being weighed for 5:1 in molar ratio, i.e., both quality is respectively 369.05mg and 157.30mg,
It is dissolved in the solution of deionized water and dehydrated alcohol composition that volume ratio is 3:1 (total 35mL), magnetic agitation 30min,
Obtain mixed liquor；
2) the resulting mixed liquor in step 1) is transferred in autoclave of the 50mL with poly- polyparaphenylene liner, with
The polyethylene pyrrole of the hexa of 0.054g, the lauryl sodium sulfate of 0.238g, 0.031g are added in backward reaction kettle
The NN- dimethylformamide Morphological control agent of pyrrolidone and 0.062g, reaction kettle is sealed, and is placed in baking oven at 200 DEG C anti-
Answer 23h；
3) to after reaction, after cooled to room temperature, obtain the product of black, ultrapure water and dehydrated alcohol are used respectively
Be centrifuged repeatedly 3 times；
4) finally, gained sample is dried in vacuo at 70 DEG C, selenium/selenizing vanadium composite material is obtained.
Embodiment 6:
1) selenium powder, selenium dioxide and vanadium chloride are weighed for 2:2:1 in molar ratio, i.e., quality be respectively 157.92mg,
221.92mg and 157.30mg is dissolved in the solution of deionized water and dehydrated alcohol composition that volume ratio is 3:1 (altogether
35mL), magnetic agitation 30min obtains mixed liquor；
2) the resulting mixed liquor in step 1) is transferred in autoclave of the 50mL with poly- polyparaphenylene liner, with
The polyethylene pyrrole of the hexa of 0.048g, the lauryl sodium sulfate of 0.275g, 0.029g are added in backward reaction kettle
The NN- dimethylformamide Morphological control agent of pyrrolidone and 0.072g, reaction kettle is sealed, and is placed in baking oven at 210 DEG C anti-
Answer 21h；
3) to after reaction, after cooled to room temperature, obtain the product of black, ultrapure water and dehydrated alcohol are used respectively
Be centrifuged repeatedly 3 times；
4) finally, gained sample is dried in vacuo at 90 DEG C, selenium/selenizing vanadium composite material is obtained.
Embodiment 7:
1) selenium powder, selenourea, sodium selenide and vanadic anhydride are weighed for 2:1:1:1 in molar ratio, i.e. quality is respectively
157.92mg, 123.02mg, 124.96mg and 182.00mg are dissolved in deionized water and anhydrous second that volume ratio is 4:1
In the solution of alcohol composition (total 35mL), magnetic agitation 30min obtains mixed liquor；
2) the resulting mixed liquor in step 1) is transferred in autoclave of the 50mL with poly- polyparaphenylene liner, with
The polyethylene pyrrole of the hexa of 0.042g, the lauryl sodium sulfate of 0.319g, 0.027g are added in backward reaction kettle
The NN- dimethylformamide Morphological control agent of pyrrolidone and 0.079g, reaction kettle is sealed, and is placed in baking oven at 220 DEG C anti-
Answer 20h；
3) to after reaction, after cooled to room temperature, obtain the product of black, ultrapure water and dehydrated alcohol are used respectively
Be centrifuged repeatedly 3 times；
4) finally, gained sample is dried in vacuo at 80 DEG C, selenium/selenizing vanadium composite material is obtained.
Embodiment 8:
1) selenium powder, selenourea, sodium selenide, ammonium metavanadate and vanadium chloride, i.e. quality are weighed for 1:1:1:0.5:0.5 in molar ratio
Respectively 78.96mg, 123.02mg, 124.96mg, 58.49mg and 78.65mg, be dissolved in volume ratio be 4:1 go from
In the solution of sub- water and dehydrated alcohol composition (total 35mL), magnetic agitation 30min obtains mixed liquor；
2) the resulting mixed liquor in step 1) is transferred in autoclave of the 50mL with poly- polyparaphenylene liner, with
The polyethylene pyrrole of the hexa of 0.059g, the lauryl sodium sulfate of 0.226g, 0.035g are added in backward reaction kettle
The NN- dimethylformamide Morphological control agent of pyrrolidone and 0.056g, reaction kettle is sealed, and is placed in baking oven at 200 DEG C anti-
It should for 24 hours；
3) to after reaction, after cooled to room temperature, obtain the product of black, ultrapure water and dehydrated alcohol are used respectively
Be centrifuged repeatedly 3 times；
4) finally, gained sample is dried in vacuo at 120 DEG C, selenium/selenizing vanadium composite material is obtained.
Embodiment 9:
1) in molar ratio for 1.5:1.5:1.5:1.5:0.4:0.2:0.2 weigh selenourea, selenium powder, selenium dioxide, sodium selenide,
Ammonium metavanadate, vanadium chloride and vanadic anhydride, i.e. quality be respectively 184.53mg, 118.44mg, 166.44mg, 46.97mg,
31.46mg and 36.40mg is dissolved in the solution of deionized water and dehydrated alcohol composition that volume ratio is 4:1 (altogether
35mL), magnetic agitation 30min obtains mixed liquor；
2) the resulting mixed liquor in step 1) is transferred in autoclave of the 50mL with poly- polyparaphenylene liner, with
The polyethylene pyrrole of the hexa of 0.040g, the lauryl sodium sulfate of 0.296g, 0.026g are added in backward reaction kettle
The NN- dimethylformamide Morphological control agent of pyrrolidone and 0.083g, reaction kettle is sealed, and is placed in baking oven at 220 DEG C anti-
Answer 19h；
3) to after reaction, after cooled to room temperature, obtain the product of black, ultrapure water and dehydrated alcohol are used respectively
Be centrifuged repeatedly 3 times；
4) finally, gained sample is dried in vacuo at 100 DEG C, selenium/selenizing vanadium composite material is obtained.
Finally it should be noted that: the above examples are only used to illustrate the technical scheme of the present invention rather than its limitations, to the greatest extent
Pipe is described the invention in detail referring to above-described embodiment, it should be understood by those ordinary skilled in the art that: still may be used
With modifications or equivalent substitutions are made to specific embodiments of the invention, and repaired without departing from any of spirit and scope of the invention
Change or equivalent replacement, should all cover in present claims range.
Claims (6)
1. a kind of selenium/selenizing vanadium compound phase material preparation method, it is characterised in that include the following steps:
1) be in molar ratio (2~6): 1 weighs selenium source and vanadium source, and being dissolved in 35mL volume ratio is (3~4): 1 deionization
In the solution of water and dehydrated alcohol composition, magnetic agitation sufficiently dissolves, and obtains mixed liquor；
2) the resulting mixed liquor in step 1) is transferred in autoclave of the 50mL with poly- polyparaphenylene liner, then to
Added in reaction kettle the hexa of 0.038~0.059g, the lauryl sodium sulfate of 0.226~0.324g, 0.023~
The NN- dimethylformamide Morphological control agent of the polyvinylpyrrolidone and 0.056~0.087g of 0.035g, reaction kettle is close
Envelope is placed in baking oven at 200~220 DEG C reaction 18~for 24 hours；
3) to which after reaction, after cooled to room temperature, the product for obtaining black is carried out with ultrapure water and dehydrated alcohol respectively
It is centrifuged repeatedly several times, obtains sample；
4) finally, gained sample is dried in vacuo, selenium/selenizing vanadium composite material is obtained.
2. preparation method as described in claim 1, it is characterised in that: the selenium source in the step 1) is selenourea, selenium powder, dioxy
Change one of selenium, sodium selenide or a variety of.
3. preparation method as described in claim 1, it is characterised in that: the vanadium source in the step 2) is vanadic anhydride, partially
One of ammonium vanadate, vanadium chloride are a variety of.
4. preparation method as described in claim 1, it is characterised in that: the magnetic agitation time is 30min in the step 1).
5. preparation method as described in claim 1, it is characterised in that: black product obtained in the step 3) is respectively with super
Pure water and dehydrated alcohol, which carry out being centrifuged repeatedly 3 times, obtains sample.
6. preparation method as described in claim 1, it is characterised in that: gained sample is at 50~120 DEG C in the step 4)
Vacuum drying, obtains selenium/selenizing vanadium composite material.
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| CN111244445A (en) * | 2020-01-16 | 2020-06-05 | 中南大学 | Lithium-sulfur battery composite positive electrode active material and preparation and application thereof |
| CN112624040A (en) * | 2020-12-22 | 2021-04-09 | 佛山(华南)新材料研究院 | Method for preparing hydrogen |
| CN114920207A (en) * | 2022-05-05 | 2022-08-19 | 哈尔滨工业大学 | Flower-shaped VSe 2 Method for synthesizing nano material |
| CN114956013A (en) * | 2022-05-19 | 2022-08-30 | 河南工业大学 | Preparation method of VSe2 metal ultrathin nanosheet similar to graphene |
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