CN106179412B - It is a kind of to prepare sheet SmS-CrS2The method that interlayer mismatches compound - Google Patents
It is a kind of to prepare sheet SmS-CrS2The method that interlayer mismatches compound Download PDFInfo
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- 150000001875 compounds Chemical class 0.000 title claims abstract description 36
- 239000011229 interlayer Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 21
- 239000000047 product Substances 0.000 claims abstract description 16
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000007789 gas Substances 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 14
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000011282 treatment Methods 0.000 claims abstract description 9
- 229910052786 argon Inorganic materials 0.000 claims abstract description 7
- 239000006227 byproduct Substances 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 7
- 230000035484 reaction time Effects 0.000 claims abstract description 7
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000003828 vacuum filtration Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- 238000007146 photocatalysis Methods 0.000 abstract description 7
- 238000004458 analytical method Methods 0.000 abstract description 5
- -1 stirs 1h Substances 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 238000001198 high resolution scanning electron microscopy Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 2
- 229940043267 rhodamine b Drugs 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000005619 thermoelectricity Effects 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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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
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
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- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
- A62D3/10—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by subjecting to electric or wave energy or particle or ionizing radiation
- A62D3/17—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by subjecting to electric or wave energy or particle or ionizing radiation to electromagnetic radiation, e.g. emitted by a laser
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
- A62D2101/20—Organic substances
- A62D2101/26—Organic substances containing nitrogen or phosphorus
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- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
- A62D2101/20—Organic substances
- A62D2101/28—Organic substances containing oxygen, sulfur, selenium or tellurium, i.e. chalcogen
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Abstract
The present invention, which discloses, a kind of preparing sheet SmS CrS2The method that interlayer mismatches compound：By a certain amount of pure CrCl of analysis6·H2O and SmCl6·H2O is with 1：0.5~6 molar ratio is dissolved in suitable quantity of water, stirs 1h, and ammonium hydroxide is added, and stirring feeds the mixture into hydro-thermal reaction in autoclave, and reaction temperature is 80 200 DEG C, and the reaction time is 6h 48h, and products therefrom is filtered and is detached, product A is obtained；In mass ratio by product A：Thioacetamide=1：5 40 mixture ground and mixed keeps the temperature 1~5h progress vulcanizing treatments with argon gas to protect gas in tube furnace at 500~1000 DEG C; products therefrom is washed with deionized until solution PH=6.8~7.2; with vacuum filtration, and 60 DEG C of dry 5h in an oven, obtain sheet SmS CrS2Interlayer mismatches compound.Sheet SmS CrS2Interlayer mismatches the photocatalysis performance that compound effectively improves SmS.
Description
Technical field
The present invention relates to field of compound preparation, more particularly to a kind of to prepare SmS-CrS2Interlayer mismatches the side of compound
Method.
Background technology
SmS is a kind of semi-conducting material of low energy gap, is had in photocatalysis field and area of solar cell larger
Application potential, but its own there is a problem of conductivity difference, so that the performance of its performance is affected.It is really necessary to improve
The photocatalysis performance of SmS makes it have more wide application prospect.
Invention content
Sheet SmS-CrS is prepared the purpose of the present invention is to provide a kind of2The method that interlayer mismatches compound, equipment
It is required that low, simple for process, easy to operate and be easy to control, prepared sheet SmS-CrS2Interlayer, which mismatches compound, makes its light
Catalytic performance is further promoted.
In order to achieve the above object, the present invention uses following technical scheme：
It is a kind of to prepare sheet SmS-CrS2The method that interlayer mismatches compound, includes the following steps：
1) pure CrCl will be analyzed6·H2O and SmCl6·H2O is soluble in water with 1: 0.5~6 molar ratio, stirs evenly shape
Ammonium hydroxide is added in mixture and stirs evenly for resulting mixture；
2) hydro-thermal reaction in autoclave is added in the mixture after addition ammonium hydroxide, obtains product A；
3) in mass ratio by product A：Thioacetamide=1: the mixture ground and mixed of 5-40, with argon gas in tube furnace
To protect gas, vulcanizing treatment is carried out；
4) products therefrom is washed with deionized until solution PH=6.8~7.2, with vacuum filtration, and in an oven
It is dry, obtain sheet SmS-CrS2Interlayer mismatches compound.
Further, 0.5mmolCrCl is added per 50mL water in step 1)6·H2O and 5-10mL ammonium hydroxide.
Further, reaction temperature is 80-200 DEG C in step 2), reaction time 6h-48h.
Further, the temperature of vulcanizing treatment is 500~1000 DEG C in step 3), and soaking time is 1~5h.
Further, drying temperature is 60 DEG C in step 4), time 5h.
Compared with the existing technology, the invention has the advantages that：
The present invention is with CrCl6·H2O and SmCl6·H2O is raw material, prepares sheet SmS-CrS2Interlayer mismatches chemical combination
The raw material of object, the reaction is easy to get and at low cost, and process equipment is simple, and using water as reaction dissolvent, safety is good, and feasibility is strong,
So it is very economical, practical, there is good industrial prospect.
SmS is a kind of semi-conducting material of low energy gap, and the material of non-laminar structure has two as graphene is this kind of
Structural material is tieed up in photocatalysis energy stores, the fields such as catalysis reaction and area of solar cell have larger application potential,
But there is conductivity difference in its own, the performance of its performance is made to be illustrated influence.Good application prospect, research
Synthesizing becomes the hot spot of research with two-dimensional structure material.CrS2It is a kind of material of the preferable layer structure of electric conductivity, closes
At the present invention in CrS2Layer has been grown above has layer structure SmS.SmS-CrS2Interlayer, which mismatches compound, greatly to be changed
The electric conductivity of kind SmS, while being a kind of SmS and CrS2Hetero-junctions, which can be formed, in interlayer will make the photocatalysis performance of SmS into one
Step is promoted, and therefore, synthesizes SmS-CrS2Interlayer, which mismatches compound, will have in crystal c axis direction in photocatalysis technology by O-
What the mode of T-O-T arranged, which will have huge application prospect potentiality in chemical catalysis and thermoelectricity field.
Description of the drawings
Fig. 1 is sheet SmS-CrS prepared by the embodiment of the present invention 22Interlayer mismatches the SEM figures of compound；
Fig. 2 is sheet SmS-CrS prepared by the embodiment of the present invention 22Interlayer mismatches compound along piece thickness direction
HRSEM schemes；
Fig. 3 is sheet SmS-CrS prepared by the embodiment of the present invention 22Interlayer mismatches compound along plate plane
HRSEM schemes；
Fig. 4 is sheet SmS-CrS prepared by the embodiment of the present invention 22Interlayer mismatches compound Visible Light Induced Photocatalytic Luo Dan
Bright B light degradation figure.
Specific implementation mode
Embodiment 1
It is a kind of to prepare sheet SmS-CrS2The method that interlayer mismatches compound, includes the following steps：
1) by a certain amount of pure CrCl of analysis6·H2O and SmCl6·H2O is dissolved in 1: 0.5 molar ratio in 50mL water, stirring
10ml ammonium hydroxide is added in mixture by 1h, stirs 30min；Wherein, CrCl6·H2O is 0.5mmol.
2) hydro-thermal reaction in autoclave is fed the mixture into, reaction temperature is 200 DEG C, and reaction time 6h produces gained
Object filters separation, obtains product A；
3) in mass ratio by product A：Thioacetamide=1: 5 mixture ground and mixed is with argon gas in tube furnace
Gas is protected, 1h is kept the temperature at 800 DEG C and carries out vulcanizing treatment；
4) products therefrom is washed with deionized until solution PH=7.0, with vacuum filtration, and in an oven 60 DEG C it is dry
Dry 5h obtains sheet SmS-CrS2Interlayer mismatches compound.
Embodiment 2
It is a kind of to prepare sheet SmS-CrS2The method that interlayer mismatches compound, includes the following steps：
1) by a certain amount of pure CrCl of analysis6·H2O and SmCl6·H2O is dissolved in 1: 1 molar ratio in 50mL water, stirring
10ml ammonium hydroxide is added in mixture by 1h, stirs 30min；Wherein, CrCl6·H2O is 0.5mmol.
2) hydro-thermal reaction in autoclave is fed the mixture into, reaction temperature is 140 DEG C, and reaction time 48h produces gained
Object filters separation, obtains product A；
3) in mass ratio by product A：Thioacetamide=1: 10 mixture ground and mixed is with argon gas in tube furnace
Gas is protected, 2h is kept the temperature at 900 DEG C and carries out vulcanizing treatment；
4) products therefrom is washed with deionized until solution PH=7.0, with vacuum filtration, and in an oven 60 DEG C it is dry
Dry 5h obtains sheet SmS-CrS2Interlayer mismatches compound.
Embodiment 3
It is a kind of to prepare sheet SmS-CrS2The method that interlayer mismatches compound, includes the following steps：
1) by a certain amount of pure CrCl of analysis6·H2O and SmCl6·H2O is dissolved in 1: 3 molar ratio in 50mL water, stirring
8ml ammonium hydroxide is added in mixture by 1h, stirs 30min；Wherein, CrCl6·H2O is 0.5mmol.
2) hydro-thermal reaction in autoclave is fed the mixture into, reaction temperature is 80 DEG C, and the reaction time is that for 24 hours, gained is produced
Object filters separation, obtains product A；
3) in mass ratio by product A：Thioacetamide=1: 40 mixture ground and mixed is with argon gas in tube furnace
Gas is protected, 4h is kept the temperature at 500 DEG C and carries out vulcanizing treatment；
4) products therefrom is washed with deionized until solution PH=6.8, with vacuum filtration, and in an oven 60 DEG C it is dry
Dry 5h obtains sheet SmS-CrS2Interlayer mismatches compound.
Embodiment 4
It is a kind of to prepare sheet SmS-CrS2The method that interlayer mismatches compound, includes the following steps：
1) by a certain amount of pure CrCl of analysis6·H2O and SmCl6·H2O is dissolved in 1: 6 molar ratio in 50mL water, stirring
5ml ammonium hydroxide is added in mixture by 1h, stirs 30min；Wherein, CrCl6·H2O is 0.5mmol.
2) hydro-thermal reaction in autoclave is fed the mixture into, reaction temperature is 120 DEG C, and reaction time 12h produces gained
Object filters separation, obtains product A；
3) in mass ratio by product A：Thioacetamide=1: 20 mixture ground and mixed is with argon gas in tube furnace
Gas is protected, 5h is kept the temperature at 1000 DEG C and carries out vulcanizing treatment；
4) products therefrom is washed with deionized until solution PH=7.2, with vacuum filtration, and in an oven 60 DEG C it is dry
Dry 5h obtains sheet SmS-CrS2Interlayer mismatches compound.
Fig. 1 is the present invention by sheet SmS-CrS prepared by embodiment 22Interlayer mismatches compound SEM figures, can from figure
To find out for product for the SmS-CrS with laminated structure2Interlayer mismatches compound.Fig. 2 is that the present invention is made by embodiment 2
Standby sheet SmS-CrS2Interlayer, which mismatches HRSEM of the compound along piece thickness direction, schemes, as we can see from the figure SmS and CrS2By suitable
Sequence ordered arrangement.Fig. 3 is the present invention by sheet SmS-CrS prepared by embodiment 22Interlayer mismatches compound along plate plane
HRSEM schemes, and is found through measuring lattice fringe, d=0.306nm, corresponding CrS2(020), d=0.345nm corresponds to SmS's
(111) crystal face illustrates to have synthesized SmS-CrS in conjunction with Fig. 1,22Interlayer mismatches compound.Fig. 4 is sheet SmS-CrS2Layer is not
With compound in the light degradation figure that 1000W xenon lamps are light source rhodamine B degradation, we can see that being in light application time from figure
When 90min, SmS-CrS2Layer mismatches compound and has reached 44% to rhodamine B degradation, and the SmS of pure phase degrades 33%,
Illustrate sheet SmS-CrS2Layer, which mismatches compound, can improve the photocatalysis performance of SmS.
Claims (2)
1. a kind of preparing sheet SmS-CrS2The method that interlayer mismatches compound, which is characterized in that include the following steps：
1) pure CrCl will be analyzed6·H2O and SmCl6·H2O is with 1：0.5~6 molar ratio is soluble in water, stirs evenly to form mixing
Ammonium hydroxide is added in mixture and stirs evenly for object；
2) hydro-thermal reaction in autoclave is added in the mixture after addition ammonium hydroxide, obtains product A；
3) in mass ratio by product A：Thioacetamide=1：The mixture ground and mixed of 5-40, in tube furnace with argon gas be protect
Gas is protected, vulcanizing treatment is carried out；
4) products therefrom is washed with deionized until pH value of solution=6.8~7.2, with vacuum filtration, and is dried in an oven,
Obtain sheet SmS-CrS2Interlayer mismatches compound；
0.5mmolCrCl is added per 50mL water in step 1)6·H2O and 5-10mL ammonium hydroxide；
Reaction temperature is 80-200 DEG C in step 2), reaction time 6h-48h；
The temperature of vulcanizing treatment is 500~1000 DEG C in step 3), and soaking time is 1~5h.
2. a kind of sheet SmS-CrS is prepared according to claim 12The method that interlayer mismatches compound, feature exist
In：Drying temperature is 60 DEG C in step 4), time 5h.
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| CN111644184B (en) * | 2020-06-16 | 2022-11-29 | 陕西科技大学 | Visible light response Sm 10.67 S 16 Photocatalyst and preparation method thereof |
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| CN102502754A (en) * | 2011-10-13 | 2012-06-20 | 陕西科技大学 | Method for preparing SmS nanocrystal by solvothermal method |
| CN103495427A (en) * | 2013-10-17 | 2014-01-08 | 大连理工大学 | Method for using low-temperature plasma to prepare supported metal sulfide catalyst |
| CN104821240A (en) * | 2015-04-29 | 2015-08-05 | 岭南师范学院 | SnS2/MoS2 composite material one-step hydrothermal synthesizing method and application thereof |
| CN105536684A (en) * | 2015-12-22 | 2016-05-04 | 镇江市高等专科学校 | Preparation method of molybdenum disulfide-silver sulfide composite nano-grade adsorption-photocatalyst |
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| CN105688945A (en) * | 2016-03-22 | 2016-06-22 | 福州大学 | Composite photo-catalyst with molybdenum disulfide (MoS2) nanosheet/cadmium sulfide (CdS) nanowire core-shell structure |
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- 2016-07-26 CN CN201610596279.3A patent/CN106179412B/en active Active
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| CN102502754A (en) * | 2011-10-13 | 2012-06-20 | 陕西科技大学 | Method for preparing SmS nanocrystal by solvothermal method |
| CN103495427A (en) * | 2013-10-17 | 2014-01-08 | 大连理工大学 | Method for using low-temperature plasma to prepare supported metal sulfide catalyst |
| CN104821240A (en) * | 2015-04-29 | 2015-08-05 | 岭南师范学院 | SnS2/MoS2 composite material one-step hydrothermal synthesizing method and application thereof |
| CN105536684A (en) * | 2015-12-22 | 2016-05-04 | 镇江市高等专科学校 | Preparation method of molybdenum disulfide-silver sulfide composite nano-grade adsorption-photocatalyst |
| CN105664977A (en) * | 2016-02-03 | 2016-06-15 | 中国科学院化学研究所 | Molybdenum disulfide-cadmium sulfide nanometer composite material and preparing method and application thereof |
| CN105688945A (en) * | 2016-03-22 | 2016-06-22 | 福州大学 | Composite photo-catalyst with molybdenum disulfide (MoS2) nanosheet/cadmium sulfide (CdS) nanowire core-shell structure |
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| "CuS/MoS2 nanocomposite with high solar photocatalytic activity";Nannan Meng et al.;《Journal of nanoparticle Research》;20150711;第17卷(第7期);第1-10页 * |
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