CN106179412A - One prepares lamellar SmS CrS2interlayer does not mate the method for compound - Google Patents
One prepares lamellar SmS CrS2interlayer does not mate the method for compound Download PDFInfo
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- CN106179412A CN106179412A CN201610596279.3A CN201610596279A CN106179412A CN 106179412 A CN106179412 A CN 106179412A CN 201610596279 A CN201610596279 A CN 201610596279A CN 106179412 A CN106179412 A CN 106179412A
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- 150000001875 compounds Chemical class 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000011229 interlayer Substances 0.000 claims abstract description 35
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 22
- 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
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000006243 chemical reaction 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
- 239000007789 gas Substances 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 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
- 230000014759 maintenance of location Effects 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- 238000007146 photocatalysis Methods 0.000 abstract description 7
- 238000001914 filtration Methods 0.000 abstract description 5
- 239000010410 layer Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 238000001198 high resolution scanning electron microscopy Methods 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 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
- 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 open one of the present invention prepares lamellar SmS CrS2Interlayer does not mate the method for compound: by a certain amount of analytical pure CrCl6·H2O and SmCl6·H2O is dissolved in suitable quantity of water with the mol ratio of 1:0.5～6, stirs 1h, adds ammonia, stirring, feeds the mixture into hydro-thermal reaction in autoclave, and reaction temperature is 80 200 DEG C, and the response time is 6h 48h, is separated by products therefrom sucking filtration, obtains product A；In mass ratio by product A: the mixture ground and mixed of thioacetamide=1:5 40; with argon for protection gas in tube furnace; at 500～1000 DEG C, it is incubated 1～5h carries out vulcanizing treatment; 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 lamellar SmS CrS2Interlayer does not mate compound.Lamellar SmS CrS2Interlayer does not mate compound and is effectively improved the photocatalysis performance of SmS.
Description
Technical field
The present invention relates to field of compound preparation, prepare SmS-CrS particularly to one2Interlayer does not mate the side of compound
Method.
Background technology
SmS is the semi-conducting material of a kind of low energy gap, has bigger in photocatalysis field and area of solar cell
Application potential, but the problem that himself there is conductance rate variance so that it is the performance of performance is affected.It is necessary in fact to improve
The photocatalysis performance of SmS so that it is there is more wide application prospect.
Summary of the invention
It is an object of the invention to provide one and prepare lamellar SmS-CrS2Interlayer does not mate the method for compound, its equipment
Require low, technique is simple, easy and simple to handle and be easily controlled, prepared lamellar SmS-CrS2Interlayer does not mate compound makes its light
Catalytic performance promotes further.
In order to achieve the above object, the present invention is by the following technical solutions:
One prepares lamellar SmS-CrS2Interlayer does not mate the method for compound, comprises the following steps:
1) by analytical pure CrCl6·H2O and SmCl6·H2O is soluble in water with the mol ratio of 1: 0.5～6, and stir shape
Resulting mixture, adds ammonia and stirs in mixture；
2) mixture after adding ammonia adds hydro-thermal reaction in autoclave, obtains product A；
3) in mass ratio by the mixture ground and mixed of product A: thioacetamide=1: 5-40, with argon in tube furnace
For protection gas, carry out vulcanizing treatment；
4) products therefrom is washed with deionized until solution PH=6.8～7.2, with vacuum filtration, and in an oven
It is dried, obtains lamellar SmS-CrS2Interlayer does not mate compound.
Further, step 1) in every 50mL water add 0.5mmolCrCl6·H2O and 5-10mL ammonia.
Further, step 2) in reaction temperature be 80-200 DEG C, the response time is 6h-48h.
Further, step 3) in the temperature of vulcanizing treatment be 500～1000 DEG C, temperature retention time is 1～5h.
Further, step 4) in baking temperature be 60 DEG C, the time is 5h.
Relative to prior art, the method have the advantages that
The present invention is with CrCl6·H2O and SmCl6·H2O is raw material, prepares lamellar SmS-CrS2Interlayer does not mate chemical combination
Thing, the raw material of this reaction is easy to get and low cost, and process equipment is simple, and using water as reaction dissolvent, safety is good, and feasibility is strong,
So very economical, practical, there is good industrial prospect.
SmS is the semi-conducting material of a kind of low energy gap, and the material of non-laminar structure has two along with Graphene is this kind of
The fields such as dimension structural material stores at photocatalysis energy, catalytic reaction and area of solar cell have bigger application potential,
But the problem that himself there is conductance rate variance so that it is the performance of performance is illustrated impact.Good application prospect, research
Synthesize and there is two-dimensional structure material become the focus of research.CrS2It is the material of the preferable layer structure of a kind of electric conductivity, closes
Become the present invention at CrS2Layer has grown above has layer structure SmS.SmS-CrS2Interlayer does not mate compound and will change greatly
The electric conductivity of kind SmS, is a kind of SmS and CrS simultaneously2Hetero-junctions can be formed at interlayer and the photocatalysis performance making SmS is entered one
Step promotes, and therefore, synthesizes SmS-CrS2Interlayer does not mate compound will be had on crystal c direction of principal axis by O-in photocatalysis technology
The mode of T-O-T arranges, and this material will have huge application prospect potentiality at chemical catalysis and thermoelectricity field.
Accompanying drawing explanation
Fig. 1 is lamellar SmS-CrS prepared by the embodiment of the present invention 22Interlayer does not mate the SEM figure of compound；
Fig. 2 is lamellar SmS-CrS prepared by the embodiment of the present invention 22Interlayer does not mate compound along sheet thickness direction
HRSEM schemes；
Fig. 3 is lamellar SmS-CrS prepared by the embodiment of the present invention 22Interlayer does not mate compound along plate plane
HRSEM schemes；
Fig. 4 is lamellar SmS-CrS prepared by the embodiment of the present invention 22Interlayer does not mate compound Visible Light Induced Photocatalytic Luo Dan
Bright B light degradation figure.
Detailed description of the invention
Embodiment 1
One prepares lamellar SmS-CrS2Interlayer does not mate the method for compound, comprises the following steps:
1) by a certain amount of analytical pure CrCl6·H2O and SmCl6·H2O is dissolved in 50mL water with the mol ratio of 1: 0.5, stirring
1h, adds 10ml ammonia, stirs 30min in mixture；Wherein, CrCl6·H2O is 0.5mmol.
2) feeding the mixture into hydro-thermal reaction in autoclave, reaction temperature is 200 DEG C, and the response time is 6h, is produced by gained
Thing sucking filtration separates, and obtains product A；
3) in mass ratio by product A: thioacetamide=1: the mixture ground and mixed of 5, in tube furnace with argon it is
Protection gas, is incubated 1h 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 do
Dry 5h, obtains lamellar SmS-CrS2Interlayer does not mate compound.
Embodiment 2
One prepares lamellar SmS-CrS2Interlayer does not mate the method for compound, comprises the following steps:
1) by a certain amount of analytical pure CrCl6·H2O and SmCl6·H2O is dissolved in 50mL water with the mol ratio of 1: 1, stirring
1h, adds 10ml ammonia, stirs 30min in mixture；Wherein, CrCl6·H2O is 0.5mmol.
2) feeding the mixture into hydro-thermal reaction in autoclave, reaction temperature is 140 DEG C, and the response time is 48h, is produced by gained
Thing sucking filtration separates, and obtains product A；
3) in mass ratio by product A: thioacetamide=1: the mixture ground and mixed of 10, in tube furnace with argon it is
Protection gas, is incubated 2h 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 do
Dry 5h, obtains lamellar SmS-CrS2Interlayer does not mate compound.
Embodiment 3
One prepares lamellar SmS-CrS2Interlayer does not mate the method for compound, comprises the following steps:
1) by a certain amount of analytical pure CrCl6·H2O and SmCl6·H2O is dissolved in 50mL water with the mol ratio of 1: 3, stirring
1h, adds 8ml ammonia, stirs 30min in mixture；Wherein, CrCl6·H2O is 0.5mmol.
2) feeding the mixture into hydro-thermal reaction in autoclave, reaction temperature is 80 DEG C, and the response time is 24h, is produced by gained
Thing sucking filtration separates, and obtains product A；
3) in mass ratio by product A: thioacetamide=1: the mixture ground and mixed of 40, in tube furnace with argon it is
Protection gas, is incubated 4h 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 do
Dry 5h, obtains lamellar SmS-CrS2Interlayer does not mate compound.
Embodiment 4
One prepares lamellar SmS-CrS2Interlayer does not mate the method for compound, comprises the following steps:
1) by a certain amount of analytical pure CrCl6·H2O and SmCl6·H2O is dissolved in 50mL water with the mol ratio of 1: 6, stirring
1h, adds 5ml ammonia, stirs 30min in mixture；Wherein, CrCl6·H2O is 0.5mmol.
2) feeding the mixture into hydro-thermal reaction in autoclave, reaction temperature is 120 DEG C, and the response time is 12h, is produced by gained
Thing sucking filtration separates, and obtains product A；
3) in mass ratio by product A: thioacetamide=1: the mixture ground and mixed of 20, in tube furnace with argon it is
Protection gas, is incubated 5h 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 do
Dry 5h, obtains lamellar SmS-CrS2Interlayer does not mate compound.
Fig. 1 is present invention lamellar SmS-CrS as prepared by embodiment 22Interlayer does not mate compound SEM figure, can from figure
With find out for product be the SmS-CrS with laminated structure2Interlayer does not mate compound.Fig. 2 is that the present invention is made by embodiment 2
Standby lamellar SmS-CrS2Interlayer does not mate the compound HRSEM figure along sheet thickness direction, SmS and CrS as we can see from the figure2By suitable
Sequence ordered arrangement.Fig. 3 is present invention lamellar SmS-CrS as prepared by embodiment 22Interlayer does not mate compound along plate plane
HRSEM schemes, and finds through measuring lattice fringe, d=0.306nm, corresponding CrS2(020), d=0.345nm correspondence SmS
(111) crystal face, has synthesized SmS-CrS in conjunction with Fig. 1,2 explanations2Interlayer does not mate compound.Fig. 4 is lamellar SmS-CrS2Layer is not
Join compound at the light degradation figure that 1000W xenon lamp is light source rhodamine B degradation, we can see that from figure in light application time and be
During 90min, SmS-CrS2Layer does not mate compound and rhodamine B degraded has been reached 44%, and the SmS of pure phase degrades 33%,
Lamellar SmS-CrS is described2Layer does not mate compound and can improve the photocatalysis performance of SmS.
Claims (5)
1. prepare lamellar SmS-CrS for one kind2Interlayer does not mate the method for compound, it is characterised in that comprise the following steps:
1) by analytical pure CrCl6·H2O and SmCl6·H2O is soluble in water with the mol ratio of 1:0.5～6, and stir formation mixing
Thing, adds ammonia and stirs in mixture；
2) mixture after adding ammonia adds hydro-thermal reaction in autoclave, obtains product A；
3) in mass ratio by product A: the mixture ground and mixed of thioacetamide=1:5-40, with argon for protecting in tube furnace
Protect gas, carry out vulcanizing treatment；
4) products therefrom is washed with deionized until solution PH=6.8～7.2, with vacuum filtration, and is dried in an oven,
Obtain lamellar SmS-CrS2Interlayer does not mate compound.
One the most according to claim 1 prepares lamellar SmS-CrS2Interlayer does not mate the method for compound, and its feature exists
In step 1) in every 50mL water add 0.5mmolCrCl6·H2O and 5-10mL ammonia.
One the most according to claim 1 prepares lamellar SmS-CrS2Interlayer does not mate the method for compound, and its feature exists
In step 2) in reaction temperature be 80-200 DEG C, the response time is 6h-48h.
One the most according to claim 1 prepares lamellar SmS-CrS2Interlayer does not mate the method for compound, and its feature exists
In step 3) in the temperature of vulcanizing treatment be 500～1000 DEG C, temperature retention time is 1～5h.
One the most according to claim 1 prepares lamellar SmS-CrS2Interlayer does not mate the method for compound, and its feature exists
In step 4) in baking temperature be 60 DEG C, the time is 5h.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610596279.3A CN106179412B (en) | 2016-07-26 | 2016-07-26 | It is a kind of to prepare sheet SmS-CrS2The method that interlayer mismatches compound |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610596279.3A CN106179412B (en) | 2016-07-26 | 2016-07-26 | It is a kind of to prepare sheet SmS-CrS2The method that interlayer mismatches compound |
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| Publication Number | Publication Date |
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| CN106179412A true CN106179412A (en) | 2016-12-07 |
| CN106179412B CN106179412B (en) | 2018-08-24 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111644184A (en) * | 2020-06-16 | 2020-09-11 | 陕西科技大学 | Visible light response Sm10.67S16Photocatalyst 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 |
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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
- 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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| Title |
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| HOULONG L.ZHUANG ET AL.: ""Computational prediction and characterization of single-layer CrS2"", 《APPLIED PHYSICS LETTERS》 * |
| NANNAN MENG ET AL.: ""CuS/MoS2 nanocomposite with high solar photocatalytic activity"", 《JOURNAL OF NANOPARTICLE RESEARCH》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111644184A (en) * | 2020-06-16 | 2020-09-11 | 陕西科技大学 | Visible light response Sm10.67S16Photocatalyst and preparation method thereof |
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Effective date of registration: 20240820 Address after: 810, 8th Floor, Building 10, Courtyard 1, Tianxing Street, Fangshan District, Beijing, 102400 Patentee after: Beijing Zhichanhui Technology Co.,Ltd. Country or region after: China Address before: No. 1, Weiyang District university garden, Xi'an, Shaanxi Province, Shaanxi Patentee before: SHAANXI University OF SCIENCE & TECHNOLOGY Country or region before: China |
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