CN111362321A - Preparation method of metal sulfide - Google Patents
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- CN111362321A CN111362321A CN202010281320.4A CN202010281320A CN111362321A CN 111362321 A CN111362321 A CN 111362321A CN 202010281320 A CN202010281320 A CN 202010281320A CN 111362321 A CN111362321 A CN 111362321A
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Abstract
The invention discloses a preparation method of a metal sulfide. The preparation method of the metal sulfide comprises the following steps: 1) dissolving trithiocyanuric acid in dimethylformamide to obtain a solution A; 2) dissolving metal acetate in DMF to obtain solution B; 3) under the condition of ultrasonic or stirring, dropwise adding the solution A into the solution B to obtain a precipitate; 4) and carrying out heat treatment on the precipitate to obtain the corresponding metal sulfide. The methodThe chemical component general formula of the metal sulfide prepared by the method is MxSyWherein M can be any one or combination of several of Co, Ni, Cu, Zn, Ag and Cd in any proportion, and S is sulfur element. The result shows that the metal sulfide prepared by the method is an aggregate of nano/submicron particles, and has high purity and good crystallinity. The preparation method disclosed by the invention is easy to operate, low in time consumption and high in yield, and has the characteristics of environmental friendliness and wide source by taking trithiocyanuric acid as a sulfur source.
Description
Technical Field
The invention belongs to the technical field of metal sulfide material preparation, and particularly relates to a process for preparing a metal sulfide.
Background
Transition Metal Sulfides (TMS) are receiving attention due to their excellent physical and chemical properties, and are widely used in various fields such as catalysis, energy, environment, photoelectricity, and the like. For example, due to MxSyCan be subjected to conversion reaction with lithium ions and the lithium ions can be in a layered MS2The TMS material is separated from the graphene and embedded, so that the TMS material has higher theoretical specific capacity than the graphene, and becomes one of main candidate materials of the lithium battery anode material. TMS has a polar thiophilic surface and strong affinity with soluble polysulfide, so that the dissolution of lithium (poly) sulfide in electrolyte in the discharging process is avoided, and the TMS is favorable for being used as a high-efficiency electrode of a lithium-sulfur battery. Two-dimensional MS2Single or multi-layer MS with strong light response capability and adjustable optical band gap, especially atomic thickness2The carrier diffusion distance can be shortened, and the charge recombination rate can be reduced, so that the carrier diffusion distance and the charge recombination rate are ideal materials for constructing high-performance electronic/optoelectronic devices. The gap between the valence band and the conduction band of TMS is relatively narrow, and TMS-based materials generally have better electrical conductivity than metal oxides, giving them remarkable electrocatalytic properties, and thus are widely used for electrolysis of water and electrocatalysis of CO2Reduction, and the like. In addition, TMS can generate reversible redox reaction in alkaline electrolyte, and is one of the most promising high-energy supercapacitor electrode materials.
In general, the current methods for preparing TMS can be briefly summarized as solvothermal methods, hydrothermal methods, vapor deposition methods, and the like. The solvothermal method and the hydrothermal method require higher reaction temperature and longer reaction time, and particularly relate to S2-、S、H2S and the likeAnd (4) adding excessive sulfur source for reaction. For example, the Lou topic group prepares core-shell structure Zn-Co-S by using core-shell structure Zn/Co-ZIF as a template and thioacetamide as a sulfur source, wherein the reaction temperature is 150 ℃, and the feeding molar ratio of metal ions to sulfur element is 1:20(p.zhang, b.y.guan, l.yu, x.w.lou, angelw.chem.int.ed.2017, 56,7141.); xiiaoei Yang et al use ethylenediamine as solvent, thiourea as sulfur source, and proceed thermal reaction at 160 deg.C for 48h in Ti3C2CdS grows on MXene substrate. Wherein the feeding molar ratio of Cd ions to thiourea is 1: 3(r.xiao, c.x.zhao, z.y.zou, x.f.yang, et al, appl.catal.b-environ.2019, 118382); hao Yu and its collaborators with MoO3Is molybdenum source, KSCN is sulfur source, the feeding molar ratio of Mo to S is 1:4, after hydrothermal for 12h at 200 ℃, the mixture is heated in TiO2MoS is successfully loaded on the nano-rod2(Y.P.Liu, Y.H.Li, F.Peng, Hao Yu, et al, appl.Catal.B-environ.2019,241, 236). The vapor deposition process is more complicated, for example, the Gengfeng Zheng topic group is NiMoO4Nanofibers and S powder as precursors, NiMoO4The feeding molar ratio of S to S is 1: 21, vacuumizing, introducing Ar as protective gas, and preparing NiS successfully by (Chemical Vapor Deposition, CVD) method at 400 DEG C2-MoS2Nanofibers (t.c.an, y.wang, j.tang, w.g.f.zheng, et a, j.mater.chem.a,2016,4, 13439). It can be seen that in the three main preparation methods described above, the utilization of the sulfur source is not high, and most of S2-、S、H2S does not participate in the reaction and is discharged as waste liquid and tail gas. Although it can be subsequently processed, there will still be a small amount of S2-Enter the atmosphere or water body and pollute the environment. The method for preparing TMS by using the trithiocyanuric acid as the sulfur source has the characteristics of easily obtained raw materials, high yield, no pollution, accordance with the sustainable development strategy and the like, and the feeding molar ratio of the trithiocyanuric acid to the metal acetate is basically consistent with the stoichiometric ratio of the metal to the sulfur in the product, so that the feeding amount of the S element in the experiment can be accurately controlled, and the utilization rate of the sulfur source is improved.
Disclosure of Invention
In view of the above-mentioned disadvantages of the prior art, the present invention aims to provide a method for preparing metal sulfide from trithiocyanuric acid, DMF and metal acetate.
The technical scheme adopted by the invention is as follows:
a method for producing a metal sulfide, comprising the steps of:
1) adding trithiocyanuric acid into dimethyl formamide to form yellow clear and transparent solution A, wherein the concentration of the trithiocyanuric acid in the solution A is 0.2-1.0 mol/L;
2) adding metal acetate into dimethyl formamide to form a clear solution B, wherein the concentration of metal ions in the solution B is 0.1-0.5 mol/L;
3) under the assistance of ultrasound or stirring, the solution A is dropwise added into the solution B, and precipitates are rapidly separated out; wherein in the mixed solution A and solution B, the feeding molar ratio of the metal ions to the trithiocyanuric acid is the same as the stoichiometric ratio of the metal to the sulfur in the target metal sulfide;
4) separating and collecting the precipitate, and performing heat treatment on the precipitate in a manner that: raising the temperature to 400-800 ℃ at a heating rate of 1-20 ℃/min in an inert atmosphere, preserving the temperature for 0.5-10 h, and then cooling to room temperature to obtain the corresponding metal sulfide.
In the invention, when cyanuric acid is used as a sulfur source and metal acetate is used as a metal source, cyanuric acid ionizes cyanuric acid and hydrogen ions in a solution, metal acetate ionizes metal ions and acetate, and cyanuric acid and metal ions are combined to generate cyanuric acid metal salt precipitate. During the subsequent heat treatment, the metal cyanurates decompose to metal sulphides. And the feeding molar ratio of the trithiocyanuric acid to the metal acetate is basically consistent with the stoichiometric ratio of the metal to the sulfur in the product, so that the feeding amount of the S element in the experiment can be accurately controlled, and the utilization rate of the sulfur source is improved. It should be noted that, in the present invention, metal acetate should be specifically used as the metal source, and other metal salts of acid groups (such as sulfate, nitrate, hydrochloride, and acetylacetone) cannot be used for preparing metal sulfide according to the method.
In the steps, the following specific reagents and parameters can be adopted for realizing:
in step 2), the metal acetate may be anhydrous or anhydrous acetate, including any one or a combination of several of cobalt acetate, nickel acetate, copper acetate, zinc acetate, silver acetate, and cadmium acetate in any proportion.
In the steps 1) and 2), the preparation temperature of the solution A and the solution B is 15-50 ℃, and the mixing temperature of the solution A and the solution B can be set to be 25-50 ℃.
In the step 4), the molar ratio of the metal ions to the trithiocyanuric acid in the mixed solution A and the mixed solution B can be set to be 1: 1-3: 1.
In step 4), the precipitate may be separated by vacuum filtration.
In the step 4), the inert atmosphere can be selected to be N2Or Ar.
The metal sulfide prepared by the preparation method comprises the following component MxSyWherein M can be any one or combination of several of Co, Ni, Cu, Zn, Ag and Cd in any proportion (specifically determined according to the added metal source), S is sulfur element, and x and y are stoichiometric numbers after the metal salt and trithiocyanuric acid react. The metal sulfide obtained by the method is an aggregate of nano/submicron particles with the size of 100-500 nm, and has high purity, good crystallinity and high yield.
The metal sulfide prepared by the method has the characteristics of high purity, good crystallinity, high yield, large specific surface area, controllable structural unit, good stability and the like, and can be used for battery electrodes, catalysts, semiconductors and the like.
Drawings
FIG. 1 is a scanning electron microscope image of the nickel sulfide prepared in example 1, wherein the morphology is that nanoparticles are agglomerated into blocks with the size of 300 nm-500 nm.
FIG. 2 is the XRD ray diffraction pattern of the nickel sulfide prepared in example 1, and it can be seen that the position of the diffraction peak is consistent with the result reported in standard card PDF #12-0041, and the phase of the product can be judged to be NiS.
FIG. 3 is a scanning electron microscope image of cobalt sulfide prepared in example 2, in which nanoparticles having a morphology of 100nm to 150nm are agglomerated to form a larger block.
FIG. 4 is the XRD ray diffraction pattern of the copper sulfide prepared in example 4, and it can be seen that the position of the diffraction peak is consistent with the result reported in standard card PDF #29-0578, and the phase of the product can be judged to be Cu1.96S。
FIG. 5 is the XRD ray diffraction pattern of the silver sulfide prepared in example 5, and it can be seen that the position of the diffraction peak is consistent with the result reported by the standard card PDF #14-0072, and the phase of the product can be judged to be Ag2S。
Detailed Description
The invention is further elucidated with reference to the figures and embodiments.
Example 1
1) Adding 0.320g of trithiocyanuric acid into 5ml of DMF, and stirring at room temperature until a yellow clear transparent solution is formed, and marking as a solution A;
2) 0.450g of nickel acetate tetrahydrate (Ni (CH)3COO)2·4H2O) is added to 5ml of DMF and stirred at 50 ℃ until a clear solution is formed, which is marked as solution B;
3) under the stirring at room temperature, dropwise adding the solution A into the solution B, and immediately turning turbid with continuous separation of brown precipitate;
4) collecting the brown precipitate by vacuum filtration, washing with distilled water and ethanol for three times, and drying at constant temperature of 60 ℃ under vacuum for 12 h;
5) carrying out heat treatment on the dried precipitate, wherein the heat treatment process comprises the following steps: in N2Heating to 600 ℃ at the speed of 5 ℃/min in the atmosphere, preserving the heat for 2h, cooling to room temperature along with the furnace, and taking out to obtain the nickel sulfide.
The scanning electron microscope picture of the nickel sulfide prepared in this example is shown in fig. 1, and the XRD ray diffraction pattern is shown in fig. 2. As can be seen, the phase of the nickel sulfide prepared in the example is NiS, and the elemental analysis shows that the mass ratio of Ni to S is 1:1, and the particle size is 300nm to 500 nm.
Example 2
1) 0.320g trithiocyanuric acid is added to 5ml DMF and stirred vigorously at 30 ℃ until a yellow clear transparent solution is formed, noted solution A
2) 0.450g of cobalt acetate tetrahydrate (Co (CH)3COO)2·4H2O) is added to 5ml of DMF and stirred vigorously at 50 ℃ until a clear solution is formed, which is marked as solution B;
3) stirring at 30 ℃, dropwise adding the solution A into the solution B, and immediately turning turbid with continuous separation of brown precipitate (the mass ratio of Co to S is 1: 1);
4) carrying out vacuum filtration on the brown precipitate, washing the brown precipitate with distilled water and ethanol for three times, and then drying the brown precipitate for 12 hours at the constant temperature of 60 ℃ under the vacuum condition;
5) carrying out heat treatment on the dried precipitate, wherein the heat treatment process comprises the following steps: in N2Respectively heating to 500 ℃ at the speed of 10 ℃/min in the atmosphere, preserving the heat for 2h, then cooling to room temperature along with the furnace, and taking out to obtain the cobalt sulfide.
A scanning electron microscope photograph of the cobalt sulfide prepared in this example is shown in fig. 3. The cobalt sulfide phase is Co1- xS, the particle size is 150 nm-200 nm.
Example 3
1) 0.320g trithiocyanuric acid is added to 5ml DMF and stirred vigorously at 40 ℃ until a yellow clear transparent solution is formed, noted solution A
2) 0.396g of zinc acetate dihydrate (Zn (CH)3COO)2·2H2O) is added into 5ml of DMF, and stirred vigorously at 50 ℃ until a clear solution is formed, and is marked as a solution B;
3) stirring at 40 ℃, dropwise adding the solution A into the solution B, and instantly turning turbid with continuous precipitation of white precipitate (the mass ratio of Zn to S is 1: 1);
4) carrying out vacuum filtration on the white precipitate, washing the white precipitate with distilled water and ethanol for three times, and then drying the white precipitate for 12 hours at a constant temperature of 60 ℃ under a vacuum condition;
5) carrying out heat treatment on the dried precipitate, wherein the heat treatment process comprises the following steps: in N2Respectively heating to 400 ℃ at the speed of 2 ℃/min in the atmosphere, preserving the heat for 2h, then cooling to room temperature along with the furnace, and taking out to obtain the zinc sulfide.
The phase of the zinc sulfide prepared in this example is ZnS, and elemental analysis shows that the mass ratio of Zn to S is 1:1, and the particle size is about 100nm to 300 nm.
Example 4
1) 0.320g trithiocyanuric acid is added to 5ml DMF and stirred vigorously at 50 ℃ until a yellow clear transparent solution is formed, noted solution A
2) 0.720g of copper acetate monohydrate (Cu (CH)3COO)2·H2O) is added to 5ml of DMF and stirred vigorously at 50 ℃ until a clear solution is formed, which is marked as solution B;
3) stirring at 50 ℃, dropwise adding the solution A into the solution B, and immediately turning turbid with continuous precipitation of vermilion (the mass ratio of Cu to S is 2: 1);
4) carrying out vacuum filtration on the vermilion precipitate, washing the vermilion precipitate with distilled water and ethanol for three times, and then drying the vermilion precipitate for 12 hours at the constant temperature of 60 ℃ under the vacuum condition;
5) carrying out heat treatment on the dried precipitate at different temperatures, wherein the heat treatment process comprises the following steps: in N2Respectively heating to 800 ℃ at the speed of 5 ℃/min in the atmosphere, preserving the heat for 2h, then cooling to room temperature along with the furnace, and taking out to obtain the copper sulfide.
The XRD ray diffraction pattern of the copper sulfide prepared in this example is shown in FIG. 4, the phase of the copper sulfide is Cu1.96And S, wherein the ratio of the mass of Cu to the mass of S is about 2:1, and the particle size is about 150nm to 300 nm.
Example 5
1) 0.320g trithiocyanuric acid is added to 5ml DMF and stirred vigorously at room temperature until a yellow clear transparent solution is formed, noted as solution A
2) 0.602g (CH)3COOAg) is added into 5ml DMF and stirred vigorously at 50 ℃ until a clear solution is formed and is marked as a solution B;
3) under the stirring at room temperature, dropwise adding the solution A into the solution B, wherein the solution becomes turbid immediately and continuously separates out with vermilion precipitate (the mass ratio of Ag to S is 2: 1);
4) carrying out vacuum filtration on the yellow precipitate, washing the yellow precipitate with distilled water and ethanol for three times, and then drying the yellow precipitate for 12 hours at the constant temperature of 60 ℃ under the vacuum condition;
5) carrying out heat treatment on the dried precipitate at different temperatures, wherein the heat treatment process comprises the following steps: in N2Respectively heating to 500 ℃ at the speed of 20 ℃/min in the atmosphere, preserving the heat for 2h, then cooling to room temperature along with the furnace, and taking out to obtain the silver sulfide.
The XRD ray diffraction pattern of the silver sulfide prepared in this example is shown in FIG. 5, and the component is Ag2And S, wherein the material mass ratio of Ag to S is 2:1, and the particle size is about 150nm to 250 nm.
Example 6
1) 0.320g trithiocyanuric acid is added to 5ml DMF and stirred vigorously at 15 ℃ until a yellow clear transparent solution is formed, noted solution A
2) 0.481g of cadmium acetate dihydrate (Cd (CH)3COO)2·2H2O) is added to 5ml of DMF and stirred vigorously at 50 ℃ until a clear solution is formed, which is marked as solution B;
3) stirring at 25 ℃, dropwise adding the solution A into the solution B, and enabling the solution to become turbid immediately and continuously separate out along with white precipitate (the mass ratio of Cd to S is 1: 1);
4) carrying out vacuum filtration on the white precipitate, washing the white precipitate with distilled water and ethanol for three times, and then drying the white precipitate for 12 hours at a constant temperature of 60 ℃ under a vacuum condition;
5) carrying out heat treatment on the dried precipitate, wherein the heat treatment process comprises the following steps: in N2Respectively heating to 700 ℃ at the speed of 5 ℃/min in the atmosphere, preserving the heat for 2h, then cooling to room temperature along with the furnace, and taking out to obtain the cadmium sulfide.
The silver sulfide component prepared in this example is CdS, and elemental analysis shows that the mass ratio of Ag to S is 1:1, and the particle size is about 100nm to 150 nm.
Example 7
1) 0.320g trithiocyanuric acid is added to 5ml DMF and stirred vigorously at 35 ℃ until a yellow clear transparent solution is formed, noted solution A
2) 0.113g of nickel acetate tetrahydrate (Ni (CH)3COO)2·4H2O) and 0.225gAdding to 5ml of DMF, and stirring vigorously at 50 ℃ until a clear solution is formed, which is marked as solution B;
3) stirring at 35 ℃, dropwise adding the solution A into the solution B, and immediately turning turbid with a tan precipitate (mass ratio of Ni, Co and S is 1:2: 4);
4) carrying out vacuum filtration on the brown precipitate, washing the brown precipitate with distilled water and ethanol for three times, and then drying the brown precipitate for 12 hours at the constant temperature of 60 ℃ under the vacuum condition;
5) carrying out heat treatment on the dried precipitate, wherein the heat treatment process comprises the following steps: in N2Respectively heating to 600 ℃ at the speed of 12 ℃/min in the atmosphere, preserving the heat for 2h, then cooling to room temperature along with the furnace, and taking out to obtain the nickel-cobalt binary sulfide.
The phase of the nickel cobalt binary sulfide prepared in this example is NiCo2S4The element analysis shows that the mass ratio of Ni, Co and S is 1:2:4, and the particle size is 150 nm-200 nm.
Finally, the above examples are only examples of the invention and are not intended to limit the invention, and many variations are possible. Therefore, all the technical solutions obtained by carrying out equivalent substitutions or equivalent transformations from the disclosure of the present invention fall within the protection scope of the present invention.
Claims (7)
1. A method for producing a metal sulfide, characterized by comprising the steps of:
1) adding trithiocyanuric acid into dimethyl formamide to form yellow clear and transparent solution A, wherein the concentration of the trithiocyanuric acid in the solution A is 0.2-1.0 mol/L;
2) adding metal acetate into dimethyl formamide to form a clear solution B, wherein the concentration of metal ions in the solution B is 0.1-0.5 mol/L;
3) under the assistance of ultrasound or stirring, the solution A is dropwise added into the solution B, and precipitates are rapidly separated out; wherein in the mixed solution A and solution B, the feeding molar ratio of the metal ions to the trithiocyanuric acid is the same as the stoichiometric ratio of the metal to the sulfur in the target metal sulfide;
4) separating and collecting the precipitate, and performing heat treatment on the precipitate in a manner that: raising the temperature to 400-800 ℃ at a heating rate of 1-20 ℃/min in an inert atmosphere, preserving the temperature for 0.5-10 h, and then cooling to room temperature to obtain the corresponding metal sulfide.
2. The preparation method according to claim 1, wherein in the step 2), the metal acetate is anhydrous or hydrous acetate and comprises any one or combination of cobalt acetate, nickel acetate, copper acetate, zinc acetate, silver acetate and cadmium acetate in any proportion.
3. The preparation method according to claim 1, wherein in steps 1) and 2), the preparation temperature of the solution A and the solution B is 15-50 ℃, and the mixing temperature of the solution A and the solution B is 25-50 ℃.
4. The method according to claim 1, wherein in the step 4), the molar ratio of the metal ion to the trithiocyanuric acid in the mixed solution A and solution B is 1:1 to 3: 1.
5. The process according to claim 1, wherein in step 4), the precipitate is separated by vacuum filtration.
6. The method of claim 1, wherein in step 4), the inert atmosphere is N2Or Ar.
7. A metal sulfide produced by the production method according to claim 1 to 5, characterized in that: component MxSyM can be any one or combination of several of Co, Ni, Cu, Zn, Ag and Cd in any proportion, S is sulfur element, and x and y are stoichiometric numbers after the metal salt reacts with trithiocyanuric acid; the obtained metal sulfide is an aggregate of nano/submicron particles with the size of 100-500 nm, and has high purity, good crystallinity and high yield.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112010353A (en) * | 2020-09-04 | 2020-12-01 | 吉林大学 | Metal sulfide nano material and preparation method and application thereof |
| CN113184894A (en) * | 2021-05-08 | 2021-07-30 | 合肥工业大学 | One-dimensional heterogeneous nano material of silver sulfide and cobalt sulfide and preparation method thereof |
| CN115007176A (en) * | 2022-05-13 | 2022-09-06 | 江苏亚泰化工有限公司 | Double-shell ZnS @ ZnxCo1-xS catalyst and synthetic method and application thereof |
| CN116495770A (en) * | 2023-04-28 | 2023-07-28 | 西安电子科技大学 | Plasmon enhanced copper-based sulfide semiconductor and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107126964A (en) * | 2017-04-24 | 2017-09-05 | 湖南大学 | A kind of preparation method of regular octahedron cadmium sulfide and application |
| CN109663599A (en) * | 2018-12-29 | 2019-04-23 | 西安交通大学 | A kind of preparation and its application of the octahedra Cd-Co binary sulfide of pattern size tunable |
-
2020
- 2020-04-10 CN CN202010281320.4A patent/CN111362321A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107126964A (en) * | 2017-04-24 | 2017-09-05 | 湖南大学 | A kind of preparation method of regular octahedron cadmium sulfide and application |
| CN109663599A (en) * | 2018-12-29 | 2019-04-23 | 西安交通大学 | A kind of preparation and its application of the octahedra Cd-Co binary sulfide of pattern size tunable |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112010353A (en) * | 2020-09-04 | 2020-12-01 | 吉林大学 | Metal sulfide nano material and preparation method and application thereof |
| CN113184894A (en) * | 2021-05-08 | 2021-07-30 | 合肥工业大学 | One-dimensional heterogeneous nano material of silver sulfide and cobalt sulfide and preparation method thereof |
| CN115007176A (en) * | 2022-05-13 | 2022-09-06 | 江苏亚泰化工有限公司 | Double-shell ZnS @ ZnxCo1-xS catalyst and synthetic method and application thereof |
| CN115007176B (en) * | 2022-05-13 | 2024-03-08 | 江苏亚泰化工有限公司 | Double-shell ZnS@Zn x Co 1-x S catalyst and synthesis method and application thereof |
| CN116495770A (en) * | 2023-04-28 | 2023-07-28 | 西安电子科技大学 | Plasmon enhanced copper-based sulfide semiconductor and preparation method and application thereof |
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