CN106927499A - A kind of preparation method of multicomponent compound metal sulfide - Google Patents
A kind of preparation method of multicomponent compound metal sulfide Download PDFInfo
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- CN106927499A CN106927499A CN201710267871.3A CN201710267871A CN106927499A CN 106927499 A CN106927499 A CN 106927499A CN 201710267871 A CN201710267871 A CN 201710267871A CN 106927499 A CN106927499 A CN 106927499A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G11/00—Compounds of cadmium
- C01G11/02—Sulfides
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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
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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
- B01J27/043—Sulfides with iron group metals or platinum group metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/12—Sulfides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/11—Sulfides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/08—Sulfides
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The present invention is a kind of preparation method of multicomponent compound metal sulfide, is comprised the following steps：1）0.1 gram to 1 gram sulfur-bearing metal complex is put into the high boiling organic solvent of the mL of 20 mL 100, uniform solution is obtained；2）By the uniform solution under stirring, heating response adds the uniform solution of another sulfur-bearing metal complex after relevant temperature is reached, and continues isothermal reaction 5 to 20 minutes；3）After cooling, centrifugal treating is carried out to product and takes gained solid, dried with hexamethylene and deionized water washed product and after being centrifuged off accessory substance and impurity in succession, obtain product composition metal sulfide.The preparation method of the new multicomponent composition metal sulfide that the present invention is provided, simple to operate, reaction environment is friendly, and controllability is strong, can efficiently separate light induced electron and hole, and adjusts the energy gap of photochemical catalyst, and then improves photocatalysis efficiency.
Description
Technical field
The invention belongs to technical field of nano material, a kind of new multicomponent composition metal sulfide is particularly related to
Preparation method.
Background technology
With society high speed development, environmental pollution and energy scarcity problem faced as human kind sustainable development two
Big challenge.As one kind cleaning, the cheap and reproducible energy, the energy and ring that are developed into solving to become increasingly conspicuous of solar energy
The key of border problem.Photocatalysis technology has because it is converted into Hydrogen Energy, self-cleaning surface technology and photocatalytic degradation in solar energy
The application of the aspects such as machine compound is increasingly paid close attention to by people.With TiO2Be represent traditional photochemical catalyst because its band gap it is wide
(3.2 eV) is narrow, can only respond ultraviolet and near ultraviolet ray, and the utilization rate to solar energy is low (about 5%), greatly restricts
Its marketing development, therefore instantly more sight have turned to transient metal sulfide.
The performance of CdS is ideal in metal sulfide, is to use more sulfide semiconductor light during photocatalysis is studied
Catalyst, its forbidden band broadband is 2.4 eV, can absorb visible ray.But single CdS is unstable under light illumination, Yi Fa
The third contact of a total solar or lunar eclipse corrodes, and its catalysis activity is declined rapidly.So we select to be combined CdS and other metal sulfides, make both shapes
Into CdS-MS (M=Zn, Cu, Ni, Fe etc.) composition metal sulfide, this way can be by adjusting Cd and M metallic atoms
Number ratio, the forbidden band of product is adjusted to the width for being best suitable for light-catalyzed reaction.
The preparation method of current metal sulfide mainly has hydro-thermal method, microemulsion method, solvent-thermal process method, sol-gel
Method and template etc..These methods all have the advantage of itself at corresponding aspect, but there is also certain defect simultaneously.Such as water
The corresponding equipment requirement of hot method is higher；The raw material that sol-gel process is used is costly and more long the time required to reaction；Template
Then there are some limitations because of matrix material in method etc.；
Therefore, in order to photocatalysis research can more effectively be applied in practice, seek a kind of new, simplicity, more perfect
Composition metal sulfide preparation method be necessary.
The content of the invention
In order to solve the above problems, the present invention provides a kind of preparation method of new multicomponent composition metal sulfide, the party
Method effectively prevents light induced electron compound with hole, improves the efficiency of its photochemical catalyzing.
In order to achieve the above object, the present invention is achieved by the following technical solutions：
The present invention is a kind of preparation method of multicomponent compound metal sulfide, and preparation method comprises the following steps：
1）0.1 gram to 1 gram sulfur-bearing metal complex is put into the high boiling organic solvent of 20 mL-100 mL, obtains homogeneous molten
Liquid；
2）By the uniform solution under stirring, heating response is added another containing sulfur metal after relevant temperature is reached
The uniform solution of complex, continues isothermal reaction 5 to 20 minutes；
3）After cooling, centrifugal treating is carried out to product and takes gained solid, in succession with hexamethylene and deionized water washed product and from
The heart is dried after removing accessory substance and impurity, obtains product composition metal sulfide；Oleic acid after centrifugation is recyclable, reduces into
This, reduces environmental pollution.
Further improvement of the present invention is：In the step 1）Employed in sulfur-bearing metal complex metallic element
Species includes：Cd、Zn、Cu、Ni、Fe、Co、Mn.
Further improvement of the present invention is：In the step 1）In, the sulfur-bearing metal complex is organic in higher boiling
Solution temperature in solvent is 100 DEG C to 160 DEG C.
Further improvement of the present invention is：In the step 2）Middle heating-up temperature is 220 DEG C to 320 DEG C, and final anti-
It is higher than another sulfur-bearing metal complex decomposition temperature to answer temperature.
Further improvement of the present invention is：In the step 1）Middle high boiling organic solvent its boiling point is matched somebody with somebody containing sulfur metal
On compound decomposition temperature.
Further improvement of the present invention is：In the step 2）In after add another sulfur-bearing metal complex heat
Decomposition temperature must be higher than step 1）The decomposition temperature of the middle sulfur-bearing metal complex for first adding.
Further improvement of the present invention is：Presoma is done with sulfur-bearing metal complex.
Further improvement of the present invention is：In the step 1）In, sulfur-bearing metal complex is closed for mercaptobenzothiazoler
Cadmium or mercaptobenzothiazoler close copper.
Further improvement of the present invention is：In the step 2）In, another sulfur-bearing metal complex is sulfydryl benzo
Thiazole closes zinc or mercaptobenzothiazoler closes copper or mercaptobenzothiazoler closes nickel.
The beneficial effects of the invention are as follows：Liquid phase thermal decomposition method of the present invention, it is simple to operate, it is environment-friendly, obtain
The composition metal sulfide that nano particle is homogeneous, size, pattern, atomic ratio are controllable, effectively prevent light induced electron with it is empty
Being combined for cave, improves the efficiency of its photochemical catalyzing.
Brief description of the drawings
Fig. 1 is the SEM figures of CdS-ZnS prepared by the embodiment of the present invention one.
Fig. 2 is the SEM figures of CdS-CuS prepared by the embodiment of the present invention three.
Fig. 3 is the SEM figures of CdS-NiS prepared by the embodiment of the present invention four.
Specific embodiment
In order to deepen the understanding of the present invention, the present invention is described further below in conjunction with drawings and Examples, should
Embodiment is only used for explaining the present invention that not low protection scope of the present invention is constituted and limited.
As Figure 1-3, the present invention is a kind of preparation method of multicomponent compound metal sulfide, it is characterised in that：It is described
Preparation method is comprised the following steps：
1）0.1 gram to 1 gram sulfur-bearing metal complex is put into the high boiling organic solvent of 20 mL-100 mL, obtains homogeneous molten
Liquid；
2）By the uniform solution under stirring, heating response is added another containing sulfur metal after relevant temperature is reached
The uniform solution of complex, continues isothermal reaction 5 to 20 minutes；
3）After cooling, centrifugal treating is carried out to product and takes gained solid, in succession with hexamethylene and deionized water washed product and from
The heart is dried after removing accessory substance and impurity, obtains product composition metal sulfide.
Wherein：In the step 1）Employed in the metallic element species of sulfur-bearing metal complex include：Cd、Zn、Cu、
Ni、Fe、Co、Mn；
In the step 1）In, solution temperature of the sulfur-bearing metal complex in high boiling organic solvent is 100 DEG C to 160
℃。
In the step 2）Middle heating-up temperature is 220 DEG C to 320 DEG C, and end reaction temperature contains sulfur metal higher than another
Complex decomposition temperature；
In the step 1）Its boiling point of middle high boiling organic solvent is on sulfur-bearing metal complex decomposition temperature.
In the step 2）In after the heat decomposition temperature of another sulfur-bearing metal complex that adds must be higher than step 1）In
The decomposition temperature of the sulfur-bearing metal complex for first adding；
Presoma is done with sulfur-bearing metal complex, sulfur-bearing metal complex is by the organic ligand containing sulfydryl（Including sulfydryl benzo thiophene
Azoles, lauryl mercaptan, Cys, mercaptoethanol, benzenethiol, TGA etc.）, it is corresponding with the synthesis of corresponding soluble metallic salt
Metal complex.
The step 1）In, sulfur-bearing metal complex is that mercaptobenzothiazoler closes cadmium or mercaptobenzothiazoler closes copper.
In the step 2）In, another sulfur-bearing metal complex is that mercaptobenzothiazoler closes zinc or mercaptobenzothiazoler is closed
Copper or mercaptobenzothiazoler close nickel.
Embodiment one
0.44 g mercaptobenzothiazolers conjunction cadmium is added in the there-necked flask of 250 mL for filling 45 mL oleic acid, is persistently stirred
Mix be heated to 100 DEG C make solid dissolving after, continuing to be heated to 240 DEG C of isothermal reactions, to thermally decompose 5 minutes complex complete, then adds
Heat closes the oleic acid solutions of zinc to addition mercaptobenzothiazoler after 285 DEG C, and its mass volume ratio is 0.16 g:15 mL, constant temperature adds
Heat stops reaction after 10 minutes, gained solid is taken after centrifugal treating is carried out to product, is washed with hexamethylene and deionized water in succession
Product is simultaneously centrifuged off accessory substance and impurity, obtains product CdS-ZnS composition metal sulfide.
Embodiment two
0.44 g mercaptobenzothiazolers conjunction copper is added in the there-necked flask of 250 mL for filling 45 mL oleic acid, is persistently stirred
Mix be heated to 120 DEG C make solid dissolving after, continuing to be heated to 260 DEG C of isothermal reactions, to thermally decompose 5 minutes complex complete, then adds
Heat closes the oleic acid solutions of zinc to addition mercaptobenzothiazoler after 285 DEG C, and its mass volume ratio is 0.16 g:15 mL, constant temperature adds
Heat stops reaction after 10 minutes, gained solid is taken after centrifugal treating is carried out to product, is washed with hexamethylene and deionized water in succession
Product is simultaneously centrifuged off accessory substance and impurity, obtains product CuS-ZnS composition metal sulfide.
Embodiment three
0.44 g mercaptobenzothiazolers conjunction cadmium is added in the there-necked flask of 250 mL for filling 45 mL oleic acid, is persistently stirred
Mix be heated to 100 DEG C make solid dissolving after, continuing to be heated to 240 DEG C of isothermal reactions, to thermally decompose 5 minutes complex complete, then adds
Heat closes the oleic acid solutions of copper to addition mercaptobenzothiazoler after 260 DEG C, and its mass volume ratio is 0.16 g:15 mL, constant temperature adds
Heat stops reaction after 10 minutes, gained solid is taken after centrifugal treating is carried out to product, is washed with hexamethylene and deionized water in succession
Product is simultaneously centrifuged off accessory substance and impurity, obtains product CdS-CuS composition metal sulfide.
Example IV
0.44 g mercaptobenzothiazolers conjunction cadmium is added in the there-necked flask of 250 mL for filling 45 mL oleic acid, is persistently stirred
Mix be heated to 100 DEG C make solid dissolving after, continuing to be heated to 240 DEG C of isothermal reactions, to thermally decompose 5 minutes complex complete, then adds
Heat closes the oleic acid solutions of nickel to addition mercaptobenzothiazoler after 270 DEG C, and its mass volume ratio is 0.16 g:15 mL, constant temperature adds
Heat stops reaction after 10 minutes, gained solid is taken after centrifugal treating is carried out to product, is washed with hexamethylene and deionized water in succession
Product is simultaneously centrifuged off accessory substance and impurity, obtains product CdS-NiS composition metal sulfide.
Embodiment five
0.44 g mercaptobenzothiazolers conjunction copper is added in the there-necked flask of 250 mL for filling 45 mL oleic acid, is persistently stirred
Mix be heated to 120 DEG C make solid dissolving after, continuing to be heated to 260 DEG C of isothermal reactions, to thermally decompose 5 minutes complex complete, then adds
Heat closes the oleic acid solutions of zinc to addition mercaptobenzothiazoler after 270 DEG C, and its mass volume ratio is 0.16 g:15 mL, constant temperature adds
Heat stops reaction after 10 minutes, gained solid is taken after centrifugal treating is carried out to product, is washed with hexamethylene and deionized water in succession
Product is simultaneously centrifuged off accessory substance and impurity, obtains product CuS-NiS composition metal sulfide.
Liquid phase thermal decomposition method of the present invention, obtains homogeneous nano particle, size, pattern, atomic ratio controllable
Composition metal sulfide, effectively prevents light induced electron compound with hole, improves the efficiency of its photochemical catalyzing.
Claims (7)
1. a kind of preparation method of multicomponent compound metal sulfide, it is characterised in that：The preparation method is comprised the following steps：
0.1 gram to 1 gram sulfur-bearing metal complex is put into the high boiling organic solvent of 20 mL-100 mL, obtains homogeneous molten
Liquid；
By the uniform solution under stirring, heating response adds another kind to match somebody with somebody containing sulfur metal after relevant temperature is reached
The uniform solution of compound, continues isothermal reaction 5 to 20 minutes；
After cooling, centrifugal treating is carried out to product and takes gained solid, with hexamethylene and deionized water washed product and be centrifuged in succession
Dried after removing accessory substance and impurity, obtain product composition metal sulfide.
2. a kind of preparation method of multicomponent compound metal sulfide according to claims 1, it is characterised in that：In the step
Rapid 1）Employed in the metallic element species of sulfur-bearing metal complex include：Cd、Zn、Cu、Ni、Fe、Co、Mn.
3. a kind of preparation method of multicomponent compound metal sulfide according to claims 1, it is characterised in that：In the step
Rapid 1）In, solution temperature of the sulfur-bearing metal complex in high boiling organic solvent is 100 DEG C to 160 DEG C.
4. a kind of preparation method of multicomponent compound metal sulfide according to claims 1, it is characterised in that：In the step
Rapid 2）Middle heating-up temperature is 220 DEG C to 320 DEG C, and end reaction temperature is higher than another sulfur-bearing metal complex decomposition temperature.
5. a kind of preparation method of multicomponent compound metal sulfide according to claims 1, it is characterised in that：In the step
Rapid 1）Its boiling point of middle high boiling organic solvent is on sulfur-bearing metal complex decomposition temperature.
6. a kind of preparation method of multicomponent compound metal sulfide according to claims 1, it is characterised in that：In the step
Rapid 2）In after the heat decomposition temperature of another sulfur-bearing metal complex that adds must be higher than step 1）It is middle first add containing sulfur metal
The decomposition temperature of complex.
7. a kind of preparation method of multicomponent compound metal sulfide according to claims 1, it is characterised in that：With sulfur-bearing gold
Metal complex does presoma.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108899222A (en) * | 2018-06-26 | 2018-11-27 | 中南大学 | A kind of preparation method of electrode material for super capacitor |
| CN109252188A (en) * | 2018-09-30 | 2019-01-22 | 河北工业大学 | A kind of preparation method of nanometer nickel sulfide film |
| CN111318720A (en) * | 2020-03-04 | 2020-06-23 | 王冲 | Cubic PtCoS alloy nano-particles and preparation method thereof |
| CN112607792A (en) * | 2020-12-17 | 2021-04-06 | 中国科学技术大学 | Sodium-ion battery negative electrode material, and preparation method and application thereof |
-
2017
- 2017-04-22 CN CN201710267871.3A patent/CN106927499B/en active Active
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108899222A (en) * | 2018-06-26 | 2018-11-27 | 中南大学 | A kind of preparation method of electrode material for super capacitor |
| CN108899222B (en) * | 2018-06-26 | 2020-06-19 | 中南大学 | Preparation method of supercapacitor electrode material |
| CN109252188A (en) * | 2018-09-30 | 2019-01-22 | 河北工业大学 | A kind of preparation method of nanometer nickel sulfide film |
| CN109252188B (en) * | 2018-09-30 | 2021-05-07 | 河北工业大学 | Preparation method of nickel sulfide nano film |
| CN111318720A (en) * | 2020-03-04 | 2020-06-23 | 王冲 | Cubic PtCoS alloy nano-particles and preparation method thereof |
| CN111318720B (en) * | 2020-03-04 | 2022-10-25 | 王冲 | Cubic PtCoS alloy nano-particles and preparation method thereof |
| CN112607792A (en) * | 2020-12-17 | 2021-04-06 | 中国科学技术大学 | Sodium-ion battery negative electrode material, and preparation method and application thereof |
| CN112607792B (en) * | 2020-12-17 | 2022-07-15 | 中国科学技术大学 | Sodium-ion battery negative electrode material, and preparation method and application thereof |
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