CN117105252A - Preparation method of aluminum sulfide - Google Patents
Preparation method of aluminum sulfide Download PDFInfo
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- CN117105252A CN117105252A CN202311016855.9A CN202311016855A CN117105252A CN 117105252 A CN117105252 A CN 117105252A CN 202311016855 A CN202311016855 A CN 202311016855A CN 117105252 A CN117105252 A CN 117105252A
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- Prior art keywords
- sulfide
- aluminum
- powder
- hours
- aluminum sulfide
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- COOGPNLGKIHLSK-UHFFFAOYSA-N aluminium sulfide Chemical compound [Al+3].[Al+3].[S-2].[S-2].[S-2] COOGPNLGKIHLSK-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 58
- 239000000843 powder Substances 0.000 claims abstract description 36
- 229910052742 iron Inorganic materials 0.000 claims abstract description 29
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229940056932 lead sulfide Drugs 0.000 claims abstract description 20
- 229910052981 lead sulfide Inorganic materials 0.000 claims abstract description 20
- 238000001816 cooling Methods 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000012216 screening Methods 0.000 claims abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 8
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 239000002341 toxic gas Substances 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- 229910002804 graphite Inorganic materials 0.000 description 7
- 239000010439 graphite Substances 0.000 description 7
- 238000000926 separation method Methods 0.000 description 7
- 229910052782 aluminium Inorganic materials 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 239000003517 fume Substances 0.000 description 4
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 239000012300 argon atmosphere Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical group [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000563 toxic property Toxicity 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/68—Aluminium compounds containing sulfur
- C01F7/70—Sulfides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The application relates to the technical field of chemical synthesis, in particular to a preparation method of aluminum sulfide. The method comprises the following steps: s1, uniformly mixing lead sulfide and aluminum powder to obtain a mixture; s2, wrapping and compacting the mixture by utilizing an iron sheet, roasting at 600-800 ℃ for 3-8 hours, and cooling to room temperature to obtain intermediate powder; s3, screening the intermediate powder to obtain primary clinker; s4, roasting the primary clinker at 860-950 ℃ for 3-8 hours, and cooling to room temperature to obtain aluminum sulfide powder. Solves the problems of severe reaction, toxic gas generation, incapability of separating products and raw materials and the like in the preparation process of the existing lead sulfide preparation method.
Description
Technical Field
The application relates to the technical field of chemical synthesis, in particular to a preparation method of aluminum sulfide.
Background
Aluminum sulfide is a gray solid inorganic compound, has the characteristics of high electrochemical activity, high specific surface area and conductivity, low decomposition potential, high energy density and the like, and has very wide application in the aspects of preparing metal and alloy compounds and the like in super capacitors, graphene oxide and secondary lithium batteries.
At present, the preparation method of aluminum sulfide comprises the following steps: the magnesium strip is used for igniting the mixture of the sulfur powder and the aluminum powder in the large crucible, but the reaction of preparing aluminum sulfide by igniting the sulfur powder and the aluminum powder by the magnesium strip is severe, and the potential explosion risk exists. The method is characterized in that the dried hydrogen sulfide is introduced into a vacuum furnace containing aluminum powder for heating, but the preparation of aluminum sulfide from the dried hydrogen sulfide and the aluminum powder has serious environmental pollution, long preparation period and high requirements on equipment, and meanwhile, the hydrogen sulfide has extremely toxic property. Loutfy et al (U.S. patent: 4265716) prepared aluminum sulfide at 1200 ℃ from pure carbon powder, sulfur powder and aluminum oxide powder. Huda et al prepared aluminum sulfide by carbosulfidation of aluminum oxide at 1200-1800 ℃. Both the above two preparation methods have the advantages of overhigh preparation temperature and CS 2 The generation of isothermal chamber gas, the separation of the prepared product and the raw material, and the low conversion rate of alumina. Hsu and the like prepare aluminum sulfide by using COS and alumina at 850 ℃, the temperature of the preparation method is reduced compared with the temperature of the COS and the alumina, but the COS used in the preparation is very environment-friendly, the preparation product and the raw materials cannot be separated, only 40% of the alumina is converted into the aluminum sulfide, and the equipment requirement is very high.
Disclosure of Invention
First, the technical problem to be solved
In view of the above-mentioned shortcomings and disadvantages of the prior art, the present application provides a method for preparing aluminum sulfide, which solves the problems of severe reaction, toxic gas generation, incapability of separating products and raw materials, etc. in the existing lead sulfide preparation method.
(II) technical scheme
In order to achieve the above purpose, the main technical scheme adopted by the application comprises the following steps:
a method for preparing aluminum sulfide, comprising the following steps:
s1, uniformly mixing lead sulfide and aluminum powder to obtain a mixture;
s2, wrapping and compacting the mixture by utilizing an iron sheet, roasting at 600-800 ℃ for 3-8 hours, and cooling to room temperature to obtain intermediate powder;
s3, screening the intermediate powder to obtain primary clinker;
s4, roasting the primary clinker at 860-950 ℃ for 3-8 hours, and cooling to room temperature to obtain aluminum sulfide powder.
Further, in the step S1, the molar ratio of the lead sulfide to the aluminum powder is 2-4: 2.
further, the firing is performed at 600℃for 6 hours in step S2.
Further, the firing is performed at 950℃for 5 hours in step S4.
Further, in the step S1, the molar ratio of the lead sulfide to the aluminum powder is 1:1.
further, step S2 is performed under vacuum or argon.
Further, step S4 is performed under vacuum or argon.
Further, the vacuum degree of the vacuum is 0.09-0.1 MPa.
Further, the vacuum degree of the vacuum was 0.1MPa.
The application also provides aluminum sulfide prepared by the preparation method of any technical scheme.
(III) beneficial effects
According to the preparation method of aluminum sulfide, lead sulfide and aluminum powder are used as raw materials, iron is used as a catalyst, the preparation method is simple, the raw materials are easy to obtain, and industrial production is easy to realize.
The preparation process has the advantages of no severe reaction, safety, controllability and no explosion risk. Meanwhile, no tail gas is generated in the preparation process, and no toxic gas participates.
The prepared product is easy to separate from raw materials, catalysts and impurities.
Drawings
FIG. 1 is a process flow diagram of a method for preparing aluminum sulfide according to the present application;
FIG. 2 is an XRD pattern of primary clinker in example 1 of the present application;
FIG. 3 is an XRD pattern of aluminum sulfide powder in example 1 of the present application.
Detailed Description
The following are specific embodiments of the present application, and the technical solutions of the present application are further described with reference to the accompanying drawings, but the present application is not limited to these embodiments.
The process flow chart of the aluminum sulfide preparation method provided by the application is shown in figure 1, and specifically comprises the following steps:
s1, uniformly mixing lead sulfide and aluminum powder to obtain a mixture;
s2, wrapping and compacting the mixture by utilizing an iron sheet, roasting at 600-800 ℃ for 3-8 hours, and cooling to room temperature to obtain intermediate powder;
s3, screening the intermediate powder to obtain primary clinker;
s4, roasting the primary clinker at 860-960 ℃ for 3-8 hours, and cooling to room temperature to obtain aluminum sulfide powder.
In the preparation method, lead sulfide and aluminum powder are used as raw materials, iron is used as a catalyst, and the reaction principle is shown in a formula (1):
specifically, in the step S1, lead sulfide and aluminum powder are placed in a mixer to be mixed uniformly, so as to obtain a mixture. Preferably, the aluminum powder is weighed in a glove box filled with high purity argon and anhydrous.
In the step S2, placing the iron sheet along the inner wall of the crucible, filling the mixture into the crucible containing the iron sheet, wrapping and compacting the mixture by using the iron sheet, roasting for 3-8 hours at the temperature of 500-800 ℃, and cooling to the room temperature to obtain intermediate powder and the iron sheet coated by lead. At this time, the intermediate powder includes lead sulfide, aluminum, and lead, wherein aluminum and lead are mostly in the shape of small round balls, and are partially polymerized into a block or irregular shape.
S3, screening the intermediate powder by adopting a mechanical separation method to obtain primary clinker, and carrying out oscillation separation on the iron sheet coated with lead to obtain lead and iron sheet. Specifically, pouring the intermediate powder and the iron sheet coated with lead into a mortar in a fume hood, taking out the iron sheet coated with lead by using tweezers, carrying out vibration separation to obtain lead and the iron sheet, and sieving the rest intermediate powder by adopting a mechanical separation method to remove aluminum and lead to obtain primary clinker. At this time, the primary clinker includes lead sulfide, aluminum sulfide, and a small amount of aluminum.
S4, placing the primary clinker into a crucible, roasting for 3-8 hours at the temperature of 860-960 ℃, removing impurities, cooling to room temperature, placing the crucible into a fume hood, and grinding to obtain aluminum sulfide powder.
In order that the above-described aspects may be better understood, exemplary embodiments of the present application are described in more detail below with reference to specific embodiments.
Example 1
The preparation method of the lead sulfide provided by the embodiment comprises the following steps:
s1, placing 0.2mol of lead sulfide and 0.2mol of aluminum powder into a mixer for uniformly mixing to obtain a mixture.
S2, placing the iron sheet along the inner wall of the graphite crucible, filling the mixture into the graphite crucible containing the iron sheet, wrapping and compacting the mixture by utilizing the iron sheet, roasting for 6 hours at 600 ℃ under the vacuum condition of 0.09MPa, and cooling to room temperature to obtain intermediate powder and the iron sheet coated with lead.
S3, placing the graphite crucible in a fume hood, pouring the intermediate powder and the iron sheet coated with lead into a mortar, taking out the iron sheet coated with lead by using tweezers, carrying out vibration separation to obtain lead and the iron sheet, and sieving the rest intermediate powder by adopting a mechanical separation method to remove aluminum and lead to obtain primary clinker. The XRD pattern of the primary clinker is shown in FIG. 2.
S4, placing the primary clinker in a vacuum furnace, roasting for 5 hours at the temperature of 950 ℃ under the vacuum condition of the vacuum degree of 0.1MPa, cooling to room temperature, placing the graphite crucible in a fume hood, and grinding to obtain aluminum sulfide powder. The XRD pattern of the obtained aluminum sulfide powder is shown in FIG. 3.
Example 2
The difference from example 1 is that in step S1 of example 2, 0.4mol of lead sulfide and 0.2mol of aluminum powder were placed in a mixer and mixed uniformly to obtain a mixture. In the step S2, an iron crucible is selected to replace a graphite crucible, roasting is carried out for 4 hours at the temperature of 700 ℃ under the vacuum condition with the vacuum degree of 0.09MPa, and intermediate powder and the iron sheet coated by lead are obtained after cooling to the room temperature. And in the step S4, roasting for 7 hours at the temperature of 860 ℃ under the vacuum condition of 0.09MPa to obtain aluminum sulfide powder.
The other components are the same as those in embodiment 1, and will not be described here again.
Example 3
The difference from example 1 is that in step S1 of example 3, 0.3mol of lead sulfide and 0.2mol of aluminum powder were placed in a mixer and mixed uniformly to obtain a mixture. And in the step S2, roasting for 8 hours at 600 ℃ in an argon atmosphere, and cooling to room temperature to obtain intermediate powder and a lead-coated iron sheet. And in the step S4, roasting for 6 hours at 870 ℃ under the vacuum condition of 0.09MPa to obtain aluminum sulfide powder.
The other components are the same as those in embodiment 1, and will not be described here again.
Example 4
The difference from example 1 is that in step S1 of example 4, 0.4mol of lead sulfide and 0.2mol of aluminum powder were placed in a mixer and mixed uniformly to obtain a mixture. In the step S2, a corundum crucible is selected to replace a graphite crucible, roasting is carried out for 3 hours at the temperature of 800 ℃ under the vacuum condition of 0.1MPa, and intermediate powder and a lead-coated iron sheet are obtained after cooling to the room temperature.
The other components are the same as those in embodiment 1, and will not be described here again.
Example 5
The difference from example 1 is that in this example 5, a nickel crucible was used instead of a graphite crucible in step S2, and the intermediate powder and the lead-coated iron sheet were obtained by baking at 600 c for 8 hours under vacuum conditions having a vacuum degree of 0.09MPa and cooling to room temperature. And in the step S4, roasting for 7 hours at 950 ℃ under the vacuum condition of 0.1MPa of vacuum degree to obtain aluminum sulfide powder.
The other components are the same as those in embodiment 1, and will not be described here again.
Example 6
The difference from example 1 is that in this example 6, the intermediate powder and the lead-coated iron sheet were obtained after baking at 600 c for 6 hours under an argon atmosphere in step S2 and cooling to room temperature. And in the step S4, roasting for 5 hours at the temperature of 890 ℃ under the vacuum condition of 0.1MPa to obtain aluminum sulfide powder.
The other components are the same as those in embodiment 1, and will not be described here again.
Example 7
The difference from example 1 is that in this example 7, the intermediate powder and the lead-coated iron sheet were obtained by baking at 600 c for 6 hours under an argon atmosphere in step S2 and cooling to room temperature. And in the step S4, roasting for 6 hours at the temperature of 920 ℃ under the vacuum condition of 0.1MPa to obtain aluminum sulfide powder.
The other components are the same as those in embodiment 1, and will not be described here again.
It should be understood that these examples are for the purpose of illustrating the application only and are not intended to limit the scope of the application. Furthermore, it is to be understood that various changes, modifications and/or variations may be made by those skilled in the art after reading the technical content of the present application, and that all such equivalents are intended to fall within the scope of the present application as defined in the appended claims.
Claims (10)
1. A method for preparing aluminum sulfide, which is characterized by comprising the following steps:
s1, uniformly mixing lead sulfide and aluminum powder to obtain a mixture;
s2, wrapping and compacting the mixture by utilizing an iron sheet, roasting at 600-800 ℃ for 3-8 hours, and cooling to room temperature to obtain intermediate powder;
s3, screening the intermediate powder to obtain primary clinker;
s4, roasting the primary clinker at 860-950 ℃ for 3-8 hours, and cooling to room temperature to obtain aluminum sulfide powder.
2. The method for preparing aluminum sulfide according to claim 1, wherein in the step S1, the molar ratio of the lead sulfide to the aluminum powder is 2 to 4:2.
3. the method of producing aluminum sulfide according to claim 2, wherein in the step S2, the baking is performed at 600 ℃ for 6 hours.
4. The method of producing aluminum sulfide according to claim 3, wherein in the step S4, the aluminum sulfide is baked at 950 ℃ for 5 hours.
5. The method of producing aluminum sulfide as claimed in claim 4, wherein in the step S1, a molar ratio of lead sulfide to aluminum powder is 1:1.
6. the method of producing aluminum sulfide according to claim 5, wherein the step S2 is performed under vacuum or argon.
7. The method of producing aluminum sulfide as claimed in claim 6, wherein the step S4 is performed under vacuum or argon.
8. The method of producing aluminum sulfide according to claim 7, wherein the vacuum degree of the vacuum is 0.09 to 0.1MPa.
9. The method for producing aluminum sulfide according to claim 8, wherein the vacuum is 0.1MPa.
10. An aluminum sulfide prepared by the preparation method according to any one of claims 1 to 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311016855.9A CN117105252A (en) | 2023-08-14 | 2023-08-14 | Preparation method of aluminum sulfide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311016855.9A CN117105252A (en) | 2023-08-14 | 2023-08-14 | Preparation method of aluminum sulfide |
Publications (1)
| Publication Number | Publication Date |
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| CN117105252A true CN117105252A (en) | 2023-11-24 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202311016855.9A Pending CN117105252A (en) | 2023-08-14 | 2023-08-14 | Preparation method of aluminum sulfide |
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| CN (1) | CN117105252A (en) |
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2023
- 2023-08-14 CN CN202311016855.9A patent/CN117105252A/en active Pending
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