CN114956163A - High-efficiency and environment-friendly synthetic method of high-purity stannous sulfide material in inert gas environment - Google Patents
High-efficiency and environment-friendly synthetic method of high-purity stannous sulfide material in inert gas environment Download PDFInfo
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- CN114956163A CN114956163A CN202210502144.1A CN202210502144A CN114956163A CN 114956163 A CN114956163 A CN 114956163A CN 202210502144 A CN202210502144 A CN 202210502144A CN 114956163 A CN114956163 A CN 114956163A
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- 239000011261 inert gas Substances 0.000 title claims abstract description 30
- DZXKSFDSPBRJPS-UHFFFAOYSA-N tin(2+);sulfide Chemical compound [S-2].[Sn+2] DZXKSFDSPBRJPS-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 title claims abstract description 19
- 238000010189 synthetic method Methods 0.000 title claims abstract description 9
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 20
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 16
- 239000010439 graphite Substances 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 12
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 9
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 13
- 239000002184 metal Substances 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 238000001308 synthesis method Methods 0.000 claims description 5
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims description 4
- 230000007613 environmental effect Effects 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 238000004073 vulcanization Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000002912 waste gas Substances 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 3
- 238000001704 evaporation Methods 0.000 abstract description 2
- 230000008020 evaporation Effects 0.000 abstract description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000002783 friction material Substances 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- AFNRRBXCCXDRPS-UHFFFAOYSA-N tin(ii) sulfide Chemical compound [Sn]=S AFNRRBXCCXDRPS-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000001050 lubricating effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000005083 Zinc sulfide Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011011 black crystal Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a high-efficiency and environment-friendly synthetic method of a high-purity stannous sulfide material in an inert gas environment. Firstly, uniformly mixing tin powder with the granularity of-40 meshes and sulfur powder with the granularity of-60 meshes according to the weight ratio of 10 to (2.6-3), putting the mixture into a high-purity graphite crucible, putting the graphite crucible into a low-vacuum sealed chamber, vacuumizing to 1-2Pa, filling inert gas into the sealed chamber to negative pressure (0.06-0.08MPa), then heating the sealed chamber to 200 ℃ and 500 ℃, preserving heat for 2-5h, and then cooling; the metallic tin powder and the sulfur powder are uniformly mixed in advance, a high-purity graphite crucible with very good heat conductivity is adopted, the vulcanization reaction is rapid and sufficient, the production efficiency can be greatly improved, the metallic tin powder and the sulfur powder are produced in an inert gas environment in a non-vacuum state, the temperature field is more uniform, the temperature balance of a synthesis environment is further improved, the evaporation phenomenon in the phase reaction process is greatly inhibited, the synthesis reaction is ensured to be sufficient, and the generation of waste gas and waste is greatly inhibited.
Description
Technical Field
The invention relates to a method for efficiently and environmentally synthesizing stannous sulfide, in particular to a method for efficiently and environmentally synthesizing a high-purity stannous sulfide material in an inert gas environment.
Background
The stannous sulfide is a gray black crystal with the density of 5.22g/cm3 and the melting point of 880 ℃, is nontoxic and is insoluble in water. Generally used for friction materials, a liquid lubricating film can be formed between a friction plate and a brake disc, so that the friction coefficient of the material is reduced, and the more liquid is separated out along with the increase of the temperature, the more obvious the lubricating effect is. Compared with a metal-containing friction material, the safety of stannous sulfide is higher, and with the improvement of the attention of Europe and North America countries to highway heavy metal pollution, the application of the tin-based friction material is greatly increased, and the application prospect is wide. In addition, the optical direct band gap and the indirect band gap of the tin sulfide are respectively 1.3-1.5 eV and 1.0-1.1 eV, and the tin sulfide has good spectral matching with visible light in solar radiation, so the tin sulfide is very suitable for being used as a light absorption layer in a solar cell and is a very potential solar cell material.
At present, the existing stannous sulfide synthesis method has the disadvantages of low synthesis efficiency, insufficient reaction and more generated waste gas and waste.
Disclosure of Invention
The invention aims to provide a high-efficiency and environment-friendly synthetic method of a high-purity stannous sulfide material in an inert gas environment, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
the high-efficiency and environment-friendly synthetic method of the high-purity stannous sulfide material in the inert gas environment comprises the following steps:
step one, uniformly mixing metal tin powder (-40 meshes) and sulfur powder (-60 meshes) according to the weight ratio of 10 to (2.6-3), putting the mixture into a high-purity graphite crucible, and putting the graphite crucible into a closed vacuum chamber;
step two, vacuumizing the closed vacuum chamber to 1-2Pa, and filling inert gas to negative pressure (0.08-0.09 MPa);
step three, heating the sealed vacuum chamber to 200-;
and step four, after cooling to room temperature, vacuumizing to 2-10MPa, then filling inert gas to 0.1MPa, and taking out the graphite crucible composition.
As a still further scheme of the invention: the granularity of the metallic tin powder and the sulfur powder in the first step is wide in application range, and the metallic tin powder and the sulfur powder are fully mixed in advance to be in a uniform state, so that the phase can be rapidly and fully synthesized.
As a still further scheme of the invention: in the first step, the container adopts a high-purity graphite crucible with high thermal conductivity, so that the heat conduction characteristic in the thermal reaction process is greatly improved, and the phase reaction is promoted to be rapid, uniform and sufficient.
As a still further scheme of the invention: and in the second step, inert gas is filled after vacuum pumping, and the reaction is synthesized under the negative pressure condition close to the atmospheric pressure, so that the uniformity of a temperature field can be ensured, few phase distillations are generated at high temperature, the reaction is rapid, the condition of generating sulfur dioxide gas is greatly reduced, and the environment-friendly and efficient reaction process is ensured.
As a still further scheme of the invention: in the third step and the fourth step, the method realizes the one-time synthesis of the high-purity stannous sulfide material, and fully embodies the high-efficiency environmental protection characteristic of the method.
Compared with the prior art, the invention has the beneficial effects that:
1. the metallic tin powder and the sulfur powder are uniformly mixed in advance, and a high-purity graphite crucible with very good heat conductivity is adopted, so that the vulcanization reaction is rapid and sufficient, and the production efficiency can be greatly improved;
2. the method is used for production in an inert gas environment in a non-vacuum state, the temperature field is more uniform, the temperature balance of the synthesis environment is further improved, the evaporation phenomenon in the phase reaction process is greatly inhibited, the synthesis reaction is ensured to be sufficient, and the generation of waste gas and waste is greatly inhibited;
3. the synthesis process achieves the aim of high efficiency and environmental protection.
Drawings
FIG. 1 is a process flow diagram of the present invention.
FIG. 2 is XRD detection diagram of stannous sulfide produced by the process of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Referring to fig. 1-2, in the embodiment of the present invention:
the first embodiment is as follows:
the high-efficiency and environment-friendly synthetic method of the high-purity stannous sulfide material in the inert gas environment comprises metallic tin powder and sulfur powder, and comprises the following steps:
step one, uniformly mixing metal tin powder (-40 meshes) and sulfur powder (-60 meshes) according to the weight ratio of 10 to (2.6-3), putting the mixture into a high-purity graphite crucible, and putting the graphite crucible into a closed vacuum chamber;
step two, vacuumizing the closed vacuum chamber to 1-2Pa, and filling inert gas to negative pressure (0.08-0.09 MPa);
step three, heating the sealed vacuum chamber to 200-;
and step four, after cooling to room temperature, vacuumizing to 2-10MPa, then filling inert gas to 0.1MPa, and taking out the graphite crucible composition.
Example two:
the high-efficiency and environment-friendly synthetic method of the high-purity stannous sulfide material in the inert gas environment comprises metallic tin powder and sulfur powder, and comprises the following steps:
step one, uniformly mixing metal tin powder (-40 meshes) and sulfur powder (-60 meshes) according to the weight ratio of 10 to (2.6-3), placing the mixture into a quartz crucible, and placing the quartz crucible into a closed vacuum chamber;
step two, vacuumizing the closed vacuum chamber to 1-2Pa, and filling inert gas to negative pressure (0.08-0.09 MPa);
step three, heating the sealed vacuum chamber to 200-;
and step four, after cooling to room temperature, vacuumizing to 2-10MPa, then filling inert gas to 0.1MPa, and taking out the quartz crucible composition.
Example three:
the high-efficiency and environment-friendly synthetic method of the high-purity stannous sulfide material in the inert gas environment comprises metallic tin powder and sulfur powder, and comprises the following steps:
step one, uniformly mixing metal tin powder (-40 meshes) and sulfur powder (-60 meshes) according to the weight ratio of 10 to (2.6-3), putting the mixture into an alumina crucible, and putting the alumina crucible into a closed vacuum chamber;
step two, vacuumizing the closed vacuum chamber to 1-2Pa, and filling inert gas to negative pressure (0.08-0.09 MPa);
step three, heating the sealed vacuum chamber to 200-;
and step four, after cooling to room temperature, vacuumizing to 2-10MPa, then filling inert gas to 0.1MPa, and taking out the alumina crucible composition.
From the first to third examples, it can be seen that the reaction is more sufficient and the efficiency is higher by the high purity graphite crucible.
The working principle of the invention is as follows:
the metal tin powder and the sulfur powder which are uniformly mixed generate a metal vulcanization reaction under the action of a proper temperature in an inert gas environment (the vulcanization process of the technical invention is also suitable for the vulcanization process of low-melting-point metal zinc so as to obtain zinc sulfide), and the reaction process can be expressed by a chemical formula as follows: sn + S-SnS, Sn + 2S-SnS 2 ，2Sn+3S＝Sn 2 S 3 Therefore, during the synthesis process, the intermediate phase may contain Sn, SnS 2 、Sn 2 S 3 S, the content of the process phase is related to the ratio of the metallic tin powder to the sulfur powder, and in order to obtain high-purity stannous sulfide and achieve the purposes of high efficiency and environmental protection, the ratio is calculated according to a theory, the mixture is uniform and the full reaction is combined, so that the high-yield stannous sulfide material with stable chemical performance and high purity can be obtained.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and/or modifications of the invention can be made, and equivalents and modifications of some features of the invention can be made without departing from the spirit and scope of the invention.
Claims (5)
1. The high-efficiency and environment-friendly synthetic method of the high-purity stannous sulfide material in the inert gas environment comprises metallic tin powder and sulfur powder, and is characterized in that:
the method comprises the following steps:
step one, uniformly mixing metal tin powder (-40 meshes) and sulfur powder (-60 meshes) according to the weight ratio of 10 to (2.6-3), putting the mixture into a high-purity graphite crucible, and putting the graphite crucible into a closed vacuum chamber;
step two, vacuumizing the closed vacuum chamber to 1-2Pa, and filling inert gas to negative pressure (0.08-0.09 MPa);
step three, heating the sealed vacuum chamber to 200-;
and step four, after cooling to room temperature, vacuumizing to 2-10MPa, then filling inert gas to 0.1MPa, and taking out the graphite crucible composition.
2. The efficient and environment-friendly synthesis method of the high-purity stannous sulfide material in the inert gas environment according to claim 1, which is characterized by comprising the following steps: the granularity of the metallic tin powder and the sulfur powder in the first step is wide in application range, and the metallic tin powder and the sulfur powder are fully mixed in advance to be in a uniform state, so that the phase can be rapidly and fully synthesized.
3. The efficient and environment-friendly synthesis method of the high-purity stannous sulfide material in the inert gas environment according to claim 1, which is characterized by comprising the following steps: in the first step, the container adopts a high-purity graphite crucible with high thermal conductivity, so that the heat conduction characteristic in the thermal reaction process is greatly improved, and the phase reaction is promoted to be rapid, uniform and sufficient.
4. The efficient and environment-friendly synthesis method of the high-purity stannous sulfide material in the inert gas environment according to claim 1, which is characterized by comprising the following steps: and in the second step, inert gas is filled after vacuum pumping, and the reaction is synthesized under the negative pressure condition close to the atmospheric pressure, so that the uniformity of a temperature field can be ensured, few phase distillations are generated at high temperature, the reaction is rapid, the condition of generating sulfur dioxide gas is greatly reduced, and the environment-friendly and efficient reaction process is ensured.
5. The efficient and environment-friendly synthesis method of the high-purity stannous sulfide material in the inert gas environment according to claim 1, which is characterized by comprising the following steps: in the third step and the fourth step, the method realizes the one-time synthesis of the high-purity stannous sulfide material, and fully embodies the high-efficiency environmental protection characteristic of the method.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115893477A (en) * | 2022-11-14 | 2023-04-04 | 昆明理工大学 | Preparation method of high-purity tin trisulfide |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105016378A (en) * | 2014-04-21 | 2015-11-04 | 渤海大学 | Preparation method of tin sulfide nanosheet |
| US20180087186A1 (en) * | 2016-09-23 | 2018-03-29 | National Chung Shan Institute Of Science And Technology | Method of producing carbide raw material |
| CN109748318A (en) * | 2019-02-18 | 2019-05-14 | 云南锡业集团（控股）有限责任公司研发中心 | A kind of preparation method of stannous sulfide |
| US20190189883A1 (en) * | 2016-05-25 | 2019-06-20 | Nippon Shokubai Co., Ltd. | Thermoelectric conversion material, thermoelectric conversion device, powder for thermoelectric conversion material, and method for producing thermoelectric conversion material |
| CN111039318A (en) * | 2019-12-05 | 2020-04-21 | 大连理工大学 | Method for preparing SnS nano material by direct current arc plasma |
| US20200207636A1 (en) * | 2017-09-07 | 2020-07-02 | Kunming Diboo Technology Co., Ltd. | Method for producing stannous sulfide |
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- 2022-05-10 CN CN202210502144.1A patent/CN114956163A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105016378A (en) * | 2014-04-21 | 2015-11-04 | 渤海大学 | Preparation method of tin sulfide nanosheet |
| US20190189883A1 (en) * | 2016-05-25 | 2019-06-20 | Nippon Shokubai Co., Ltd. | Thermoelectric conversion material, thermoelectric conversion device, powder for thermoelectric conversion material, and method for producing thermoelectric conversion material |
| US20180087186A1 (en) * | 2016-09-23 | 2018-03-29 | National Chung Shan Institute Of Science And Technology | Method of producing carbide raw material |
| US20200207636A1 (en) * | 2017-09-07 | 2020-07-02 | Kunming Diboo Technology Co., Ltd. | Method for producing stannous sulfide |
| CN109748318A (en) * | 2019-02-18 | 2019-05-14 | 云南锡业集团（控股）有限责任公司研发中心 | A kind of preparation method of stannous sulfide |
| CN111039318A (en) * | 2019-12-05 | 2020-04-21 | 大连理工大学 | Method for preparing SnS nano material by direct current arc plasma |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115893477A (en) * | 2022-11-14 | 2023-04-04 | 昆明理工大学 | Preparation method of high-purity tin trisulfide |
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