CN112978693A - Method for preparing tin triphosphate by vapor phase method - Google Patents
Method for preparing tin triphosphate by vapor phase method Download PDFInfo
- Publication number
- CN112978693A CN112978693A CN202110255692.4A CN202110255692A CN112978693A CN 112978693 A CN112978693 A CN 112978693A CN 202110255692 A CN202110255692 A CN 202110255692A CN 112978693 A CN112978693 A CN 112978693A
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- Prior art keywords
- tin
- triphosphate
- vapor phase
- reactor
- preparing
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- XCWCJGRYIMDVQP-UHFFFAOYSA-A [O-]P([O-])(=O)OP(=O)([O-])OP(=O)([O-])[O-].[Sn+4].[O-]P([O-])(=O)OP(=O)([O-])OP(=O)([O-])[O-].[O-]P([O-])(=O)OP(=O)([O-])OP(=O)([O-])[O-].[O-]P([O-])(=O)OP(=O)([O-])OP(=O)([O-])[O-].[Sn+4].[Sn+4].[Sn+4].[Sn+4] Chemical compound [O-]P([O-])(=O)OP(=O)([O-])OP(=O)([O-])[O-].[Sn+4].[O-]P([O-])(=O)OP(=O)([O-])OP(=O)([O-])[O-].[O-]P([O-])(=O)OP(=O)([O-])OP(=O)([O-])[O-].[O-]P([O-])(=O)OP(=O)([O-])OP(=O)([O-])[O-].[Sn+4].[Sn+4].[Sn+4].[Sn+4] XCWCJGRYIMDVQP-UHFFFAOYSA-A 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000012808 vapor phase Substances 0.000 title claims abstract description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 11
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 8
- 239000012298 atmosphere Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 5
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 4
- 239000011574 phosphorus Substances 0.000 claims abstract description 4
- 239000007795 chemical reaction product Substances 0.000 claims abstract 2
- 238000001035 drying Methods 0.000 claims abstract 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- -1 tin triphosphite Chemical compound 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 9
- 238000009776 industrial production Methods 0.000 abstract description 3
- 239000010453 quartz Substances 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 238000000498 ball milling Methods 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 239000010431 corundum Substances 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/08—Other phosphides
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
Abstract
The invention discloses a method for preparing tin triphosphate by a vapor phase method, which comprises the steps of adding phosphorus and tin into a reactor, heating the reactor filled with materials to 550-600 ℃ in 1-5 h under a vacuum atmosphere or an inert atmosphere, reacting at a constant temperature for more than 24h, then cooling to 530 ℃ in 1-8 h, preserving heat for more than 2h, finally naturally cooling to room temperature, and washing and drying reaction products to obtain the tin triphosphate; the method greatly reduces the preparation cost of the tin triphosphate, simplifies the preparation conditions of the tin triphosphate, and is suitable for industrial production and market popularization and application.
Description
Technical Field
The invention relates to a method for preparing tin triphosphate by a vapor phase method, belonging to the field of preparation of phosphorized chemical materials.
Background
The tin triphosphate is a two-dimensional metal phosphide which is easy to strip and has a stable layered structure, and has high carrier mobility and adjustable band gap, so the tin triphosphate has good application prospects in the fields of sensing, energy storage, flame retardance and catalysis. At present, the main preparation method of tin triphosphate is a ball milling method, and the main preparation steps are that red phosphorus and tin powder are put into a high-energy ball mill, the high-energy ball mill is transferred to a glove box, and then the materials are ball milled to obtain the tin triphosphate; the glove box and the high-energy ball mill are expensive in equipment, and the high-energy ball mill has small space and cannot prepare tin triphosphate in large scale, so that the application of the material is rarely researched.
Disclosure of Invention
The invention provides a method for preparing tin triphosphate by a gas phase method, which is suitable for industrial production and aims to solve the problems of harsh conditions, high cost, complex operation and the like in the existing ball milling method for preparing tin triphosphate.
The molar ratio of phosphorus to tin is 2-4: 1.
The washing is sequentially washing by using hydrogen peroxide, ethanol and deionized water.
The reactor is a quartz reactor, a corundum reactor or a metal reactor.
The heating equipment is a resistance heater such as a tubular furnace, a muffle furnace and the like.
The invention has the following beneficial effects:
compared with the existing ball milling method for preparing tin triphosphate, the method effectively solves the problems of expensive equipment and low yield of tin triphosphate preparation, can complete the preparation by adopting a quartz reactor, a corundum reactor and a metal reactor with low cost, greatly reduces the preparation cost of tin triphosphate, simplifies the preparation conditions of tin triphosphate, and is suitable for industrial production and market popularization and application.
Drawings
FIG. 1 is a pictorial representation of a tin triphosphate prepared in example 1;
figure 2 is an XRD pattern of tin triphosphate prepared in example 3.
Detailed Description
The present invention is further illustrated by the following examples, but the scope of the invention is not limited to the above-described examples.
Example 1
Sealing red phosphorus and tin powder into a quartz tube in a vacuum atmosphere according to the molar ratio of 3:1, heating the quartz tube to 550 ℃ in 2h by using a muffle furnace, gasifying the red phosphorus, liquefying tin, reacting at 550 ℃ for 24h, cooling to 530 ℃ in 1h, reacting at constant temperature for 2h, naturally cooling to room temperature, taking out a product, and sequentially washing with hydrogen peroxide, absolute ethyl alcohol and deionized water for 1 time respectively to obtain a tin triphosphate product (figure 1).
Example 2
Sealing red phosphorus and tin powder into a quartz tube in a vacuum atmosphere according to a molar ratio of 4:1, heating the quartz tube to 600 ℃ in 4h by using a muffle furnace, gasifying the red phosphorus, liquefying tin, reacting at a constant temperature of 600 ℃ for 26h, cooling to 530 ℃ in 2h, reacting at a constant temperature for 3h, naturally cooling to room temperature, taking out a product, and sequentially washing with hydrogen peroxide, absolute ethyl alcohol and deionized water for 1 time respectively to obtain a tin triphosphate product.
Example 3
Sealing red phosphorus and tin powder at a molar ratio of 8:3 in a quartz tube under nitrogen atmosphere, heating the quartz tube to 580 deg.C in a muffle furnace within 3h, gasifying the red phosphorus, liquefying tin, reacting at 580 deg.C for 25h, and reacting at 5h
Cooling to 530 ℃ for constant temperature reaction for 3h, naturally cooling to room temperature, taking out the product, and washing with hydrogen peroxide, absolute ethyl alcohol and deionized water for 1 time respectively in sequence to obtain a tin triphosphate product; carrying out XRD characterization analysis on the sample; the results are shown in FIG. 2, and it can be seen that diffraction peaks appear in the sample at 21.87 °, 24.10 °, 32.78 °, 36.91 °, 41.15 °, 44.60 °, 49.44 ° and 60.63 °, which is consistent with the previous reports, and the tin triphosphite prepared by the method of the invention is proved.
Claims (3)
1. A method for preparing tin triphosphate by a vapor phase method is characterized by comprising the following steps: adding phosphorus and tin into a reactor, heating the reactor filled with materials to 550-600 ℃ in a vacuum atmosphere or an inert atmosphere within 1-5 h, reacting at a constant temperature for more than 24h, then cooling to 530 ℃ within 1-8 h, keeping the temperature for more than 2h, finally naturally cooling to room temperature, and washing and drying reaction products to obtain the tin triphosphite.
2. The method for preparing tin triphosphate according to claim 1, characterized in that: the molar ratio of phosphorus to tin is 2-4: 1.
3. The method for preparing tin triphosphate according to claim 1, characterized in that: the washing is to wash with hydrogen peroxide, ethanol and deionized water in turn.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110255692.4A CN112978693A (en) | 2021-03-09 | 2021-03-09 | Method for preparing tin triphosphate by vapor phase method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110255692.4A CN112978693A (en) | 2021-03-09 | 2021-03-09 | Method for preparing tin triphosphate by vapor phase method |
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| Publication Number | Publication Date |
|---|---|
| CN112978693A true CN112978693A (en) | 2021-06-18 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110255692.4A Pending CN112978693A (en) | 2021-03-09 | 2021-03-09 | Method for preparing tin triphosphate by vapor phase method |
Country Status (1)
| Country | Link |
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| CN (1) | CN112978693A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0637056A1 (en) * | 1993-07-30 | 1995-02-01 | Patent-Treuhand-Gesellschaft für elektrische Glühlampen mbH | High pressure discharge lamp |
| CN109534308A (en) * | 2019-01-12 | 2019-03-29 | 河南大学 | A kind of preparation method of large-size particle shape phosphatization tin compound |
| CN111020697A (en) * | 2019-12-06 | 2020-04-17 | 深圳市中科墨磷科技有限公司 | Sn-doped tin4P3Method for efficiently preparing two-dimensional black phosphorus crystal for catalyst |
-
2021
- 2021-03-09 CN CN202110255692.4A patent/CN112978693A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0637056A1 (en) * | 1993-07-30 | 1995-02-01 | Patent-Treuhand-Gesellschaft für elektrische Glühlampen mbH | High pressure discharge lamp |
| CN109534308A (en) * | 2019-01-12 | 2019-03-29 | 河南大学 | A kind of preparation method of large-size particle shape phosphatization tin compound |
| CN111020697A (en) * | 2019-12-06 | 2020-04-17 | 深圳市中科墨磷科技有限公司 | Sn-doped tin4P3Method for efficiently preparing two-dimensional black phosphorus crystal for catalyst |
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Application publication date: 20210618 |