CN112939065A - Preparation method of black phosphorus catalyst - Google Patents
Preparation method of black phosphorus catalyst Download PDFInfo
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- CN112939065A CN112939065A CN202110272728.XA CN202110272728A CN112939065A CN 112939065 A CN112939065 A CN 112939065A CN 202110272728 A CN202110272728 A CN 202110272728A CN 112939065 A CN112939065 A CN 112939065A
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- Prior art keywords
- tin
- quartz tube
- black phosphorus
- preparation
- phosphorus catalyst
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- 239000003054 catalyst Substances 0.000 title claims abstract description 27
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000010453 quartz Substances 0.000 claims abstract description 29
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 29
- QPBYLOWPSRZOFX-UHFFFAOYSA-J tin(iv) iodide Chemical compound I[Sn](I)(I)I QPBYLOWPSRZOFX-UHFFFAOYSA-J 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 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 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 6
- -1 tin iodide compound Chemical class 0.000 claims description 4
- JTDNNCYXCFHBGG-UHFFFAOYSA-L tin(ii) iodide Chemical compound I[Sn]I JTDNNCYXCFHBGG-UHFFFAOYSA-L 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 2
- 230000008021 deposition Effects 0.000 abstract 1
- 238000011068 loading method Methods 0.000 description 9
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 8
- 230000033558 biomineral tissue development Effects 0.000 description 2
- 238000001228 spectrum Methods 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
- 238000012512 characterization method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/006—Compounds containing, besides tin, two or more other elements, with the exception of oxygen or hydrogen
-
- 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
- B01J27/14—Phosphorus; Compounds thereof
-
- 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
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/455—Phosphates containing halogen
-
- 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)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
- Glass Compositions (AREA)
Abstract
The invention discloses a preparation method of a black phosphorus catalyst, belonging to the field of novel phosphorization materials; uniformly mixing tin triphosphate and tin iodide, placing the mixture in one end of a quartz tube, placing the quartz tube in a double-temperature-zone tube furnace, heating the raw material end to 500-550 ℃ within 3-5 h under an inert atmosphere or vacuum condition, heating the other end of the quartz tube to 450-490 ℃, preserving heat for 7-9 h, and obtaining a black phosphorus catalyst Sn at the other end of the quartz tube24P19.3I8(ii) a The method of the invention provides a new idea of vapor transport deposition for the preparation of the supported catalyst.
Description
Technical Field
The invention relates to a black phosphorus catalyst Sn24P19.3I8Belonging to the field of preparation of phosphorization chemical materials.
Background
Sn24P19.3I8Is a catalyst for preparing black phosphorus by a mineralization method; the mineralization method is simple to operate, mild in preparation conditions and low in cost, and is considered as the most possible method for realizing the industrial preparation of black phosphorus for many years; and Sn24P19.3I8The mechanical strength of the catalyst is low, the specific surface area is small, and the condition of industrial production of the catalyst cannot be met, so the catalyst needs to be loaded; among the various loading methods, the gas phase method is the preferred loading method because of its uniform loading. And at Sn24P19.3I8In the preparation, the traditional preparation method is to mix the metallic tin, the tin tetraiodide and the red phosphorus evenly and then carry out heat treatment to obtain Sn24P19.3I8Can only be generated in situ on metallic tin. However, tin cannot be vaporized at the preparation temperature, so that the catalyst loading must be realized by firstly loading tin on the carrier and then vaporizing other raw materials to react with the tin on the carrier, but the high surface tension of tin inevitably causes that the tin cannot be uniformly loaded on the carrier, and further causes that the catalyst cannot be uniformly loaded on the carrier, which increases the Sn24P19.3I8Difficulty of loading in the gas phase process.
Disclosure of Invention
For black phosphorus catalyst Sn24P19.3I8The invention provides a black phosphorus catalyst Sn suitable for gas phase loading, which has the problem of great difficulty in gas phase loading caused by the fact that Sn is required to be used as a raw material for preparation24P19.3I8The preparation method comprises the steps of uniformly mixing tin triphosphate and tin iodide, placing the mixture at one end of a quartz tube, placing the quartz tube into a double-temperature-zone tube furnace, heating the end, where the raw materials are placed, to 500-550 ℃ within 3-5 hours under an inert atmosphere or vacuum condition, heating the other end of the quartz tube to 450-490 ℃, preserving heat for 7-9 hours, and obtaining a black phosphorus catalyst Sn at the other end of the quartz tube24P19.3I8。
The tin iodide compound is tin diiodide or tin tetraiodide.
The mass ratio of the tin iodide compound to the tin triphosphate is 1: 1-5.
The invention has the following beneficial effects:
the invention and the prior black phosphorus catalyst Sn24P19.3I8Compared with the preparation method, the method has the advantages that the metallic tin which can not be vaporized at the preparation temperature is replaced by the vaporized tin triphosphate, so that the problem of the black phosphorus catalyst Sn is effectively solved24P19.3I8The problem of incapability of gas phase transportation preparation, namely the black phosphorus catalyst Sn24P19.3I8The gas phase loading of (a) provides a process.
Drawings
FIG. 1 shows Sn prepared in example 124P19.3I8A real object diagram of (1);
FIG. 2 shows Sn prepared in example 324P19.3I8XRD pattern of (a); the upper spectrum is the product of example 3, and the lower spectrum is Sn24P19.3I8The standard card of (1).
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
Uniformly mixing tin triphosphate and tin diiodide according to the mass ratio of 3:1, adding the mixture into one end of a quartz tube, putting the quartz tube into a double-temperature-zone tube furnace, heating the end of the quartz tube, which is provided with raw materials, to 500 ℃ within 3h under a vacuum condition, heating the other end of the quartz tube to 490 ℃, preserving heat for 8h, and obtaining a black phosphorus catalyst Sn at the other end of the quartz tube24P19.3I8The product (FIG. 1).
Example 2
Uniformly mixing tin triphosphate and tin tetraiodide according to a mass ratio of 4:1, adding the mixture into one end of a quartz tube, putting the quartz tube into a double-temperature-zone tube furnace, and heating the end, provided with the raw materials, of the quartz tube to the temperature of the end, provided with the raw materials, of the quartz tube in a vacuum atmosphere within 5hThe temperature of the other end of the quartz tube is increased to 490 ℃ at 530 ℃, and after the temperature is kept for 7 hours, the black phosphorus catalyst Sn is obtained at the other end of the quartz tube24P19.3I8And (3) obtaining the product.
Example 3
Uniformly mixing tin triphosphate and tin tetraiodide according to the mass ratio of 2:1, adding the mixture into one end of a quartz tube, putting the quartz tube into a double-temperature-zone tube furnace, and performing reaction on the quartz tube in a N-shaped furnace2Under the condition, the temperature of one end of the quartz tube, which is provided with the raw materials, is increased to 540 ℃ within 4h, the temperature of the other end of the quartz tube is increased to 450 ℃, and after the temperature is maintained for 9h, the black phosphorus catalyst Sn is obtained at the other end of the quartz tube24P19.3I8A product; carrying out XRD characterization analysis on the product; the results are shown in FIG. 2, and the XRD diffraction peak of the sample and the Sn catalyst of black phosphorus can be seen24P19.3I8Corresponding to the standard card (PDF # 52-0212), the method is proved to be capable of preparing the black phosphorus catalyst Sn24P19.3I8。
Claims (3)
1. A preparation method of a black phosphorus catalyst is characterized by comprising the following steps: uniformly mixing tin triphosphate and tin iodide, placing the mixture in one end of a quartz tube, placing the quartz tube in a double-temperature-zone tube furnace, heating the raw material end to 500-550 ℃ within 3-5 h under an inert atmosphere or vacuum condition, heating the other end of the quartz tube to 450-490 ℃, preserving heat for 7-9 h, and obtaining a black phosphorus catalyst Sn at the other end of the quartz tube24P19.3I8。
2. The method for preparing a black phosphorus catalyst according to claim 1, wherein: the tin iodide compound is tin diiodide or tin tetraiodide.
3. The method for preparing a black phosphorus catalyst according to claim 1, wherein: the mass ratio of the tin iodide compound to the tin triphosphate is 1: 1-5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110272728.XA CN112939065A (en) | 2021-03-12 | 2021-03-12 | Preparation method of black phosphorus catalyst |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110272728.XA CN112939065A (en) | 2021-03-12 | 2021-03-12 | Preparation method of black phosphorus catalyst |
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| Publication Number | Publication Date |
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| CN112939065A true CN112939065A (en) | 2021-06-11 |
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| CN202110272728.XA Pending CN112939065A (en) | 2021-03-12 | 2021-03-12 | Preparation method of black phosphorus catalyst |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109305661A (en) * | 2017-07-27 | 2019-02-05 | 南京工业大学 | A method of preparing rhombic system black phosphorus monocrystalline |
| US20190382268A1 (en) * | 2018-06-15 | 2019-12-19 | Black P2 (USA) INC. | Method for Producing Black Phosphorus |
| CN111111712A (en) * | 2019-12-19 | 2020-05-08 | 昆明理工大学 | Multi-section temperature rise and fall preparation of black phosphorus catalyst AxByCzMethod (2) |
| CN111439734A (en) * | 2020-03-26 | 2020-07-24 | 深圳市中科墨磷科技有限公司 | By SnP3Method for efficiently preparing two-dimensional black phosphorus crystal for catalyst |
-
2021
- 2021-03-12 CN CN202110272728.XA patent/CN112939065A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109305661A (en) * | 2017-07-27 | 2019-02-05 | 南京工业大学 | A method of preparing rhombic system black phosphorus monocrystalline |
| US20190382268A1 (en) * | 2018-06-15 | 2019-12-19 | Black P2 (USA) INC. | Method for Producing Black Phosphorus |
| CN111111712A (en) * | 2019-12-19 | 2020-05-08 | 昆明理工大学 | Multi-section temperature rise and fall preparation of black phosphorus catalyst AxByCzMethod (2) |
| CN111439734A (en) * | 2020-03-26 | 2020-07-24 | 深圳市中科墨磷科技有限公司 | By SnP3Method for efficiently preparing two-dimensional black phosphorus crystal for catalyst |
Non-Patent Citations (3)
| Title |
|---|
| SHENG LI ET AL.: "New Strategy for Black Phosphorus Crystal Growth through Ternary Clathrate", 《CRYST. GROWTH DES.》 * |
| 侯冉冉等: "黑磷的矿化法制备及其形成机制研究进展", 《磷肥与复肥》 * |
| 卢秋菊等: "高纯黑磷的低成本宏量制备研究", 《磷肥与复肥》 * |
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Application publication date: 20210611 |
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