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Preparation method of black phosphorus catalyst

A catalyst, black phosphorus technology, applied in chemical instruments and methods, physical/chemical process catalysts, phosphorus compounds, etc., can solve the problem of difficult gas phase loading

Pending Publication Date: 2021-06-11
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] For black phosphorus catalyst Sn 24 P 19.3 I 8 It must be prepared with Sn as a raw material, which leads to the problem that the gas phase loading is difficult. The present invention provides a black phosphorus catalyst Sn suitable for gas phase loading. 24 P 19.3 I 8 The preparation method of the method is that tin triphosphide and tin iodine compound are mixed and placed at one end of the quartz tube, and the quartz tube is put into a double-temperature zone tube furnace, and in an inert atmosphere or a vacuum condition, in 3~5h The temperature at the end where the raw material is placed inside is raised to 500~550°C, the temperature at the other end of the quartz tube is raised to 450~490°C, and after 7~9 hours of heat preservation, the black phosphorus catalyst Sn 24 P 19.3 I 8

Method used

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  • Preparation method of black phosphorus catalyst
  • Preparation method of black phosphorus catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] According to the mass ratio of 3:1, mix tin triphosphide and tin diiodide and add them into one end of the quartz tube, put the quartz tube into a tube furnace with two temperature zones, under vacuum conditions, in 3h The temperature at one end of the quartz tube where the raw material is placed is raised to 500°C, and the temperature at the other end of the quartz tube is raised to 490°C. After 8 hours of heat preservation, the black phosphorus catalyst Sn is obtained at the other end of the quartz tube. 24 P 19.3 I 8 product( figure 1 ).

Embodiment 2

[0014] According to the ratio of mass ratio of 4:1, mix tin phosphide and tin tetraiodide evenly and add them to one end of the quartz tube, put the quartz tube into a tube furnace with two temperature zones, under vacuum atmosphere, in 5h The temperature at one end of the quartz tube where the raw material is placed is raised to 530°C, and the temperature at the other end of the quartz tube is raised to 490°C. After 7 hours of heat preservation, the black phosphorus catalyst Sn is obtained at the other end of the quartz tube. 24 P 19.3 I 8 product.

Embodiment 3

[0016] Mix tin phosphide and tin tetraiodide in a mass ratio of 2:1 and add them to one end of the quartz tube, put the quartz tube into a double-temperature zone tube furnace, and 2 Under these conditions, within 4 hours, the temperature at the end of the quartz tube where the raw material is placed is raised to 540 ° C, and the temperature at the other end of the quartz tube is raised to 450 ° C. After 9 hours of heat preservation, the black phosphorus catalyst Sn 24 P 19.3 I 8 product; XRD characterization analysis was carried out on the product; the results are shown in figure 2 , it can be seen from the figure that the XRD diffraction peak of the sample is consistent with that of the black phosphorus catalyst Sn 24 P 19.3 I 8 Corresponding to the standard card (PDF#52-0212), it proves that this method can prepare black phosphorus catalyst Sn 24 P 19.3 I 8 .

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PUM

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Abstract

The invention discloses a preparation method of a black phosphorus catalyst, and belongs to the field of new phosphating materials. The method comprises the steps of uniformly mixing tin triphosphide and a tin-iodine compound, putting the mixture into one end of a quartz tube, putting the quartz tube into a double-temperature-zone tubular furnace, heating the raw material end to 500550 DEG C within 3-5 hours in an inert atmosphere or a vacuum condition, heating the other end of the quartz tube to 450-490 DEG C, and preserving heat for 7-9 hours to obtain the black phosphorus catalyst Sn24P19.3I8 at the other end of the quartz tube. The method provided by the invention provides a new idea of vapor transport deposition for preparation of a supported catalyst.

Description

technical field [0001] The invention relates to a black phosphorus catalyst Sn 24 P 19.3 I 8 The preparation method belongs to the field of phosphorus chemical material preparation. Background technique [0002] sn 24 P 19.3 I 8 It is a catalyst for the preparation of black phosphorus by the mineralization method; because the mineralization method is simple to operate, the preparation conditions are mild, and the cost is low, it has been considered as the most likely method for the industrialization of black phosphorus for many years; and Sn 24 P 19.3 I 8 The low mechanical strength and small specific surface area cannot meet the conditions for industrial production of catalysts, so it must be loaded; among many loading methods, the gas phase method is currently the preferred loading method because of its uniform loading. And in Sn 24 P 19.3 I 8 In the preparation of , the traditional preparation method is to mix metal tin, tin tetraiodide and red phosphorus evenl...

Claims

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Application Information

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IPC IPC(8): C01G19/00C01B25/455B01J27/14
CPCC01G19/006C01B25/455B01J27/14C01P2002/72
Inventor 梅毅吴际朱远蹠谢德龙王驰廉培超宋现成汪万乘
Owner KUNMING UNIV OF SCI & TECH
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