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Continuous preparation method of black phosphorus

A black phosphorus and mineralizer technology, applied in the field of phosphorus chemical industry, can solve the problems of difficult industrial continuous production, poor crystallinity of black phosphorus, unfavorable large-scale production, etc., and achieve full utilization, low cost and mild conditions Effect

Active Publication Date: 2018-06-08
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The methods proposed by CN104630879A, CN106087050, and CN105460910A have the advantages of good crystallinity and low cost of the prepared black phosphorus, but the black phosphorus obtained by this method needs to further remove impurities, the process is cumbersome and the cost is high, which is not conducive to large-scale production
CN106185849A discloses a method for preparing nano-scale black phosphorus. Red phosphorus is added to a high-energy ball mill, and black phosphorus is obtained through ball milling for several hours. This method can obtain black phosphorus with high purity, but the crystallinity of black phosphorus is not good , which is unfavorable to the subsequent application of black phosphorus
Moreover, the above methods can only prepare black phosphorus intermittently, and it is difficult to carry out industrial continuous production. Therefore, it is of great significance to develop a method that can continuously prepare high-purity black phosphorus to promote the application of black phosphorus

Method used

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  • Continuous preparation method of black phosphorus
  • Continuous preparation method of black phosphorus
  • Continuous preparation method of black phosphorus

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The gaseous yellow phosphorus and mineralizers (Sn and SnI 4 Mixed according to the mass ratio of 1:1) slowly pass into the microreactor, the temperature inside the microreactor is 550 ° C, after making it fully mixed and reacted in the microreactor, the obtained gaseous product is further passed into the black phosphorus In the grower, the temperature in the black phosphorus grower is 200°C. Black phosphorus grows in the black phosphorus grower. At the same time, the mineralizer is separated from the black phosphorus in gaseous form and mixed with the initial mineralizer to continue to use. After a period of reaction , open the black phosphorus grower, you can get high-purity black phosphorus, the purity is greater than 99.9%, the obtained black phosphorus physical map and XRD pattern are as follows figure 2 with image 3 shown by image 3 It can be seen that the four obvious characteristic peaks of black phosphorus are at 17.03°, 26.61°, 34.32°, and 52.42° respecti...

Embodiment 2

[0027] Gaseous yellow phosphorus and mineralizers (Bi, PbI 2 , BiI 3 According to the mass ratio of 1:1:2) slowly pass into the microreactor, the temperature in the microreactor is 570 ° C, after it is fully mixed and reacted in the microreactor, the gaseous product obtained is further passed into the In the black phosphorus grower, the temperature inside the black phosphorus grower is 250°C, the black phosphorus grows in the black phosphorus grower, and the mineralizer is separated from the black phosphorus in gaseous form and mixed with the initial mineralizer to continue to use, reacting for a period of time After a period of time, turn on the black phosphorus grower to obtain high-purity black phosphorus with a purity greater than 99.9%. The XRD pattern of the black phosphorus that present embodiment prepares is as follows Figure 4 As shown, it can be seen from the figure that the four obvious characteristic peaks of black phosphorus are at 17.05°, 26.40°, 34.23°, and ...

Embodiment 3

[0029] Gaseous yellow phosphorus and mineralizers (In and NH 4 I is mixed according to the mass ratio of 3:1) slowly into the microreactor, the temperature in the microreactor is 600 °C, after it is fully mixed and reacted in the microreactor, the gaseous product obtained is further passed into the black In the phosphorus grower, the temperature in the black phosphorus grower is 300°C, and the black phosphorus grows in the black phosphorus grower. At the same time, the mineralizer is separated from the black phosphorus in gaseous form and mixed with the initial mineralizer to continue to use, and react for a period of time Finally, turn on the black phosphorus grower to obtain high-purity black phosphorus with a purity greater than 99.9%. The XRD pattern of the black phosphorus that present embodiment prepares is as follows Figure 5 As shown, it can be seen from the figure that the four obvious characteristic peaks of black phosphorus are at 17.22°, 26.53°, 34.62°, and 52.41...

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Abstract

The invention discloses a continuous preparation method of black phosphorus, and belongs to the technical field of phosphorus chemical industry. The method disclosed by the invention comprises the following steps: introducing gaseous phosphorus and a mineralizer into a microreactor in which the temperature is 550 to 750 DEG C, after sufficiently mixing the reactants inside the microreactor to react sufficiently, further introducing obtained gaseous products into a black phosphorus grower in which the temperature is 200 to 500 DEG C, growing black phosphorus inside the black phosphorus grower,simultaneously separating the mineralizer from black phosphorus in a gaseous state, and mixing with an initial mineralizer for continuous utilization. According to the preparation method, high-purityblack phosphorus can be prepared, and continuous preparation of black phosphorous can be realized, so that the device is low in cost, simple and easy to operate, the device can be engaged with production equipment of yellow phosphorous and red phosphorous in industrial engineering at present, and the production cost is reduced.

Description

technical field [0001] The invention relates to a continuous preparation method of black phosphorus, which belongs to the technical field of phosphorus chemical industry. Background technique [0002] Black phosphorus is one of the most stable allotropes of phosphorus. A large number of theoretical and experimental studies have shown that black phosphorus has excellent properties, such as high carrier mobility and on-off ratio, and directly adjustable layers. Band gap, high anisotropy, excellent biocompatibility, etc., have shown great potential application value in solar cells, energy storage batteries, biomedicine, field effect transistors, sensors, catalysis and other fields. [0003] However, the current research on black phosphorus has just started, and many aspects still need to be further studied. In particular, the development of an efficient method for preparing black phosphorus is extremely important to promote the development of the application field of black phos...

Claims

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Application Information

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IPC IPC(8): C01B25/02
CPCC01B25/02
Inventor 廉培超汤永威王波梅毅何路东
Owner KUNMING UNIV OF SCI & TECH
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