Method for catalytic preparation of high-purity black phosphorus by adopting fixed bed

Abstract

The invention discloses a method for catalytic preparation of high-purity black phosphorus by adopting a fixed bed. According to the invention, gaseous phosphorus enters a fixed-bed reactor from the bottom part of the fixed-bed reactor; a solid-state catalyst fills the fixed-bed reactor; under the action of the solid-state catalyst, gaseous phosphorus molecules are converted into gaseous black phosphorus molecules; the gaseous black phosphorus molecules enter black phosphorus crystallizers from the top part of the fixed-bed reactor; the fixed-bed reactor is connected with two black phosphoruscrystallizers; when one of the black phosphorus crystallizers is full, the pipeline valve of the black phosphorus crystallizer is closed, while the pipeline valve of the other black phosphorus crystallizer is opened for collection via the other black phosphorus crystallizer; the gaseous black phosphorus molecules are continuously collected by two black phosphorus crystallizers in turn; gaseous black phosphorus in the black phosphorus crystallizers is condensed into black phosphorus crystals; and catalytically-unreacted gaseous phosphorus returns to the fixed-bed reactor. The method provided bythe invention can prepare high-purity block-shaped black phosphorus, can prepare high-purity nanometer black phosphorus by adjustment and control of the temperature and time of crystallization, and has the advantages of small catalyst loss, low preparation cost and simple operation.

Description

technical field [0001] The invention relates to a method for preparing high-purity black phosphorus by using fixed-bed catalysis, and belongs to the technical field of new phosphorus chemical industry materials. Background technique [0002] Black phosphorus is a thermodynamically stable allotrope of phosphorus at normal temperature and pressure. A large number of theoretical and experimental results show that black phosphorus has many excellent properties, such as high anisotropy and high carrier mobility. And switching ratio, direct bandgap with adjustable layer number, excellent biocompatibility, etc., have shown good application prospects in fields such as field effect transistors, solar cells, energy storage batteries, biomedicine, sensors, and catalysis. [0003] But the application of black phosphorus is limited by its preparation method. So far, a variety of methods have been developed for the preparation of black phosphorus, and the high-pressure method is the earl...

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Problems solved by technology

CN106185849A discloses a method for preparing nano-scale black phosphorus by ball milling, but the crystallinity of black phosphorus is not good, which is unfavorable for the subsequent application of black phosphorus

Moreover, the above methods can only prepare black phosphorus in batches, and it is difficult to carry out industrialized continuous production.

CN108128761A discloses a method for continuous preparation of black phosphorus. However, during the growth of black phosphorus, the mineralizer exists in gaseous form, and when the temperature is lowered, the mineralizer will condense, resulting in the existence of impurities in the black phosphorus, the purity of which is not high, and the catalyst After condensation, it cannot be recycled to the reactor to participate in the reaction again, resulting in loss of catalyst, resulting in higher production cost of black phosphorus

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