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A kind of controllable preparation method of nanometer red phosphorus hollow sphere

A hollow sphere, red phosphorus technology, applied in nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problems of unsuitability for the production of red phosphorus-based nanomaterials, high toxicity, etc., to reduce the difficulty of industrialization, and to easily obtain raw materials , the effect of cheap raw materials

Active Publication Date: 2022-04-05
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the above several methods, the impurities produced by the reaction are difficult to remove, and the reagents used in the reaction are all highly flammable and explosive substances, and are highly toxic, so they are not suitable for the actual production of red phosphorus-based nanomaterials.

Method used

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  • A kind of controllable preparation method of nanometer red phosphorus hollow sphere
  • A kind of controllable preparation method of nanometer red phosphorus hollow sphere
  • A kind of controllable preparation method of nanometer red phosphorus hollow sphere

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Step 1. Weigh 0.02g-0.06g of red phosphorus, then transfer it to an empty agate mortar, grind it with a pestle for 5-20 minutes, and then sieve with a 200-mesh sieve to obtain 200-mesh red phosphorus powder.

[0030] Step 2, transfer the red phosphorus powder obtained above to a quartz tube with a diameter of 15 mm through necking treatment, vacuumize, and then pass in nitrogen protective gas.

[0031] Step 3: Repeat the content of step 2 for 3 to 4 times to finally obtain red phosphorus powder under negative pressure and nitrogen atmosphere.

[0032] Step 4. Preheat the above-mentioned quartz tube containing red phosphorus powder with a flame gun, and then direct the flame at the constriction of the quartz tube and heat for 2 minutes to obtain a completely sealed quartz tube under a vacuum state and a nitrogen atmosphere.

[0033] Step 5, placing the above-mentioned quartz tube in the middle of the tube furnace. Raise the temperature at 5°C / min to 300-500°C, keep it w...

Embodiment 2

[0038] Step 1. Weigh 0.1g-0.4g of red phosphorus, then transfer it to an empty agate mortar, grind with a pestle for 5-20 minutes, and then sieve with a 200-mesh sieve to obtain 200-mesh red phosphorus powder.

[0039] Step 2, transfer the red phosphorus powder obtained above to a quartz tube with a diameter of 15 mm through necking treatment, vacuumize, and then pass in nitrogen protective gas.

[0040] Step 3: Repeat the content of step 2 for 3 to 4 times to finally obtain red phosphorus powder under negative pressure and nitrogen atmosphere.

[0041] Step 4. Preheat the above-mentioned quartz tube containing red phosphorus powder with a flame gun, and then direct the flame at the constriction of the quartz tube and heat for 2 minutes to obtain a completely sealed quartz tube under a vacuum state and a nitrogen atmosphere.

[0042] Step 5, placing the above-mentioned quartz tube in the middle of the tube furnace. Raise the temperature at 5°C / min to 500-800°C, keep it warm f...

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Abstract

The invention relates to a controllable preparation method of nano red phosphorus hollow spheres, belonging to the technical field of material preparation. The method of the invention comprises: preparing a vacuum-sealed quartz tube filled with industrial red phosphorus; and preparing hollow nanometer red phosphorus spheres. Wherein, by adjusting the calcination temperature, the holding time and the addition amount of red phosphorus, the particle diameter of the nano-red phosphorus hollow spheres is controlled, and the diameter range of the nano-red phosphorus hollow spheres is adjustable, ranging from tens of nanometers to hundreds of nanometers. The invention has simple process and convenient synthesis; solid-phase reaction is adopted, and no impurities are generated in the reaction process; energy consumption is low, sustainable, time is short, and cost is low; yield is high, and scale is easy, and red phosphorus can be endowed with a hollow structure because of its hollow structure. Large specific surface area, rich pore structure and reduced density of red phosphorus powder make nano-red phosphorus hollow spheres show excellent effects in many fields. It is the best choice for nano-red phosphorus hollow spheres used in red phosphorus-based composite materials General synthetic method.

Description

technical field [0001] The invention relates to a controllable preparation method of nano red phosphorus hollow spheres, belonging to the technical field of material preparation. Specifically, it is a method for preparing nanometer red phosphorus hollow spheres. Background technique [0002] Prior Art 1 via NaN 3 with PCl 5 The solvothermal reaction between (10NaN 3 +2PCl 5 →2P+10NaCl+15N 2 ) to generate elemental red phosphorus, and uniform red phosphorus hollow nanospheres were prepared by the Kirkendall effect. Then prior art 2 uses molten NaCl–KCl–AlCl 3 In the salt system, the oxidation-reduction reaction between the nano-magnesium metal surface and phosphorus pentachloride generates red phosphorus, and the Kirkendall effect is used to control the morphology of the red phosphorus hollow spheres. The prior art 3 prepares iodine-doped nano-red phosphorus hollow spheres by redox reaction of phosphorus triiodide and ethylene glycol to produce red phosphorus by means ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/023B82Y30/00B82Y40/00
CPCC01B25/023B82Y30/00B82Y40/00
Inventor 潘也唐袁永帅杨荣杰
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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