Method for preparing boron alkene with high crystallinity and uniform thickness by hydrochloric acid assisted liquid phase oxidation

A high crystallinity, auxiliary liquid technology, applied in the direction of boron, boron/boride, etc., can solve the problem of poor removal of magnesium ions between layers, and achieve the effect of low method cost and simple and mild reaction conditions

Pending Publication Date: 2021-06-25
SHAANXI NORMAL UNIV
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, limited by the electron-deficient characteristics of boron, the boron nanosheets prepared

Method used

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  • Method for preparing boron alkene with high crystallinity and uniform thickness by hydrochloric acid assisted liquid phase oxidation
  • Method for preparing boron alkene with high crystallinity and uniform thickness by hydrochloric acid assisted liquid phase oxidation
  • Method for preparing boron alkene with high crystallinity and uniform thickness by hydrochloric acid assisted liquid phase oxidation

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0031] Example 1

[0032] 1, 2.54 g (10 mmol) iodine was added to 300 ml of acetonitrile, rapidly stirring to it completely dissolved, and then 0.46 g (10 mmol) of magnesium boron is continued under a nitrogen atmosphere, and the precursor dispersion was obtained.

[0033] 2. Under nitrogen protection and stirring, a 3 ml mass fraction was added to 36% hydrochloric acid in a precursor dispersion, and 14 days were taken at room temperature, followed by centrifugation at 15000 r / min for 20 min, and the lower level precipitation was re-dispersed. In 20 mL of acetonitrile, the washing was washed and centrifuged again, and the step 5 times was repeated. Subsequently with deoxidation deionized water, the unhydrate ethanol was washed 3 times, respectively, and solid substances were obtained.

[0034] 3. Taking the solid substance obtained by step 2 is dispersed in 50 ml of acetonitrile, and the dispersion is ultrasonic treatment for 120 min, and the ultrasonic power is 400 W. The dispe...

Example Embodiment

[0040] Example 2

[0041] In step 2 of Example 1, the time of the prototype reaction was sequentially replaced with 7 days, 14 days, 21 days, and the other steps were identical to the first embodiment to obtain the corresponding product. From Figure 12It can be seen that when the reaction time reaches 7 days, the characteristic diffraction peak of the boron is completely disappeared, and the parallel crystal surface diffraction peaks of bohane (104) and (208) appear.When the reaction was 14 days, the above parallel crystal surface diffraction peak intensity was the highest, and the remaining diffraction peaks were small, the effect was best.After 21 days, (208) crystal plane diffraction peak gradually disappeared, accompanied by other diffraction peaks, it was proved that the reaction was optimal for 14 days.

Example Embodiment

[0042] Example 3

[0043] In step 3 of Example 1, the ultrasonic time was sequentially replaced with 60 min, 90 min, 120 min, 150 min, and the other steps were the same as in Example 1, resulting in the corresponding product.From Figure 13 It can be seen that the edge portion of the product obtained after 60 min is thinned, but the central region is still a block shape.After 120 minutes, the product exhibited a uniform sheet shape, and the effect was good.The lateral dimensions of the product obtained after 180min were gradually reduced, which was related to the crushing of bohane nanofilates for long-term ultrasound.Therefore, the present invention preferably has an ultrasonic time of 90 to 150 min, and the ultrasonic 120min is optimal.

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Abstract

The invention discloses a method for preparing boron alkene with high crystallinity and uniform thickness by hydrochloric acid assisted liquid phase oxidation. The method comprises the following steps: by taking layered magnesium diboride as a boron source, acetonitrile as a solvent and an iodine elementary substance as an oxidant, stirring and reacting at normal temperature in an inert atmosphere under the condition of adding hydrochloric acid, oxidizing an electronegative boron layer by the iodine elementary substance, hydrochloric acid promotes interlayer magnesium ions to be removed from the interlayer in an ion exchange and chelation coordination mode, and then ultrasonic stripping is carried out to prepare the nano flaky boron alkene. The obtained boron alkene structure is high in order degree, the thickness of the nanosheet is 2.92-5.32 nm, and the transverse size is 100 nm-1. 5 [mu] m. The method is mild in reaction condition and low in production cost, does not need a high-vacuum environment, does not need to add and prepare a substrate, and can realize preparation of borane with high crystallinity and adjustable thickness.

Description

technical field [0001] The invention belongs to the technical field of preparation of two-dimensional materials, and in particular relates to a method for preparing boronene with high crystallinity and uniform thickness through hydrochloric acid-assisted liquid phase oxidation. Background technique [0002] Two-dimensional layered materials represented by graphene, black phosphorus, and MXene have the characteristics of large specific surface area, high electrochemical activity, and structural anisotropy, and can be widely used in electrochemical energy storage, electrocatalysis, adsorption and separation, etc. area has attracted much attention. In the study of new two-dimensional materials, boronene is considered to be a special material with great application potential due to its diverse structure and superconducting properties, ultra-high strength, and adjustable band gap. [0003] At present, the preparation methods of boron are mainly divided into two categories: botto...

Claims

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Application Information

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IPC IPC(8): C01B35/02
CPCC01B35/023Y02E60/10
Inventor 刘宗怀张锋贾聪颖
Owner SHAANXI NORMAL UNIV
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