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A kind of high-efficiency preparation method of boron nitride nanosheet and its organic dispersion

A boron nitride, nanosheet technology, applied in chemical instruments and methods, nitrogen compounds, inorganic chemistry, etc., can solve the problems of low preparation efficiency, complex transfer technology, complex preparation process, etc.

Active Publication Date: 2019-12-24
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the requirements for the structure and composition of these functional small molecular compounds or polymers are relatively high, and the related synthetic process routes are often complicated, which is not conducive to industrial application.
[0009] In addition, the preparation of BNNSs by CVD technology has the disadvantages of high preparation cost, many structural defects of the obtained product, and complicated transfer technology.
[0010] In conclusion, although some progress has been made in the preparation technology research of BNNSs, the existing technology generally has some deficiencies such as low preparation efficiency, complex preparation process, and poor product structure control level. Low-cost preparation is still a key technical problem to be solved in this field

Method used

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  • A kind of high-efficiency preparation method of boron nitride nanosheet and its organic dispersion
  • A kind of high-efficiency preparation method of boron nitride nanosheet and its organic dispersion
  • A kind of high-efficiency preparation method of boron nitride nanosheet and its organic dispersion

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Experimental program
Comparison scheme
Effect test

Embodiment 1、2

[0080] Embodiment 1, 2, comparative example 1, 2

[0081] 1. Sample preparation

[0082] (1) The preparation of embodiment 1 sample is carried out as follows:

[0083] Step 1: Under the protection of ethylene, add 50.0 mL of anhydrous dichloromethane to a Schlenk double-layer reaction flask with a capacity of 250 mL, keep the temperature of the system at 35 ° C by stirring, and then add 0.10 g of acetonitrile α-diethylene oxide Amine palladium catalyst (1, concentration 2.0 g / L), at a constant temperature of 35° C. and ethylene pressure of 0.1 MPa, the polymerization was continued for 24 h by stirring. After the reaction, the obtained product was poured into 50 mL of methanol containing 1 wt% hydrochloric acid, and stirred to terminate the polymerization. After further drying the solvent, the obtained product was dissolved with an appropriate amount of THF, and a small amount of hydrogen peroxide and hydrochloric acid were added, stirred at room temperature for 1 h to dissol...

Embodiment 3， comparative example 3、4、5

[0098] 1. Sample preparation

[0099] (1) The preparation of embodiment 3 sample is carried out as follows:

[0100] Step 1: Under the protection of ethylene, add 50.0 mL of anhydrous dichloromethane to a Schlenk double-layer reaction flask with a capacity of 250 mL, keep the system temperature at 15 ° C by stirring, and then add 0.10 g of acetonitrile α-diethylene oxide Amine palladium catalyst (1, concentration 2.0g / L) and 2.50g methyl acrylate (MA, 0.58mol / L) were injected into the reaction flask, and the polymerization was continued for 24h by stirring at a constant temperature of 15°C and ethylene pressure of 0.1MPa . After the reaction, the resulting product was poured into 50 mL of acidified methanol with a concentration of 1 wt%, and stirred to terminate the polymerization. After further drying the solvent, the obtained product was dissolved with an appropriate amount of THF, and a small amount of hydrogen peroxide and hydrochloric acid were added, stirred at room te...

Embodiment 4

[0125] Embodiment 4, comparative example 6

[0126] 1. Sample preparation

[0127] (1) The preparation of embodiment 4 sample is carried out as follows:

[0128] Step 1: Under the protection of ethylene, add 50.0 mL of anhydrous dichloromethane to a Schlenk double-layer reaction flask with a capacity of 250 mL, keep the system temperature at 15 ° C by stirring, and then add 0.10 g of acetonitrile α-diethylene oxide Amine palladium catalyst (1, concentration 2.0g / L) and 4.50g butyl acrylate (BA, 0.70mol / L) were injected into the reaction flask, and the polymerization was continued for 24h by stirring at a constant temperature of 15°C and ethylene pressure of 0.1MPa . After the reaction, the resulting product was poured into 50 mL of acidified methanol with a concentration of 1 wt%, and stirred to terminate the polymerization. After further drying the solvent, the obtained product was dissolved with an appropriate amount of THF, and a small amount of hydrogen peroxide and hyd...

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Abstract

The invention provides an efficient preparation method of a boron nitride nanosheet and organic dispersion liquid thereof. The efficient preparation method comprises the following steps: a first step, adding boron nitride powder A, polymer and an organic solvent D in proportion, sealing, and then carrying out ultrasonic treatment to obtain initial dispersion liquid E, wherein the polymer is at least one of hyperbranched polyethylene B and hyperbranched polyethylene copolymer C; a second step, fully standing or centrifuging the initial dispersion liquid E obtained from the step 1 at low speed to obtain BNNSs dispersion liquid F containing excessive polymer; a third step, carrying out high-speed centrifuging or vacuum suction filtration and drying on the BNNSs dispersion liquid F containing the excessive polymer obtained from the step 2 to obtain a boron nitride nanosheet G; and a fourth step, adding the boron nitride nanosheet powder G and an organic solvent H which are obtained from the step 3 in the container, sealing and then carrying out ultrasonic treatment to obtain the boron nitride nanosheet dispersion liquid. By the efficient preparation method of the boron nitride nanosheet and the organic dispersion liquid thereof, the low-defect boron nitride nanosheet and the dispersion liquid thereof are effectively prepared controllably at low cost.

Description

technical field [0001] The invention relates to a method for preparing boron nitride nanosheets (BNNSs) and its organic dispersion, in particular to a method for efficiently preparing BNNSs and its organic dispersion by using hyperbranched polyethylene or its copolymers in an ordinary low-boiling point organic solvent. Dispersion method. Background technique [0002] In recent years, the upsurge of research on graphene has attracted widespread academic and industrial attention to other two-dimensional materials, such as transition metal dichalcogenides (TMDs), hexagonal boron nitride (h-BN), molybdenum disulfide (MoS 2 )Wait. Among them, h-BN and natural graphite have a similar two-dimensional layered structure, and there are also van der Waals forces between the layers, and the layers are also composed of sp 2 Therefore, boron nitride nanosheets (BNNSs) obtained by exfoliation are called "white graphene", which not only have excellent thermal conductivity and mechanical p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/064C08F10/02C08F4/26
CPCC01B21/064C01P2002/82C08F10/02C08F4/26
Inventor 徐立新卢铁梅叶会见
Owner ZHEJIANG UNIV OF TECH
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