CN108503890B - Preparation method of organic silicon functionalized boron nitride nanosheet - Google Patents

Preparation method of organic silicon functionalized boron nitride nanosheet Download PDF

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CN108503890B
CN108503890B CN201810326080.8A CN201810326080A CN108503890B CN 108503890 B CN108503890 B CN 108503890B CN 201810326080 A CN201810326080 A CN 201810326080A CN 108503890 B CN108503890 B CN 108503890B
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boron nitride
organic silicon
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谢政
刘世鑫
周树云
曾海波
吉建平
宋秀峰
陈萍
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Technical Institute of Physics and Chemistry of CAS
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Abstract

The invention discloses a preparation method of an organic silicon functionalized boron nitride nanosheet, which comprises the following steps: amination is carried out on the boron nitride powder to obtain aminated boron nitride; and reacting the obtained aminated boron nitride with organic silicon to obtain the organic silicon functionalized boron nitride nanosheet. Meanwhile, the solubility and the dispersibility of the boron nitride nanosheet in the matrix are improved, and the doping concentration of the boron nitride nanosheet in the matrix is increased.

Description

Preparation method of organic silicon functionalized boron nitride nanosheet
Technical Field
The invention relates to the field of preparation of boron nitride nanosheets. More particularly, relates to a preparation method of an organosilicon functionalized boron nitride nanosheet.
Background
Boron Nitride (BN), an important group III-V compound consisting of a group III element boron and a group V element nitrogen. Boron nitride has excellent physical and chemical properties such as wide band gap, high thermal conductivity, oxidation resistance and the like, and has huge application prospects in the aspects of high temperature, high frequency, high power, photoelectron, radiation resistance and the like. Therefore, the preparation of boron nitride nanosheets, the measurement of nanostructures, the assembly of nano devices, the test of boron nitride reinforced ceramics and optical and electrical properties and the like become important research directions in the field of current inorganic nano materials. The boron nitride nano material comprises quantum dots, nano wires, nano belts, nano tubes, nano sheets, nano crystals and the like, and the traditional preparation method comprises a mechanical stripping method, an arc discharge method, a laser ablation method, a ball milling method, a plasma jet method, a chemical vapor deposition method and the like. Because a single nanomaterial cannot be put into practical use, it is necessary to dope the nanomaterial with an organic or inorganic matrix to prepare a composite material and a device. If the physical blending is directly carried out, the defects of uneven doping, poor dispersibility and the like are caused. Suitable functionalization of the nanomaterial is therefore required to improve its solubility and dispersion in the matrix.
Therefore, there is a need to provide a new method for functionalizing boron nitride to improve the existing problems.
Disclosure of Invention
The invention aims to provide a preparation method of an organic silicon functionalized boron nitride nanosheet, which realizes organic functionalization of the boron nitride nanosheet, improves the solubility and the dispersibility of the boron nitride nanosheet in a matrix, and improves the doping concentration of the boron nitride nanosheet in the matrix.
In order to achieve the purpose, the invention provides a preparation method of an organic silicon functionalized boron nitride nanosheet, which comprises the following steps:
amination is carried out on the boron nitride powder to obtain aminated boron nitride;
and reacting the obtained aminated boron nitride with organic silicon to obtain the organic silicon functionalized boron nitride nanosheet.
In the preparation method, the granularity of the boron nitride powder can be preferably between 2 and 5 mu m, and the method comprises the steps of firstly aminating boron nitride and then reacting the aminated boron nitride with organic silicon to obtain the organic silicon functionalized boron nitride nanosheet with high doping concentration in the matrix. Wherein the substrate may include, but is not limited to, vinyl alcohol, methyl methacrylate, methyl triethoxysilane, aminopropyl triethoxysilane, and the like.
Preferably, the method for amination of boron nitride powder includes, but is not limited to, one of the following two methods:
mixing boron nitride powder with an amino organic compound, ball-milling under the atmosphere of inert protective gas, washing, and drying to obtain the aminated boron nitride; or the like, or, alternatively,
and performing microwave treatment on the boron nitride powder under the ammonia atmosphere at the pressure of below 0.3Pa to obtain the aminated boron nitride.
In the above method, the productivity can be improved by amination of boron nitride powder by a ball milling method.
Preferably, the mass ratio of the aminoorganic compound to the boron nitride powder is greater than 1: 1.
Preferably, the amino organic compound is selected from one or more of urea, tetraethylenepentamine and triphenylamine;
preferably, the ball milling time is more than 6h, and the ball milling temperature is 0-150 ℃;
preferably, the organic silicon contains a group capable of reacting with an amino group, preferably but not including one or more selected from epoxy group, carboxyl group and isocyanate group.
Preferably, the isocyanate group is selected from one or more of 3-isocyanate propyl trimethoxy silane and 3-isocyanate propyl triethoxy silane.
Preferably, the reaction of the aminated boron nitride with silicone comprises the following steps: and carrying out reflux reaction on the aminated boron nitride and organic silicon in a solvent under the atmosphere of inert protective gas, and after the reaction is finished, purifying and centrifuging to obtain the dispersion liquid of the organic silicon functionalized boron nitride nanosheets. It can be understood that after the solvent is removed, pure organosilicon functionalized boron nitride nanosheets are obtained. Wherein, the removal of the solvent can be a conventional method in the art, such as evaporation, and the like, and is not described herein.
Preferably, the inert shielding gas is selected from nitrogen, argon.
Preferably, the conditions of the reflux reaction are: the temperature is 25-100 ℃, and the time is 3-24 h.
Preferably, the addition amount of the aminated boron nitride is 1-50 parts by weight, and the addition amount of the organic silicon is 10-100 parts by weight.
Preferably, the solvent is selected from one or a mixture of acetone, petroleum ether and ethanol.
More preferably, the addition amount of the aminated boron nitride is 1-50 parts by weight, the addition amount of the organic silicon is 10-100 parts by weight, and the addition amount of the solvent is 10-200 parts by weight.
The invention has the following beneficial effects:
according to the invention, the boron nitride powder is stripped into the boron nitride nanosheets, so that a large number of boron nitride nanosheets can be obtained.
The preparation method realizes the organic functionalization of the boron nitride nanosheet, improves the solubility and the dispersibility of the boron nitride nanosheet in the matrix, and improves the doping concentration of the boron nitride nanosheet in the matrix.
The method for preparing the organic silicon functionalized boron nitride nanosheet has the characteristics of wide applicability, simplicity in operation and the like.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
Fig. 1 shows a schematic diagram of the preparation of silicone functionalized boron nitride nanoplates in example 1.
Figure 2 shows a fourier infrared spectrum of an aminated boron nitride, silicone functionalized boron nitride nanosheet prepared in example 1.
Fig. 3 shows transmission electron micrographs of aminated boron nitride nanoplates (a) and silicone functionalized boron nitride nanoplates (b) in example 1.
Fig. 4 shows a photograph of a dispersion of silicone-functionalized boron nitride nanoplates in petroleum ether in example 1.
Fig. 5 shows a photograph of the organic glass composite doped with 0.1 wt% silicone functionalized boron nitride nanoplates obtained in example 1.
Fig. 6 shows a photograph of a dispersion of the silicone-functionalized boron nitride nanoplates of example 2 in ethanol.
Fig. 7 shows a photograph of the organic glass composite doped with 0.5 wt% silicone functionalized boron nitride nanoplates obtained in example 3.
Fig. 8 shows a photograph of a dispersion of the boron nitride powder of comparative example 1 in water.
Fig. 9 shows a photograph of an organic glass composite doped with unfunctionalized boron nitride nanoplates of comparative example 5.
Fig. 10 shows a photograph of an organic glass composite doped with 0.5 wt% unfunctionalized boron nitride nanoplates of comparative example 6.
Detailed Description
In order to more clearly illustrate the invention, the invention is further described below with reference to preferred embodiments and the accompanying drawings. Similar parts in the figures are denoted by the same reference numerals. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
Example 1
The preparation method of the organic silicon functionalized boron nitride nanosheet comprises the following steps:
under the atmosphere of nitrogen, adding 40g of boron nitride powder and 80g of urea into a No. 1 ball mill, carrying out ball milling for 15h at the temperature of 0 ℃, and taking out a ball-milled mixture; washing with deionized water, and drying to obtain the aminated boron nitride.
Weighing 25g of aminated boron nitride, adding 100ml of petroleum ether and the weighed aminated boron nitride into a reactor 2#, carrying out ultrasonic treatment for 60min to obtain milky suspension, adding 50g of 3-isocyanatopropyltriethoxysilane, continuously stirring at the temperature of 100 ℃, and carrying out reflux treatment for 24 h; after the reaction is finished, washing with petroleum ether, and centrifuging at the rotating speed of 12000rpm to obtain the petroleum ether dispersion liquid of the organic silicon functionalized boron nitride nanosheet, wherein the solubility is 0.5 mg/ml. The particle size of the nano-sheet is 100nm, and the thickness of the lamella is 3 nm. The reaction scheme is shown in figure 1.
Referring to fig. 2, which is a fourier infrared spectrum of the aminated boron nitride, silicone functionalized boron nitride nanosheets prepared in example 1; as can be seen in the figure, at 1373.6cm-1At a sum of 816.5cm-1The characteristic absorption peaks correspond to B-N in-plane stretching vibration and B-N-B out-of-plane bending vibration of boron nitride respectively; at 3443cm-1The corresponding absorption peak is caused by the adsorption of water in the air on the surface of the sample; with respect to the infrared spectrum of the aminated boron nitride, 3240cm in the vicinity of the absorption peak of water was observed-1An absorption peak is formed at the position, which is caused by the stretching vibration of the N-H bond; infrared light for organosilicon functionalized boron nitrideSpectrum, can be seen at 3240cm-1The absorption peak disappears, and is 1081cm-1、1695cm-1、2927cm-1The absorption peaks at (A) correspond to Si-O bond, amide bond and alkane bond, respectively, which confirmed the presence of 3-isocyanatopropyltriethoxysilane, and were not found at 2272cm-1An absorption peak of an isocyanate group appears nearby, which shows that unreacted organic silicon is completely removed, and an absorption peak corresponding to an amido bond appears simultaneously, which shows that amino groups on boron nitride and the isocyanate group are subjected to chemical reaction, and shows that the organic silicon functionalized boron nitride nanosheet is successfully prepared, wherein the particle size of the nanosheet is 130nm, and the thickness of the nanosheet is 5 nm.
Referring to fig. 3, it is a transmission electron micrograph of the aminated boron nitride nanosheets and the organosilicon functionalized boron nitride nanosheets; the prepared boron nitride nanosheet is of a two-dimensional lamellar structure, the thickness of the lamellar is small, and the edge of the nanosheet is curled.
See fig. 4, which is a photograph of a dispersion of silicone functionalized boron nitride nanoplates in petroleum ether. A significant tyndall effect was seen under laser irradiation, demonstrating the formation of a stable dispersion.
Doping an organic silicon functionalized boron nitride nanosheet into a methyltriethoxysilane matrix by a sol-gel method, wherein the specific method comprises the following steps:
and mixing the obtained dispersion liquid with a methyltriethoxysilane monomer, reacting, and curing and molding a reaction product to obtain the organic glass composite material doped with the organic silicon functionalized boron nitride nanosheet.
Referring to the attached figure 5, which is a photograph of the obtained organic glass composite material doped with 0.1 wt% of organic silicon functionalized boron nitride nanosheets, it can be seen that the organic silicon functionalized boron nitride nanosheets are uniformly dispersed in the composite material, and no aggregation phenomenon of the nanosheets is observed. The haze value of the organic glass can be used for measuring the dispersion degree of the nano material in the matrix, and the lower the haze value, the better the dispersion of the material. The haze value of this glass was 13.1%. It should be noted that, in the drawings, the english letters are only words on the background paper, and can be used for visually observing the light transmittance of the glass and the dispersion degree of the nano material in the matrix, but have no other significance. The same applies to fig. 7, 9 and 10 below.
Example 2
The preparation method of the organic silicon functionalized boron nitride nanosheet comprises the following steps:
under the atmosphere of nitrogen, adding 20g of boron nitride powder and 100g of tetraethylenepentamine into a No. 1 ball mill, carrying out ball milling for 20h at 150 ℃, and taking out a ball-milled mixture; washing with deionized water, and drying to obtain the aminated boron nitride.
Weighing 10g of aminated boron nitride, adding 50ml of petroleum ether and the weighed aminated boron nitride into a reactor 2#, carrying out ultrasonic treatment for 40min to obtain milky suspension, adding 40g of 3-isocyanatopropyl trimethoxy silane, continuously stirring at the temperature of 70 ℃, and carrying out reflux treatment for 10 h; after the reaction is finished, removing solvent petroleum ether by a rotary evaporation device, washing with ethanol, and centrifuging at the rotating speed of 5000rpm to obtain the ethanol dispersion liquid of the organic silicon functionalized boron nitride nanosheet, wherein the solubility is 1.3mg/ml, the particle size of the nanosheet is 90nm, and the thickness of the nanosheet is 2 nm.
The organic silicon functionalized boron nitride nanosheets obtained in example 2 were doped in the same polymer matrix by a sol-gel method, achieving an effect similar to that of example 1, and a haze value of 11.4% at a doping concentration of 0.1 wt%.
See fig. 6, which is a photograph of a dispersion of silicone functionalized boron nitride nanoplates in ethanol. A significant tyndall effect was seen under laser irradiation, demonstrating the formation of a stable dispersion.
Example 3
The preparation method of the organic silicon functionalized boron nitride nanosheet comprises the following steps:
under the atmosphere of nitrogen, adding 2g of boron nitride powder and 20g of triphenylamine into a No. 1 ball mill, carrying out ball milling for 10h at room temperature, and taking out a ball-milled mixture; and (3) washing and drying by using deionized water to obtain the aminated boron nitride.
Weighing 1g of aminated boron nitride, adding 10ml of acetone and the weighed aminated boron nitride into a reactor 2#, carrying out ultrasonic treatment for 10min to obtain milky suspension, adding 10g of 3-isocyanatopropyltriethoxysilane, continuously stirring at the temperature of 25 ℃, and carrying out reflux treatment for 3 h; after the reaction is finished, acetone is used for washing, and the mixture is centrifuged at the rotating speed of 500rpm to obtain the acetone dispersion liquid of the organic silicon functionalized boron nitride nanosheet, wherein the solubility is 1.4 mg/ml. The particle size of the nano-sheet is 110nm, and the thickness of the sheet layer is 1 nm.
The organosilicon functionalized boron nitride nanosheets are doped into the aminopropyltriethoxysilane matrix by a sol-gel method, which is the same as in example 2.
Referring to the attached figure 7, which is a photograph of the obtained organic glass composite material doped with 0.5 wt% of organic silicon functionalized boron nitride nanosheets, it can be seen that the concentration of the doped organic silicon functionalized boron nitride nanosheets reaches 0.5 wt%, the nanosheets are uniformly dispersed in the matrix, and the haze value of the glass is 16.2%.
Example 4
The preparation method of the organic silicon functionalized boron nitride nanosheet comprises the following steps:
and (3) placing 2g of boron nitride powder in a microwave oven, pumping to a low pressure of 0.1Pa, introducing 30sccm ammonia gas, and performing microwave treatment for 20min to obtain the aminated boron nitride.
Weighing 2g of aminated boron nitride, adding 20ml of acetone and the weighed aminated boron nitride into a reactor 2#, carrying out ultrasonic treatment for 15min to obtain milky suspension, adding 15g of 3-isocyanatopropyltriethoxysilane, continuously stirring at the temperature of 50 ℃, and carrying out reflux treatment for 5 h; after the reaction is finished, acetone is used for washing, and the mixture is centrifuged at the rotating speed of 1000rpm to obtain the acetone dispersion liquid of the organic silicon functionalized boron nitride nanosheet, wherein the solubility is 1.8 mg/ml. The particle size of the nano-sheet is 130nm, and the thickness of the sheet layer is 1.4 nm.
The organic silicon functionalized boron nitride nanosheet obtained in example 4 is doped into a methyltriethoxysilane matrix by a sol-gel method, the effect achieved by the method is similar to that of example 1, and the haze value is 10.3% when the doping concentration is 0.1 wt%.
Comparative example 1
Example 1 was repeated except that the silicone-functionalized boron nitride nanoplates were replaced with boron nitride powder, the remaining conditions were unchanged, and the boron nitride powder was dissolved in water.
The solubility of the obtained non-functionalized boron nitride powder in water was 0.002 mg/ml.
See fig. 8, which is a photograph of a dispersion of boron nitride powder in water. As can be seen from the figures, the solubility of boron nitride powder in water is very low and most of the powder precipitates.
Comparative example 2
Example 1 was repeated except that the silicone-functionalized boron nitride nanosheets were replaced with unfunctionalized boron nitride nanosheets, the remaining conditions were unchanged, and the unfunctionalized boron nitride nanosheets were dissolved in petroleum ether. The preparation method of the unfunctionalized boron nitride nanosheet comprises the following steps:
a certain amount of boron nitride powder is taken and dispersed in a solvent, and ultrasonic treatment is carried out for a period of time under high power. And centrifuging the dispersion liquid obtained after the ultrasonic treatment at a certain rotating speed to finally obtain the non-functionalized boron nitride nanosheet dispersion liquid. The solvent can be removed by rotary evaporation or distillation to obtain the nanosheet powder.
The solubility of the obtained non-functionalized boron nitride nanosheet in petroleum ether was 0.13 mg/ml.
Comparative example 3
Example 2 was repeated except that the silicone-functionalized boron nitride nanosheets were replaced with unfunctionalized boron nitride nanosheets, the remaining conditions were unchanged, and the unfunctionalized boron nitride nanosheets were dissolved in ethanol. The preparation method of the unfunctionalized boron nitride nanosheet is the same as that of comparative example 1. The solubility of the organosilicon functionalized boron nitride nanosheet in ethanol is greater than that of the non-functionalized boron nitride nanosheet, and is 1 mg/ml.
Comparative example 4
Example 3 was repeated except that the silicone-functionalized boron nitride nanosheets were replaced with unfunctionalized boron nitride nanosheets, the remaining conditions were unchanged, and the unfunctionalized boron nitride nanosheets were dissolved in acetone. The preparation method of the unfunctionalized boron nitride nanosheet is the same as that of comparative example 1. The solubility of the organosilicon functionalized boron nitride nanosheet in acetone is greater than that of the non-functionalized boron nitride nanosheet, and the corresponding solubility is 0.7 mg/ml.
Comparative example 5
Example 1 was repeated except that the non-functionalized boron nitride nanoplates of comparative example 1 were doped into the methyltriethoxysilane matrix by a sol-gel method, which was the same as example 1.
Referring to fig. 9, which is a photograph of organic glass composite material doped with unfunctionalized boron nitride nanosheets, it can be seen that the nanosheets have an obvious aggregation phenomenon in the composite material, and the doping concentration is only 0.1 wt%. The haze value was 54.7%.
Comparative example 6
Example 3 was repeated except that the unfunctionalized boron nitride nanoplates were doped into the aminopropyltriethoxysilane matrix by a sol-gel process, which was the same as example 3.
Referring to fig. 10, which is a photograph of an organic glass composite doped with 0.5 wt% non-functionalized boron nitride nanosheets, it can be seen that the nanosheets have a significant aggregation phenomenon in the composite. The haze value was 70.6%.
It should be understood that the above-mentioned embodiments of the present invention are only examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention, and it will be obvious to those skilled in the art that other variations or modifications may be made on the basis of the above description, and all embodiments may not be exhaustive, and all obvious variations or modifications may be included within the scope of the present invention.

Claims (4)

1. The preparation method of the organic silicon functionalized boron nitride nanosheet is characterized by comprising the following steps:
amination is carried out on the boron nitride powder to obtain aminated boron nitride;
reacting the obtained aminated boron nitride with organic silicon to obtain organic silicon functionalized boron nitride nanosheets;
wherein, the addition amount of the aminated boron nitride is 1-50 parts by weight, and the addition amount of the organic silicon is 10-100 parts by weight;
the organic silicon is selected from one or more of 3-isocyanate propyl trimethoxy silane and 3-isocyanate propyl triethoxy silane;
the method for amination of boron nitride powder is as follows:
and performing microwave treatment on the boron nitride powder under the ammonia atmosphere at the pressure of below 0.3Pa to obtain the aminated boron nitride.
2. The method of claim 1, wherein the reaction of the aminated boron nitride with silicone comprises the steps of: and carrying out reflux reaction on the aminated boron nitride and organic silicon in a solvent under the atmosphere of inert protective gas, and after the reaction is finished, purifying and centrifuging to obtain the dispersion liquid of the organic silicon functionalized boron nitride nanosheets.
3. The method according to claim 2, wherein the reflux reaction is carried out under the following conditions: the temperature is 25-100 ℃, and the time is 3-24 h.
4. The preparation method according to claim 2, wherein the solvent is selected from one or more of acetone, petroleum ether and ethanol.
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