CN110921638A - Method for preparing modified boron nitride nanosheet by aqueous phase shearing method - Google Patents
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Abstract
A method for preparing modified boron nitride nanosheets by a water phase shearing method belongs to the technical field of two-dimensional nanomaterial preparation. Dispersing the layered h-BN into an aqueous solution, simultaneously adding a surfactant to stably disperse the h-BN, then shearing and stripping the h-BN in a shear reactor to obtain OH-BNNSs with less than 10 layers, and obtaining OH-BNNSs powder by high-speed centrifugation, suction filtration and freeze drying. The prepared OH-BNNSs has few layers and high yield, and covalent functionalization is simultaneously carried out in the stripping process to generate hydroxyl, thereby further improving the stability and the dispersibility of the OH-BNNSs in a polar solution. The method provided by the invention has the advantages of controllable stripping process, high efficiency, simple operation, low cost and industrial application prospect.
Description
Technical Field
The invention belongs to the technical field of two-dimensional nano material preparation, and particularly relates to application of a liquid phase shearing and stripping method in the field of preparation of two-dimensional nano materials. In particular to a method for preparing a small number of BNNSs by using h-BN as a raw material through shearing force generated in a shearing type reactor and simultaneously performing covalent functionalization to obtain hydroxylated boron nitride OH-BNNSs.
Background
With the development of scientific technology, the demand for miniaturized and lightweight electronic devices is increasing, and many challenges are presented in terms of heat dissipation in order to avoid overheating of the devices. To solve this problem, inorganic (ceramic) materials such as Silica (SiO)2) Aluminum oxide (Al)2O3) Boron Nitride (BN), silicon carbide (SiC) and aluminum nitride (AlN)Is used as the heat conductive member. Among them, hexagonal boron nitride is widely used as a heat conductive filler due to its excellent physicochemical properties, such as high thermal conductivity (thermal conductivity of boron nitride nanosheets is 2000W/m · k), high heat resistance, high temperature insulation, high temperature stability, low thermal expansion coefficient, strong oxidation resistance, strong corrosion resistance and stable chemical properties. Notably, hexagonal boron nitride has a layered structure similar to graphite and can be exfoliated to produce sheets with two-dimensional nanostructures. These nanosheet fillers have significant advantages over traditional fillers, such as: lower percolation range (about 0.1-2 vol.%), the association between particles gives a significant reduction in filler content (less than 0.001%), a large amount of interfacial area per volume of particles (10%)3-104m2/ml) and a very short distance between the particles (distance of 10-50nm when added in an amount of 1-8 vol.%). These excellent properties make hexagonal boron nitride (BNNSs) more thermally conductive. At present, although few-layer BNNSs can be prepared, the preparation method is difficult to scale, and the scale application of the BNNSs is limited. Therefore, solving this problem becomes a focus of attention of researchers.
At present, BNNSs are prepared by a plurality of methods, mainly including: chemical vapor deposition, mechanical lift-off, liquid phase lift-off, and the like. These methods each have advantages and disadvantages, in which the mechanical peeling method is primarily repeated sticking by a transparent tape, and the adhesive force of the tape is used to overcome weak van der waals force between molecular layers to obtain BNNSs, although this method has a simple process and the obtained BNNSs have few defects and complete crystal lattice. However, the method also has the defects of low preparation efficiency, difficult scale-up and the like. The ball milling method adopted later has higher efficiency, can obtain a large amount of BNNSs, but has thicker thickness, lower efficiency and application limitation. Chemical vapor deposition is a typical method for synthesizing hexagonal nitridation nano-sheets from bottom to top, a reaction substance is gasified and reacted, and then is cooled and deposited on the surface of a heated substrate to form single-layer BNNSs, although the BNNSs prepared by the method has controllable layer number, high quality and higher yield than a mechanical stripping method, the method has high requirements on experimental equipment, the reaction needs high temperature and high pressure, the energy consumption is high, and the number of layers is greatly increasedAdding to the production cost and having more limitations for the subsequent application. To date, the liquid phase exfoliation method is the most likely method for preparing two-dimensional nanomaterials on a large scale at low cost, and among them, the ultrasonic liquid phase exfoliation method and the shear type liquid phase exfoliation method are most studied. The ultrasonic liquid phase peeling method mainly uses a liquid cavitation effect to perform peeling, but generates a local high temperature (several thousand K), a local high pressure (several thousand atmospheric pressure) and a rapid heating and cooling rate (several billion K.S) in the process of generating bubbles-1) These harsh conditions can cause the resulting BNNSs to be non-uniform in size, and the ultrasonic exfoliation has a small throughput and is difficult to scale up, which limits the studies on the application of BNNSs. The shear type liquid phase separation method has received much attention from scientists because of its simplicity of operation and effectiveness of action. Although various shearing type machine structures are different, the principle is consistent, and the inter-layer Van der Waals force of the laminated material is overcome through the shearing force generated by the viscous liquid-phase medium in a high-speed gradient region, so that the peeling preparation is realized, wherein the shearing force in any direction can be decomposed into the shearing force (longitudinal shearing force) in the direction vertical to the plane of the material and the shearing force (transverse shearing force) in the direction parallel to the plane of the material, the longitudinal shearing force cuts the laminated material in the direction vertical to the plane of the material, the size of the laminated material is reduced, the defect occurs at the cutting edge, and the laminated material is peeled by the transverse shearing force in the direction parallel to the plane of the material, so that the thickness of the laminated material is reduced.
To date, Jonathan n, Coleman, et al have experimentally demonstrated that layered Materials can be used to prepare two-dimensional nanomaterials (Paton kr., Varrla E, Backes c., Smith RJ., Khan u., O' Neill a., Coleman JN., etc. nature Materials 2014,6, 624-. A large number of experiments and researches prove that the graphene can be obtained by stripping the graphite which is a layered material through a shearing technology, for example, Chinese patent CN 107217305A discloses that through cavitation effect generated by ultrasonic waves and multiple composite actions such as centrifugal extrusion, hydraulic shearing and the like generated by a high-shear homogenizing device, Van der Waals force between layers of a crystal material can be effectively broken, and a high-quality two-dimensional material with single layer or few layers and good thickness uniformity is obtained; chinese patent CN 105271206 a discloses the use of a continuously rotating co-rotating intermeshing screw machine to uniformly disperse a graphite pre-mix in the direction of screw rotation, forming a lamellar orientation, shear stripping in the direction of the intermeshing screw elements orientation; chinese patent CN 107814380B discloses that a shear thickening system is mixed with graphite, and the mixed liquid is in a shear thickening high viscosity state through mechanical shearing, so that the shear stress between the shear thickening system and a graphite interface can be obviously enhanced, and the efficiency of preparing graphene by stripping graphite is improved; chinese patent CN 106995212 a discloses that graphite mixed solution is subjected to high shear stripping to obtain graphene solution and the like. However, the research depth of the liquid phase shear stripping of h-BN for preparing BNNSs is not as deep as that of graphene at present, and because of the solvent resistance of the h-BN, the solvent used for stripping the h-BN is generally an organic solvent, for example, Chinese patent CN 104803363A discloses that hexagonal boron nitride powder and a polar organic solvent (such as dodecyl pyrrolidone, isopropanol, N-methyl pyrrolidone, dimethylformamide and N-methyl formamide) are mixed and stirred uniformly according to a certain proportion, and then the mixture is sheared and stripped by a high shear dispersion emulsifying machine under certain temperature, shearing speed and shearing time. The organic solvent is basically a high-boiling point solvent, is difficult to remove and harmful to human bodies, and pollutes the environment, so that the post-treatment steps of experiments are increased, and the harm to the human health and the environmental protection is also generated. Therefore, the deionized water which is less researched and environmentally friendly is considered to be selected as the stripping solvent, and the research and development of the liquid phase stripping technology are in the direction.
Compared with a large number of reports on functionalized graphene, only a few papers and patents on functionalized h-BN are published, such as Chinese patent CN 109573965A which discloses that BNNSs are dispersed in an aqueous solution of sodium hydroxide and are treated by a hydrothermal method to prepare hydroxyl modified boron nitride nanosheets (BNOH); chinese patent CN 110343291a discloses adding BNNSs into a strong alkali solution, and stirring at high temperature to obtain a hydroxylated boron nitride nanosheet. Furthermore, The conventional methods for preparing hydroxylated Boron Nitride nanoparticles include concentrated nitric acid hydrothermal oxidation, molten sodium hydroxide oxidation, high temperature and high pressure Water thermal oxidation, etc., which require high temperature, high pressure, strong acid, strong base, and strong oxidant, which increase The risk and complexity of The experiment, and are not favorable for The popularization and expansion of The experiment, while Yi Lin experimentally proves that The B-N bond at The defect edge of BNNSs has higher reactivity than The intact B-N inside BNNSs (Lin Y, Williams T V, Xu T B, et al, aqueous dispersion of Few-Layered and monomeric Hexagon Boron Nitride nanoparticles from Sound-Assisted Hydrolysis: Critical roll of Water [ J ] Journal of chemical chemistry C, chemistry, 115, 2679). The cavitation effect brought by the ultrasound can crush h-BN, so that defects are generated at the edge of the prepared BNNSs, but the crushing effect brought by the ultrasound effect is obviously not obvious without shearing force, for example, KaiWu et al obtain hydroxylated boron nitride nanosheets by a water-based ball milling one-step method, namely, the crushing effect of ball milling is utilized, but the high-strength non-specific ball milling effect can damage the lattice structure on the surface of the boron nitride, so that the performance of the boron nitride is reduced, and the method has some defects. The patent of directly stripping the functionalized boron nitride nanosheets at one time in a water environment by a liquid phase shearing and stripping technology is not reported, and the method is more efficient, low in cost, convenient and rapid.
The method takes deionized water as a solvent, and prepares the OH-BNNSs which have high quality, few layers, large yield and covalent functionalization in a simple, high-efficiency and economic way under the treatment of a shear type reactor. The main advantages of using deionized water as the solvent are: (1) compared with other liquids such as organic solvents and ionic liquids, the deionized water has the advantages of environmental protection, low cost, simple post-treatment and the like. (2) In the stripping process, high-speed longitudinal shearing force breaks H-BN into small pieces with the size of about 200nm, B-N bonds are broken at the edges of BNNSs in the breaking process, a large number of defects appear, in the stripping experiment process, water molecules are used as an oxidant to attack the B-N bonds at the edges of the defects of the BNNSs to produce hydroxyl groups, so that the covalent functionalization of the BNNSs is realized, and the effect of the BNNSs in a polar solvent (H) is improved2O, DMF, NMP, IPA).
Disclosure of Invention
The invention provides a novel method for preparing modified boron nitride nanosheets by using an aqueous phase shearing method.
The invention discloses a method for preparing modified boron nitride nanosheets, namely hydroxylated boron nitride OH-BNNSs, by an aqueous phase shearing method, which is characterized by comprising the following steps:
1) dissolving a surfactant in deionized water until the surfactant is completely dispersed;
2) dispersing blocky boron nitride h-BN serving as a raw material into the surfactant aqueous solution in the step 1) to prepare a suspension, carrying out shearing and stripping treatment in a shearing type reactor, and taking supernatant to obtain OH-BNNSs.
The surfactant in the step 1) includes but is not limited to anionic surfactant-sodium dodecyl sulfate, sodium cholate; amphoteric surfactant-dodecyl hydroxypropyl sulfobetaine, lauryl alanine diethanolamine salt; nonionic surfactants-triton, polyvinyl alcohol, and the like.
The concentration of the surfactant in the suspension in the step 2) is 0-1 mg/ml, and the concentration of the h-BN in the suspension is 5-30 mg/ml. Further preferably, the mass ratio of the surfactant to the h-BN is 1:20 to 1: 200.
Shear reactors include, but are not limited to: shear homogenizers, rotating packed beds, high pressure homogenizers, and the like. The stripping time is 0.25-20h, such as 500-6000rpm for shear homogenizer and rotating packed bed, and the mean pressure is 100MPa for high-pressure homogenizer
The OH-BNNSs prepared by the method has few layers (less than 10 layers of OH-BNNSs) and high yield, and covalent functionalization is simultaneously carried out in the stripping process to generate hydroxyl, so that the stability and the dispersibility of the OH-BNNSs in a polar solution are further improved. The method provided by the invention has the advantages of controllable stripping process, high efficiency, simple operation, low cost and industrial application prospect.
Drawings
The embodiments of the present invention will be further described with reference to the drawings;
FIG. 1 is a schematic diagram of the exfoliation and functionalization process for preparing OH-BNNSs according to the present invention;
FIG. 2 SEM image of OH-BNNSs prepared by stripping of example 1 of the present invention;
FIG. 3 TEM image of OH-BNNSs prepared by exfoliation in example 1 of the present invention;
FIG. 4 AFM image of OH-BNNSs prepared by exfoliation in example 1 of the present invention;
FIG. 5 IR spectrum of OH-BNNSs prepared by exfoliation in example 13 of the invention.
FIG. 6 XPS spectra of OH-BNNSs prepared in example 13, example 17 and example 19 of the present invention;
FIG. 7 TGA of OH-BNNSs prepared in example 13 of the present invention and BNNSs prepared in example 20.
Detailed Description
To facilitate an understanding of the invention, reference will now be made in detail to the following examples, the scope of which is to be construed as including but not limited to the full breadth of the appended claims and any and all modifications that would occur to one skilled in the art without departing from the scope of the invention.
Example 1, boron nitride nanoplates were prepared;
firstly, 0.5g of sodium dodecyl sulfate is weighed and dissolved in 500ml of deionized water, then 10g h-BN is weighed and dispersed in the prepared sodium dodecyl sulfate aqueous solution, and the mass ratio of the sodium dodecyl sulfate to the h-BN is 1: 20.
And shearing and stripping the prepared h-BN suspension by using a shearing homogenizer at the rotating speed of 6000r/min for 14 h. And then centrifuging the suspension, wherein the centrifugal separation rotating speed is 6000r/min, the time is 10min, and taking supernatant to obtain OH-BNNSs dispersion liquid, wherein the concentration of the supernatant is 0.88 mg/ml. Repeatedly filtering and washing the obtained supernatant, and freeze-drying to obtain OH-BNNSs powder.
The shearing type homogenizer is a FJ300-SH type digital display high-speed dispersion homogenizer produced by Shanghai Biaogao model factory.
Example 2
Except for example 1 where the surfactant used was dodecyl hydroxypropyl sulfobetaine, the procedure was otherwise identical and the concentration of the supernatant after shear stripping was 0.82 mg/ml.
Example 3
Except for the difference from example 1 that the surfactant used was polyvinyl alcohol, the procedure was otherwise identical, and the concentration of the supernatant after shear peeling was 0.93 mg/ml.
Example 4
Except that 15g h-BN was weighed out in the same manner as in example 1 and the supernatant concentration after shear peeling was 0.72 mg/ml.
Example 5
Except that 5g h-BN was weighed in the same manner as in example 1 and the supernatant concentration after shear peeling was 0.60 mg/ml.
Example 6
Except that 0.375g of sodium lauryl sulfate was weighed out in the same manner as in example 1, and the concentration of the supernatant after shear peeling was 0.75 mg/ml.
Example 7
Except that 0.05g of sodium lauryl sulfate was weighed out in the same manner as in example 1, and the concentration of the supernatant after shear peeling was 0.29 mg/ml.
Example 8
The difference from example 1 is that the peeling speed is 5000r/min, the rest processes are consistent, and the concentration of the supernatant after shearing and peeling is 0.65 mg/ml. .
Example 9
The difference from example 1 is that the peeling speed is 3000r/min, the rest processes are consistent, and the supernatant concentration after shearing peeling is 0.27 mg/ml.
Example 10
The difference from example 1 is that the stripping time was 15h, the rest of the process was consistent, and the supernatant concentration after shear stripping was 0.80 mg/ml.
Example 11
The difference from example 1 is that the stripping time was 12h, the rest of the process was consistent, and the supernatant concentration after shear stripping was 0.70 mg/ml.
Example 12
The difference from example 1 is that the stripping time was 11h, the rest of the process was consistent, and the supernatant concentration after shear stripping was 0.66 mg/ml.
Example 13
Except that no surfactant was added as in example 1, the process was otherwise identical and after shear stripping, 0.27mg/ml was added. The IR spectrum of the obtained OH-BNNSs is shown in FIG. 5.
Example 14
The difference from example 1 is that the shear reactor is a rotary packed bed, the rotating speed is 2000r/min, the rest processes are consistent, and the concentration of the supernatant after shear stripping is 0.40 mg/ml.
The rotary packed bed of the invention is a supergravity rotary bed device which is already disclosed, and comprises a supergravity rotary bed reactor in the forms of packed beds, baffled spiral channels and the like (refer to application numbers of 91109255.2, 91111028.3, 01268009.5, 200520100685.3, 02114174.6 and 200510032296.6).
Example 15
The difference from example 14 is that the rotation speed is 1000r/min, the rest process is consistent, and the concentration of the supernatant after shear stripping is 0.21 mg/ml.
Example 16
The difference from example 14 is that the stripping time was 20h, the rest of the process was identical, and the supernatant concentration after shear stripping was 0.45 mg/ml.
Example 17
Except that no surfactant was added as in example 16, the procedure was identical and the supernatant concentration after shear stripping was 0.24 mg/ml.
Example 18
The difference from example 1 is that the shearing reactor is a high-pressure homogenizer, the stripping time is 15min, the mean pressure is 100Mpa, the equipment does not relate to the rotating speed, the other processes are consistent, and the concentration of the supernatant after shearing and stripping is 0.78 mg/ml.
The high-pressure homogenizer is a Scientz-150 type high-pressure homogenizer manufactured by Ningbo Xinzhi Biotechnology GmbH.
Example 19
Except that no surfactant was added as in example 18, the procedure was identical and the supernatant concentration after shear stripping was 0.70 mg/ml.
Example 20
The difference from example 13 is that the stripping apparatus is an ultrasonic apparatus, the other process is the same, and the supernatant concentration after ultrasonic stripping is 0.53 mg/ml.
The ultrasonic equipment is a KQ5200DE ultrasonic cleaner produced by Kunshan ultrasonic instruments Limited.
Claims (7)
1. A method for preparing modified boron nitride nanosheets namely hydroxylated boron nitride (OH-BNNSs) by an aqueous phase shearing method is characterized by comprising the following steps:
1) dissolving a surfactant in deionized water until the surfactant is completely dispersed;
2) dispersing blocky boron nitride h-BN serving as a raw material into the surfactant aqueous solution in the step 1) to prepare a suspension, and carrying out shear stripping treatment in a shear type reactor to obtain OH-BNNSs.
2. The method for preparing modified boron nitride nanosheets (hydroxylated boron nitride (OH-BNNSs) according to claim 1, wherein the surfactant of step 1) is one or more selected from anionic surfactants, amphoteric surfactants and nonionic surfactants.
3. The method for preparing modified boron nitride nanosheets, namely hydroxylated boron nitride OH-BNNSs, according to claim 1 wherein the surfactant is selected from the group consisting of sodium lauryl sulfate, sodium cholate, lauryl hydroxypropyl sulfobetaine, lauryl alanine diethanolamine salt, triton, polyvinyl alcohol.
4. The method for preparing the modified boron nitride nanosheets namely the hydroxylated boron nitride OH-BNNSs by the aqueous phase shearing method according to claim 1, wherein the concentration of the surfactant in the suspension in the step 2) is 0-1 mg/ml, and the concentration of the h-BN is 5-30 mg/ml.
5. The method for preparing the modified boron nitride nanosheets namely the hydroxylated boron nitride OH-BNNSs by the aqueous phase shearing method according to claim 4, wherein the mass ratio of the surfactant to the h-BN is selected to be 1:20-1: 200.
6. The method for preparing modified boron nitride nanosheets (hydroxylated boron nitride (OH-BNNSs) according to claim 1 by an aqueous phase shear process, wherein the shear reactor includes but is not limited to: shearing homogenizer, rotary packed bed, high pressure homogenizer, and stripping time of 0.25-20 hr.
7. The method for preparing modified boron nitride nanosheets (namely hydroxylated boron nitride OH-BNNSs) according to claim 6, wherein the mean pressure is 100MPa in the case of shear homogenizer, rotating packed bed, etc. at the rotation speed of 1000-.
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| CN113264778A (en) * | 2021-05-17 | 2021-08-17 | 厦门理工学院 | Boron nitride composite ceramic and preparation method and application thereof |
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