CN112028036A - Preparation method of boron nitride nanosheet dispersion liquid - Google Patents
Preparation method of boron nitride nanosheet dispersion liquid Download PDFInfo
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- CN112028036A CN112028036A CN202010952703.XA CN202010952703A CN112028036A CN 112028036 A CN112028036 A CN 112028036A CN 202010952703 A CN202010952703 A CN 202010952703A CN 112028036 A CN112028036 A CN 112028036A
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
- C01B21/0648—After-treatment, e.g. grinding, purification
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/004—Reflecting paints; Signal paints
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/32—Radiation-absorbing paints
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
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- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention provides a preparation method of boron nitride nanosheet dispersion, which can be used for preparing hexagonal boron nitride nanosheets with average thickness of 2-3 layers and external dimension of 0.3-0.5 mu m, and the yield is higher than 85%. The preparation method comprises the following steps: taking the micro-morphology of a disc shape, the diameter of the disc is 3-20 mu m, and the surface area is 2-6m in parts by mass21 portion of hexagonal boron nitride powder per gram, 10 to 30 portions of pure water, 3 to 5 portions of ammonium fluoride, 2 to 3 portions of sodium fluoride and 0.5 to 1.5 portions of sodium fluoride, and pulping at 160-Treating the mixture for 500 hours under the hydrothermal condition of 180 ℃ and stirring; and cooling the feed liquid after the hydrothermal treatment to room temperature, and removing free ions by an ion exchange method or an electrodialysis method to obtain the feed liquid containing the boron nitride nanosheets. The obtained feed liquid containing the boron nitride nanosheets can be prepared into powder in a vacuum drying method, a spray drying method and other manners, and can be stored or used by adding a proper amount of stabilizer and suspending agent, or replacing the contained water with other solvents.
Description
Technical Field
The invention belongs to the technical field of coating raw materials, and particularly relates to a preparation method of a boron nitride nanosheet dispersion liquid.
Background
The hexagonal boron nitride nanosheet is a functional material which is researched more in recent years and is similar to the structure of graphene; however, as the bonding force between adjacent sheet layers in the hexagonal boron nitride is larger than that between graphite layers, the nano-sheet is difficult to be prepared from the hexagonal boron nitride with micron size by the traditional methods of intercalation, stripping and the like.
In the prior art, a process for stripping hexagonal boron nitride powder into boron nitride nanosheets by a concentrated acid method and a concentrated alkali method also comprises NH4F, peeling the hexagonal boron nitride powder into the fluorinated boron nitride nanosheets, for example, chemically peeling the hexagonal boron nitride powder with the overall dimension of 3-8 microns and the thickness of about 100nm to nanosheets with the thickness of 1nm or 3-5 layers, but the yield of the nanosheets is low, the hexagonal boron nitride powder which is not peeled or is peeled to a greater extent needs to be separated out by a centrifugal method, and the separation process is difficult to realize.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of boron nitride nanosheets, which can be used for preparing hexagonal boron nitride nanosheets with average thickness of 2-3 layers and external dimension of 0.3-0.5 mu m, and the yield is higher than 85%.
The preparation method of the boron nitride nanosheet comprises the following steps: taking the micro-morphology of a disc shape, the diameter of the disc is 3-20 mu m, and the surface area is 2-6m in parts by mass21 part of hexagonal boron nitride powder per gram, 10 to 30 parts of pure water, 2 to 3 parts of ammonium fluoride and 0.5 to 1.5 parts of sodium fluoride are added, and the mixture is pulped and treated for 500 hours under the hydrothermal condition of 180 ℃ and the stirring temperature of 160-; and cooling the feed liquid after the hydrothermal treatment to room temperature, and removing free ions by an ion exchange method or an electrodialysis method to obtain the feed liquid containing the boron nitride nanosheets.
The feed liquid before and after the removal of free ions by the ion exchange method or the electrodialysis method is sampled and injected with green or red laser beams, and uniform and stable tyndall effect can be observed, no solid matter can be seen, and the transparency of the slurry is obviously different from that of the slurry before hydrothermal treatment.
The obtained feed liquid containing the boron nitride nanosheets can be prepared into powder by a vacuum drying method, a spray drying method and the like, and can be stored or used by adding a proper stabilizer and a proper suspending agent, or can be stored or used by replacing the contained water with an organic solvent such as propylene glycol methyl ether acetate and ethanol.
Detailed Description
The technical solution of the present invention is further illustrated below with reference to examples, but the present invention is not limited thereto.
Example 1
The surface area was 4.5m, taking the shape as a disk, the average diameter of the disk being 16 μm (the disk-like shape and the average diameter are determined from the scanning electron micrograph)2Putting 300g of hexagonal boron nitride powder with the mass purity of 99.6% in a 12L plastic barrel, adding 6000g of pure water, adding 750g of ammonium fluoride and 300g of sodium fluoride, stirring uniformly, pouring into a 10L pressure kettle with a polytetrafluoroethylene lining, stirring well, heating to 165 ℃ and continuously treating for 400 hours, stirring uniformly for 5 minutes without 2 hours in the period, cooling to room temperature after treatment, taking a plurality of material liquids with different depths in the kettle, respectively putting 15ml of each material liquid in a 20ml glass test tube, respectively injecting green and red laser beams along the central axis direction of the test tube, and observing uniform and stable Tyndall effect without solid matter; measuring the volume of feed liquid after hydrothermal treatment to 6530ml, removing free ions through a mixed bed of strong acid ion exchange resin and strong base ion exchange resin (the height-diameter ratio is 15, pure water between resin microspheres is removed by blowing from top to bottom before exchange), removing feed liquid between resin microspheres by blowing from top to bottom after exchange to obtain 6490ml of exchange liquid, placing the exchange liquid in a 12L plastic barrel, taking a plurality of feed liquids with different depths, placing 15ml of each feed liquid in a 20ml glass test tube, respectively injecting green and red laser beams along the central axis direction of the test tube, observing uniform and stable Tyndall effect, not seeing solid matter, sampling 100ml, drying in a normal temperature vacuum drying method, and measuring the surface area of the obtained powder to be more than 500m2The hexagonal boron nitride nanosheet can not be seen through a scanning electron microscope, and can be judged to be a hexagonal boron nitride nanosheet through scanning electron microscope images and photographs, wherein the hexagonal boron nitride nanosheet is 3 layers in average thickness (less than 5 layers in thickness) and 0.7 micrometer in average external dimension. The yield of the hexagonal boron nitride nanosheet is 88% through chemical analysis. Thus, 6490ml of the resulting exchange solution was a hexagonal boron nitride nanosheet feed solution having a mass concentration of 4.0% and pure water as the dispersion medium.
Taking 1000ml of hexagonal boron nitride nanosheet feed liquid with pure water as a dispersion medium and a mass concentration of 4.0%, adding 1250ml of propylene glycol methyl ether acetate, distilling, refluxing to remove water, cooling to room temperature, adding 2.4 titanate coupling agents, uniformly stirring, treating for 1 hour, adding 10.8 parts of polyvinyl alcohol, uniformly stirring, and treating for 1 hour to form 1200ml of dispersion liquid. The mass concentration of the hexagonal boron nitride nanosheets in the obtained propylene glycol monomethyl ether acetate dispersion liquid is 3.3%, the average thickness is 3 layers, the overall dimension is 0.7 mu m, and the content of the titanate-containing coupling agent is 0.2% and the content of polyvinyl alcohol is 2.7%; even if a green or red laser beam is irradiated along the central axis of the test tube, a uniform and stable Tyndall effect can be observed, and no solid can be observed.
Adding 1000g of organic silicon modified polyurethane resin into a shearing machine, starting a shearing motor, adding 150g of propylene glycol methyl ether acetate dispersion liquid, treating for 1h until boron nitride nanosheets are uniformly dispersed in the organic silicon modified polyurethane resin, adding 3g of ultraviolet absorbent UV-P and 10g of polyether modified siloxane, and uniformly mixing to obtain the shading and heat insulating coating. A judgment basis for uniform dispersion of the boron nitride nanosheets in the organic silicon modified polyurethane resin or the paint is that a mixed solution or paint is filled into a 20ml glass test tube until the glass test tube is nearly full, a green or red laser beam is emitted along the central axis direction of the test tube, a uniform and stable Tyndall effect can be observed, and no solid matter can be observed.
Preparing a coating on a clean glass plate by a blade coating mode, heating to 65 ℃ for curing for 60min, gradually volatilizing a solvent in the curing process, gradually polymerizing resin components, separating the obtained film layer, measuring the thickness to be about 42 mu m, and achieving 41% of visible light transmittance, 0.2% of ultraviolet transmittance, 62% of near infrared ray + ultraviolet ray reflectance and 42% of visible light scattering reflectance. After the coating is dried in the sun for 1000 hours in summer and autumn, the visible light transmittance, the ultraviolet transmittance, the near infrared ray + ultraviolet ray reflectance, the visible light reflectance, the color and the uniformity are tested to be unchanged.
The organic silicon modified polyurethane resin is a product of Sanjin pigment Limited liability company in Xigyang county, and is of the brand SJ-5021, wherein the resin content is 50%; the cured coating can resist ultraviolet light for a long time without color change, the light transmittance of the coating below 30 mu m can be kept above 90%, and the coating has good hardness and toughness and scratch resistance. The main component of the ultraviolet absorbent UV-P is 2- (2 '-hydroxy-5' -methylphenyl) benzotriazole. The titanate coupling agent is a titanate coupling agent TC-3 of a chemical auxiliary oil plant in the day of the Tianchan city.
Claims (4)
1. A preparation method of boron nitride nanosheets comprises the following steps: taking the micro-morphology as a disk, the diameter of the disk is 3-20 mu m, and the surface area is 2-10m in parts by mass21 part of hexagonal boron nitride powder per gram, 10 to 30 parts of pure water, 2 to 3 parts of ammonium fluoride and 0.5 to 1.5 parts of sodium fluoride are added, and the mixture is pulped and treated for 500 hours under the hydrothermal condition of 180 ℃ and 160-; and removing free ions from the slurry after the hydrothermal treatment by an ion exchange method or an electrodialysis method to obtain feed liquid containing the boron nitride nanosheets.
2. A method of producing boron nitride nanoplates as in claim 1, wherein the boron nitride nanoplates have an average thickness of 2-3 layers and an external dimension of 0.3-0.5 μm.
3. The method for preparing boron nitride nanosheets according to claim 1, wherein the feed solution containing boron nitride nanosheets is prepared into a powder by a vacuum drying method or a spray drying method.
4. The method for producing a boron nitride nanosheet dispersion of claim 1, wherein the feed liquid containing boron nitride nanosheets is stored or used by replacing water contained therein with an organic solvent.
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US20100081732A1 (en) * | 2003-10-14 | 2010-04-01 | National Taiwan University | Method of using hyperbranched polyamine to exfoliate inorganic clay into random form of nanosilicate platelet |
CN102532956A (en) * | 2010-12-22 | 2012-07-04 | 财团法人工业技术研究院 | Organic dispersion of inorganic nano-sheet and method for producing same |
CN103641130A (en) * | 2013-12-12 | 2014-03-19 | 山东大学 | Method for preparing fluorinated boron nitride in fluorinating and stripping manners |
CN103865311A (en) * | 2012-12-07 | 2014-06-18 | 财团法人工业技术研究院 | Organic dispersion, method for preparing the same and coating composition using the same |
CN107236346A (en) * | 2017-06-16 | 2017-10-10 | 凤台精兴生物科技有限公司 | A kind of preparation method of radiation proof thermal insulation coatings |
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-
2020
- 2020-09-11 CN CN202010952703.XA patent/CN112028036A/en not_active Withdrawn
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US20100081732A1 (en) * | 2003-10-14 | 2010-04-01 | National Taiwan University | Method of using hyperbranched polyamine to exfoliate inorganic clay into random form of nanosilicate platelet |
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CN103865311A (en) * | 2012-12-07 | 2014-06-18 | 财团法人工业技术研究院 | Organic dispersion, method for preparing the same and coating composition using the same |
US20180094182A1 (en) * | 2013-01-18 | 2018-04-05 | United States Of America As Represented By The Administrator Of Nasa | Highly Thermally Conductive Hexagonal Boron Nitride/Alumina Composite Made From Commercial Hexagonal Boron Nitride |
CN103641130A (en) * | 2013-12-12 | 2014-03-19 | 山东大学 | Method for preparing fluorinated boron nitride in fluorinating and stripping manners |
CN103641130B (en) * | 2013-12-12 | 2015-03-25 | 山东大学 | Method for preparing fluorinated boron nitride nanosheet in fluorinating and stripping manners |
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