CN106554514A - A kind of method for modifying boron nitride nanosheet surface with poly-dopamine - Google Patents
A kind of method for modifying boron nitride nanosheet surface with poly-dopamine Download PDFInfo
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- CN106554514A CN106554514A CN201610962015.5A CN201610962015A CN106554514A CN 106554514 A CN106554514 A CN 106554514A CN 201610962015 A CN201610962015 A CN 201610962015A CN 106554514 A CN106554514 A CN 106554514A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The present invention relates to a kind of method for modifying boron nitride nanosheet with poly-dopamine.It is an object of the invention to provide the method that a kind of mixed solvent ultrasound of use polar organic solvent water is peeled off hexagonal boron nitride and modifies boron nitride nanosheet surface with poly-dopamine.The boron nitride nanosheet that the present invention is obtained good dispersion, yield in the mixed solvent of polar organic solvent water is high, the holding time is long.By poly-dopamine surface modification boron nitride nanosheet prepared by the inventive method, easily storage, good dispersion in a solvent.A kind of method for modifying boron nitride nanosheet with poly-dopamine provided by the present invention has simple to operate, safety, low cost and other advantages.
Description
Technical field
The present invention relates to new material technology field, more particularly to a kind of poly-dopamine modifies boron nitride nanosheet surface
Method.
Technical background
Boron nitride (BN) with good non-oxidizability, electrical insulating property, corrosion resistance, have it is amorphous, cube and six sides etc.
Various crystal formations.Wherein, six square boron nitride (h-BN) are by alternate B and N atoms sp2The hexagon two dimension honeybee of hydridization composition
Nest shape lattice structure, layer structure is similar to graphite, therefore chemical property is the most stable.Hexagonal boron nitride nanosheet shows many
Excellent property, such as good mechanical performance (700～900GPa of Young's moduluss, 120～160GPa of fracture strength, breaking strain
0.28～0.33%), high thermal stability (oxidation resistance temperature～850 DEG C) and high-termal conductivity (2000 W of heat conductivity in room temperature face
m-1·K-1) etc., while boron nitride nanosheet also has electrical insulating property (band gap of about 5eV～6eV), low thermal coefficient of expansion (10-6, be only second to quartz), chemical resistance, lubricity, the performance characteristics such as hydrophobicity and electro permanent magnetic.
Boron nitride nanosheet has many preparation methoies.Chemical vapour deposition technique, chemical stripping method, mental retardation ball-milling method and sound wave
The methods such as edman degradation Edman can be obtained the less boron nitride nanosheet of size.103539085 A of Chinese patent CN disclose one kind to be made
With the method that ammonium fluoroborate and sodium borohydride are Material synthesis hexagonal boron nitride nanosheet.104803363 A of Chinese patent CN are public
A kind of method that utilization high-shearing dispersion emulsifying machine shearing stripping prepares boron nitride nanosheet is opened.Chinese patent CN
103626141 A disclose a kind of method that utilization chemical stripping prepares hexagonal boron nitride nanosheet, the method phase after the reaction
Need to be washed to repeatedly acid solution PH between 6～8, last handling process is comparatively laborious.Above method is to a certain degree
On be prepared for boron nitride nanosheet, but obtained boron nitride nanosheet easily occurs to reunite, and boron nitride nanosheet surface has
Stronger inertia and its hydrophobicity.Additionally, when boron nitride nanosheet is prepared with mechanical stripping method, selected dispersion liquid is to nitridation
Boron nanometer sheet peeling effect has a great impact, from such as water, isopropanol, dehydrated alcohol, DMF, dodecane
The single solvents such as base ketopyrrolidine, dimethylformamide, N-METHYLFORMAMIDE can be obtained boron nitride to h-BN mechanical strippings and receive
Rice piece, but obtained boron nitride nanosheet easily reunites, keeps that the dispersity time is short, low yield, therefore be unfavorable for nitrogenizing
The large-scale industrial production of boron nanometer sheet, storage and apply.
The content of the invention
In order to solve the above problems, the invention provides a kind of mixed solvent of use polar organic solvent-water is used as dispersion
Liquid ultrasound stripping prepares boron nitride nanosheet, then with the method on the prepared boron nitride nanosheet surface of poly-dopamine modification,
The mixed solvent of described polar organic solvent-water is favorably improved the dispersion of boron nitride nanosheet, and boron nitride nanosheet exists
In the mixed solvent, the retention time is long, is difficult sedimentation of reuniting, improves the preparation efficiency of boron nitride nanosheet；The poly-dopamine
The boron nitride nanosheet of modification has good dispersibility, prevents the reunion of boron nitride nanosheet well, effectively improves
The storage and application of boron nitride nanosheet.
It is an object of the invention to provide a kind of method for modifying boron nitride nanosheet surface with poly-dopamine.
A kind of method for modifying boron nitride nanosheet surface with poly-dopamine, it is characterised in that with following process and step
Suddenly：
A. the preparation of boron nitride nanosheet：
A-1. by polar organic solvent and water mixing and stirring according to a certain percentage, obtain the mixing of polar organic solvent-water
Solvent, described polar organic solvent are isopropanol, dehydrated alcohol, DMF, dimethylformamide, N- methyl
Any one in Methanamide；Described polar organic solvent is 3 with the mass ratio of water: (1~2)；
A-2. by the mixed solvent of the polar organic solvent-water for having been prepared in hexagonal boron nitride powder and above-mentioned steps a-1 by one
The ratio of the mixed solvent of fixed ratio mixing and stirring, described hexagonal boron nitride powder and polar organic solvent-water is 1
g : 90 mL ~ 1 g : 110 mL；
A-3. carry out ultrasonic stripping under certain temperature, ultrasonic splitting time and ultrasonic power by acting on for ultrasound, it is described
Ultrasonic exfoliation temperature at 20～50 DEG C, ultrasonic splitting time is 0.5～3 hour, and ultrasonic power is in 360～1600 W；
A-4. ultrasound peel off after the completion of, by mixed liquor centrifugation rate be 1500 rpm～5000 rpm under conditions of carry out from
The heart, collecting supernatant carries out pumping rate, washing, is dried, and finally gives hexagonal boron nitride nanosheet；
B. the modification with poly-dopamine to boron nitride nanosheet：
B-1. alkaline buffer is prepared, three (methylol) aminomethane hydrochloride of 0.01mol/L～0.03mol/L is prepared
（Tris-Cl）Buffer solution or borate buffer solution, pH are 8.5 ~ 10.0；
B-2. above-mentioned hexagonal boron nitride nanosheet and dehydrated alcohol dispersion solvent are added in reaction vessel, stirring mixing is
Even, the ratio of boron nitride nanosheet and dehydrated alcohol dispersion solvent is 0.02g:1 mL~ 0.1 g:1mL；
B-3. alkaline buffer obtained in above-mentioned steps b-1 is added in above-mentioned reaction vessel, is uniformly mixed；Institute
The ratio of the buffer solution and boron nitride nanosheet of addition is 50mL:1g ~ 150mL:1g；
B-4. under the conditions of having noble gases or inert free gas, Dopamine Hydrochloride is added in above-mentioned reaction vessel, is stirred
The mass ratio of mix homogeneously, Dopamine Hydrochloride and boron nitride nanosheet is 1:3 ~ 1:8；
B-5. the reaction system is continuous at 20 DEG C ~ 25 DEG C of room temperature under stirring condition of the rotating speed for 300 rpm ~ 800 rpm
5 h ~ 8 h of stirring reaction；Then it is in colourless neutrality to repeat sucking filtration, wash to filtrate；Again temperature be 80 DEG C ~ 110 DEG C bars
It is dried under part, obtains the boron nitride nanosheet of surface poly-dopamine grafting and modifying.
The present invention includes following beneficial effect：
First, the invention provides a kind of ultrasound in the mixed solvent of polar organic solvent-water peels off the side of boron nitride nanosheet
Method, the mixed solvent of this kind of polar organic solvent-water are favorably improved the dispersion of boron nitride nanosheet, and boron nitride nanosheet exists
In the mixed solvent, the retention time is long, is difficult sedimentation of reuniting.
2nd, the present invention develops a kind of method of modifying of boron nitride nanosheet surface poly-dopamine, the process is simple, power consumption
It is low, easy to control.
3rd, good dispersion of the present invention by the boron nitride nanosheet of poly-dopamine modification in ethanol or water, holding time
Grow and be not susceptible to reunite.
4th, boron nitride nanosheet prepared by the inventive method, solves boron nitride nanosheet surface inertness, cannot and be polymerized
Thing matrix is compatible and the low problem of polymeric matrix interaction force, can improve boron nitride/polymer composites mechanics strong
The performance such as degree, heat conductivity, corrosion-resistant, can promote application of the boron nitride in polymer composites.
Description of the drawings
Fig. 1 is prepared during boron nitride nanosheet is dispersed in the mixed solvent of polar organic solvent-water for the embodiment of the present invention 1 and is put
Photo after putting 1 hour, after 1 month and after 6 months.
Fig. 2 is that boron nitride nanosheet prepared by the embodiment of the present invention 1 is dispersed in aqueous isopropanol (a, b are left for figure) and this
The boron nitride nanosheet of poly-dopamine modification prepared by inventive embodiments 3 is dispersed in aqueous isopropanol (a, b are right for figure) respectively
Photo (figure a) after placing 1 hour and the photo (figure b) after 3 months.
Fig. 3 is that the high-resolution-ration transmission electric-lens of boron nitride nanosheet prepared by the embodiment of the present invention 1 and SEAD shine
Piece.
Fig. 4 be the embodiment of the present invention 3 prepare poly-dopamine modification boron nitride nanosheet high-resolution-ration transmission electric-lens with
SEAD photo.
Fig. 5 is that the surface sweeping electromicroscopic photograph (figure a) and the present invention of boron nitride nanosheet prepared by the embodiment of the present invention 1 are implemented
The surface sweeping electromicroscopic photograph (figure b) of the boron nitride nanosheet of poly-dopamine modification prepared by example 3.
Fig. 6 is the poly-dopamine modification that boron nitride nanosheet prepared by the embodiment of the present invention 1 is prepared with the embodiment of the present invention 3
Boron nitride nanosheet X-ray micro-zone analysis（EDS）Comparison diagram, (a) figure represent the X micro-zone analysis of boron nitride nanosheet, (b)
Figure represents the X micro-zone analysis of the boron nitride nanosheet of poly-dopamine modification, and KeV refers to kiloelectron-volt that B, C, N and O are represented respectively
Boron, carbon, nitrogen and oxygen element.
Fig. 7 is the poly-dopamine modification that boron nitride nanosheet prepared by the embodiment of the present invention 1 is prepared with the embodiment of the present invention 3
Boron nitride nanosheet infrared spectrogram, wherein BNNSs represents that boron nitride nanosheet, BNNSs@PDA represent that poly-dopamine is repaiied
The boron nitride nanosheet of decorations.
Fig. 8 is the poly-dopamine modification that boron nitride nanosheet prepared by the embodiment of the present invention 1 is prepared with the embodiment of the present invention 3
Boron nitride nanosheet thermogravimetric curve figure, wherein BNNSs represents that boron nitride nanosheet, BNNSs@PDA represent poly-dopamine
The boron nitride nanosheet of modification.
Specific embodiment
Below by specific embodiment, the present invention is further described.
Embodiment 1：First, the isopropanol and deionized water of certain mass are taken so that the quality of isopropanol and deionized water
Than for 3:2, prepare the mixed solvent of polar organic solvent and water；Then, take 3 g hexagonal boron nitride powders to add to reaction vessel
In, then in reaction vessel, add 300 mL to be 3 in mass ratio:The mixed solvent of the 2 isopropanol-deionized waters for preparing,
Mixing and stirring；Finally, by reaction system ultrasonic exfoliation temperature be 20～50 DEG C, power is that the condition of 1350 W is first reacted
2 hours；After the completion of ultrasound is peeled off, mixed liquor is carried out being centrifuged under conditions of centrifugation rate is 3000 rpm, supernatant is collected
Carry out pumping rate, washing（Absolute ethanol washing 2 ~ 3 times）, be dried, finally give hexagonal boron nitride nanosheet.Sucking filtration film is aperture
For 0.22 μm of organic membrane.
Embodiment 2：First, the DMF and deionized water of certain mass are taken so that N, N- dimethyl methyl
The mass ratio of amide and deionized water is 3:2, prepare the mixed solvent of polar organic solvent and water；Then, take 3 g, six sides nitridation
Boron powder is added into reaction vessel, then in reaction vessel, add 300 mL to be 3 in mass ratio:2 N for preparing, N- bis-
The mixed solvent of methylformamide-deionized water, mixing and stirring；Finally, by reaction system ultrasonic exfoliation temperature be 20
～50 DEG C, power is that the condition of 1350 W first reacts 2 hours；Ultrasound peel off after the completion of, mixed liquor is carried out in centrifugation rate be
It is centrifuged under conditions of 3000 rpm, collecting supernatant carries out pumping rate, washing（Deionized water wash 2 ~ 3 times, absolute ethanol washing
2 ~ 3 times）, be dried, finally give hexagonal boron nitride nanosheet.Sucking filtration film is the organic membrane that aperture is 0.22 μm.
Embodiment 3：The Tris-Cl buffer of 0.01 mol/L is configured first（pH=8.5）300 mL, take 2 g by the present invention
Boron nitride nanosheet prepared by the method for embodiment 1 is placed in beaker, then adds 100 mL dehydrated alcohol in beaker, then plus
Enter the Tris-Cl buffer that 300 configured mL concentration are 0.01 mol/L, stir, add 600 mg hydrochloric acid DOPA
Amine stirs, finally by reaction system under the conditions of the rotating speed about magnetic agitation of 400 rpm room temperature reaction 6 hours.Obtain
Product sucking filtration, washing（Deionized water wash 3 ~ 5 times, absolute ethanol washing 3 ~ 5 times）, be dried, obtain poly-dopamine and repair
The boron nitride nanosheet of decorations, sucking filtration film are the organic membrane that aperture is 0.22 μm.
Embodiment 4：The Tris-Cl buffer of 0.01 mol/L is configured first（pH=8.5）300 mL, take 2 g by the present invention
Hexagonal boron nitride nanosheet prepared by the method for embodiment 2 is put in three neck round bottom flask, and 100 mL are then added in beaker
Dehydrated alcohol, adds the Tris-Cl buffer that 300 configured mL concentration are 0.01 mol/L, stirs, Xiang Sankou
Nitrogen is passed through in round-bottomed flask, 600 mg Dopamine Hydrochloride is added and is stirred, evacuation continues logical in three neck round bottom flask
Nitrogen, finally by reaction system room temperature reaction 6 hours in the magnetic agitation that rotating speed is 500 rpm and under conditions of logical nitrogen.
The product sucking filtration that arrives, washing（Deionized water wash 2 ~ 3 times, absolute ethanol washing 4 ~ 5 times）, be dried, obtain poly-dopamine
The boron nitride nanosheet of modification, sucking filtration film are the organic membrane that aperture is 0.22 μm.
Embodiment 5：Borax pH standard buffer solutions are configured first（pH=9.18）500 mL, take 8 g hexagonal boron nitride nanosheets
It is put in beaker, 150 mL dehydrated alcohol is then added in beaker, then measures and add configured Borax pH standard buffer solutions
450 mL, stir, and add 1000 mg Dopamine Hydrochloride and stir, reaction system is about 600 in rotating speed finally
Room temperature reaction 6 hours under the conditions of the magnetic agitation of rpm.The product sucking filtration that obtains, washing（Deionized water wash 3 ~ 5 times, it is anhydrous
Washing with alcohol 3 ~ 5 times）, be dried, obtain poly-dopamine modification boron nitride nanosheet, it is 0.22 μm that sucking filtration film is aperture
Organic membrane.
Claims (1)
1. a kind of method for modifying boron nitride nanosheet surface with poly-dopamine, it is characterised in that with following process and step
Suddenly：
A. the preparation of boron nitride nanosheet：
A-1. by polar organic solvent and water mixing and stirring according to a certain percentage, obtain the mixing of polar organic solvent-water
Solvent, described polar organic solvent are isopropanol, dehydrated alcohol, DMF, dimethylformamide, N- methyl
Any one in Methanamide；Described polar organic solvent is 3 with the mass ratio of water: (1~2)；
A-2. by the mixed solvent of the polar organic solvent-water for having been prepared in hexagonal boron nitride powder and above-mentioned steps a-1 by one
The ratio of the mixed solvent of fixed ratio mixing and stirring, described hexagonal boron nitride powder and polar organic solvent-water is 1
g : 90 mL ~ 1 g : 110 mL；
A-3. carry out ultrasonic stripping under certain temperature, ultrasonic splitting time and ultrasonic power by acting on for ultrasound, it is described
Ultrasonic exfoliation temperature at 20～50 DEG C, ultrasonic splitting time is 0.5～3 hour, and ultrasonic power is in 360～1600 W；
A-4. ultrasound peel off after the completion of, by mixed liquor centrifugation rate be 1500 rpm～5000 rpm under conditions of carry out from
The heart, collecting supernatant carries out pumping rate, washing, is dried, and finally gives hexagonal boron nitride nanosheet；
B. the modification with poly-dopamine to boron nitride nanosheet：
B-1. alkaline buffer is prepared, three (methylol) aminomethane hydrochloride of 0.01mol/L～0.03mol/L is prepared
（Tris-Cl）Buffer solution or borate buffer solution, pH are 8.5 ~ 10.0；
B-2. above-mentioned hexagonal boron nitride nanosheet and dehydrated alcohol dispersion solvent are added in reaction vessel, stirring mixing is
Even, the ratio of boron nitride nanosheet and dehydrated alcohol dispersion solvent is 0.02g:1 mL~ 0.1 g:1mL；
B-3. alkaline buffer obtained in above-mentioned steps b-1 is added in above-mentioned reaction vessel, is uniformly mixed；Institute
The ratio of the buffer solution and boron nitride nanosheet of addition is 50mL:1g ~ 150mL:1g；
B-4. under the conditions of having noble gases or inert free gas, Dopamine Hydrochloride is added in above-mentioned reaction vessel, is stirred
The mass ratio of mix homogeneously, Dopamine Hydrochloride and boron nitride nanosheet is 1:3 ~ 1:8；
B-5. the reaction system is continuous at 20 DEG C ~ 25 DEG C of room temperature under stirring condition of the rotating speed for 300 rpm ~ 800 rpm
5 h ~ 8 h of stirring reaction；Then it is in colourless neutrality to repeat sucking filtration, wash to filtrate；Again temperature be 80 DEG C ~ 110 DEG C bars
It is dried under part, obtains the boron nitride nanosheet of surface poly-dopamine grafting and modifying.
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