CN107337185A - A kind of hydrophily boron nitride nanosheet and its preparation method and application - Google Patents
A kind of hydrophily boron nitride nanosheet and its preparation method and application Download PDFInfo
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- CN107337185A CN107337185A CN201710500266.6A CN201710500266A CN107337185A CN 107337185 A CN107337185 A CN 107337185A CN 201710500266 A CN201710500266 A CN 201710500266A CN 107337185 A CN107337185 A CN 107337185A
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- 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
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- C01P2004/00—Particle morphology
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention belongs to technical field of nano material, discloses a kind of hydrophily boron nitride nanosheet and its preparation method and application.Preparation method specifically includes following steps：A, hexagonal boron nitride powder is dispersed in alcohols solvent, adds a certain amount of alkali saturated aqueous solution；B, the alcohols dispersion liquid of boron nitride powder is put into reactor and sealed, a period of time is reacted under the conditions of high-temperature closed；C, room temperature is cooled to, is washed with deionized after vacuum filtration to neutrality, basic ion intercalation boron nitride complex powder is can obtain after freeze-drying；D, composite powder is dispersed in deionized water again, is the aqueous dispersions that can obtain boron nitride nanosheet after supersound process 10min and dialysis purification.Preparation method technique provided by the invention is simple, easily operated, and cost is low and environmentally friendly, and obtained boron nitride nanosheet yield is high, has good water dispersible and stability.There is potential application prospect in fields such as pharmaceutical carrier, bio-sensings.
Description
Technical field
The invention belongs to technical field of nano material, more particularly to a kind of hydrophily boron nitride nanosheet and preparation method thereof
And application.
Background technology
Hexagonal boron nitride (Hexagonal boron nitride, h-BN) is also referred to as " white graphite ".As graphite
A kind of analogue, because its unique physics, chemical property receive the extensive concern of domestic and international researcher.Low-dimensional h-BN
Nano material has excellent biocompatibility, the outstanding luminescence generated by light for carrying medicine load capacity and uniqueness and electroluminescent special
Property, become the study hotspot of the biomedical sectors such as pharmaceutical carrier, bio-sensing, bio-imaging and oncotherapy.Six
Square boron nitride powder is by that can obtain individual layer or the less boron nitride nanosheet of layer after peeling off layer by layer.Boron nitride nanosheet quilt
It is considered an excellent carrier of medicine and protein delivery, huge application potential is shown in biomedicine field.
The method mainly method from top to bottom of boron nitride nanosheet is prepared, i.e., by physically or chemically means by boron nitride powder
Body material peels off the boron nitride nanosheet for obtaining small size.The method for much preparing boron nitride nanosheet at present is all from graphene
Preparation method be derived, but it is many prepare graphene method it is bad for the peeling effect of boron nitride, this is due to
Except Van der Waals force be present between boron nitride nanosheet, very strong ionic bond also be present and acting on.Therefore, for boron nitride material
The exploration of extensive stripping means is still a difficult point and focus for Material Field research.At present, the preparation nitridation reported
The main method of boron nanometer sheet includes vapour deposition process (Nano letters, 2010,10 (8):3209-3215.), ultrasonic solvent
Up-stripping method (Advanced Materials, 2009,21 (28):2889-2893.), ball-milling method (Ceramics
International,2016,42(6):7155-7163.Nature communications, 2015,6.), fusion method
(Advanced Materials,2013,25(15):2200-2204.), ion insertion method (Angewandte Chemie,
2014,126(14):3719-3723.), liquid nitrogen vaporization method (Angewandte Chemie, 2016,128 (36):10924-
10928.) etc..Although can successfully prepare boron nitride nanosheet by above method, still exist the reaction time it is long,
Experimentation is cumbersome, severe reaction conditions and the shortcomings of reaction reagent costliness.The method for preparing boron nitride nanosheet reported
Yield is still relatively low, and the size of prepared boron nitride nanosheet is larger, water dispersible is poor, also significantly limit it in life
Application in terms of thing medical science.Therefore, develop a kind of simple and environmentally-friendly and can be received applied to large-scale production hydrophily boron nitride
The method of rice piece is still a challenge.
The content of the invention
In order to overcome shortcoming and deficiency present in prior art, primary and foremost purpose of the invention is to provide a kind of hydrophily
The preparation method of boron nitride nanosheet；This method simple and fast, Environmental Safety, yield are high.
The hydrophily boron nitride nanosheet obtained another object of the present invention is to provide a kind of above-mentioned preparation method.
It is still another object of the present invention to provide the application of above-mentioned hydrophily boron nitride nanosheet.
The purpose of the present invention is achieved through the following technical solutions：
A kind of preparation method of hydrophily boron nitride nanosheet, this method are that basic ion is slotting as solvent using alcohols
Layer reagent, boron nitride nanosheet is prepared by solvent-thermal method.
Above-mentioned preparation method, specifically includes following steps：
(1) preparation of basic ion intercalation nitridation boron compound：
A, hexagonal boron nitride powder is dispersed in alcohol reagent, dispersion liquid is made, configured six in obtained dispersion liquid
The concentration of square boron nitride powder is 0.5~2mg/mL；The aqueous slkali that concentration is 2.5mol/L, ultrasound are added into the dispersion liquid again
Mix and mixed liquor is made；The volume ratio of the alcohol reagent and aqueous slkali is 30：1~5；
B, the obtained mixed liquors of step A are transferred in reactor, sealed；It is placed on the baking oven that temperature is 100~180 DEG C
6~24h of interior reaction, is cooled to room temperature, after being filtered by vacuum and being washed with deionized collect be deposited on it is white on miillpore filter
Color powder, it is put into vacuum drying chamber and dries the unnecessary moisture of removal, you can obtains basic ion intercalation nitridation boron compound；
(2) preparation of boron nitride nanosheet：
C, by step (1) obtain basic ion intercalation nitridation boron compound be scattered in again the aqueous solution be ultrasonically treated 10~
60min, centrifugation remove the hexagonal boron nitride powder being not peeled off, you can obtain the aqueous dispersions of boron nitride nanosheet；
D, by the obtained dispersion liquids of step C be transferred to molecular cut off be 8000~14000Da bag filter in dialyse to
Neutrality, remove remnants basic ion, the boron nitride nanosheet aqueous dispersions purified；Boron nitride nanosheet aqueous dispersions are cold
Freeze that boron nitride nanosheet powder can be obtained by vacuum freeze drying after ice.
Alcohol reagent described in step A is ethanol, ethylene glycol, glycerine, and abundance, cheap, toxicity is low, dirty
Contaminate small, and can preferably disperse hexagonal boron nitride powder；Described aqueous slkali is sodium hydroxide solution, potassium hydroxide solution or hydrogen
Lithia solution, its ion size are less than boron nitride piece interlamellar spacing, can effectively carry out intercalation and stripping.
Ultrasonic power described in step A is 118~122W.
Reactor described in step B is polytetrafluoroethyllining lining reactor；Filter membrane used in the vacuum filtration is to have
Machine filter film, aperture 0.22um, most of product peeled off and obtained can be retained.
The time of dialysis described in step D is 2~3 days, changes a deionized water within each 6 hours, until neutral, energy
It is enough effectively to remove unnecessary basic ion.
Vacuum freeze drying described in step D be temperature be -40~-90 DEG C, air pressure be 8~20Pa under conditions of it is cold
It is lyophilized dry, obtain boron nitride nanosheet powder.
A kind of hydrophily boron nitride nanosheet being prepared according to above-mentioned preparation method.
Application of the above-mentioned hydrophily boron nitride nanosheet in pharmaceutical carrier, bio-sensing field.
The present invention is had the following advantages relative to prior art and effect：
(1) present invention prepares boron nitride nanosheet using solvent-thermal method, and required alcohols solvent is cheap and easy to get, and toxicity is low, right
Environmental pollution is small, and can effectively disperse hexagonal boron nitride powder, contact of the increase hexagonal boron nitride powder with intercalating ions.
(2) alkali is common industrial chemicals, cheap, can effectively intercalation and peel off hexagonal boron nitride powder, institute
The boron nitride nanosheet purity and yield of acquisition are all higher, and have good water dispersible and stability.
(3) preparation method of the present invention is easy to operate, and required experimental facilities is simple, and production cost is low and the cycle is short, it is expected to real
Existing industrial mass production.
Brief description of the drawings
Fig. 1 is the high resolution transmission electron microscopy piece of boron nitride nanosheet prepared by embodiment 1.
Fig. 2 is the atomic force microscopy diagram of boron nitride nanosheet prepared by embodiment 1.
Fig. 3 is Tyndall phenomenon figure of the boron nitride nanosheet aqueous dispersions of the preparation of embodiment 1 under laser irradiation.
Fig. 4 is the X-ray diffractogram of hexagonal boron nitride powder prepared by embodiment 1 and boron nitride nanosheet.
Embodiment
With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.
Embodiment 1：
(1) preparation of basic ion intercalation nitridation boron compound
A. hexagonal boron nitride powder is dispersed in 30mL ethanol, dispersion liquid is made, configured six in obtained dispersion liquid
The concentration of square boron nitride powder is 1mg/mL；It is water-soluble that the potassium hydroxide that 2mL concentration is 2.5mol/L is added into the dispersion liquid again
Liquid, ultrasound, which mixes, is made mixed liquor；
B. the obtained mixed liquors of step A are uniformly transferred in reactor by graduated cylinder, sealed；Being placed on temperature is
Reaction 12h, is cooled to room temperature in 180 DEG C of baking oven, is collected after being filtered by vacuum and being washed with deionized and is deposited on micropore filter
White powder on film, it is put into vacuum drying chamber and dries the unnecessary moisture of removal, you can it is compound to obtain basic ion intercalation boron nitride
Thing.
(2) preparation of boron nitride nanosheet
C. step (1) is obtained into basic ion intercalation nitridation boron compound and is scattered in aqueous solution supersound process 20min again, from
The heart removes the hexagonal boron nitride powder being not peeled off, you can obtains the aqueous dispersions of boron nitride nanosheet.
D. by the obtained dispersion liquids of step C be transferred to molecular cut off be 8000~14000Da bag filter in dialyse to
Neutrality, remove remnants basic ion, the boron nitride nanosheet aqueous dispersions purified.Boron nitride nanosheet aqueous dispersions are cold
Freeze that boron nitride nanosheet powder can be obtained by vacuum freeze drying after ice.
Fig. 1 is the high resolution TEM picture for the boron nitride nanosheet that embodiment 1 obtains, and is made as we can see from the figure
The boron nitride nanosheet obtained is in film-form lamella, and surface has many folds, and this is due to that surface many oxygen-containing officials occurs
Caused by rolling into a ball, this phenomenon is oxidized to after graphite oxide similar to graphite there is the phenomenon of fold.Fig. 2 is embodiment 1
The atomic force microscopy diagram of obtained boron nitride nanosheet, there is figure to understand that the thickness of boron nitride nanosheet is only 1.5nm or so, say
It is bright that few layer of boron nitride nanosheet is successfully peeled off into by alkali intercalation solution heat treatment process hexagonal boron nitride powder.Fig. 3 is real
Apply the X-ray diffractogram of boron nitride nanosheet that example 1 obtains and hexagonal boron nitride powder, it is known that hexagonal boron nitride powder is in 2=
26.68 ° have a spike, and corresponding is hexagonal boron nitride (002) crystal face, and boron nitride nanosheet occurs one at 2=27.73 °
Weaker peak, peak width become big.Fig. 4 is after the boron nitride nanosheet aqueous dispersions that embodiment 1 obtains are placed one week, in laser pen
Under irradiation, it is observed that obvious Tyndall phenomenon.
Embodiment 2
(1) preparation of basic ion intercalation nitridation boron compound
A. hexagonal boron nitride powder is dispersed in 30mL ethylene glycol, dispersion liquid is made, configured in obtained dispersion liquid
The concentration of hexagonal boron nitride powder is 0.5mg/mL；The sodium hydroxide that 1mL concentration is 2.5mol/L is added into the dispersion liquid again
The aqueous solution, ultrasound, which mixes, is made mixed liquor；
B. the obtained mixed liquors of step A are uniformly transferred in reactor by graduated cylinder, sealed；Being placed on temperature is
Reaction 16h, is cooled to room temperature in 160 DEG C of baking oven, is collected after being filtered by vacuum and being washed with deionized and is deposited on micropore filter
White powder on film, it is put into vacuum drying chamber and dries the unnecessary moisture of removal, you can it is compound to obtain basic ion intercalation boron nitride
Thing.
(2) preparation of boron nitride nanosheet
C. step (1) is obtained into basic ion intercalation nitridation boron compound and is scattered in aqueous solution supersound process 30min again, from
The heart removes the hexagonal boron nitride powder being not peeled off, you can obtains the aqueous dispersions of boron nitride nanosheet.
D. by the obtained dispersion liquids of step C be transferred to molecular cut off be 8000~14000Da bag filter in dialyse to
Neutrality, remove remnants basic ion, the boron nitride nanosheet aqueous dispersions purified.Boron nitride nanosheet aqueous dispersions are cold
Freeze that boron nitride nanosheet powder can be obtained by vacuum freeze drying after ice.
Embodiment 3
(1) preparation of basic ion intercalation nitridation boron compound
A. hexagonal boron nitride powder is disperseed in 30mL glycerine, dispersion liquid is made, configured six in obtained dispersion liquid
The concentration of square boron nitride powder is 2mg/mL；It is water-soluble that the lithium hydroxide that 4mL concentration is 2.5mol/L is added into the dispersion liquid again
Liquid, ultrasound, which mixes, is made mixed liquor；
B. the obtained mixed liquors of step A are uniformly transferred in reactor by graduated cylinder, sealed；Being placed on temperature is
Reaction 24h, is cooled to room temperature in 120 DEG C of baking oven, is collected after being filtered by vacuum and being washed with deionized and is deposited on micropore filter
White powder on film, it is put into vacuum drying chamber and dries the unnecessary moisture of removal, you can it is compound to obtain basic ion intercalation boron nitride
Thing.
(2) preparation of boron nitride nanosheet
C. step (1) is obtained into basic ion intercalation nitridation boron compound and is scattered in aqueous solution supersound process 20min again, from
The heart removes the hexagonal boron nitride powder being not peeled off, you can obtains the aqueous dispersions of boron nitride nanosheet.
D. by the obtained dispersion liquids of step C be transferred to molecular cut off be 8000~14000Da bag filter in dialyse to
Neutrality, remove remnants basic ion, the boron nitride nanosheet aqueous dispersions purified.Boron nitride nanosheet aqueous dispersions are cold
Freeze that boron nitride nanosheet powder can be obtained by vacuum freeze drying after ice.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (9)
- A kind of 1. preparation method of hydrophily boron nitride nanosheet, it is characterised in that：This method is as solvent, alkali using alcohols Ion is intercalation reagent, and boron nitride nanosheet is prepared by solvent-thermal method.
- 2. preparation method according to claim 1, it is characterised in that：This method specifically includes following steps：(1) preparation of basic ion intercalation nitridation boron compound：A, hexagonal boron nitride powder is dispersed in alcohol reagent, dispersion liquid is made, configure six side's nitrogen in obtained dispersion liquid The concentration for changing boron powder is 0.5~2mg/mL；The aqueous slkali that concentration is 2.5mol/L is added into the dispersion liquid again, ultrasound mixes Mixed liquor is made；The volume ratio of the alcohol reagent and aqueous slkali is 30：1~5；B, the obtained mixed liquors of step A are transferred in reactor, sealed；It is placed on anti-in the baking oven that temperature is 100~180 DEG C 6~24h is answered, is cooled to room temperature, the white powder being deposited on miillpore filter is collected after being filtered by vacuum and being washed with deionized End, it is put into vacuum drying chamber and dries the unnecessary moisture of removal, you can obtains basic ion intercalation nitridation boron compound；(2) preparation of boron nitride nanosheet：C, step (1) is obtained into basic ion intercalation nitridation boron compound and is scattered in the aqueous solution 10~60min of supersound process again, from The heart removes the hexagonal boron nitride powder being not peeled off, you can obtains the aqueous dispersions of boron nitride nanosheet；D, the obtained dispersion liquids of step C are transferred in the bag filter that molecular cut off is 8000~14000Da and dialysed to neutrality, Remove remaining basic ion, the boron nitride nanosheet aqueous dispersions purified；Boron nitride nanosheet aqueous dispersions are freezed and tied Boron nitride nanosheet powder can be obtained by vacuum freeze drying after ice.
- 3. preparation method according to claim 2, it is characterised in that：Alcohol reagent described in step A is ethanol, second two Alcohol, glycerine；Described aqueous slkali is sodium hydroxide solution, potassium hydroxide solution or lithium hydroxide solution.
- 4. preparation method according to claim 2, it is characterised in that：Ultrasonic power described in step A be 118~ 122W。
- 5. preparation method according to claim 2, it is characterised in that：Reactor described in step B is polytetrafluoroethylene (PTFE) Liner reactor；Filter membrane used in the vacuum filtration is organic filter membrane, aperture 0.22um.
- 6. preparation method according to claim 2, it is characterised in that：The time of dialysis described in step D is 2~3 days, A deionized water is changed within each 6 hours, until neutral.
- 7. preparation method according to claim 2, it is characterised in that：Vacuum freeze drying described in step D is in temperature Spend for -40~-90 DEG C, air pressure is freeze-dried under conditions of being 8~20Pa, obtains boron nitride nanosheet powder.
- A kind of 8. hydrophily boron nitride nanosheet that preparation method according to claim any one of 1-7 is prepared.
- 9. application of the hydrophily boron nitride nanosheet according to claim 8 in pharmaceutical carrier, bio-sensing field.
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Cited By (13)
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| CN108003864A (en) * | 2017-12-04 | 2018-05-08 | 西南科技大学 | A kind of luminol lighting function nm-class boron nitride and preparation method thereof |
| CN108529575A (en) * | 2018-07-16 | 2018-09-14 | 齐鲁师范学院 | A method of preparing boron nitride nanosheet using solvent thermal reaction |
| CN108584891A (en) * | 2018-07-20 | 2018-09-28 | 芜湖清柏白露智能信息科技有限公司 | A kind of preparation method of boron nitride nanometer band |
| CN109353996A (en) * | 2018-10-09 | 2019-02-19 | 北京科技大学 | A kind of preparation method of few layer hexagonal boron nitride nanosheet |
| CN109573965A (en) * | 2018-12-26 | 2019-04-05 | 合肥学院 | A kind of preparation method of hydroxyl modification boron nitride nanosheet dispersion liquid |
| CN110577197A (en) * | 2018-06-11 | 2019-12-17 | 中国科学院深圳先进技术研究院 | Preparation method of boron nitride nanosheet |
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| CN109353996A (en) * | 2018-10-09 | 2019-02-19 | 北京科技大学 | A kind of preparation method of few layer hexagonal boron nitride nanosheet |
| CN109573965A (en) * | 2018-12-26 | 2019-04-05 | 合肥学院 | A kind of preparation method of hydroxyl modification boron nitride nanosheet dispersion liquid |
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| CN110746563A (en) * | 2019-10-24 | 2020-02-04 | 江苏理工学院 | PEG ball-milling intercalation h-BN modified polyurethane heat-conducting composite material and preparation method thereof |
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| CN111137866A (en) * | 2020-01-10 | 2020-05-12 | 中国南方电网有限责任公司电网技术研究中心 | Method for preparing boron nitride nanosheet by efficiently stripping h-BN |
| CN113604047A (en) * | 2021-09-02 | 2021-11-05 | 大同共聚(西安)科技有限公司 | Preparation method of boron nitride graphene oxide polyimide composite material |
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Application publication date: 20171110 |