CN105582889B - A kind of preparation method of three-dimensional carbon boron nitride nanometer material - Google Patents
A kind of preparation method of three-dimensional carbon boron nitride nanometer material Download PDFInfo
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- CN105582889B CN105582889B CN201610068404.3A CN201610068404A CN105582889B CN 105582889 B CN105582889 B CN 105582889B CN 201610068404 A CN201610068404 A CN 201610068404A CN 105582889 B CN105582889 B CN 105582889B
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Abstract
The present invention is a kind of preparation method of three-dimensional carbon boron nitride nanometer material.The preparation method uses three-step synthesis method：The first step, with solvent-thermal process diboron trioxide triethanolamine presoma colloid；Second step, the precursor powder of melamine hypoboric acid is synthesized with hydro-thermal method；3rd step, ground uniformly after the presoma obtained in step 1 and step 2 is mixed, under reaction atmosphere, high temperature pyrolysis obtains the homogeneous three-dimensional carbon boron nitride nanometer material of high-specific surface area, pattern.The present invention has the advantages that cost is low, yield is high, green non-pollution, application are strong, can obtain existing method not getable high-specific surface area, high quality, high-purity and have concurrently carbon, boron nitride superior function new boron carbonitrides three-dimensional nanometer material.
Description
Technical field
Technical scheme is related to carbon, boron nitride nanometer material technology synthesis field, specially a kind of three-dimensional carbon-to-nitrogen
Change synthetic method and the application of boron nano material.
Background technology
Nanoscale science and technology is the emerging technology for modern age emerging and developing rapidly, and nano material is in fine ceramics, doctor
Had a wide range of applications in the fields such as the, energy, environment, sensor.Carbon nanomaterial has unique microstructure and unusual
Electricity, mechanics, mechanical property and quantum size effect, and in new energy, environment, biology, medicine, information, space flight etc.
Field shows many excellent properties.Hexagonal boron nitride (h-BN) nano material, is isoelectronic species with graphite, has excellent height
Warm inoxidizability, chemical stability, excellent greasy property, high thermal conductance, good wave transparent performance etc., therefore be widely used in
The field such as machinery, metallurgy, electronics, Aero-Space.
Three-dimensional carbon-boron nitride nanometer material that this patent proposes is that fusion carbon nanomaterial and boron nitride nanometer material are superior
Property in the novel three-dimensional nano material of one, its microscopic appearance is to stack the bulk that forms by lamella, and the cross section of bulk is again
By being mutually communicated or blind bore hole forms cellular three-dimensional structure.Three-dimensional carbon-boron nitride nanometer material has excellent thing
Rationality energy, inoxidizability, chemical stability are strong, absorption property is strong, specific surface area is big, hole is abundant, nontoxic, thus extremely
It is suitably applied in drinking water purification and sewage disposal.
In recent years, many work are directed to the research of three-dimensional carbon and three-dimensional boron nitride nanometer material.2011, Cao et al.
By synthesize new presoma obtain tridimensional network graphene (Xiehong Cao, Yumeng Shi, Wenhui Shi,
Gang Lu,Xiao Huang,Qingyu Yan,Qichun Zhang and Hua Zhang；small；2011,7,No.22,
3163–3168.).2013, Wang et al. utilizations blew sugared method and three-dimensional foam graphene net have been synthesized on polymeric matrix
(Xuebin Wang,Yuanjian Zhang,Chunyi Zhi,Xi Wang,Daiming Tang,Yibin Xu,Qunhong
Weng,Xiangfen Jiang,Masanori Mitome,Dmitri Golberg&Yoshio Bando；nature
communications；2013,16,Dec,4:2905.).Lian et al. obtained hexagonal phase in 2011 with simple solid phase method
Three-dimensional boron nitride nanometer spends (Gang Lian, Xiao Zhang, Miao Tan, Shunjie Zhang, Deliang Cui and
Qilong Wang；J.Mater.Chem.,2011,21,9201.).The same year, Liu et al. is using template-free method synthesis cross network
Structure three-dimensional boron nitride (Dan Liu, Weiwei Lei, Si Qin＆Ying Chen；physical chemistry two-
dimensional materials(2013)4:4453.).Recent Zhao et al. is obtained using foaming agent auxiliary gas foaming method
The three-dimensional boron nitride thin-walled of multi-levelization (Huijie Zhao, Xiufeng Song and Haibo Zeng；3 NPG Asia
Materials(2015)7,e168.).Up to the present, it can also be prepared without preparation method efficiently, safe and have carbon concurrently
With three-dimensional carbon-boron nitride nanometer material that the low cost, high-purity, pattern of the superior function of boron nitride are homogeneous, specific surface area is big.
The content of the invention
The technical problems to be solved by the invention are：A kind of new three-dimensional carbon-boron nitride nanometer material and its system are provided
Preparation Method.The use of the colloid of diboron trioxide and triethanolamine solvent-thermal process is precursors in this method, product one
The brand-new carbon-to-nitrogen boron complex three-dimensional nanostructured of kind.The preparation method have cost is low, yield is high, green non-pollution, application
The advantages that property is strong.The present invention uses three-step synthesis method：The first step, with solvent-thermal process diboron trioxide triethanolamine presoma glue
Body；Second step, the precursor powder of melamine hypoboric acid is synthesized with hydro-thermal method；3rd step, by what is obtained in step 1 and step 2
Ground after presoma mixing it is uniform, under reaction atmosphere, high temperature pyrolysis obtain the homogeneous three-dimensional carbon of high-specific surface area, pattern-
Boron nitride nanometer material.Obtain the not getable high-specific surface area of existing method institute, high quality, high-purity and have carbon, nitrogen concurrently
Change New Type of Carbon-boron nitride three-dimensional nanometer material of the superior function of boron.
The technical scheme is that：
A kind of preparation method of three-dimensional carbon-boron nitride nanometer material, comprises the following steps：
(1) diboron trioxide and triethanolamine are mixed to join in reactor, stirred 5-60 minutes；Wherein, mol ratio
For boron atom:Nitrogen-atoms=1:3~3:1；
(2) reactor is sealed, insulation reaction 10-24 hours, then allow reactor to naturally cool at 150-200 DEG C
Room temperature, obtain the colloid mixture of diboron trioxide-triethanolamine；
(3) melamine and boric acid are placed in water, add the reactor with reflux after stirring 1-2 hours, in advance
Hot 80-90 DEG C dissolves it and is incubated 2-15 hours, and the mixed solution of melamine-boric acid-water is made, then cools down solution
To 10-25 DEG C, cooling velocity is 1-50 DEG C per minute, there is precipitating crystalline precipitation；1-5 days are incubated again, are filtrated to get crystal settling
Thing；Material proportion is that every milliliter of water contains 0.005-0.1 grams of melamine and 0.002-0.1 grams of boric acid；
(4) sediment obtained in step (3) is put into drying 3-8 hours in 60-80 DEG C of drying boxes, obtains white powder
End；
(5) grind, obtain a homogeneous mixture after colloid and the white powder mixing obtained step (2) and step (4)；Its
In, quality is than colloid and white powder=1:1–1:10；
(6) mixture that will be prepared in step (5), the 800-1500 DEG C of heat treatment under reaction atmosphere, heating rate is every
1-20 DEG C of minute, soaking time is 2-6 hours, is cooled under reaction atmosphere；Black foam shape solid matter be three-dimensional carbon-
Boron nitride nanometer material.
Reactor is polytetrafluoroethylliner liner in described step (1), the closed reactor of stainless steel external member.
Reaction atmosphere in described step (6) is argon gas, nitrogen or ammonia.
The gas flow rate of reaction atmosphere is 50-500 milliliters/per minute in described step (6).
Reaction mass volume is preferably the 70%-80% of reactor inner bag volume in described step (1).
The substantive distinguishing features of the present invention：
Raw material diboron trioxide is dissolved in triethanolamine at 150-200 DEG C, and the second of diboron trioxide three is obtained after cooling
Hydramine presoma colloid (steps 1 and 2)；Raw material melamine and boric acid are dissolved in 80-90 DEG C of aqueous solution, are separated out through cooling, mistake
Filter and melamine hypoboric acid molecular crystal precursor powder (step 3,4) is obtained after drying；Obtained presoma colloid and presoma
The effect of powder is well mixed, and colloid plays binding agent during this, precursor powder plays support (step 5)；Afterwards
In high-temperature heat treatment process, precursor mixture bulge foaming, substantial amounts of CO is discharged2, NH3Deng gas, ultimately form three-dimensional carbon-
Boron nitride nanometer material (step 6).
The beneficial effects of the invention are as follows：
1. the product obtained by the inventive method is the cellular three-dimensional carbon of high-purity-boron nitride nanometer material.XRD spectra
The diffraction maximum of (Fig. 1) is clear, is graphite and hexagonal boron nitride, occurs without the diffraction maximum of other dephasigns；SEM schemes (Fig. 2 and Fig. 3)
The monolithic structure that three-dimensional carbon-boron nitride nanometer material of the prepared this method synthesis of display is accumulated for lamella, the size of bulk
For 10-100 microns, the cross section of monolithic structure be it is cellular, wherein mesoporous pore size be 30 rans, macropore diameter be
250 rans, product purity are about 95%；Fig. 4 shows three-dimensional carbon-boron nitride nanometer material that this method obtains at low temperature
The absorption of nitrogen and desorption isotherm specific surface area can reach 344.133m2/g。
2. superior function and feature of the inventive method based on carbon and boron nitride nanometer material, had both possessed carbon material organic
Excellent performance in the absorption of pollutant, wherein, suction to methylene blue especially prominent to methylene blue and Congo red absorption
Attached amount is up to 408mg g-1, far above a kind of porous boron nitride nanofiber (patent No. CN201510026727.1)；Again simultaneously
Obtain the suction of outstanding adsorption of metal ions characteristic that boron nitride material is shown for example to cadmium ion, nickel ion, cobalt ions
It is attached etc..
3. raw material of the present invention is diboron trioxide, triethanolamine, boric acid and melamine, raw material it is common and
It is cheap.
4. the three-dimensional carbon that the present invention synthesizes-boron nitride nanometer material morphology is homogeneous, purity is high, specific surface area is big, method letter
It is single, reliable, and it is adapted to scale to be combined to.Resulting three-dimensional carbon-boron nitride is a kind of novel nano-material, is shown extremely excellent
It is elegant to organic pollution and the absorption property of metal ion, waste water control can be applied to well.
Brief description of the drawings
Fig. 1 is the X-ray diffraction spectrogram of three-dimensional carbon-boron nitride in embodiment 1.
Fig. 2 is the scanning electron microscope diagram of three-dimensional carbon-boron nitride in embodiment 1.
Fig. 3 is the scanning electron microscope diagram of three-dimensional carbon-boron nitride in embodiment 1.
Fig. 4 is the low temperature nitrogen adsorption and desorption thermoisopleth of three-dimensional carbon-boron nitride in embodiment 1.
Adsorption isotherms of the Fig. 5 for three-dimensional carbon-boron nitride in embodiment 1 to methylene blue.
Embodiment
The present invention is further described with instantiation below in conjunction with the accompanying drawings.
The autoclave and high temperature process furnances used in the embodiment of the present invention is known device.
Embodiment 1
(1) 20.9g diboron trioxides, 29.8g triethanolamines are weighed, and the two is mixed to the hydro-thermal for being placed in that volume is 50ml
In kettle inner bag.Now the boron of diboron trioxide and triethanolamine/nitrogen mol ratio is 3 in reaction mass:1, its volume of mixture is about
Account for the 80% of inner bag capacity.Add magneton and 1 hour is quickly stirred on magnetic stirring apparatus so that reactant is sufficiently mixed；
(2) the reactor inner bag that step 1) is configured with to reaction mass is placed in reactor, sealing, is incubated at 180 DEG C
Carry out solvent heat treatment (triethanolamine plays a part of reactant and solvent simultaneously) within 10 hours, then allow reactor natural cooling
To room temperature, the colloid mixture of diboron trioxide-triethanolamine is obtained after unloading kettle；
(3) 2.52 grams of boric acid and 2.47 grams of melamines are taken to be added separately in 100 milliliters of deionized water, stirring 1 is small
When after add with reflux reactor, preheating 80 DEG C dissolve it and be incubated 8 hours；Solution is then cooled to 25
DEG C, cooling velocity is 5 DEG C per minute, there is crystal precipitation precipitation.Insulation 1 day, is filtrated to get solid precipitation thing；
(4) sediment obtained in step (3) is put into 60 DEG C of drying bakers, is incubated 8 hours, obtains white powder；
(5) white powder obtained in the colloid obtained in 0.5g steps (2), and 2.5g steps (4) is weighed, according to matter
Measure ratio 1:5 are put into mortar, and carry out physical grinding and be well mixed, and obtain mix products as heat treatment presoma；
(6) mix precursor that will be obtained in step (5), it is used as under reaction atmosphere 1100 DEG C to be heat-treated in nitrogen, its
Middle air velocity is 80mL per minute, and heating rate is 5 DEG C per minute, and soaking time is 4 hours, afterwards in a nitrogen atmosphere under
Cooling.It is more three-dimensional carbons-boron nitride nanometer material to obtain black foam shape solid matter.
Tested through XRD, it is graphite and hexagonal boron nitride that Fig. 1 diffraction maximum, which shows product, and does not have spreading out for other dephasigns
Peak appearance is penetrated, illustrates that the purity through the three-dimensional carbon prepared by the inventive method-boron nitride nanometer material is high.Scheme through SEM (Fig. 2 and
Fig. 3) find out the three-dimensional monolithic structure that there is three-dimensional carbon-boron nitride nanometer material lamella to accumulate, the size of bulk is that 10-100 is micro-
Rice or so, the cross section of monolithic structure is three-dimensional honeycomb (foam) shape, wherein mesoporous pore size be 30 rans, macropore diameter be
250 rans.By surveying BET (Fig. 4), the specific surface area that can calculate three-dimensional carbon-boron nitride nanometer material is
344.133m2/ g, illustrate that prepared three-dimensional carbon-boron nitride nanometer material has high specific surface area.Above collection of illustrative plates explanation is originally
What invention obtained is three-dimensional carbon-boron nitride nanometer material that pattern is homogeneous, purity is high, specific surface area is big.By to methylene blue
Adsorption experiment is carried out, and fits its Langmuir adsorption isotherm (Fig. 5), it is known that its absorption to organic dyestuff methylene blue
Amount is up to 408mg g-1.By three-dimensional carbon-boron nitride nanometer material to Cr2+、Ni2+、Cd2+Adsorption experiment is carried out Deng metal ion,
Gone to adsorb 200mL with 50mg three-dimensional carbon-boron nitride, ion concentration is 50mg L-1, above-mentioned metal ion solution, in 2 minutes
It is i.e. adsorbable complete.Thus, it can be seen that the three-dimensional carbon synthesized-boron nitride nanometer material have it is extremely outstanding to organic dyestuff and
The absorption property of metal ion.
Embodiment 2, example 3
By in the step of embodiment 1 (1), the weighed amount of diboron trioxide is set to respectively：6.96g, 2.32g, i.e., by three oxidations
It is 1 that the dosage of two boron and triethanolamine makes into according to boron atom and nitrogen-atoms mol ratio respectively:1、1:3 are mixed to join reactor
In inner bag, other operations are same as Example 1, and obtained product is the same as embodiment 1.
Embodiment 4, example 5
The weighed amount of the step of embodiment 1 (3) mesoboric acid is set to 0.5g, 5g respectively；Maintain the amount of melamine constant.I.e.
Only reactant mesoboric acid concentration is changed into every milliliter of water respectively contains 0.005 gram, 0.05 gram of boric acid, maintains other operations
Same as Example 1, obtained product is the same as embodiment 1.
Embodiment 6, example 7
The weighed amount of melamine in the step of embodiment 1 (3) is set to 0.5g, 5g respectively；Maintain the amount of boric acid constant.I.e.
The concentration of melamine in reactant is only changed to every milliliter of water respectively and contains 0.005 gram, 0.05 gram of melamine, it is other each
Item operation is same as Example 1, and obtained product is the same as embodiment 1.
Embodiment 8
The weighed amount of colloid and white powder in the step of embodiment 1 (5) is set to 1.0g, 1.0g respectively, i.e., by colloid with
White powder is changed to mass ratio and is adjusted to 1:1, and physical grinding is well mixed, other operations are identical with example 1, obtain
The product arrived is the same as embodiment 1.
Embodiment 9, example 10
Heat treatment temperature in the step of embodiment 1 (6) is changed to 800 DEG C, 1300 DEG C respectively, other operations with
Embodiment 1 is identical, and obtained product is the same as embodiment 1.
Embodiment 11,12
Reaction atmosphere (nitrogen) in the step of embodiment 1 (6) is changed to argon gas, ammonia respectively, other operations are equal
Same as Example 1, obtained product is the same as embodiment 1.
Unaccomplished matter of the present invention is known technology.
Claims (4)
- A kind of 1. preparation method of three-dimensional carbon-boron nitride nanometer material, it is characterized in that comprising the following steps：（1）Diboron trioxide and triethanolamine are mixed to join in reactor, stirred 5-60 minutes；Wherein, mol ratio is Boron atom:Nitrogen-atoms=1: 3 ~ 3 : 1；（2）Reactor is sealed, the insulation reaction 10-24 hours at 150-200 DEG C, then allow reactor natural cooling To room temperature, the colloid mixture of diboron trioxide-triethanolamine is obtained；（3）Melamine and boric acid are placed in water, stirring adds the reactor with reflux, preheating after 1-2 hour 80-90 DEG C dissolve it and are incubated 2-15 hours, the mixed solution of melamine-boric acid-water are made, then by solution 10-25 DEG C are cooled to, cooling velocity is 1-50 DEG C per minute, there is precipitating crystalline precipitation；1-5 day is incubated again, is filtered Obtain crystal precipitation；Material proportion is that every milliliter of water contains 0.005-0.1 gram of melamine and 0.002-0.1 gram of boron Acid；（4）By step（3）In obtained sediment be put into 60-80 DEG C of drying boxes and dry 3-8 hours, obtain white powder End；（5）By step（2）And step（4）Grind, obtain a homogeneous mixture after obtained colloid and white powder mixing；Wherein, Quality is than colloid and white powder=1: 1 – 1 : 10 ；（6）By step（5）The mixture of middle preparation, 800-1500 DEG C of heat treatment under reaction atmosphere, heating rate are every point 1-20 DEG C of clock, soaking time are 2-6 hours, are cooled under reaction atmosphere；It is three-dimensional to obtain black foam shape solid matter Carbon-to-nitrogen boron nano material；Described step（6）In reaction atmosphere be argon gas, nitrogen or ammonia.
- 2. the preparation method of three-dimensional carbon as claimed in claim 1-boron nitride nanometer material, it is characterized in that described step（1） Middle reactor is polytetrafluoroethylliner liner, the closed reactor of stainless steel external member.
- 3. the preparation method of three-dimensional carbon as claimed in claim 1-boron nitride nanometer material, it is characterized in that described step（6） The gas flow rate of middle reaction atmosphere be 50-500 milliliters/it is per minute.
- 4. the preparation method of three-dimensional carbon as claimed in claim 1-boron nitride nanometer material, it is characterized in that described step（1） Middle reaction mass volume is preferably 70 % -80 % of reactor inner bag volume.
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| CN1206931A (en) * | 1998-08-22 | 1999-02-03 | 吉林大学 | Method for preparing cubic boron nitride monocrystal-diamond film hetru P-N junction |
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