CN105502342A - Method for preparing nanometer hollow carbon spheres with dopamine serving as carbon source - Google Patents
Method for preparing nanometer hollow carbon spheres with dopamine serving as carbon source Download PDFInfo
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- CN105502342A CN105502342A CN201610008245.8A CN201610008245A CN105502342A CN 105502342 A CN105502342 A CN 105502342A CN 201610008245 A CN201610008245 A CN 201610008245A CN 105502342 A CN105502342 A CN 105502342A
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- C01—INORGANIC CHEMISTRY
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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
- C01P2004/34—Spheres hollow
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- C01P2004/60—Particles characterised by their size
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- C01P2006/14—Pore volume
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Abstract
The invention discloses a method for preparing nanometer hollow carbon spheres with dopamine serving as the carbon source. The method includes the steps of firstly, preparing SiO2 nanometer spheres through a method (please see the method in the description); secondly, directly adding dopamine to a reaction system, and preparing SiO2Pdop by wrapping dopamine on the surfaces of SiO2 through in situ polymerization; thirdly, roasting the prepared SiO2Pdop under the atmosphere of nitrogen to obtain SiO2Carbon; fourthly, dispersing the prepared SiO2Carbon in an ammonia water solution to be etched. By means of the method, preparation of the SiO2 nanometer spheres and wrapping of dopamine are completed through a one-pot method, the preparation cycle is shortened, the energy consumption is saved, operation is easy, large-scale production can be easily achieved, nanometer hollow carbon spheres which are uniform in size, controllable in shell thickness and particle size and stable in morphology structure can be prepared, and application prospects are wide.
Description
Technical field
It is the method that carbon source prepares nano hollow carbon ball with Dopamine HCL that the present invention relates to a kind of, belongs to technical field of nanometer material preparation.
Background technology
Due to small-size effect, nano material has a lot of unique performances and special application, and high-specific surface area makes it be sent to great expectations in fields such as effective catalyst, hydrogen storage material, low melting materials.The change of appearance of nano material also causes remarkable change to the physicals of material itself, as: nano material has lower luminous reflectivity, can convert solar energy into electrical energy efficiently and heat energy, and also there is as additive the function strengthening toughness and intensity.Nano material has huge applications space and potential value in fields such as electronics, magnetics, acoustics, and nano material is also widely used in physics, chemistry, biology, material and field of medicaments simultaneously.Simultaneously the quantum size effect of nano material and macro quanta tunnel effect make Application of micron in electrical element, sensor field.
Along with the development of nanotechnology, nano hollow sphere material has due to it peculiar property that density is low, specific surface area is large, attracts wide attention, and becomes a study hotspot of technical field of nano material.Nano hollow carbon ball is the one in nano hollow sphere material, because it has good adsorptivity and perviousness, and hollow cavity can be used for holding guest molecule, produce microcosmic " parcel " effect, therefore nano hollow carbon ball is as a kind of novel functional materials, has broad application prospects in fields such as support of the catalyst, super capacitor, controlled drug transmission and slowly-releasings.
Usually adopt silicon-dioxide as presoma at present, then modifying on the surface of presoma by controlling carbon source, forming a kind of solid nucleocapsid structure, then remove presoma by the method for heating or chemical reaction, carbon source generation carbonization is made by high-temperature roasting, thus obtained hollow carbon sphere.
Research shows: Dopamine HCL and silicon-dioxide have good biocompatibility, and environmental friendliness is pollution-free, and the nitrogen element contained in Dopamine HCL can make the carbon source obtained by it in ultracapacitor, have good application prospect.Therefore existing is at present the report that carbon source prepares nano hollow carbon ball with Dopamine HCL, but current preparation method also exists following defect:
First, being carbon source when being prepared hollow carbon sphere at present with Dopamine HCL, is by presoma SiO
2nanometer ball is put in the dopamine solution prepared, by Dopamine HCL to presoma SiO
2nanometer ball is modified, the presoma SiO used
2nanometer ball is divided into two kinds of situations:
(1) SiO that market is directly bought is adopted
2nanometer ball: this method eliminates SiO
2the preparation of nanometer ball thus saved the preparation time of hollow carbon sphere, but, with the SiO that market is bought
2nanometer ball, can not meet in experiment SiO
2the flexible requirements of nanometer ball, the hollow carbon sphere prepared is more single, can not meet the demand of test or market diversification;
(2) SiO adopting laboratory now to make
2nanometer ball: this method can directly experimentally demand prepare different SiO
2nanometer ball, more flexibly; But when adopting now processed in this way, in order to ensure SiO
2the effect that the quality of nanometer ball and Dopamine HCL are modified, SiO
2after nanometer ball generates in reaction soln, all need the SiO first will prepared
2nanometer ball is separated, and then carries out the process such as a series of cleaning, drying to it, the SiO finally will handled well
2nanometer ball reacts with Dopamine HCL again, and making to prepare hollow carbon sphere needs just can complete through two steps, and this method inevitably wastes a large amount of time and reagent, causes the double loss of time and the energy.
Secondly, when preparing hollow carbon sphere at present, in etch step, usually use HF as etching agent to SiO
2nanometer ball etches, because HF is a kind of hypertoxicity material of severe corrosive, volatile, large to human body and environmental hazard, is therefore unfavorable for prepared by mass-producing.
Summary of the invention
For the problems referred to above that prior art exists, the object of this invention is to provide a kind of simple to operate, applied widely, what can realize mass-producing take Dopamine HCL as the method that carbon source prepares nano hollow carbon ball.
For achieving the above object, the technical solution used in the present invention is as follows:
Take Dopamine HCL as the method that carbon source prepares nano hollow carbon ball, comprise the steps:
A) first adopt
legal system is for SiO
2nanometer ball, then directly adds Dopamine HCL in reaction system, makes Dopamine HCL be coated on SiO by in-situ polymerization
2surface, obtained composite nano materials, referred to as: SiO
2pdop;
B) by obtained composite nano materials: SiO
2pdop, carries out calcination process under nitrogen atmosphere: be warming up to 450 ~ 550 DEG C with the temperature rise rate of 8 ~ 12 DEG C/min, is then incubated 4 ~ 6 hours, obtain the composite nano materials of carbonization, referred to as: SiO
2carbon;
C) by the composite nano materials of obtained carbonization: SiO
2carbon is dispersed in ammonia soln, carries out insulation etching 10 ~ 16 hours at 130 ~ 150 DEG C, obtains described nano hollow carbon ball, referred to as: voidCarbon.
Preferably, described step a) comprises following operation:
To the mixed solution and dripping tetraethyl orthosilicate (i.e. TEOS) of alcohol water and ammoniacal liquor, at room temperature stir 12 ~ 24 hours, make tetraethyl orthosilicate complete hydrolysis generate SiO
2nanometer ball; Then add Dopamine HCL directly in reaction soln, at room temperature continue stirring 12 ~ 72 hours, reaction terminates, centrifugation, washs, dry to the solid collected, and namely obtains SiO
2pdop.
As further preferred version, 1mL tetraethyl orthosilicate uses the mixing solutions of 8 ~ 245mL alcohol water and ammoniacal liquor.
As further preferred version, described alcohol water is formed for 1:1 ~ 20:1 (with 2:1 ~ 15:1 for the best) by volume by alcoholic solvent and water.
As further preferred version, the mixing solutions of described alcohol water and ammoniacal liquor is formed for 5:1 ~ 50:1 (with 8:1 ~ 45:1 for the best) by volume by alcohol water and ammoniacal liquor.
By regulating the SiO of alcohol water ratio, the amount of ammoniacal liquor, the adjustable generation of amount of tetraethyl orthosilicate
2the size of nanometer ball, adopts above-mentioned optimum ratio, can prepare the SiO of particle diameter at 120 ~ 450nm
2nanometer ball.
By regulating the carbon thickness of the shell of the nano hollow carbon ball of the adjustable generation of consumption of Dopamine HCL, if control the SiO of Dopamine HCL and generation
2the mass ratio of nanometer ball is 1:5 ~ 5:1, can prepare the nano hollow carbon ball that carbon thickness of the shell is 6 ~ 16nm; The SiO of generation described here
2the quality of nanometer ball carries out Theoretical Calculation by the TEOS added to obtain, and 1mLTEOS theory can generate 0.27gSiO
2nanometer ball.
Preferably, the concentration etching ammonia soln used is 5 ~ 15wt%.
Compared with prior art, the present invention has following significance beneficial effect:
1, the present invention before coated Dopamine HCL without the need to presoma SiO
2nanometer ball carries out centrifugation and washing, obviously shortens preparation cycle, has saved energy consumption, has improve productive rate;
2, carbonization calcination process of the present invention is without the need to the stage treatment of complexity, only need be warming up to 450 ~ 550 DEG C with the temperature rise rate of 8 ~ 12 DEG C/min, then be incubated 4 ~ 6 hours, not only simple to operate, and the damage avoided coated inner core materials, applied widely;
3, the present invention adopts and etches in ammonia soln, can not only stablize the pattern obtaining good nucleocapsid structure, and be conducive to large-scale production;
4, especially, experiment shows: the nano hollow carbon ball prepared by the inventive method, has appearance structure better, and specific surface area is large, and the advantages such as catalytic performance is excellent, have good use value and application prospect in fields such as environment; Further, owing to adopting Dopamine HCL to modify, containing nitrogen element in Dopamine HCL, make it in ultracapacitor, also have very large application prospect.
Accompanying drawing explanation
Fig. 1 is scanning electron microscope (SEM) photograph and the transmission electron microscope picture of the nano hollow carbon ball of preparation in embodiment 1;
Fig. 2 is the nitrogen physisorption test pattern of the nano hollow carbon ball of preparation in embodiment 1;
Fig. 3 is that the composite nano materials of the poly-Dopamine HCL coated silica prepared in embodiment 1-3 is (referred to as SiO
2pdop) transmission electron microscope picture;
Fig. 4 is the SiO of preparation in embodiment 1 and 4
2the scanning electron microscope (SEM) photograph of nanometer ball;
Fig. 5 is the SiO of preparation in embodiment 5
2the scanning electron microscope (SEM) photograph of nanometer ball;
Fig. 6 is that the composite nano materials of the poly-Dopamine HCL coated silica of preparation in embodiment 6 is (referred to as SiO
2pdop) scanning electron microscope (SEM) photograph;
Fig. 7 is that the Large stone of preparation in embodiment 7 gathers the composite nano materials of Dopamine HCL coated silica (referred to as SiO
2pdop) scanning electron microscope (SEM) photograph and transmission electron microscope picture;
Fig. 8 is the scanning electron microscope (SEM) photograph of the nano hollow carbon ball of preparation in embodiment 8.
Embodiment
Below in conjunction with embodiment and application examples, technical solution of the present invention is described in further detail and completely.
Embodiment 1
A) ammoniacal liquor being 32wt% by 40mL dehydrated alcohol, 4mL water and 1mL concentration joins in a clean beaker, after stirring makes it to mix, under agitation dropwise add 0.2mLTEOS (tetraethyl orthosilicate, CAS#78-10-4, density: 0.9346g/mL), at room temperature stir 12 hours, then directly add 200mg Dopamine HCL, at room temperature continue stirring 24 hours; Centrifugation (6000rpm, 3min), drying after washing 3 times respectively with water and ethanol successively to the solid collected, namely obtains the composite nano materials of poly-Dopamine HCL coated silica (referred to as SiO
2pdop);
B) by obtained SiO
2pdop is placed in tube furnace, under nitrogen protection, be warming up to 500 DEG C and be incubated roasting 5 hours at this temperature with the temperature rise rate of 10 DEG C/min, obtains the coated silicon-dioxide of carbon-coating (referred to as SiO
2carbon);
C) by obtained SiO
2in the mixing solutions that the ammoniacal liquor that it is 32wt% that Carbon is dispersed in by 30mL water and 10mL concentration is formed, and ultrasonic making is uniformly dispersed, then be transferred in reactor, insulation etching 12h at 140 DEG C, etching terminates rear centrifugation, three times are washed respectively, final drying with water and ethanol successively to the solid collected, obtain described nano hollow carbon ball (referred to as: voidCarbon).
Embodiment 2
The difference of the present embodiment and embodiment 1 is only: the amount of the Dopamine HCL added is replaced with 300mg by 200mg, and all the other contents are all identical with described in embodiment 1.
Embodiment 3
The difference of the present embodiment and embodiment 1 is only: the amount of the Dopamine HCL added is replaced with 300mg by 200mg, and replaces with 72 hours by adding the continuation of the room temperature after Dopamine HCL churning time by 24 hours, and all the other contents are all identical with described in embodiment 1.
Embodiment 4
The difference of the present embodiment and embodiment 1 is only: by step a) in add 1mL concentration be that the ammoniacal liquor of 32wt% replaces with and adds the ammoniacal liquor that 2mL, 3mL and 5mL concentration is 32wt% respectively, all the other contents are all identical with described in embodiment 1.
Embodiment 5
The difference of the present embodiment and embodiment 1 is only: by step a) in add 0.2mLTEOS and replace with and add 0.6mL, 1.2mL, 2.4mL and 5mLTEOS respectively, all the other contents are all identical with described in embodiment 1.
Embodiment 6
The difference of the present embodiment and embodiment 1 is only: by step a) in add 40mL dehydrated alcohol, 4mL water (that is: alcohol water than for 10:1) replaces with and adds alcohol water respectively than being the dehydrated alcohol of 2:1,4:1,6:1,8:1,15:1 and water, all the other contents are all identical with described in embodiment 1.
Embodiment 7
The difference of the present embodiment and embodiment 1 is only: by step a) in add 1mL concentration be that the ammoniacal liquor of 32wt% replaces with and adds the ammoniacal liquor that 5mL concentration is 32wt%; To add 0.2mLTEOS to replace with and add 5mLTEOS, all the other contents are all identical with described in embodiment 1.
Embodiment 8
The difference of the present embodiment and embodiment 1 is only: by step a) in add 40mL dehydrated alcohol, 4mL water (that is: alcohol water than for 10:1) replaces with and adds alcohol water than being the dehydrated alcohol (25mL) of 25:15 and water (15mL), be that the ammoniacal liquor of 32wt% replaces with and adds the ammoniacal liquor that 3.14mL concentration is 32wt% by adding 1mL concentration, to add 0.2mLTEOS to replace with and add 3.75mLTEOS, all the other contents are all identical with described in embodiment 1.
Below in conjunction with accompanying drawing, the present invention is further described:
Fig. 1 is scanning electron microscope (SEM) photograph and the transmission electron microscope picture of nano hollow carbon ball prepared by embodiment 1, wherein: a is the scanning electron microscope (SEM) photograph of the nano hollow carbon ball etching preparation in 12 hours in embodiment 1; B and c is the transmission electron microscope picture in etching 6 hours and 8 hours isolated nano hollow carbon balls of difference in embodiment 1 respectively; D is the transmission electron microscope picture of the nano hollow carbon ball etching preparation in 12 hours in embodiment 1; Visible in conjunction with b, c, d figure: under the same conditions, etching time has impact to the completely hollow carbon ball of acquisition, and etching time is too short, will obtain not exclusively hollow carbon ball; Visible in conjunction with a and d: homogeneous, the completely hollow nano hollow carbon ball of size can be prepared according to embodiment 1 condition.
Fig. 2 is the nitrogen physisorption test result of the nano hollow carbon ball of preparation in embodiment 1, can calculate the specific surface area (BET) of nano hollow carbon ball prepared by embodiment 1 up to 635m by Fig. 2
2/ g, mesopore volume is 0.63cm
3/ g, mesoporous size is 3.99nm, superior performance.It should be noted that, the nitrogen physisorption test result of nano hollow carbon ball prepared by other embodiment of the present invention is all fine, is only illustrated with embodiment 1 at this herein.
Fig. 3 is that the composite nano materials of the poly-Dopamine HCL coated silica prepared in embodiment 1-3 is (referred to as SiO
2pdop) transmission electron microscope picture, wherein: a and b is SiO prepared by embodiment 1 (200mg Dopamine HCL stirs 24 hours)
2the transmission electron microscope picture of Pdop; C and d is SiO prepared by embodiment 2 (300mg Dopamine HCL stirs 24 hours)
2the transmission electron microscope picture of Pdop; E and f is SiO prepared by embodiment 3 (300mg Dopamine HCL stirs 72 hours)
2the transmission electron microscope picture of Pdop; The thickness of poly-Dopamine HCL shell is wherein respectively 6nm (a, b), 10nm (c, d), 16nm (e, f); As can be seen here: the add-on along with Dopamine HCL increases and adds the prolongation in the reaction times after Dopamine HCL, the thickness of the poly-Dopamine HCL shell of preparation can be made to increase thereupon, illustrate by regulating the amount of the Dopamine HCL added and adding the reaction times after Dopamine HCL, can regulate and control the thickness of the shell of the nano hollow carbon ball of preparation.
Fig. 4 is the SiO of preparation in embodiment 1 and 4
2the scanning electron microscope (SEM) photograph of nanometer ball, wherein: a and b is the SiO adding the generation of 1mL ammoniacal liquor in embodiment 1
2the scanning electron microscope (SEM) photograph of nanometer ball; C and d is the SiO adding the generation of 2mL ammoniacal liquor in embodiment 4
2the scanning electron microscope (SEM) photograph of nanometer ball; E and f is the SiO adding the generation of 3mL ammoniacal liquor in embodiment 4
2the scanning electron microscope (SEM) photograph of nanometer ball; G and h is the SiO adding the generation of 5mL ammoniacal liquor in embodiment 4
2the scanning electron microscope (SEM) photograph of nanometer ball; As seen from Figure 4: along with increasing of ammoniacal liquor add-on, the SiO generated
2the particle diameter of nanometer ball also increases thereupon, and size changes to 250nm by 150nm, illustrates that the add-on of ammoniacal liquor is to generated SiO
2the particle diameter of nanometer ball has impact.
Fig. 5 is the SiO of preparation in embodiment 5
2the scanning electron microscope (SEM) photograph of nanometer ball, wherein: a and b is the SiO adding 0.6mLTEOS generation in embodiment 5
2the scanning electron microscope (SEM) photograph of nanometer ball; C and d is the SiO adding 1.2mLTEOS generation in embodiment 5
2the scanning electron microscope (SEM) photograph of nanometer ball; E and f is the SiO adding 2.4mLTEOS generation in embodiment 5
2the scanning electron microscope (SEM) photograph of nanometer ball; G and h is the SiO adding 5mLTEOS generation in embodiment 5
2the scanning electron microscope (SEM) photograph of nanometer ball; As seen from Figure 5: along with increasing of TEOS add-on, the SiO generated
2the particle diameter of nanometer ball also increases thereupon, and size changes to 175nm by 130nm, illustrates that the add-on of TEOS is to generated SiO
2the particle diameter of nanometer ball has impact.
Fig. 6 is that the composite nano materials of the poly-Dopamine HCL coated silica of preparation in embodiment 6 is (referred to as SiO
2pdop) scanning electron microscope (SEM) photograph, wherein: the alcohol water of a, b is than being 2:1, c, and the alcohol water of d is than being 4:1, e, and the alcohol water ratio of f is 6:1, g, the alcohol water of h is than being 8:1, i, and the alcohol water of j is than being 10:1, k, and the alcohol water of l is than being 15:1; As seen from Figure 6: the SiO that the comparison of alcohol water generates
2the particle diameter of nanometer ball has certain influence.
Fig. 7 is that the Large stone of preparation in embodiment 7 gathers the composite nano materials of Dopamine HCL coated silica (referred to as SiO
2pdop) scanning electron microscope (SEM) photograph and transmission electron microscope picture, wherein: the SiO generated when a and b is and adds 5mL ammoniacal liquor, 5mLTEOS
2the scanning electron microscope (SEM) photograph of Pdop, its particle diameter is 408nm; C and d is the Large stone SiO of preparation in 7
2the transmission electron microscope picture of Pdop; 5mLTEOS in 5mL ammoniacal liquor and embodiment 5 in embodiment 4, embodiment 7, by increasing the amount of ammoniacal liquor and TEOS simultaneously, can obtain the SiO of Large stone
2pdop.
Fig. 8 is the scanning electron microscope (SEM) photograph of nano hollow carbon ball prepared by embodiment 8, and wherein: a and b is the scanning electron microscope (SEM) photograph under high power lens, its particle diameter is 448nm; C and d is the scanning electron microscope (SEM) photograph under low power lens; As seen from Figure 8: the amount of alcohol water ratio, ammoniacal liquor and the amount of TEOS can affect the particle diameter of the final nano hollow carbon ball generated, illustrate by regulating and controlling the particle diameter of the nano hollow carbon ball of preparation the adjustment of above-mentioned parameter.
Current is the preparation that carbon source carries out nano hollow carbon ball with Dopamine HCL, is all first by presoma SiO
2nanometer ball is put in the dopamine solution prepared, by Dopamine HCL to presoma SiO
2nanometer ball is modified, and then carries out high-temperature roasting and HF etching to the product obtained.And present invention achieves SiO
2the preparation of nanometer ball and the one kettle way that is coated with of Dopamine HCL complete, without the need to the SiO as presoma
2nanometer ball carries out separating treatment, not only shortens preparation cycle, has saved energy consumption, and simple to operate, is easy to realize mass-producing; Further, maturing temperature of the present invention can drop to about 500 DEG C by 800 DEG C of the prior art, is not only conducive to energy efficient, and not easily causes the high-temperature damage to kernel; Especially, the present invention also can realize etching with dilute ammonia solution (concentration is only required to be 5 ~ 15wt%), and the environmental pollution can effectively avoiding strong acid (such as HF) to produce and murder by poisoning, be more conducive to industrializing implementation.Adopting the inventive method, can to prepare size homogeneous, and the thick and size controllable of shell, the nano hollow carbon ball that appearance structure is stable, have a extensive future.
Finally need to herein means out: be only part preferred embodiment of the present invention above; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.
Claims (6)
1. be the method that carbon source prepares nano hollow carbon ball with Dopamine HCL, it is characterized in that, comprise the steps:
A) first adopt
legal system is for SiO
2nanometer ball, then directly adds Dopamine HCL in reaction system, makes Dopamine HCL be coated on SiO by in-situ polymerization
2surface, obtained composite nano materials, referred to as: SiO
2pdop;
B) by obtained composite nano materials: SiO
2pdop, carries out calcination process under nitrogen atmosphere: be warming up to 450 ~ 550 DEG C with the temperature rise rate of 8 ~ 12 DEG C/min, is then incubated 4 ~ 6 hours, obtain the composite nano materials of carbonization, referred to as: SiO
2carbon;
C) by the composite nano materials of obtained carbonization: SiO
2carbon is dispersed in ammonia soln, carries out insulation etching 10 ~ 16 hours at 130 ~ 150 DEG C, obtains described nano hollow carbon ball, referred to as: voidCarbon.
2. the method for claim 1, is characterized in that, described step a) comprises following operation:
To the mixed solution and dripping tetraethyl orthosilicate of alcohol water and ammoniacal liquor, at room temperature stir 12 ~ 24 hours, make tetraethyl orthosilicate complete hydrolysis generate SiO
2nanometer ball; Then add Dopamine HCL directly in reaction soln, at room temperature continue stirring 12 ~ 72 hours, reaction terminates, centrifugation, washs, dry to the solid collected, and namely obtains SiO
2pdop.
3. method as claimed in claim 2, is characterized in that: 1mL tetraethyl orthosilicate uses the mixing solutions of 8 ~ 245mL alcohol water and ammoniacal liquor.
4. method as claimed in claim 2 or claim 3, is characterized in that: described alcohol water is formed for 1:1 ~ 20:1 by volume by alcoholic solvent and water.
5. method as claimed in claim 2 or claim 3, is characterized in that: the mixing solutions of described alcohol water and ammoniacal liquor is formed for 5:1 ~ 50:1 by volume by alcohol water and ammoniacal liquor.
6. the method for claim 1, is characterized in that: the concentration etching ammonia soln used is 5 ~ 15wt%.
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