CN102815689B - Preparation method of carbon micron ball material with even particle size - Google Patents
Preparation method of carbon micron ball material with even particle size Download PDFInfo
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- CN102815689B CN102815689B CN201210300689.0A CN201210300689A CN102815689B CN 102815689 B CN102815689 B CN 102815689B CN 201210300689 A CN201210300689 A CN 201210300689A CN 102815689 B CN102815689 B CN 102815689B
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Abstract
The invention belongs to the technical field of an inorganic nonmetallic material preparation method, and particularly relates to a preparation method of carbon micron ball material with even particle size. The preparation method adopts a hydrothermal reduction method, and comprises the steps of: taking ethylene glycol (EG) as carbon source and solvent, dissolving FeCl3, polyvinyl pyrrolidone (PVP) and AgNO3 and finally adding concentrated hydrochloric acid (HCl) into the solution; maintaining the conditions of high temperature and high pressure in a constant temperature drying oven and a reaction kettle with an inner liner made of polytetrafluoroethylene; and finally, preparing the carbon micron ball material. After being observed by a scanning electron microscope and detected by an electronic data system (EDS), the carbon micron ball material which is high in yield and even in particle size can be prepared by the method. Compared with the original preparation method, the hydrothermal method adopted by the preparation method is low in needed temperature and short in time; meanwhile, the carbon micron ball material prepared by the method is narrow in particle size distribution range and high in yield.
Description
Technical field
The invention belongs to ceramic preparation method technical field, particularly the preparation method of the uniform carbon micro-spheres material of a kind of particle diameter.
Background technology
Carbon is one of the abundantest element of occurring in nature content, and it can be used as single-element and forms the diverse material of many structure and properties.Its performance coverage from the most firmly to the softest, from isolator to good conductor, from thermal insulation to good heat conduction, from full extinction to full impregnated light etc. (Zhang Yongchao. the synthetic and performance study [D] of the hydrothermal method of carbosphere. Harbin: Heilongjiang University, 2008.), therefore the range of application of carbon material is also very extensive, too numerous to enumerate.In recent years, increasing research starts to pay close attention to new carbon, particularly Graphene, CNT (carbon nano-tube) and spherical carbon material etc., and its tempo is very rapidly surprising, and new carbon will be brought immeasurable impellent for the progress of human society.
Nineteen sixties, people find that in the forming process of research coke pitch compounds changes in the middle of can occurring in heat treatment process mutually, the spherical carbon material of phase in the middle of generating, it has the performance of a lot of excellences, as good electrical and thermal conductivity, high-bulk-density, self sintering and unreactiveness etc., thereby be widely used in the aspects such as template synthesis hollow ball-shape material, ion secondary battery cathode material lithium, support of the catalyst, high-density high-strength carbon material, activated carbon with high specific surface area and high-performance liquid chromatography filler.
In recent years, along with the appearance of the material preparation method becoming increasingly abundant, global researchist starts to prepare carbon micron-spheres with non-asphalt stock.Conventional preparation method has hydrothermal method, metal deoxidization, chemical vapor deposition (CVD) method, arc discharge method, supercritical methanol technology and template etc. at present.Wherein, hydrothermal method is simple to operate because of it, and product purity is high, becomes and adopts more preparation method, and its raw material adopts glucose, sucrose, Mierocrystalline cellulose etc. mostly.For example, the people such as Mi are just take glucose as principal reaction thing, at 500 ℃ of Water Under thermal response 12 h, obtain appearance attractive in appearance, size uniform is distributed in carbon ball (the Yuanzhu Mi between 1 micron ~ 2 microns, Weibing Hu, Youmeng Dan, Yingliang Liu. Synthesis of carbon micro-spheres by a glucose hydrothermal method[J]. Materials Letters, 2008,62 (8-9): 1194 – 1196.).
Summary of the invention
The preparation method who the object of this invention is to provide the uniform carbon micro-spheres material of a kind of particle diameter, is characterized in that, in the method, the carbon source of carbon micro-spheres material and solvent are EG solution, and the concrete steps of the method are as follows:
A. with electronic balance, weigh respectively the FeCl that mass ratio is 1:1
3and AgNO
3two kinds of reactants, in dry beaker, then weigh PVP and are placed in FeCl is housed
3beaker in, wherein FeCl
3with the mass ratio of PVP be 1:12; With graduated cylinder, measure a dense HCl and two parts of EG solution as solvent respectively, two parts of EG solution is labeled as respectively EG1 solvent and EG2 solvent is stand-by, and its volume ratio is dense HCl: EG1 solvent: EG2 solvent=1:1:2;
B. to FeCl is housed
3with in the beaker of PVP, add measured EG2 solvent, with glass stick, stir to be placed on magnetic stirring apparatus and stir until FeCl
3be dispersed in EG2 solvent with PVP, obtain yellow solution;
C. measured EG1 solvent is poured into AgNO is housed
3beaker in, with glass stick, stir to be placed on magnetic stirring apparatus and stir until AgNO
3be dispersed in EG1 solvent, obtain colourless transparent solution;
D. under magnetic agitation, by the water white transparency AgNO obtaining in step c
3solution evenly splashes into the FeCl obtaining in step b
3in the yellow mixing solutions of PVP, after stirring, add measured dense HCl solution, continue to stir this mixing solutions until mix, obtain yellow solution;
E. the faint yellow homogeneous mixture solotion obtaining in steps d is poured in the reactor that liner is tetrafluoroethylene, put into loft drier and react;
F. reaction finishes rear taking-up reactor, opens reactor after being cooled at normal temperatures room temperature, pours the solution in liner into beaker;
G. pour the solution in beaker into centrifuge tube, symmetry is put into whizzer, uses ethanol centrifuge washing three times, the final colloid being comprised of carbon micro-spheres material that obtains.
In described step e, the temperature of loft drier is 150 ℃ ~ 170 ℃.
In described step e, the reaction times is 7 h ~ 11 h.
Beneficial effect of the present invention is:
The present invention adopt hydrothermal method than in the past conventional preparation method temperature required low, the time is short, the carbon micro-spheres material particle size narrow distribution range of simultaneously preparing with this method, output is high.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the carbon micro-spheres material prepared by the present invention;
Fig. 2 is the EDS collection of illustrative plates of embodiment 1.
Embodiment
The invention provides the preparation method of the uniform carbon micro-spheres material of a kind of particle diameter, below in conjunction with the drawings and specific embodiments, the present invention will be further described.
Embodiment 1
Prepare the uniform carbon micro-spheres material of a kind of particle diameter, its concrete steps are as follows:
A. with electronic balance, weigh respectively 0.0163 g FeCl
3, 0.0170 g AgNO
3in two dry beakers, then weigh 0.2000 g PVP and be placed in FeCl is housed
3beaker in; With graduated cylinder, measure the dense HCl of a 5.0 ml, a 10.0 ml EG solvents and a 5.0 ml EG solvents respectively stand-by;
B. to FeCl is housed
3with in the beaker of PVP, pour measured 10.0 ml EG solvents into, with glass stick, stir to be placed on magnetic stirring apparatus and stir until FeCl
3be dispersed in EG with PVP, obtain yellow solution;
C. measured 5.0 ml EG solvents are poured into AgNO is housed
3beaker in, with glass stick, stir to be placed on magnetic stirring apparatus and stir until AgNO
3be dispersed in EG, obtain colourless transparent liquid;
D. under magnetic agitation, by the AgNO in step c
3solution evenly adds the FeCl in step b
3in PVP mixing solutions, after stirring, add the dense HCl solution of measured 5.0 ml, continue to stir this mixing solutions until stir, obtain yellow solution;
E. the faint yellow homogeneous mixture solotion of 20.0 ml of gained in steps d being poured into volume is that in the liner of the 25.0 ml reactor that is tetrafluoroethylene, the loft drier of putting into 160 ℃ carries out hydro-thermal reaction;
F. after reacting 9 h, take out reactor, open reactor after being cooled at normal temperatures room temperature, the solution in liner is poured in beaker;
G. pour the solution in beaker in step f into centrifuge tube, put into whizzer, rotating speed be 8000 rpm, time are under the condition of 10 min with centrifugal three times of ethanol, finally obtain carbon micro-spheres material.
With dropper, in centrifuge tube, draw a small amount of solution containing prepared carbon micro-spheres material, drop on the conductive resin being attached in sample table, after being dried, by scanning electron microscope (SEM), observe its pattern, as shown in Figure 1; As shown in Figure 2, through EDS, detect, the composition of prepared carbon micro-spheres material is carbon.
Claims (1)
1. a preparation method for the uniform carbon micro-spheres material of particle diameter, is characterized in that, in the method, the carbon source of carbon micro-spheres material and solvent are EG solution, and the concrete steps of the method are as follows:
A. with electronic balance, weigh respectively the FeCl that mass ratio is 1:1
3and AgNO
3two kinds of reactants, in dry beaker, then weigh PVP and are placed in FeCl is housed
3beaker in, wherein FeCl
3with the mass ratio of PVP be 1:12; With graduated cylinder, measure a dense HCl and two parts of EG solution as solvent respectively, two parts of EG solution is labeled as respectively EG1 solvent and EG2 solvent is stand-by, and its volume ratio is dense HCl:EG1 solvent: EG2 solvent=1:1:2;
B. to FeCl is housed
3with in the beaker of PVP, add measured EG2 solvent, with glass stick, stir to be placed on magnetic stirring apparatus and stir until FeCl
3be dispersed in EG2 solvent with PVP, obtain yellow solution;
C. measured EG1 solvent is poured into AgNO is housed
3beaker in, with glass stick, stir to be placed on magnetic stirring apparatus and stir until AgNO
3be dispersed in EG1 solvent, obtain colourless transparent solution;
D. under magnetic agitation, by the water white transparency AgNO obtaining in step c
3solution evenly splashes into the FeCl obtaining in step b
3in the yellow mixing solutions of PVP, after stirring, add measured dense HCl solution, continue to stir this mixing solutions until mix, obtain yellow solution;
E. the faint yellow homogeneous mixture solotion obtaining in steps d is poured in the reactor that liner is tetrafluoroethylene, put into loft drier and react;
F. reaction finishes rear taking-up reactor, opens reactor after being cooled at normal temperatures room temperature, pours the solution in liner into beaker;
G. pour the solution in beaker into centrifuge tube, symmetry is put into whizzer, uses ethanol centrifuge washing three times, the final colloid being comprised of carbon micro-spheres material that obtains;
In described step e, the temperature of loft drier is 150 ℃～170 ℃;
In described step e, the reaction times is 7h～11h.
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| CN201210300689.0A CN102815689B (en) | 2012-08-22 | 2012-08-22 | Preparation method of carbon micron ball material with even particle size |
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| CN102815689B true CN102815689B (en) | 2014-04-16 |
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| CN101665250A (en) * | 2009-09-25 | 2010-03-10 | 福州大学 | Polymerizing-pyrolytic method for preparing mesocarbon microbead in asphaltic base |
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