CN102765712A - Method for preparing carbon microspheres - Google Patents
Method for preparing carbon microspheres Download PDFInfo
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- CN102765712A CN102765712A CN2012102356399A CN201210235639A CN102765712A CN 102765712 A CN102765712 A CN 102765712A CN 2012102356399 A CN2012102356399 A CN 2012102356399A CN 201210235639 A CN201210235639 A CN 201210235639A CN 102765712 A CN102765712 A CN 102765712A
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Abstract
The invention provides a method for preparing carbon microspheres. The method comprises the steps of: taking glucose as a carbon source, dissolving the glucose in water, and then carrying out microwave hydrothermal reaction, washing and drying on the solution, thereby obtaining the carbon microspheres. The diameter and yield of the carbon microspheres can be controlled by controlling the temperature, pressure and time of the microwave hydrothermal reaction. The carbon microspheres obtained by the method provided by the invention is even in particle size distribution and high in purity; and the diameter of the carbon microspheres is about 100-500 nm. The method for preparing the carbon microspheres provided by the invention is friendly to the environment without pollution, short in reaction time, low in reaction temperature, simple in operation, good in repeatability and the like.
Description
Technical field
The invention belongs to the nano-carbon material preparing technical field, relate to a kind of method for preparing carbosphere.
Background technology
Since the eighties in last century, CNT was found, worldwide started the carbon material research boom, the new carbon of different structure and pattern is synthesized in succession, like C60 (soccerballene), Graphene etc.Carbosphere is as one of research focus of carbon material in recent years; Have that density is low, the intrinsic damp performance is good, the performance of thermostability and multiple excellences such as chemicalstability is high, controllable specific surface area and good biocompatibility, have broad application prospects in fields such as lightweight structural material, metal-based damping material, support of the catalyst, lithium ion battery negative material, electrode material for super capacitor and fuel cells.
At present, the method for preparing carbosphere has a lot, mainly can be divided into template, liquid phase synthesizing method, vapor-phase thermal cracking method etc.Wherein liquid phase synthesizing method utilizes water or organic solvent to be media, and under the autogenous pressure of certain temperature and solvent, a kind of compound method that raw material reacts has the advantage that synthesis temperature is lower, product purity is higher.Yet prepare needs adding metal catalyst in the carbon material process for most organic solvent, raw material and product have toxicity, not environmental protection.Therefore, the liquid phase preparation process that seek a kind of raw material of environmental protection cheaply, need not catalyzer becomes the focus of carbosphere synthetic technology.Min Li etc. are at Hydrothermalsynthesis; Characterization; Adopt hydrothermal synthesis method among the and KOH activation of carbon spheres from glucose [Carbohydrate Research346 (2011) 999-1004]; With glucose is that raw material has made carbosphere, and microsphere diameter is at 350 ~ 600nm.Yet the reaction times, general length needed could synthesize carbosphere more than 5 hours, and efficient is lower.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method who prepares the carbosphere of simple, efficient, environmental protection, and this method is to be starting material with glucose, utilizes microwave-assisted hydrothermal synthesis of carbon microballoon.The prepared carbosphere purity of this method is high, particle diameter is even, controllable size; Adopt the hydrothermal synthesis method of microwave-assisted have the reaction times short, temperature of reaction is low; Simple to operate, advantages such as good reproducibility are that the starting material environmental friendliness is pollution-free, with low cost with glucose.
For realizing above-mentioned purpose, the invention provides a kind of method for preparing carbosphere, with glucose carbon source; After its dissolving, after the microwave hydrothermal reaction, spinning; Collection obtains the carbosphere that diameter is 100 ~ 500nm; Wherein, the condition of microwave hydrothermal reaction is: temperature: 150 ~ 250 ℃, and the time: 1 ~ 3 hour.
The invention provides a kind of method for preparing carbosphere, may further comprise the steps:
Step 1: glucose is dissolved in water, be configured to solution, the concentration of glucose is 10～100g/L in the solution;
Step 2: the glucose solution that step 1 is obtained adds in the micro-wave digestion jar, the micro-wave digestion jar is moved in the microwave hydrothermal synthesizer carry out building-up reactions, and reaction naturally cools to room temperature after finishing; Temperature of reaction is controlled between 150 ℃ ~ 250 ℃, and the reaction times is controlled at 1h ~ 3h.
Step 3: the product that step 3 obtains is collected through spinning,, promptly obtained the final product carbosphere after the oven dry then respectively through deionized water and absolute ethanol washing.
The carbosphere even particle size distribution that the present invention obtains, purity is high, and the diameter of carbosphere is controlled in 100～500nm scope.
The method that the present invention prepares carbosphere has the following advantages at least: the present invention is starting material with glucose, environmental protection, with low cost, and the reaction product environmental friendliness is pollution-free.It is short to adopt the hydrothermal synthesis method of microwave-assisted to have the reaction times, can control the carbosphere diameter through controlled microwave hydrothermal temperature, pressure and time.The carbosphere epigranular that the present invention obtains, purity is high, and diameter is controlled between 100～500nm.The present invention provides that the method for preparing carbosphere has the product purity height, environmental friendliness is pollution-free, advantage such as simple to operate, good reproducibility.
Description of drawings
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates by the carbosphere of the present invention's preparation;
Fig. 2 is ESEM (SEM) photo of the carbosphere for preparing of the present invention.Wherein (a) is 150 ℃, the 1h reaction product; (b) be 200 ℃, the reaction product of 2h; (c) be 250 ℃, the reaction product of 3h; (d) be 200 ℃, the reaction product of 3h;
Embodiment
Embodiment 1:
Step 1: glucose is dissolved in water, be configured to solution, the concentration of glucose is 10g/L in the solution;
Step 2: the glucose solution that step 1 is obtained adds in the micro-wave digestion jar, the micro-wave digestion jar is moved in the microwave hydrothermal synthesizer carry out building-up reactions, and reaction naturally cools to room temperature after finishing; Temperature of reaction is controlled at 150 ℃, and the reaction times is controlled at 1h.
Step 3: the product that step 3 obtains is collected through spinning,, promptly obtained the final product carbosphere after the oven dry then respectively through deionized water and absolute ethanol washing.
The diameter of present embodiment gained carbosphere is about 100nm.
Embodiment 2:
Step 1: glucose is dissolved in water, be configured to solution, the concentration of glucose is 50g/L in the solution;
Step 2: the glucose solution that step 1 is obtained adds in the micro-wave digestion jar, the micro-wave digestion jar is moved in the microwave hydrothermal synthesizer carry out building-up reactions, and reaction naturally cools to room temperature after finishing; Temperature of reaction is controlled at 200 ℃, and the reaction times is controlled at 2h.
Step 3: the product that step 3 obtains is collected through spinning,, promptly obtained the final product carbosphere after the oven dry then respectively through deionized water and absolute ethanol washing.
The diameter of present embodiment gained carbosphere is about about 300nm.
Embodiment 3:
Step 1: glucose is dissolved in water, be configured to solution, the concentration of glucose is 100g/L in the solution;
Step 2: the glucose solution that step 1 is obtained adds in the micro-wave digestion jar, the micro-wave digestion jar is moved in the microwave hydrothermal synthesizer carry out building-up reactions, and reaction naturally cools to room temperature after finishing; Temperature of reaction is controlled at 250 ℃, and the reaction times is controlled at 3h.
Step 3: the product that step 3 obtains is collected through spinning,, promptly obtained the final product carbosphere after the oven dry then respectively through deionized water and absolute ethanol washing.
The diameter of present embodiment gained carbosphere is about about 500nm.
Embodiment 4
Step 1: glucose is dissolved in water, be configured to solution, the concentration of glucose is 10g/L in the solution;
Step 2: the glucose solution that step 1 is obtained adds in the micro-wave digestion jar, the micro-wave digestion jar is moved in the microwave hydrothermal synthesizer carry out building-up reactions, and reaction naturally cools to room temperature after finishing; Temperature of reaction is controlled at 200 ℃, and the reaction times is controlled at 3h.
Step 3: the product that step 3 obtains is collected through spinning,, promptly obtained the final product carbosphere after the oven dry then respectively through deionized water and absolute ethanol washing.
The diameter of present embodiment gained carbosphere is about about 200nm.
Below, see also shown in Figure 1ly, it is the XRD figure spectrum by the carbosphere of the inventive method preparation.Can be found out by figure: the carbosphere of the present invention's preparation is the decolorizing carbon structure.
See also shown in Figure 2ly, it is the SEM pattern of the carbosphere for preparing of the present invention.Can be found out by figure: the diameter of the carbosphere of the present invention's preparation is between 100～500nm.
Claims (2)
1. a method for preparing carbosphere is characterized in that: be carbon source with glucose, after its dissolving; After the microwave hydrothermal reaction, spinning is collected and is obtained the carbosphere that diameter is 100 ~ 500nm; Wherein, the condition of microwave hydrothermal reaction is: temperature: 150 ~ 250 ℃, and the time: 1 ~ 3 hour.
2. method for preparing carbosphere is characterized in that: may further comprise the steps:
Step 1: glucose is dissolved in water, be configured to solution, the concentration of glucose is 10～100g/L in this solution;
Step 2: the glucose solution that step 1 is obtained adds in the micro-wave digestion jar, the micro-wave digestion jar is moved in the microwave hydrothermal synthesizer carry out building-up reactions, and reaction naturally cools to room temperature after finishing; The temperature of microwave hydrothermal reaction is controlled between 150 ℃ ~ 250 ℃, and the reaction times is controlled at 1h ~ 3h;
Step 3: the product that step 3 obtains is collected through spinning,, promptly obtained the final product carbosphere after the oven dry then respectively through deionized water and absolute ethanol washing.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103274385A (en) * | 2013-04-26 | 2013-09-04 | 北大先行科技产业有限公司 | Lithium ion battery cathode material carbon microsphere and preparation method thereof |
| CN103864056A (en) * | 2014-04-04 | 2014-06-18 | 南京瑞盈环保科技有限公司 | Preparation method of carbon microspheres |
| CN104179003A (en) * | 2014-08-11 | 2014-12-03 | 中北大学 | Preparation method of carbon nanosphere-carbon fiber multi-scale reinforcement |
| CN104876621A (en) * | 2015-05-07 | 2015-09-02 | 陕西科技大学 | C/SiC porous composite ceramic with bionic structure and preparation method of C/SiC porous composite ceramic |
| CN104944405A (en) * | 2014-03-27 | 2015-09-30 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of carbon spheres |
| CN105609722A (en) * | 2015-12-28 | 2016-05-25 | 黑龙江科技大学 | Preparation method of double-modified SnO<2>@C/graphene nano composite anode material |
| CN105879931A (en) * | 2016-05-10 | 2016-08-24 | 中国科学院青岛生物能源与过程研究所 | Method for preparing carbon microsphere weak cation exchange chromatographic column filler |
| CN106334524A (en) * | 2016-11-08 | 2017-01-18 | 山东大学 | Preparation method and application core-shell structure laminated double-metal hydroxide composite particles |
| CN107317042A (en) * | 2017-08-25 | 2017-11-03 | 河南师范大学 | Microwave-hydrothermal method prepares sulphur, nitrogen, the method for iron codope carbon material fuel battery negative pole elctro-catalyst |
| CN107482232A (en) * | 2017-08-25 | 2017-12-15 | 河南师范大学 | A kind of fuel cell oxygen reduction electrocatalyst phosphorus, the preparation method of nitrogen co-doped carbon material |
| CN107492666A (en) * | 2017-08-25 | 2017-12-19 | 河南师范大学 | A kind of fuel battery negative pole elctro-catalyst sulphur, the preparation method of nitrogen co-doped carbon material |
| CN107492668A (en) * | 2017-08-25 | 2017-12-19 | 河南师范大学 | Microwave-hydrothermal method prepares phosphorus, nitrogen, the method for nickel co-doped carbon material electrode catalyst |
| CN108584913A (en) * | 2018-07-18 | 2018-09-28 | 陕西科技大学 | A kind of method that lignin Microwave-assisted firing prepares hollow micro-nano carbon ball |
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| CN102408231A (en) * | 2011-08-29 | 2012-04-11 | 山西省电力公司晋城供电分公司 | Preparation method of hollow Ni-Zn ferrite microsphere |
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| CN101254913A (en) * | 2008-04-03 | 2008-09-03 | 天津大学 | Method for preparing carbon nano-tube or rod by hydrothermal process |
| CN102408231A (en) * | 2011-08-29 | 2012-04-11 | 山西省电力公司晋城供电分公司 | Preparation method of hollow Ni-Zn ferrite microsphere |
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103274385A (en) * | 2013-04-26 | 2013-09-04 | 北大先行科技产业有限公司 | Lithium ion battery cathode material carbon microsphere and preparation method thereof |
| CN104944405A (en) * | 2014-03-27 | 2015-09-30 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of carbon spheres |
| CN103864056A (en) * | 2014-04-04 | 2014-06-18 | 南京瑞盈环保科技有限公司 | Preparation method of carbon microspheres |
| CN103864056B (en) * | 2014-04-04 | 2016-03-09 | 南京瑞盈环保科技有限公司 | A kind of preparation method of carbosphere |
| CN104179003A (en) * | 2014-08-11 | 2014-12-03 | 中北大学 | Preparation method of carbon nanosphere-carbon fiber multi-scale reinforcement |
| CN104179003B (en) * | 2014-08-11 | 2016-06-01 | 中北大学 | The preparation method of Nano carbon balls-carbon fiber multi-scale reinforcing body |
| CN104876621A (en) * | 2015-05-07 | 2015-09-02 | 陕西科技大学 | C/SiC porous composite ceramic with bionic structure and preparation method of C/SiC porous composite ceramic |
| CN105609722B (en) * | 2015-12-28 | 2017-11-21 | 黑龙江科技大学 | A kind of SnO of dual modification2The preparation method of@C/ graphene nanometer composite negative materials |
| CN105609722A (en) * | 2015-12-28 | 2016-05-25 | 黑龙江科技大学 | Preparation method of double-modified SnO<2>@C/graphene nano composite anode material |
| CN105879931A (en) * | 2016-05-10 | 2016-08-24 | 中国科学院青岛生物能源与过程研究所 | Method for preparing carbon microsphere weak cation exchange chromatographic column filler |
| CN106334524A (en) * | 2016-11-08 | 2017-01-18 | 山东大学 | Preparation method and application core-shell structure laminated double-metal hydroxide composite particles |
| CN106334524B (en) * | 2016-11-08 | 2019-07-05 | 山东大学 | Nucleocapsid structure layered double hydroxide compound particle preparation method and application |
| CN107317042A (en) * | 2017-08-25 | 2017-11-03 | 河南师范大学 | Microwave-hydrothermal method prepares sulphur, nitrogen, the method for iron codope carbon material fuel battery negative pole elctro-catalyst |
| CN107482232A (en) * | 2017-08-25 | 2017-12-15 | 河南师范大学 | A kind of fuel cell oxygen reduction electrocatalyst phosphorus, the preparation method of nitrogen co-doped carbon material |
| CN107492666A (en) * | 2017-08-25 | 2017-12-19 | 河南师范大学 | A kind of fuel battery negative pole elctro-catalyst sulphur, the preparation method of nitrogen co-doped carbon material |
| CN107492668A (en) * | 2017-08-25 | 2017-12-19 | 河南师范大学 | Microwave-hydrothermal method prepares phosphorus, nitrogen, the method for nickel co-doped carbon material electrode catalyst |
| CN108584913A (en) * | 2018-07-18 | 2018-09-28 | 陕西科技大学 | A kind of method that lignin Microwave-assisted firing prepares hollow micro-nano carbon ball |
| CN108584913B (en) * | 2018-07-18 | 2021-06-18 | 陕西科技大学 | Method for preparing hollow micro-nano carbon spheres by microwave-assisted heating of lignin |
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Application publication date: 20121107 |