CN101698479B - Preparation method of carbon ball with big size - Google Patents
Preparation method of carbon ball with big size Download PDFInfo
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- CN101698479B CN101698479B CN2009102103618A CN200910210361A CN101698479B CN 101698479 B CN101698479 B CN 101698479B CN 2009102103618 A CN2009102103618 A CN 2009102103618A CN 200910210361 A CN200910210361 A CN 200910210361A CN 101698479 B CN101698479 B CN 101698479B
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Abstract
The invention provides a preparation method of a carbon ball with big size, comprising the following steps: (1) glucose is dissolved in zinc brine solution to obtain mixed solution; the glucose concentration in the mixed solution is 2.5-10g/L and zinc ion concentration in the mixed solution is 0.005-0.1mol/L; (2) the mixed solution is added in a reaction kettle, and the temperature is 140-250DEG C for 180-600min, and then the temperature is cooled to be room temperature; (3) the product is taken out, and the carbon ball is obtained after washing, filtering and drying processes are carried out. The preparation method has the beneficial effects that: (1) the size of the carbon ball is controlled to be 5-10mum by adjusting the glucose concentration and the zinc brine solution; (2) the needed equipment is simple, the production process is simple and the cost is low.
Description
Technical field
The present invention relates to a kind of preparation method of carbon ball, especially relate to a kind of preparation method of micron order carbon ball.
Background technology
Along with the discovery of carbon materials such as CNT (carbon nano-tube), soccerballene and Graphene, people recognize the importance of carbon material in Development of Human Civilization.Carbon material has high chemical stability, good high-temperature resistance toheat, and extensive application prospect in biological field and electronic applications has also caused people's very big attention.Wherein, spherical carbon material (carbon ball) also is used as medicine, catalyst support material, biomass parting material, medicament slow release material etc.
The preparation method of carbon ball material has a lot, as chemical vapor deposition (CVD), pyrolysis, arc process and carbohydrate evaporation etc.CVD and arc process required equipment costliness, complicated operation; Pyrolysis method not only needs high temperature service, also needs atmosphere protection.And the carbohydrate evaporation, desired raw material is simple, reaction conditions is gentle (＜300 ℃), is suitable for scale operation.
The carbohydrate evaporation is put into water heating kettle with sugar soln exactly, reacts for some time at a certain temperature, makes the sugar dehydration, finally forms the carbon ball.The resulting carbon ball of this method size is generally all at nanometer and submicron order, and particle diameter is less.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of preparation method of micron order carbon ball; This method can obtain micron-sized carbon ball by adding zinc salt, and diameter dimension and can effectively be controlled carbon ball size by regulating glucose concn and zinc salt concentration between 5-10 μ m; Simultaneously, this method equipment input is little, technology is simple, cost is low, is suitable for large-scale industrial production.
For solving the problems of the technologies described above, the preparation method of a kind of micron order carbon of the present invention ball comprises the steps:
(1) glucose is dissolved in the zinc salt solution, get mixed solution; Glucose concn in the described mixed solution is 2.5-10g/L, and the zinc ion concentration in the described mixed solution is 0.005-0.1mol/L;
(2) above-mentioned mixed solution is packed in the reactor,, be cooled to room temperature at 140-250 ℃ of insulation 180-600min down;
(3) product is taken out, through routine washing, suction filtration and drying process, get final product carbon ball product.
Further, described zinc salt is the mixture of one or more arbitrary proportions in zinc nitrate, zinc sulfate, zinc acetate, the zinc oxalate.
The present invention has following beneficial effect:
(1) can control carbon ball size greatly between 5-10 μ m by regulating glucose concn and zinc salt concentration;
(2) required equipment is simple, production technique is simple and cost is low.
Description of drawings
Fig. 1 is scanning electron microscope (SEM) photo of example 1 prepared carbon ball.
Embodiment
In order to show substantive distinguishing features of the present invention and marked improvement, further specify embodiment and effect with following indefiniteness embodiment.
Embodiment 1
A kind of preparation method of micron order carbon ball comprises the steps:
(1) glucose is dissolved in the zinc nitrate aqueous solution, get mixed solution; Glucose concn in the described mixed solution is 2.5g/L, and the zinc ion concentration in the described mixed solution is 0.005mol/L;
(2) above-mentioned mixed solution is packed in the reactor,, be cooled to room temperature at 140 ℃ of insulation 180min down;
(3) product is taken out, through routine washing, suction filtration and drying process, get final product carbon ball product.
Characterize through scanning electronic microscope, the diameter dimension of carbon ball is 5.0-9.2 μ m.
Embodiment 2
A kind of preparation method of micron order carbon ball comprises the steps:
(1) glucose is dissolved in the zinc sulfate solution, get mixed solution; Glucose concn in the described mixed solution is 4g/L, and the zinc ion concentration in the described mixed solution is 0.006mol/L;
(2) above-mentioned mixed solution is packed in the reactor,, be cooled to room temperature at 165 ℃ of insulation 300min down;
(3) product is taken out, through routine washing, suction filtration and drying process, get final product carbon ball product.
Characterize through scanning electronic microscope, the diameter dimension of carbon ball is 7.0-9.4 μ m.
Embodiment 3
A kind of preparation method of micron order carbon ball comprises the steps:
(1) glucose is dissolved in the zinc acetate aqueous solution, get mixed solution; Glucose concn in the described mixed solution is 6g/L, and the zinc ion concentration in the described mixed solution is 0.007mol/L;
(2) above-mentioned mixed solution is packed in the reactor,, be cooled to room temperature at 190 ℃ of insulation 400min down;
(3) product is taken out, through routine washing, suction filtration and drying process, get final product carbon ball product.
Characterize through scanning electronic microscope, the diameter dimension of carbon ball is 5.2-7.1 μ m.
Embodiment 4
A kind of preparation method of micron order carbon ball comprises the steps:
(1) glucose is dissolved in the zinc oxalate aqueous solution, get mixed solution; Glucose concn in the described mixed solution is 7g/L, and the zinc ion concentration in the described mixed solution is 0.008mol/L;
(2) above-mentioned mixed solution is packed in the reactor,, be cooled to room temperature at 215 ℃ of insulation 500min down;
(3) product is taken out, through routine washing, suction filtration and drying process, get final product carbon ball product.
Characterize through scanning electronic microscope, the diameter dimension of carbon ball is 5.2-6.5 μ m.
Embodiment 5
A kind of preparation method of micron order carbon ball comprises the steps:
(1) glucose is dissolved in the mixed aqueous solution of zinc nitrate and zinc sulfate, get mixed solution; Glucose concn in the described mixed solution is 8g/L, and the zinc ion concentration in the described mixed solution is 0.009mol/L; The ratio of weight and number of described zinc nitrate and zinc sulfate is 1: 1;
(2) above-mentioned mixed solution is packed in the reactor,, be cooled to room temperature at 230 ℃ of insulation 600min down.
(3) product is taken out, through routine washing, suction filtration and drying process, get final product carbon ball product.
Characterize through scanning electronic microscope, the diameter dimension of carbon ball is 5.4-8.6 μ m.
Embodiment 6
The preparation method of a kind of micron order carbon of the present invention ball comprises the steps:
(1) glucose is dissolved in the mixed aqueous solution of zinc nitrate, zinc sulfate, zinc acetate and zinc oxalate, get mixed solution; Glucose concn in the described mixed solution is 2.5g/L, and the zinc ion concentration in the described mixed solution is 0.025mol/L; The mol ratio of described zinc nitrate, zinc sulfate, zinc acetate and zinc oxalate is 1: 2: 4: 3;
(2) above-mentioned mixed solution is packed in the reactor,, be cooled to room temperature at 250 ℃ of insulation 600min down;
(3) product is taken out, through routine washing, suction filtration and drying process, get final product carbon ball product.
Characterize through scanning electronic microscope, the diameter dimension of carbon ball is 7.5-9.8 μ m.
Obviously, the above embodiment of the present invention only is for example of the present invention clearly is described, and is not to be qualification to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here can't give exhaustive to all embodiments.Everyly belong to the row that conspicuous variation that technical scheme of the present invention extends out or change still are in protection scope of the present invention.
Claims (2)
1. the preparation method of a micron order carbon ball is characterized in that, comprises the steps:
(1) glucose is dissolved in the zinc salt solution, get mixed solution; Glucose concn in the described mixed solution is 2.5-10g/L, and the zinc ion concentration in the described mixed solution is 0.005-0.1mol/L;
(2) above-mentioned mixed solution is packed in the reactor,, be cooled to room temperature at 140-250 ℃ of insulation 180-600min down;
(3) product is taken out, through washing, suction filtration and drying process, get final product carbon ball product;
Described micron order carbon ball, its diameter dimension is between 5-10 μ m.
2. the preparation method of micron order carbon ball according to claim 1 is characterized in that: described zinc salt is the mixture of one or more arbitrary proportions in zinc nitrate, zinc sulfate, zinc acetate, the zinc oxalate.
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| CN2009102103618A CN101698479B (en) | 2009-10-30 | 2009-10-30 | Preparation method of carbon ball with big size |
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| CN2009102103618A CN101698479B (en) | 2009-10-30 | 2009-10-30 | Preparation method of carbon ball with big size |
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| CN101698479A CN101698479A (en) | 2010-04-28 |
| CN101698479B true CN101698479B (en) | 2011-08-17 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103183342B (en) * | 2013-04-02 | 2014-11-12 | 中国矿业大学 | Controllable synthetic method for phosphorus doped graphitization carbon spheres with hollow structures |
| CN104649246A (en) * | 2013-11-18 | 2015-05-27 | 湖南师范大学 | Low temperature hydrothermal preparation method of biomass carbon microsphere / nanosphere |
| CN103979525B (en) * | 2014-05-22 | 2016-08-24 | 辽宁大学 | A kind of preparation method of the rich spherical material with carbon element of acidic group |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007044614A2 (en) * | 2005-10-06 | 2007-04-19 | Headwaters Technology Innovation Llc | Carbon nanostructures manufactured from catalytic templating nanoparticles |
| CN101224883A (en) * | 2008-02-03 | 2008-07-23 | 山东大学 | Method for preparing hollow carbon balls |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007044614A2 (en) * | 2005-10-06 | 2007-04-19 | Headwaters Technology Innovation Llc | Carbon nanostructures manufactured from catalytic templating nanoparticles |
| CN101224883A (en) * | 2008-02-03 | 2008-07-23 | 山东大学 | Method for preparing hollow carbon balls |
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