CN104150465A - Method for preparing hollow carbon ball - Google Patents
Method for preparing hollow carbon ball Download PDFInfo
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- CN104150465A CN104150465A CN201410390340.XA CN201410390340A CN104150465A CN 104150465 A CN104150465 A CN 104150465A CN 201410390340 A CN201410390340 A CN 201410390340A CN 104150465 A CN104150465 A CN 104150465A
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- hollow carbon
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Abstract
The invention discloses a method for preparing a hollow carbon ball and belongs to the field of inorganic non-metallic material preparation. The hollow carbon ball is prepared from an oxygen-containing organic matter, an ammonium salt and water as raw materials by a hydrothermal method. Bubbles produced by ammonium salt decomposition in a hydro-thermal process are used as soft templates, the oxygen-containing organic matter is carbonized on surfaces of the bubbles, and then the finished product is obtained by pumping filtration, washing and drying. The method has short reaction time and simple processes. The hollow carbon ball has high water solubility and a high void ratio of volume, can be controllably prepared and massively produced and can be used in fields of adsorption materials, drug carriers and super capacitors.
Description
technical field:
The present invention relates to a kind of preparation method of hollow carbon balls, belong to ceramic preparation field.
background technology:
Hollow carbon balls material has large specific surface area, large pore volume, unreactiveness and good mechanical stability, and these special performances have determined its wide application prospect in fields such as catalysis, sorbent material, electrode materials, electrical condenser, energy storage materials.
At present, the method for preparing hollow carbon balls is mainly: template, vapour deposition process, arc discharge method etc.
Template is the most a kind of method of preparing hollow carbon balls adopting.Template can be divided into again hard template method and soft template method according to its material character.Hard template method major part is that some monodispersed silicon balls of application, polymer drops, metal oxide etc. are template, then make polymkeric substance at its surface aggregate, obtain the compound ball of polymkeric substance embedding hard template, charing afterwards, then select suitable method to remove hard template to obtain Carbon Hollow ball.Jang etc. [Jang J, Lim B. Advanced Materials, 2002,14 (19): 1390-1393.] utilize surface by the SiO of modified
2as template, Vinylstyrene is carbon source, has prepared the hollow carbon balls of big or small about 22nm.Although hollow carbon sphere prepared by hard template method has size homogeneous, the advantage that core-shell structure is controlled.But first hard template method need to synthesize uniform mould material, also need afterwards template to remove, not only complex operation, and all can have product loss in each step operation, the yield of the target product therefore finally obtaining is very low; Remove in operating process and be easy to cause shell wall to damage in template, the rigidity of the shell wall of the product therefore obtaining is very poor, and even some template is difficult to remove.
Chemical vapour deposition (CVD) method is one of common method of synthetic carbon hollow ball.Its principle is: flowing under atmosphere, organic gas as carbon source in high-temperature zone pyrolysis, in the process of catalyst surface deposition growing solid carbon.Wang etc. [Wang Z L, Yin J S. Chemical physics letters, 1998,289 (1): 189-192.] adopt MnO at first
2as catalyzer, pass through CH
4synthesize 900-1050 DEG C of pyrolysis carbon hollow ball and the hollow calabash shaped carbon structure that diameter is 800nm.Because the synthetic carbon hollow ball of CVD method is generally made catalyzer with metal oxide, but less to the study on mechanism of catalyzer, thereby how to generate with a large amount of by products, and carbon hollow ball purity is not high.
Chinese patent CN1454839 A discloses a kind of method that arc discharge method is prepared hollow carbon balls, its embodiment is: in the electric arc reaction chamber of containing graphite anode and graphite cathode, pass into a rare gas element, apply a voltage between above-mentioned negative electrode and positive electrode with a pulsed current, thereby produce arc-over reaction, the product that collection is deposited on graphite cathode can obtain the product taking hollow nano carbon microsphere as principal product.The method has carbon ball and is easy to purifying a little, but needs the electric arc reaction chamber of a high pressure, and cost is higher.
summary of the invention:
Technical problem to be solved by this invention is higher, the low problem of carbon ball purity produced of hollow carbon balls preparing technique process complexity, cost in the past.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
Prepare a method for hollow carbon balls, carry out according to following step:
(a) after according to a certain percentage oxygen-bearing organic matter, ammonium salt is water-soluble, join in stainless steel cauldron
(b) stainless steel cauldron that raw material is housed is put into the process furnace with temperature programming function, be warming up to 130 ~ 300 DEG C from room temperature program with the heat-up rate of 1-10 DEG C/min, and be incubated 10min ~ 10h, and then stop heating, make reactor in stove, naturally cool to room temperature.
(c) the above-mentioned reaction solution of suction filtration, and use deionized water wash products, finally product is dried after 3 hours at 60 DEG C, obtain finished product.
Wherein the described oxygen-bearing organic matter of step (a) includes but not limited to monobasic sugar, binary carbohydrate and the starch such as glucose, sucrose, fructose.
Wherein the described ammonium salt of step (a) is one or more in bicarbonate of ammonia, volatile salt, ammonium sulfate, ammonium chloride, ammonium nitrate, ammonium acetate.
In technique scheme, preferably, the mass ratio of oxygen-bearing organic matter and water is 0.004-1, and the mass ratio of oxygen-bearing organic matter and ammonium salt is 0.1-20.
In technique scheme, preferably, hollow carbon balls external diameter is 0.02-10 μ m, and wall thickness is 2-200nm.
The major technique advantage of the method for preparing hollow carbon balls of the present invention is embodied in: 1, taking oxygen-bearing organic matters such as glucose as carbon source, raw materials cost is low; 2, prepare hollow carbon balls with the method for hydro-thermal, the reaction times is short, and owing to not needing to add metal oxide catalyst, the carbon ball purity of preparing is high; 3, technical process is short, and postprocessing working procedures is simple, and carbon ball yield is higher.
brief description of the drawings:
Fig. 1 is the TEM figure of the hollow carbon balls that makes of embodiment 1;
Fig. 2 is the TEM figure of the hollow carbon balls that makes of embodiment 2;
Fig. 3 is the TEM figure of the hollow carbon balls that makes of embodiment 2.
Embodiment
Embodiment 1:
1, take 0.2g glucose, 0.1g ammonium sulfate is dissolved in 35ml deionized water, after mixing, join in 50ml stainless steel cauldron.
2, above-mentioned stainless steel cauldron is put into the stove that adds with temperature programming function, setting temperature rise rate is 1 DEG C/min, rises to after 150 DEG C, and constant temperature 3 hours, then stops heating, makes reactor in stove, naturally cool to room temperature.
3, the above-mentioned reaction solution of suction filtration, and use deionized water wash products, finally product is dried after 4 hours at 60 DEG C, obtain hollow carbon balls product.Fig. 1 is the TEM figure of the hollow carbon balls that makes of embodiment 1
Embodiment 2:
1, take 1g glucose, 0.5g ammonium sulfate is dissolved in 35ml deionized water, after mixing, join in 50ml stainless steel cauldron.
2, above-mentioned stainless steel cauldron is put into the stove that adds with temperature programming function, setting temperature rise rate is 2 DEG C/min, rises to after 180 DEG C, and constant temperature 2 hours, then stops heating, makes reactor in stove, naturally cool to room temperature.
3, the above-mentioned reaction solution of suction filtration, and use deionized water wash products, finally product is dried after 4 hours at 60 DEG C, obtain hollow carbon balls product.Fig. 2 is the TEM figure of the hollow carbon balls that makes of embodiment 2, and Fig. 3 is the TEM figure of the hollow carbon balls that makes of embodiment 2.
Embodiment 3:
1, take 5g glucose, 0.5g ammonium chloride is dissolved in 35ml deionized water, after mixing, join in 50ml stainless steel cauldron.
2, above-mentioned stainless steel cauldron is put into the stove that adds with temperature programming function, setting temperature rise rate is 1 DEG C/min, rises to after 150 DEG C, and constant temperature 3 hours, then stops heating, makes reactor in stove, naturally cool to room temperature.
3, the above-mentioned reaction solution of suction filtration, and use deionized water wash products, finally product is dried after 4 hours at 60 DEG C, obtain hollow carbon balls product.
Embodiment 4:
1, take 1g glucose, 0.5g monoammonium sulfate is dissolved in 35ml deionized water, after mixing, join in 50ml stainless steel cauldron.
2, above-mentioned stainless steel cauldron is put into the stove that adds with temperature programming function, setting temperature rise rate is 1 DEG C/min, rises to after 130 DEG C, and constant temperature 2 hours, then stops heating, makes reactor in stove, naturally cool to room temperature.
3, the above-mentioned reaction solution of suction filtration, and use deionized water wash products, finally product is dried after 4 hours at 60 DEG C, obtain hollow carbon balls product.
Embodiment 5:
1, take 1g glucose, 0.5g bicarbonate of ammonia is dissolved in 35ml deionized water, after mixing, join in 50ml stainless steel cauldron.
2, above-mentioned stainless steel cauldron is put into the stove that adds with temperature programming function, setting temperature rise rate is 1 DEG C/min, rises to after 130 DEG C, and constant temperature 2 hours, then stops heating, makes reactor in stove, naturally cool to room temperature.
3, the above-mentioned reaction solution of suction filtration, and use deionized water wash products, finally product is dried after 4 hours at 60 DEG C, obtain hollow carbon balls product.
Embodiment 6:
1, take 0.4g sucrose, 0.1g monoammonium sulfate is dissolved in 35ml deionized water, after mixing, join in 50ml stainless steel cauldron.
2, above-mentioned stainless steel cauldron is put into the stove that adds with temperature programming function, setting temperature rise rate is 1 DEG C/min, rises to after 130 DEG C, and constant temperature 2 hours, then stops heating, makes reactor in stove, naturally cool to room temperature.
3, the above-mentioned reaction solution of suction filtration, and use deionized water wash products, finally product is dried after 4 hours at 60 DEG C, obtain hollow carbon balls product.
Embodiment 7:
1, take 0.8g fructose, 0.2g ammonium sulfate is dissolved in 35ml deionized water, after mixing, join in 50ml stainless steel cauldron.
2, above-mentioned stainless steel cauldron is put into the stove that adds with temperature programming function, setting temperature rise rate is 1 DEG C/min, rises to after 130 DEG C, and constant temperature 2 hours, then stops heating, makes reactor in stove, naturally cool to room temperature.
3, the above-mentioned reaction solution of suction filtration, and use deionized water wash products, finally product is dried after 4 hours at 60 DEG C, obtain hollow carbon balls product.
Claims (5)
1. prepare a method for hollow carbon balls, it is characterized in that carrying out according to following step:
(a) after according to a certain percentage oxygen-bearing organic matter, ammonium salt is water-soluble, join in stainless steel cauldron
(b) stainless steel cauldron that raw material is housed is put into the process furnace with temperature programming function, be warming up to 130 ~ 300 DEG C from room temperature program with the heat-up rate of 1-10 DEG C/min, and be incubated 10min ~ 10h, and then stop heating, make reactor in stove, naturally cool to room temperature;
(c) the above-mentioned reaction solution of suction filtration, and use deionized water wash products, finally product is dried after 3 hours at 60 DEG C, obtain finished product.
2. a kind of method of preparing hollow carbon balls according to claim 1, is characterized in that wherein the described oxygen-bearing organic matter of step (a) includes but not limited to monobasic sugar, binary carbohydrate and the starch such as glucose, sucrose, fructose.
3. a kind of method of preparing hollow carbon balls according to claim 1, is characterized in that the described ammonium salt of step (a) is wherein one or more in bicarbonate of ammonia, volatile salt, ammonium sulfate, ammonium chloride, ammonium nitrate, ammonium acetate.
4. a kind of method of preparing hollow carbon balls according to claim 1, the mass ratio that it is characterized in that oxygen-bearing organic matter and water is 0.004-1, the mass ratio of oxygen-bearing organic matter and ammonium salt is 0.1-20.
5. a kind of method of preparing hollow carbon balls according to claim 1, is characterized in that hollow carbon balls external diameter is 0.02-10 μ m, and wall thickness is 2-200nm.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104759241A (en) * | 2015-03-16 | 2015-07-08 | 上海交通大学 | Preparation method of carbon hollow microspheres having nonsymmetrical structure |
| CN104900416A (en) * | 2015-06-01 | 2015-09-09 | 南通江海电容器股份有限公司 | Preparation method of novel nickel @combined carbon electrode material |
| CN105460918A (en) * | 2015-12-23 | 2016-04-06 | 海安常州大学高新技术研发中心 | Preparation method of hollow carbon sphere |
| CN105502335A (en) * | 2015-12-23 | 2016-04-20 | 海安常州大学高新技术研发中心 | Novel method for preparing hollow carbon spheres |
| CN105502334A (en) * | 2015-12-21 | 2016-04-20 | 常州轻工职业技术学院 | Hollow carbon ball and preparation method thereof |
| CN105712317A (en) * | 2016-01-30 | 2016-06-29 | 山西大学 | Preparation method of nano-contained hollow carbon material |
| CN106044921A (en) * | 2016-06-20 | 2016-10-26 | 昆明理工大学 | Preparation method and application of carbon sphere loaded nanoscale zero valent iron composite material |
| CN106185865A (en) * | 2016-07-19 | 2016-12-07 | 西安交通大学 | A kind of preparation method of hollow nano carbon microsphere |
| CN107108216A (en) * | 2014-12-22 | 2017-08-29 | 秀博瑞殷株式公社 | Aoxidize carbon nano-particles and preparation method thereof, organic mineral complex comprising the oxidation carbon nano-particles and preparation method thereof |
| CN108203086A (en) * | 2016-12-19 | 2018-06-26 | 海安常州大学高新技术研发中心 | A kind of hollow carbon balls processing method |
| CN108203085A (en) * | 2016-12-19 | 2018-06-26 | 海安常州大学高新技术研发中心 | A kind of preparation method of Novel hollow carbon ball |
| CN108203087A (en) * | 2016-12-19 | 2018-06-26 | 海安常州大学高新技术研发中心 | A kind of processing method of Novel hollow carbon ball |
| CN115724419A (en) * | 2021-09-01 | 2023-03-03 | 中国科学院大连化学物理研究所 | Method for preparing hollow carbon spheres by one-pot method and application |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2018508442A (en) * | 2014-12-22 | 2018-03-29 | ソウルブレイン シーオー．， エルティーディー． | Carbon oxide nanoparticles, method for producing the same, organic / inorganic composite containing the same, and method for producing the organic / inorganic composite |
| CN107108216A (en) * | 2014-12-22 | 2017-08-29 | 秀博瑞殷株式公社 | Aoxidize carbon nano-particles and preparation method thereof, organic mineral complex comprising the oxidation carbon nano-particles and preparation method thereof |
| CN104759241B (en) * | 2015-03-16 | 2017-03-01 | 上海交通大学 | A kind of carbon hollow microsphere preparation method with unsymmetric structure |
| CN104759241A (en) * | 2015-03-16 | 2015-07-08 | 上海交通大学 | Preparation method of carbon hollow microspheres having nonsymmetrical structure |
| CN104900416A (en) * | 2015-06-01 | 2015-09-09 | 南通江海电容器股份有限公司 | Preparation method of novel nickel @combined carbon electrode material |
| CN105502334A (en) * | 2015-12-21 | 2016-04-20 | 常州轻工职业技术学院 | Hollow carbon ball and preparation method thereof |
| CN105502335A (en) * | 2015-12-23 | 2016-04-20 | 海安常州大学高新技术研发中心 | Novel method for preparing hollow carbon spheres |
| CN105460918A (en) * | 2015-12-23 | 2016-04-06 | 海安常州大学高新技术研发中心 | Preparation method of hollow carbon sphere |
| CN105712317A (en) * | 2016-01-30 | 2016-06-29 | 山西大学 | Preparation method of nano-contained hollow carbon material |
| CN106044921A (en) * | 2016-06-20 | 2016-10-26 | 昆明理工大学 | Preparation method and application of carbon sphere loaded nanoscale zero valent iron composite material |
| CN106044921B (en) * | 2016-06-20 | 2019-05-14 | 昆明理工大学 | A kind of preparation method and applications of carbon ball load nano zero-valence iron composite material |
| CN106185865A (en) * | 2016-07-19 | 2016-12-07 | 西安交通大学 | A kind of preparation method of hollow nano carbon microsphere |
| CN108203086A (en) * | 2016-12-19 | 2018-06-26 | 海安常州大学高新技术研发中心 | A kind of hollow carbon balls processing method |
| CN108203085A (en) * | 2016-12-19 | 2018-06-26 | 海安常州大学高新技术研发中心 | A kind of preparation method of Novel hollow carbon ball |
| CN108203087A (en) * | 2016-12-19 | 2018-06-26 | 海安常州大学高新技术研发中心 | A kind of processing method of Novel hollow carbon ball |
| CN115724419A (en) * | 2021-09-01 | 2023-03-03 | 中国科学院大连化学物理研究所 | Method for preparing hollow carbon spheres by one-pot method and application |
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