CN1587032A - Hollow charcoal and its synthetic method and use - Google Patents
Hollow charcoal and its synthetic method and use Download PDFInfo
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- CN1587032A CN1587032A CN 200410060849 CN200410060849A CN1587032A CN 1587032 A CN1587032 A CN 1587032A CN 200410060849 CN200410060849 CN 200410060849 CN 200410060849 A CN200410060849 A CN 200410060849A CN 1587032 A CN1587032 A CN 1587032A
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Abstract
One kind of hollow carbon is spherical and consists of carbon shell and hollow core. The preparation process of the hollow carbon includes adsorbing organic monomer reaction solution to spherical silica gel, initiating reaction to coat the silica gel with organic polymer, carbonizing the organic polymer, and dissolving the silica gel component in the core with alkali solution or acid solution. The hollow carbon in porous structure has great specific surface area and powerful adsorption capacity, and may be used in the treatment of waste water, pollutant, etc. and the hollow carbon in hollow core structure may be used as template material for the synthesis of other spherical material.
Description
Technical field
The present invention relates to a kind of hollow charcoal and preparation method and use thereof.
Background technology
The raw material of wood-charcoal material demonstrates good prospects for application at aspects such as catalysis, absorption, sensing, electrode materials, energy storages, and the raw material of wood-charcoal material of different apertures, different-shape shows different application potential, Given this, the research focus of raw material of wood-charcoal material concentrates on aperture control, morphology control two broad aspect at present.
Usually the raw material of wood-charcoal material is by organism being got through Pintsch process, charing, adopt this class methods synthetic raw material of wood-charcoal material, poor reproducibility, and pattern, aperture are restive, have brought inconvenience to application.
A kind of new synthetic technology---the template synthetic technology has caused investigator's extensive concern at present.Many research groups adopt mould plate technique to synthesize the raw material of wood-charcoal material of various novel structures, comprise micropore carbon material, ordered mesoporous carbon material, macropore carbon material or the like, have realized the aperture of raw material of wood-charcoal material, the regulation and control of pore structure.With the exception of this, the investigator has also realized the pattern regulation and control of raw material of wood-charcoal material by mould plate technique, as carbon nanotube, carbon rod, charcoal ball, charcoal integral post material or the like.
Though various raw material of wood-charcoal material are synthesized in succession, influenced by pattern, pore structure bigger because it uses potential, therefore is necessary to develop the raw material of wood-charcoal material of more novel textures.Based on this, the present invention proposes hollow raw material of wood-charcoal material of a kind of novel texture and its production and use.
Summary of the invention
The invention provides a kind of hollow raw material of wood-charcoal material and preparation method and use thereof.
Technical scheme provided by the invention is: be template with the spherical silica gel, carbon laydown gets hollow carbon sphere at spherical surface with the corrosion of silica gel template.
Above-mentioned hollow charcoal is made up of outer charcoal shell and hollow core, and hollow carbon granule directly is 0.05 μ m-50 μ m, and its outer charcoal thickness of the shell is 10nm-1 μ m, and its hollow core diameter is 30nm-49 μ m.
The present invention also provides the synthetic method of above-mentioned hollow carbon sphere: the organic monomer reaction liquid of absorption on spherical silica gel, by initiation reaction, be coated with organic polymer at silica gel, then with the organic polymer charing, and with alkali lye or acid fluid dissolves core silica gel component, thereby obtain hollow charcoal.
The above-mentioned organic monomer reaction solution that is used to be adsorbed on the spherical silica gel can be vinylbenzene, Vinylstyrene, divinyl, furfuryl alcohol, resol or carbohydrate organism.
Above-mentioned charing mode with organic polymer can be with the vitriol oil at 333K～573K with the organics dehydration carbonization and/or under the condition of secluding air and oxygen, in 673K～1473K pyroprocessing and with organic carbon.
The above-mentioned alkali lye that is used to dissolve core silica gel component is aqueous sodium hydroxide solution, potassium hydroxide aqueous solution, and acid solution is a hydrofluoric acid.Used alkali lye or acid strength do not have particular requirement (can adopt the solution of any concentration), and its preferred concentration is that concentration of lye is 0.5mol/L-5mol/L; Fluohydric acid content is HF: H
2O=5%-60% (V/V).
Hollow charcoal of the present invention can be used as sorbing material or microreactor.
Hollow charcoal of the present invention is owing to have vesicular structure, and specific surface is bigger, and strong adsorptive power is arranged, and can be used for the processing of waste water, pollutent etc.; Hollow charcoal has the hollow core structure, can be used as mould material, is used for the synthetic of other sphere materials.
Embodiment
Embodiment 1: hollow carbon sphere synthetic: behind 5ml vinylbenzene, 5ml Vinylstyrene, 500mg Diisopropyl azodicarboxylate thorough mixing, logical nitrogen 10min gets particle diameter 3 μ m spherical silica gels and puts into above-mentioned mixed solution, takes out behind the immersion 2h, sealing is put into baking oven in 343K reaction 5h.Thereafter material is taken out and places crucible, with gac with the whole embedding of crucible, under the condition of this secluding air and oxygen, 1173K calcination 2h in retort furnace, behind the naturally cooling, wash with the 5mol/L aqueous sodium hydroxide washes and promptly to get hollow raw material of wood-charcoal material for 3 times, this hollow carbon granule directly is 3.05 μ m, the about 50nm of its outer charcoal thickness of the shell, its hollow core diameter is 3 μ m.
Embodiment 2: hollow carbon sphere synthetic: at first press sucrose: the vitriol oil: water=2.5g: 0.3g: 10mL disposes sucrose and sulfuric acid mixture liquid.Particle diameter 25 μ m spherical silica gels are immersed in this mixed solution, and treating that abundant wetting back is taken out dries, and behind the complete drying, from room temperature, the heat-up rate of 2K/min is warming up to 433K and keeps 5h, allows the abundant dehydration carbonization of sucrose.This process repeats 5 times, gets silica gel-carbon composite.Handle this matrix material 3 times with the hydrofluoric acid aqueous solution of the 0.5mol/L KOH aqueous solution or 40%, can get spherical hollow raw material of wood-charcoal material, this hollow carbon granule directly is 26 μ m, the about 1 μ m of its outer charcoal thickness of the shell, and its hollow core diameter is about 25 μ m.
Embodiment 3: hollow carbon sphere synthetic: particle diameter 50nm spherical silica gel is immersed in the furfuryl alcohol, takes out after soaking into 3h, the sealing back is in 363K reaction 15h.This step repeats once.Thereafter material is placed retort furnace, the heat-up rate of 2K/min is warming up to 1073K maintenance 5h in the nitrogen atmosphere, and take out the cooling back, gets silica gel-carbon composite.With the 3mol/L KOH aqueous solution or 5% (HF/H
2O, hydrofluoric acid aqueous solution v/v) handle this matrix material 3 times, can get spherical hollow raw material of wood-charcoal material, and this hollow carbon granule directly is 55nm, the about 15nm of its outer charcoal thickness of the shell, and its hollow core diameter is 40nm.
Embodiment 4: hollow carbon sphere is used for the absorption of environmental pollutant
Polycyclic aromatic hydrocarbons is the more common environmental pollutant of a class.Get a water sample that contains polycyclic aromatic hydrocarbons, survey its uv-absorbing at 254nm, because the existence of polycyclic aromatic hydrocarbons, water sample has tangible uv-absorbing.To be filled in the stainless steel column by the hollow raw material of wood-charcoal material of embodiment 1 synthetic, and allow water sample pass through this stainless steel column, and again water sample be carried out uv-absorbing and detect.The water sample of discovery after hollow charcoal is handled do not have uv-absorbing, and visible hollow charcoal has stronger adsorptive power to polycyclic aromatic hydrocarbons, is suitable for the removal of environmental pollutant.
Embodiment 5: hollow charcoal is used for microreactor
Hollow charcoal is owing to have the hollow core structure, and this hollow core can communicate with the external world by the vesicular structure on the outer charcoal shell simultaneously, therefore can utilize the hollow cavity of hollow charcoal to serve as microreactor, carries out building-up reactions.Zirconium oxychloride, water, ethanol are pressed 1g: 3mL: the mixed of 5mL, get by the hollow charcoal of the embodiment of the invention 3 synthetic, soak in above-mentioned zirconyl chloride solution, hollow charcoal fully adsorb saturated after, take out suction filtration a moment, put into baking oven 343K reaction 12h.Zirconium oxychloride colloidal sol carries out sol gel reaction in hollow charcoal cavity, the drying calcination is handled, and can get the Zirconium powder material, and its powder granularity size is close with hollow charcoal hollow core diameter.
Claims (9)
1. hollow charcoal, it is characterized in that: charcoal outward appearance spherical in shape, it is made up of outer charcoal shell and hollow core.
2. according to the described hollow charcoal of claim 1, it is characterized in that: hollow carbon granule directly is 0.05 μ m-50 μ m, and its outer charcoal thickness of the shell is 10nm-1 μ m, and its hollow core diameter is 30nm-49 μ m.
3. according to claim 1 or 2 described hollow charcoals, it is characterized in that: outer charcoal shell is a vesicular structure, and the hollow core of hole and raw material of wood-charcoal material interconnects.
4. the synthetic method of claim 1 or 2 described hollow charcoals, it is characterized in that: the organic monomer reaction liquid of absorption on spherical silica gel, by initiation reaction, be coated with organic polymer at silica gel, then with the organic polymer charing, and with alkali lye or acid fluid dissolves core silica gel component, thereby obtain hollow charcoal.
5. according to the described method of claim 4, it is characterized in that: the organic monomer reaction solution that is adsorbed on the spherical silica gel can be vinylbenzene, Vinylstyrene, divinyl, furfuryl alcohol, resol or carbohydrate organism, it is saturated that its adsorptive capacity is controlled to be absorption, and its absorption number of times can be one or many absorption.
6. according to claim 4 or 5 described methods, it is characterized in that: the charing mode of organic polymer for the vitriol oil at 333K～573K with the organics dehydration carbonization; Perhaps under the condition of secluding air and oxygen, in 673K～1473K pyroprocessing and with organic carbon.
7. according to claim 4 or 5 described methods, it is characterized in that: the alkali lye that is used to dissolve the silica gel component is aqueous sodium hydroxide solution, potassium hydroxide aqueous solution, and acid solution is a hydrofluoric acid.
8. according to the described method of claim 7, it is characterized in that: concentration of lye is 0.5mol/L-5mol/L; Fluohydric acid content is HF: H
2O=5%-60%, described per-cent are volume ratio.
9. claim 1 or 2 described hollow charcoals are as the purposes of sorbing material, microreactor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410060849 CN1260122C (en) | 2004-09-14 | 2004-09-14 | Hollow charcoal and its synthetic method and use |
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| CN 200410060849 CN1260122C (en) | 2004-09-14 | 2004-09-14 | Hollow charcoal and its synthetic method and use |
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| CN1587032A true CN1587032A (en) | 2005-03-02 |
| CN1260122C CN1260122C (en) | 2006-06-21 |
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| CN 200410060849 Expired - Fee Related CN1260122C (en) | 2004-09-14 | 2004-09-14 | Hollow charcoal and its synthetic method and use |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100372761C (en) * | 2006-06-22 | 2008-03-05 | 上海交通大学 | Method for preparing hollow Nano carbon balls in graphite structure under solid state |
| CN100423819C (en) * | 2006-06-23 | 2008-10-08 | 武汉大学 | Hollow carbon fibre, its synthesis and use |
| CN100423820C (en) * | 2006-06-23 | 2008-10-08 | 武汉大学 | Hollow inorganic oxide fibre, its synthesis and use |
| CN101817519A (en) * | 2010-04-01 | 2010-09-01 | 中国科学院上海硅酸盐研究所 | Preparation method and use of millimetre-sized mesoporous carbon spheres |
| CN103395773A (en) * | 2013-08-09 | 2013-11-20 | 中南大学 | Nano carbon hollow sphere and preparation method thereof |
| CN104743542A (en) * | 2014-11-05 | 2015-07-01 | 北京化工大学 | Hollow mesoporous carbon ball and preparation method thereof |
| CN106006605A (en) * | 2016-05-31 | 2016-10-12 | 赵常然 | Preparation method of highly-pure nanocarbon |
-
2004
- 2004-09-14 CN CN 200410060849 patent/CN1260122C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100372761C (en) * | 2006-06-22 | 2008-03-05 | 上海交通大学 | Method for preparing hollow Nano carbon balls in graphite structure under solid state |
| CN100423819C (en) * | 2006-06-23 | 2008-10-08 | 武汉大学 | Hollow carbon fibre, its synthesis and use |
| CN100423820C (en) * | 2006-06-23 | 2008-10-08 | 武汉大学 | Hollow inorganic oxide fibre, its synthesis and use |
| CN101817519A (en) * | 2010-04-01 | 2010-09-01 | 中国科学院上海硅酸盐研究所 | Preparation method and use of millimetre-sized mesoporous carbon spheres |
| CN101817519B (en) * | 2010-04-01 | 2012-05-30 | 中国科学院上海硅酸盐研究所 | Preparation method and use of millimetre-sized mesoporous carbon spheres |
| CN103395773A (en) * | 2013-08-09 | 2013-11-20 | 中南大学 | Nano carbon hollow sphere and preparation method thereof |
| CN104743542A (en) * | 2014-11-05 | 2015-07-01 | 北京化工大学 | Hollow mesoporous carbon ball and preparation method thereof |
| CN106006605A (en) * | 2016-05-31 | 2016-10-12 | 赵常然 | Preparation method of highly-pure nanocarbon |
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| Publication number | Publication date |
|---|---|
| CN1260122C (en) | 2006-06-21 |
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