CN102502575B - Method for preparing carbon foam by using foaming agent - Google Patents
Method for preparing carbon foam by using foaming agent Download PDFInfo
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- CN102502575B CN102502575B CN2011103261851A CN201110326185A CN102502575B CN 102502575 B CN102502575 B CN 102502575B CN 2011103261851 A CN2011103261851 A CN 2011103261851A CN 201110326185 A CN201110326185 A CN 201110326185A CN 102502575 B CN102502575 B CN 102502575B
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Abstract
The invention relates to a method for preparing carbon foam by using a foaming agent. The method comprises the following steps of: performing ball milling on the foaming agent and deionized water at room temperature and stirring until the foaming agent is completely dissolved; adding carbon powder with a self-sintering capacity in a ratio, and stirring and foaming without applied pressure to obtain stable wet carbon foam; removing water in a drying box to obtain blank carbon foam; raising the temperature to be between 200 and 300 DEG C, and oxidizing at constant temperature; raising the temperature to be between 800 and 1,500 DEG C, and carbonizing to obtain carbon foam; and raising the temperature of the carbon foam to be between 2,300 and 3,000 DEG C under the protection of argon, and graphitizing to obtain a highly graphitized carbon foam material. The environment-friendly foaming agent is applied, and heating and pressurizing processes in a process for preparing the carbon foam are eliminated, so that energy and cost are saved, and the porosity and pore size of the product are adjustable and controllable; and the dried and demoulded blank carbon foam cannot be deformed in the oxidation, carbonization and graphitization processes, so that the carbon foam has uniform density.
Description
Technical field
The present invention relates to a kind of method for preparing the charcoal foam with whipping agent.
Background technology
The charcoal foam based on performances such as its good thermostability, low density, low-thermal-expansion, high heat shock resistance and vibrations, has become dual-use novel material since the sixties in last century come out, enjoy attention and development rapidly.Especially along with the improving constantly and the continuous appearance of various novel preparation process of control charcoal foamy structure level, the Application Areas of charcoal foam and range of application also obtain continuing expansion.At present it is used and has spreaded all over environmental protection, energy-conservation, chemical industry, smelting, pharmacy, nuclear energy and a plurality of industrial circles such as biomedical.
Common charcoal foam preparation processes is take mesophase pitch as raw material, adopts high temperature to produce the method preparation of pressure.The charcoal foamy structure is to be made of the crafters of centre and regularly arranged graphite flake layer ligament on every side, because mesophase pitch foams under molten state, not only energy consumption is high, and cost is high, and how foaming process controls the temperature field and pressure is the key point of the even charcoal foam in preparation aperture.And the structure formation of the arrangement mode of graphite microcrystal and macroscopic view has determined that intermediate phase pitch-based charcoal foam has low density, high heat conduction/conduction, low performances such as thermal expansivity.Graphite microcrystal is arranged in parallel at banded graphite flake layer ligament structure place, can present good directional property; Action of gravitation can make the graphite microcrystal structure, mechanical property of charcoal foam and microwave absorbing property along vertical and be parallel to gravity direction and have anisotropy, has also caused the inhomogeneous of charcoal foam density simultaneously.Especially arrange irregularity at node place graphite microcrystal, be polytropism.And also there is more crackle in the middle of these structures, thereby causes the intensity of charcoal foam lower.The method that has research adopt to add nano carbon fiber and MCMB improves the charcoal foamy body, although improved the intensity of charcoal foam, thus the continuity of also having destroyed the stone mill crystallite has reduced the thermal characteristics of charcoal foam.So be badly in need of at present simple, environmentally friendly, the controlled method for preparing the charcoal foam of a kind of technique, make the charcoal foam reach satisfied void content, and can control preferably aperture and distribution thereof, shape, three-dimensional arrangement etc.
Summary of the invention
The invention discloses and a kind ofly prepare the method for charcoal foam with whipping agent, its purpose is to overcome prior art such as high temperature from the standby required high energy consumption of process of the legal system that foams, and charcoal foamy body expensive, that prepare is low, microtexture is difficult for the problems such as adjustment.Adopt the charcoal foam of the inventive method preparation, can bubble without under the impressed pressure; Significantly be better than adopting in the traditional method high temperature to produce the preparation method of pressure.Save the heating and pressurizing technique in the preparation charcoal foam process, not only energy efficient and cost, and the whipping agent environmentally safe that adopts.
A kind ofly prepare the method for charcoal foam with whipping agent, it is characterized in that preparation process is as follows:
(1) whipping agent mixes with the weight ratio of 1:100～4:5 with deionized water, and ball grinding stirring to natural compounds dissolves fully under the room temperature; Described whipping agent is any one in collagenic protein, albumen protein or the whey protein;
(2) in the solution that step (1) obtains, add the carbon powder from caking power of having of 1～100g/100ml, and be stirred to uniform sizing material;
(3) uniform sizing material that obtains in the step (2) is foamed with alr mode, make hygrometric state charcoal foam;
(4) the hygrometric state charcoal foam that obtains in the step (3) is ladled out to mould, in the baking oven of-25～100 ° of C, removed moisture and obtain base substrate charcoal foam;
(5) the base substrate charcoal foam that obtains in the step (4) is placed oxidized still, the temperature rise rate with 0.1～5 ° of C/min in air is warming up to 200～300 ° of C, and constant temperature carried out oxide treatment in 1～10 hour under this temperature;
(6) the base substrate charcoal foam of oxide treatment in the step (5) being crossed places charring furnace, temperature rise rate with 3～100 ° of C/min under nitrogen protection is warmed up to 800～1500 ° of C, and keeps carrying out in 0.1～10 hour charing process and to obtain the charcoal foam under this temperature;
(7) the charcoal foam that obtains in the step (6) is warmed up to 2300～3000 ° of C with 10～50 ° of C/min speed under argon shield, is incubated 1～5 hour and carries out obtaining high-graphitized charcoal foam materials after the greying.
The carbon powder from caking power of having described in the step (2) comprises in coal-tar pitch, oil delay coke, gilsonite, the mesophase pitch any one.
The invention has the advantages that:
1. to adopt environment amenable natural compounds be whipping agent in the present invention, and technical process need not pressurization, so required equipment is simple, and low cost of manufacture is beneficial to large-scale application of the present invention.
2. traditional charcoal foam technology of preparing of the present invention's solution is not easy the problem of microtexture.By selecting different natural compoundss and consumption thereof, product has porosity controllable adjustment, aperture controllable adjustment.Base substrate charcoal foam through the super-dry demoulding can not produce distortion in oxidation, carbonization and graphitizing process in addition, avoids the Density inhomogeneity of traditional charcoal foam.
3. Carbon foam that the present invention produces is formed by powder accumulation, has extremely low thermal conductivity and thermal conductivity.
Embodiment
Below with embodiment the technology of the present invention content is described in further detail, but present embodiment is not limited to the present invention, every employing similarity method of the present invention and similar variation thereof all should be listed protection scope of the present invention in.
Embodiment 1
The collagenic protein of getting 1g mixes with the 100ml deionized water, and rear adding 1g coal-tar pitch stirs.Stirring bubbles obtains stable hygrometric state charcoal foam.Through-25 ° of C lyophilizes, dried charcoal foam is positioned in the box-type furnace and carries out sintering with nitrogen protection.Program is as follows: be warmed up to 200 ° of C with 0.1 ° of speed of C/ minute, the fixing processing of oxidation was carried out in insulation in 1 hour under this temperature; Pass into nitrogen protection, be raised to 800 ° of C with 3 ° of speed of C/ minute, the charcoal foam after insulation obtained charing in 3 hours under this temperature.Resulting charcoal foam is put into graphitizing furnace, under argon shield, be warming up to 2300 ° of C with 10 ° of speed of C/ minute, and under this temperature, be incubated 1 hour, obtain the graphitized carbon foam.The charcoal foam has the macropore pattern of 200-500 μ m sphere, and the window that causes the 20-100 μ m that interconnects is arranged at hole wall.Open-cell porosity is 90%, and compressive strength is 0.6MPa.
Embodiment 2
Experimental technique is identical with embodiment 1 with condition, but whipping agent is albumen protein, and consumption is 20g.Adding oil delay coke is 8g.Hygrometric state charcoal foam is at room temperature dry.Be warmed up to 210 ° of C with 1 ° of speed of C/ minute, oxidation is fixed 2 hours.Be warmed up to 1000 ° of C with 10 ° of speed of C/ minute, charing 7 hours.Be warmed up to 2500 ° of C with 15 ° of speed of C/ minute, greying 5 hours.Obtaining charcoal foam open-cell porosity is 80%, and compressive strength is 1.2MPa.
Embodiment 3
Experimental technique is identical with embodiment 1 with condition, but whipping agent is whey protein, and consumption is 55g.The adding gilsonite is 33g.Hygrometric state charcoal foam is dry under 40 ° of C.Be warmed up to 250 ° of C with 3 ° of speed of C/ minute, oxidation is fixed 8 hours.Be warmed up to 1200 ° of C with 50 ° of speed of C/ minute, charing 10 hours.Be warmed up to 2800 ° of C with 35 ° of speed of C/ minute, greying 4 hours.Obtaining charcoal foam open-cell porosity is 75%, and compressive strength is 4.5MPa.
Embodiment 4
Experimental technique is identical with embodiment 1 with condition, but whipping agent is whey protein, and consumption is 80g.The adding mesophase pitch is 100g.Hygrometric state charcoal foam is dry under 100 ° of C.Be warmed up to 300 ° of C with 5 ° of speed of C/ minute, oxidation is fixed 10 hours.Be warmed up to 1500 ° of C with 100 ° of speed of C/ minute, charing 0.1 hour.Be warmed up to 3000 ° of C with 50 ° of speed of C/ minute, greying 2 hours.Obtaining charcoal foam open-cell porosity is 65%, and compressive strength is 7.0MPa.
Claims (2)
1. one kind prepares the method for charcoal foam with foaming, it is characterized in that preparation process is as follows:
(1) whipping agent mixes with the weight ratio of 1:100～4:5 with deionized water, and ball grinding stirring to whipping agent dissolves fully under the room temperature; Described whipping agent is any one in collagenic protein, albumen protein or the whey protein;
(2) in the solution that step (1) obtains, add the carbon powder from caking power of having of 1～100g/100ml, and be stirred to uniform sizing material;
(3) uniform sizing material that obtains in the step (2) is foamed with alr mode, make hygrometric state charcoal foam;
(4) the hygrometric state charcoal foam that obtains in the step (3) is ladled out to mould, in the baking oven of-25～100 ° of C, removed moisture and obtain base substrate charcoal foam;
(5) the base substrate charcoal foam that obtains in the step (4) is placed oxidized still, the temperature rise rate with 0.1～5 ° of C/min in air is warming up to 200～300 ° of C, and constant temperature carried out oxide treatment in 1～10 hour under this temperature;
(6) the base substrate charcoal foam of oxide treatment in the step (5) being crossed places charring furnace, temperature rise rate with 3～100 ° of C/min under nitrogen protection is warmed up to 800～1500 ° of C, and keeps carrying out in 0.1～10 hour charing process and to obtain the charcoal foam under this temperature;
(7) the charcoal foam that obtains in the step (6) is warmed up to 2300～3000 ° of C with 10～50 ° of C/min speed under argon shield, after being incubated 1～5 hour and carrying out greying, obtains high-graphitized charcoal foam materials.
2. according to claim 1ly a kind ofly prepare the method for charcoal foam with whipping agent, it is characterized in that: the carbon powder from caking power of having described in the step (2) comprises in coal-tar pitch, oil delay coke, gilsonite, the mesophase pitch any one.
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| CN2011103261851A CN102502575B (en) | 2011-10-24 | 2011-10-24 | Method for preparing carbon foam by using foaming agent |
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| CN2011103261851A CN102502575B (en) | 2011-10-24 | 2011-10-24 | Method for preparing carbon foam by using foaming agent |
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| CN102502575A CN102502575A (en) | 2012-06-20 |
| CN102502575B true CN102502575B (en) | 2013-10-30 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103058706A (en) * | 2012-11-27 | 2013-04-24 | 中国人民解放军国防科学技术大学 | Method for preparing foamed ceramic sound absorption material through protein foaming |
| CN103101904B (en) * | 2013-03-06 | 2015-06-17 | 广西大学 | Preparation method of foam carbon with pressure-resistant and shock-absorbing characteristics |
| CN103112843B (en) * | 2013-03-06 | 2014-12-24 | 广西大学 | Method for preparing foam carbon with high thermal conductivity |
| CN104446614B (en) * | 2014-11-13 | 2017-07-14 | 湖北富邦科技股份有限公司 | A kind of multi-functional composite balls charcoal and preparation method thereof |
| CN106115655B (en) * | 2016-06-25 | 2018-06-05 | 惠安三兴石材有限公司 | A kind of preparation method that Carbon foam is prepared using biomass fermentation infusion |
| CN106278367B (en) * | 2016-08-04 | 2018-11-13 | 辽宁科技大学 | Microwave heating prepares the device and method of coal-based carbon foam under normal pressure |
| CN110606699B (en) * | 2018-06-15 | 2021-06-22 | 国家能源投资集团有限责任公司 | Heat-conducting carbon material and preparation method thereof |
| CN109479694A (en) * | 2018-11-07 | 2019-03-19 | 新昌县天姥园艺发展有限公司 | The suspended bed device of indoor water plant planting |
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|---|---|---|---|---|
| CN101434388A (en) * | 2008-12-05 | 2009-05-20 | 华东理工大学 | Preparation of small pore diameter carbon foam |
| CN101927996A (en) * | 2010-07-30 | 2010-12-29 | 广州有色金属研究院 | Method for preparing pitch-based foam carbon |
| CN102060287A (en) * | 2010-11-23 | 2011-05-18 | 烟台鲁航炭材料科技有限公司 | Production method of low density foam carbon heat insulating material for inert atmosphere furnace |
| JP5024919B2 (en) * | 2005-11-30 | 2012-09-12 | マルトモ株式会社 | Filling the bonito packaging pack |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH0524919A (en) * | 1991-07-24 | 1993-02-02 | Hitachi Chem Co Ltd | Production of carbon material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5024919B2 (en) * | 2005-11-30 | 2012-09-12 | マルトモ株式会社 | Filling the bonito packaging pack |
| CN101434388A (en) * | 2008-12-05 | 2009-05-20 | 华东理工大学 | Preparation of small pore diameter carbon foam |
| CN101927996A (en) * | 2010-07-30 | 2010-12-29 | 广州有色金属研究院 | Method for preparing pitch-based foam carbon |
| CN102060287A (en) * | 2010-11-23 | 2011-05-18 | 烟台鲁航炭材料科技有限公司 | Production method of low density foam carbon heat insulating material for inert atmosphere furnace |
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