CN103265005A - Nano-carbon material/carbon aerogel (CA) microwave synthesis method - Google Patents
Nano-carbon material/carbon aerogel (CA) microwave synthesis method Download PDFInfo
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- CN103265005A CN103265005A CN2013101430341A CN201310143034A CN103265005A CN 103265005 A CN103265005 A CN 103265005A CN 2013101430341 A CN2013101430341 A CN 2013101430341A CN 201310143034 A CN201310143034 A CN 201310143034A CN 103265005 A CN103265005 A CN 103265005A
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Abstract
The invention discloses a nano-carbon material/carbon aerogel (CA) microwave synthesis method. The nano-carbon material/CA microwave synthesis method comprises that resorcinol and formaldehyde as raw materials are synthesized into organic wet gel as an intermediate by a microwave synthesis method; acetone is added into the organic wet gel to extract water and impurities in the organic wet gel; and the treated organic wet gel is subjected to high temperature charing at a temperature of 900 DEG C in the nitrogen protective atmosphere for 2h to produce CA. The CA has the particle sizes less than 50nm and has a large specific surface area and high porosity. The nano-carbon material/CA microwave synthesis method has the advantages of fast synthesis speed, low energy consumption and small pollution.
Description
Technical field
The invention belongs to macromolecular material and electrochemical applications technical field, being specifically related to a kind of is raw material with Resorcinol (R) and formaldehyde (F), the applied microwave technology prepares the method for carbon nano-material/charcoal-aero gel (CA), this carbon nano-material/charcoal-aero gel is a kind of novel light porous material, has multiple high-performance, as low density, homogeneity, high-specific surface area, high conductivity, with respect to traditional porous carbon materials such as gac, activated carbon fiber, its performance is better.Can be used for aspects such as catalyzer, ultracapacitor, water treatment and Chu Qing.
Background technology
The raw material of wood-charcoal material gets more and more people's extensive concerning for a long time with characteristics such as its chemical stability, thermostability, biocompatibility, electroconductibility and low price, wide material sources always.Scientist's prophesy: after entering 21 century, the raw material of wood-charcoal material will replace a large amount of iron and silicon that use at present, become the key material that supports advanced industry.
In recent years, novel charcoal material such as carbon molecular sieve, carbon nanotube, charcoal nanofiber etc. are one of fields, forward position of international scientific research in the huge applications potentiality that every field such as the energy, chemical industry, environmental protection exist always.Along with raw material of wood-charcoal material science constantly develops, the appearance of novel charcoal nano-porous materials " charcoal-aero gel " has caused that people pay close attention to widely.
Charcoal-aero gel (CA) is a kind of mesopore raw material of wood-charcoal material with unique three-dimensional manometer network structure, this is a kind of nano level raw material of wood-charcoal material of novelty, it is big to have specific surface area, the porosity height, characteristics such as density is low and adjustable are owing to its unique electricity, optics, calorifics, magnetics, catalytic performance make it have broad application prospects in military affairs, space flight, environmental protection, the energy, medicine and other fields.
The conventional preparation of people carbon nano-material charcoal-aero gel method, Resorcinol and formaldehyde is soluble in water with the mol ratio of 1:2, add catalyzer, sealing places 80 ℃ of water-bath 7d to generate organic wet gel.Then dry 5h in thermostatic drying chamber obtains organic aerogel.In the high temperature carbonization stove, carry out charing, be warming up to 900 ℃～1000 ℃, and want blanketing with inert gas, obtain charcoal-aero gel (CA) powder of black at last.More than excessive for the power consumption of traditional method technological process, and can not be used for mass production.
Summary of the invention
Purpose of the present invention aims to provide the microwave method synthetic method of a kind of carbon nano-material/charcoal-aero gel (CA), has studied the synthetic condition of intermediate product organic aerogel microwave emphatically to the influence of charcoal-aero gel status color.Integrated survey the influence of different catalyzer, microwave time, microwave power, catalyst proportion and productive rate in the microwave method process.This method technological process is simple, and art breading is convenient, and microwave is introduced experiment, has shortened the reaction times greatly, has improved chemical reaction rate, the productive rate height, and product property is stable.
In order to realize above-mentioned task, the present invention takes following technical solution:
The microwave method synthetic method of a kind of carbon nano-material/charcoal-aero gel (CA) is characterized in that, synthesizes by following concrete steps:
Be raw material with Resorcinol (R) and formaldehyde (F), Resorcinol (R) is 1:2 with the mol ratio of formaldehyde (F), be under the condition of 400W～800W at microwave power, in raw material, add proper amount of deionized water and anhydrous sodium carbonate, stir, radiated time to raw material is 20min～40min, and temperature of reaction is 80 ℃, synthetic intermediate;
Intermediate is further at 80 ℃ of down aging 4d of insulation.Add acetone soln then at normal temperatures and pressures the moisture in the intermediate and impurity are removed, obtain wine-colored organic aerogel.
The organic aerogel that obtains carries out dry 0.5h in infrared drying oven, 110 ℃ of following dry 5h in thermostatic drying chamber then are at last at rare gas element (N
2) carbonization in the protection pipe type stove, be warming up to 900 ℃ with 5 ℃/min～10 ℃/min, then at 900 ℃ of following carbonization 2h, the naturally cooling cooling obtains charcoal-aero gel (CA) powder of black.
The microwave method synthetic method of carbon nano-material/charcoal-aero gel of the present invention (CA), the mode of employing carry out microwave radiation heating makes Resorcinol (R) and formaldehyde (F) generate the organic wet gel of intermediate rapidly.The result shows that microwave heating has improved synthesis rate and the productive rate of products therefrom greatly, and product charcoal-aero gel (CA) stable in properties, the aperture is relative with particle diameter less and porosity is higher, and specific surface area is bigger, is mainly used in aspects such as catalyzer, ultracapacitor, water treatment and Chu Qing.Characteristics such as the present invention has shortened the reaction times by the microwave chemical technology, has simplified synthesis technique, and it is simple that this technology has process, and resultant velocity is fast, and is energy-conservation, pollutes and lacks, and product property is stable.
Embodiment
Technical thought of the present invention is, is raw material with Resorcinol and formaldehyde, the applied microwave synthetic technology, and under microwave condition, adding deionized water and catalyzer carry out polyreaction and generate organic wet gel, need continuous stirring in the microwave building-up process.Aging 4d at a certain temperature, recycling acetone is removed impurity, and high temperature carbonization obtains charcoal-aero gel (CA) more at last.
Concrete synthetic method is: be raw material with Resorcinol and formaldehyde, the mol ratio of Resorcinol and formaldehyde is 1:2, in raw material, add deionized water and catalyzer, stir, being 400W～800W with microwave power, is 20min～40min to the radiated time of raw material, and temperature of reaction is 80 ℃, obtain the sticky shape of a kind of light red, transparent organic wet gel; Then organic wet gel is placed 80 ℃ of down aging 4d, in infrared drying oven and thermostatic drying chamber, carry out drying and dehydrating again, at last at rare gas element (N
2) carbonization in the protection pipe type stove.Carbonization process is to be warming up to 900 ℃ with 5 ℃～10 ℃ temperature rise rates, and then at 900 ℃ of following carbonization 2h, naturally cooling is lowered the temperature, and obtains charcoal-aero gel (CA) powder of black.
Catalyzer adopts anhydrous sodium carbonate, and optimum amount is Resorcinol/anhydrous sodium carbonate=500.
The synthetic required microwave best power of intermediate is 500W, and best radiated time is 25min, and optimal reaction temperature is 80 ℃.
The organic wet gel of intermediate removes impurity with acetone and moisture extracts 3 times at least.
Even in order to guarantee material, product property is stable, reacts completely.Usually will control microwave power, sufficient radiated time is provided, optimum microwave power is 500W, and optimum radiated time is 25min, and optimum hydrolysis temperature is 80 ℃, obtains scarlet to ruddy sticky shape, transparent organic wet gel.Through obtaining charcoal-aero gel (CA) powder of black behind removal of impurities, drying and the high temperature carbonization.The body structure surface of the product that obtains presents a large amount of comparatively ordered porous reticulated structures, and its particle diameter and aperture are all in 50nm.
Be a series of embodiment that the contriver provides below, these embodiment are more excellent examples, and the present invention does not limit to these embodiment.
Embodiment 1: catalyst type and proportioning are to the influence of charcoal-aero gel synthesis rate
Referring to table 1, be that 1:2 mixes with the mol ratio with Resorcinol (R) and formaldehyde (F), add different catalysts and different proportionings, with water as solvent, put into three-necked bottle, add magnetic stir bar, under microwave field, microwave power is 500W, and the adjusting microwave irradiation time is 25min, setting temperature of reaction is 80 ℃, obtain the sticky shape of light red, transparent organic wet gel, place infrared drying oven to dry 0.5h organic wet gel then, 5h dewaters in the thermostatic drying chamber, get the organic aerogel of hard porous, temperature is controlled at 110 ℃; At last with organic aerogel in the high temperature carbonization stove at nitrogen (N
2) protection down carries out charing, controls temperature rise rate at 5～10 ℃, at 900 ℃ of following charing 2h.Naturally cooling is lowered the temperature, and obtains charcoal-aero gel (CA) powder of black.From table 1, can obtain anhydrous Na
2CO
3It is more satisfactory catalyzer.
Table 1: catalyst type and proportioning are to the influence of charcoal-aero gel synthesis rate
Embodiment 2: the time is to the influence of charcoal-aero gel color state
Be that 1:2 mixes with the mol ratio with Resorcinol (R) and formaldehyde (F), add anhydrous sodium carbonate and make catalyzer, R/C=500, with water as solvent, put into three-necked bottle, add magnetic stir bar, under microwave field, microwave power is 500W, regulate microwave irradiation time, table 2 be the time to the influence of charcoal-aero gel color state, setting temperature of reaction is 80 ℃, gets organic wet gel, place infrared drying oven to dry 0.5h organic wet gel then, the 5h that dewaters in the thermostatic drying chamber gets the organic aerogel of hard porous, and temperature is controlled at 110 ℃; At last with organic aerogel in the high temperature carbonization stove at nitrogen (N
2) protection down carries out charing, controls temperature rise rate at 5～10 ℃, at 900 ℃ of following charing 2h.Naturally cooling is lowered the temperature, and obtains charcoal-aero gel (CA) powder of black.As can be seen from Table 2, the organic wet gel of thick redness is preferable, is 25min so choose the microwave time.
Table 2: the microwave time is to the influence of organic wet gel color state
Embodiment 3: microwave power influences organic wet gel color state
Be that 1:2 mixes with the mol ratio with Resorcinol (R) and formaldehyde (F), add anhydrous sodium carbonate and make catalyzer, R/C=500, with water as solvent, put into three-necked bottle, add magnetic stir bar, under microwave field, regulate microwave power, microwave power influences referring to table 3 organic wet gel color state, the setting microwave irradiation time is 25min, and temperature of reaction is 80 ℃, gets organic wet gel, place infrared drying oven to dry 0.5h organic wet gel then, the 5h that dewaters in the thermostatic drying chamber gets the organic aerogel of hard porous, and temperature is controlled at 110 ℃; At last with organic aerogel in the high temperature carbonization stove at nitrogen (N
2) protection down carries out charing, controls temperature rise rate at 5～10 ℃/min, at 900 ℃ of following charing 2h.Naturally cooling is lowered the temperature, and obtains charcoal-aero gel (CA) powder of black.Can obtain preferable and convenient transfer of color state when 500W from table 3, be 500W so choose microwave power.
Table 3: microwave power influences organic wet gel color state
Embodiment 4: catalyst proportion (R/C) influences organic wet gel color state
Be the mixed of 1:2 with the mole with Resorcinol (R) and formaldehyde (F), add anhydrous sodium carbonate and make catalyzer, table four is that different catalysts proportioning (R/C) influences organic wet gel color state, with water as solvent, put into three-necked bottle, add magnetic stir bar, under microwave field, regulate microwave power, table 4 is that microwave power influences organic wet gel color state, the adjusting microwave irradiation time is 25min, and setting temperature of reaction is 80 ℃, gets organic wet gel, place infrared drying oven to dry 0.5h organic wet gel then, the 5h that dewaters in the thermostatic drying chamber gets the organic aerogel of hard porous, and temperature is controlled at 110 ℃; At last with organic aerogel in the high temperature carbonization stove at nitrogen (N
2) protection down carries out charing, controls temperature rise rate at 5～10 ℃/min, at 900 ℃ of following charing 2h.Naturally cooling is lowered the temperature, and obtains charcoal-aero gel (CA) powder of black.Can obtain catalyst proportion from table four is an important factors, and the increase gradually along with catalyst proportion causes sol-gel process incomplete, the phenomenon of part white occurs.Along with the increase of catalyst proportion, aperture and the particle diameter of charcoal-aero gel also increase simultaneously,
In order to keep it in 50nm, select R/C=500.
Table 4: catalyst proportion is to organic wet gel color state influence influence
Claims (5)
1. the microwave method synthetic method of a carbon nano-material/charcoal-aero gel (CA) is characterized in that, synthesizes by following concrete steps:
Step 1, be raw material with Resorcinol (R) and formaldehyde (F), Resorcinol (R) is 1:2 with the mol ratio of formaldehyde (F), be under the condition of 400～800W at microwave power, adding proper amount of deionized water and anhydrous sodium carbonate in the raw material, stir, is 20～40min to the radiated time of raw material, temperature of reaction is 80 ℃, synthetic intermediate;
Step 2 further is being incubated 80 ℃ of down aging 4d with synthetic intermediate.Add acetone soln then at normal temperatures and pressures the moisture in the intermediate and impurity are removed, obtain wine-colored organic aerogel.
Step 3 is carried out dry 0.5h with the organic aerogel that obtains in infrared drying oven, 110 ℃ of following dry 5h in thermostatic drying chamber then are at last at rare gas element (N
2) carbonization in the protection pipe type stove.Slowly be warming up to 900 ℃, then at 900 ℃ of following carbonization 2h, naturally cooling is lowered the temperature, and obtains charcoal-aero gel (CA) powder of black.
2. method according to claim 1 is characterized in that the consumption of described anhydrous sodium carbonate is: Resorcinol (R)/anhydrous sodium carbonate=500.
3. method according to claim 1 is characterized in that the microwave power in the microwave building-up process of described step 1 is 500W, and radiated time is 25min, and temperature of reaction is 80 ℃.
4. method according to claim 1 is characterized in that, the intermediate of described step 2 needs to remove impurity and moisture extract 3 times at least with acetone.
5. method according to claim 1 is characterized in that, the organic aerogel of described step 3 when high temperature carbonization temperature rise rate control in 5 ℃/min～10 ℃/min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107026028A (en) * | 2017-03-03 | 2017-08-08 | 南京林业大学 | A kind of method that utilization biological material quickly prepares ultracapacitor carbon aerogels |
| CN113292061A (en) * | 2021-05-28 | 2021-08-24 | 浙江工业大学 | Carbon aerogel catalyst synthesized under microwave action and synthesis method and application thereof |
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| CN1895770A (en) * | 2006-06-21 | 2007-01-17 | 中国工程物理研究院激光聚变研究中心 | Carbon-gas gel powder and its preparation |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1895770A (en) * | 2006-06-21 | 2007-01-17 | 中国工程物理研究院激光聚变研究中心 | Carbon-gas gel powder and its preparation |
Non-Patent Citations (4)
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| E.G.CALVO ET AL: "Fast microwave-assisted synthesis of tailored mesoporous carbon xerogels", 《JOURNAL OF COLLOID AND INTERFACE SCIENCE》, vol. 357, no. 2, 18 February 2011 (2011-02-18), XP028370244, DOI: doi:10.1016/j.jcis.2011.02.034 * |
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| EJ JUÁREZ-PÉREZ ET AL: "Precise determination of the point of sol–gel transition in carbon gel synthesis using a microwave heating method", 《CARBON》, vol. 48, no. 11, 13 May 2010 (2010-05-13) * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107026028A (en) * | 2017-03-03 | 2017-08-08 | 南京林业大学 | A kind of method that utilization biological material quickly prepares ultracapacitor carbon aerogels |
| CN113292061A (en) * | 2021-05-28 | 2021-08-24 | 浙江工业大学 | Carbon aerogel catalyst synthesized under microwave action and synthesis method and application thereof |
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