CN101468795A - Preparation of high specific surface carbon aerogel - Google Patents
Preparation of high specific surface carbon aerogel Download PDFInfo
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- CN101468795A CN101468795A CNA2007100509755A CN200710050975A CN101468795A CN 101468795 A CN101468795 A CN 101468795A CN A2007100509755 A CNA2007100509755 A CN A2007100509755A CN 200710050975 A CN200710050975 A CN 200710050975A CN 101468795 A CN101468795 A CN 101468795A
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- carbon aerogel
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Abstract
The invention provides a method for preparing high specific surface carbon aerogel. The method is characterized by comprising the following steps: weighing hydroxyphenol with certain amount to be dissolved by furfural with certain amount to form an A solution; dissolving a catalyst, a dispersing agent and the like by ethanol with certain amount to form a B solution; dripping the B solution into the A solution under a stirring state at normal temperature to form an organosol prepolymer; gelatinating the organosol prepolymer in a sealed container at a temperature of between 30 and 90 DEG C to age for 3 to 15 days to form organic ethanol aerogel; drying the organic ethanol aerogel by opening a sealing cover at a temperature of between 30 and 80 DEG C to form the organic aerogel; maintaining the gel under inert gas protection at a temperature of between 700 and 1,100 DEG C to form the carbon aerogel; activating the carbon aerogel with strong base which is 1 to 5 times of the carbon aerogel for 1 to 2 days; washing the carbon aerogel to neutrality, and drying the neutral carbon aerogel; sintering the carbon aerogel under inert gas protection at a temperature of between 650 and 900 DEG C for 1 to 3 hours; and washing the carbon aerogel to neutrality, and drying the neutral carbon aerogel. The method prepares the carbon aerogel with specific surface of between 1,500 and 3,000m2/g and pore volume of between 0.5 and 1.5ml/g.
Description
Technical field
The invention belongs to field of material preparation, refer in particular to the preparation technology of high specific surface carbon aerogel.
Background technology
The preparation method of carbon aerogels has following several usually
1, normal pressure solvent exchange method with Resorcinol and the formaldehyde mixed in molar ratio with 1:2, is a catalyzer with yellow soda ash, with the deionization water as solvent, stir, insert after the sealing in the baking oven, handle 1d, 1d and 3d with 25 ℃, 50 ℃ and 90 ℃ respectively, generate the RF wet gel at last.Resorcinol is called for short ratio with the mol ratio of catalyzer, and the mass percent that Resorcinol and formaldehyde account for total solution is called for short the M value.Carry out solvent replacing and soak sample with acetone, after drying under the room temperature condition of normal pressure, can obtain the RF aerogel, obtain carbon aerogels by high temperature cabonization at last.
2, supercritical solvent substitution method, with Resorcinol, formaldehyde, deionized water and Na2CO3 mixed in molar ratio with 1:2:17.5:0.0008, after stirring, the input horizon spacing is thermal treatment in the rearmounted people's baking oven of sealing between the sheet glass mould that do not wait of 1～3mm, 30 ℃, 50 ℃ each 24h, 90 ℃ of following 72h, reaction promptly obtains organic wet gel sheet material of different thickness through so-gel.After with acetone the replacement such as catalyzer completely of the water in organic wet gel and unreacted being come out, carry out the supercritical solvent displacement, under protection of nitrogen gas,, after activating under the atmosphere of CO2, promptly obtain smooth carbon aerogels thin slice in 1050 ~ C high temperature cabonization.
3, starch pasting method: after starch (analytical pure) and water mixed by a certain percentage, form translucent solution t naturally cooling 90 ℃ of following heated and stirred and promptly get starch gel. use low-concentration ethanol successively behind the starch gel ageing 24h with gained, high concentration ethanol and soaked in absolute ethyl alcohol to gel all becomes hard white solid, promptly get the starch alcogel. the alcogel of gained is put in people's supercritical drying device, supercritical drying, promptly get the starch aerogel, in Nz atmosphere, gained starch aerogel is carried out temperature-programmed pyrolysis, constant temperature 3h in the time of 1300 ℃ promptly gets the carbon aerogels sample behind the naturally cooling.
Summary of the invention
The objective of the invention is to prepare a kind of high specific surface carbon aerogel powder.
The realization the solution of the present invention is to carry out according to the following procedure:
(1) Resorcinol that takes by weighing some amount dissolves with a certain amount of furfural, forms A liquid.
(2) catalyzer, dispersion agent etc. are formed B liquid with a certain amount of alcohol dissolving.Alcohol is monohydroxy-alcohol, particular methanol, ethanol, Virahol, more preferably ethanol or Virahol.
(3) the A drop is added to forms the organosol performed polymer in the B liquid under the whipped state at normal temperatures.
(4) sealed vessel gel under 30-90 ℃ of condition also formed organic alcogel in aging 3-15 days.Between 30-90 ℃ preferred 60-90 ℃ more preferably 70-80 ℃.Sealing refers to can not or seldom have solvent evaporates in gelation process.
(5) open wide sealing and be placed on the 30-80 ℃ of dry down organic aerogel that forms.
(6) this gel is kept 1-3 hour formation carbon aerogels in 700-1100 ℃ of following protection of inert gas.
(7) again with this carbon aerogels and 1-5 highly basic or strong acid admixture activation 1-2 days doubly.Highly basic or strong acid can be KOH, NaOH, Na2CO3 or H3PO4, HNO3 etc.1-5 times, preferred 2-5 times, more preferably 2-4 times, most preferably 3-4 times (weight ratio).
(8) under protection of inert gas in 650-900 ℃ of sintering 1-3 hour.Protection of inert gas can be a kind of in all rare gas elementes such as N2, Ar2.
(9) reduce to room temperature water and be washed till the neutral dry finished product that gets.
It is 1500-3000m2/g that this method has made specific surface; The carbon aerogels of pore volume 0.5-1.5ml/g.
Specific embodiment
The present invention will be further described below in conjunction with specific embodiment.
Example 1
Take by weighing the 2g Resorcinol with the dissolving of 4g furfural, form A liquid, hexamethylenetetramine is dissolved in forms B liquid in the 10ml Virahol again.At normal temperatures the A drop is added to and forms the organosol performed polymer in the B liquid under the whipped state, pour in the sealed vessel under 75 ℃ of conditions gel into and formed organic alcogel in aging 3-15 days, unlimited sealing is placed on 60 ℃ of dry down organic aerogels that form, this gel is kept 2 hours formation carbon aerogels in 900 ℃ of following protection of inert gas, and it is 800m2/g that this method has made specific surface; The carbon aerogels of pore volume 0.65ml/g.
Example 2
Take by weighing the 2g Resorcinol with the dissolving of 4g furfural, form A liquid, hexamethylenetetramine is dissolved in forms B liquid in the 20ml Virahol again.At normal temperatures the A drop is added to and forms the organosol performed polymer in the B liquid under the whipped state, pour in the sealed vessel under 75 ℃ of conditions gel into and formed organic alcogel in aging 3-15 days, unlimited sealing is placed on 60 ℃ of dry down organic aerogels that form, this gel is kept 2 hours formation carbon aerogels in 900 ℃ of following protection of inert gas, and it is 900m2/g that this method has made specific surface; The carbon aerogels of pore volume 0.69ml/g.
Example 3
Take by weighing the 2g Resorcinol with the dissolving of 4g furfural, form A liquid, hexamethylenetetramine is dissolved in forms B liquid in the 20ml Virahol again.At normal temperatures the A drop is added to and forms the organosol performed polymer in the B liquid under the whipped state, pour in the sealed vessel under 75 ℃ of conditions gel into and formed organic alcogel in aging 3-15 days, unlimited sealing is placed on 60 ℃ of dry down organic aerogels that form, this gel is kept 2 hours formation carbon aerogels in 900 ℃ of following protection of inert gas, NaOH with this carbon aerogels and 1:1 activates 24h again, under protection of inert gas in 750 ℃ of sintering 2 hours, reduce to room temperature water and be washed till the neutral dry finished product that gets, it is 1500m2/g that this method has made specific surface; The carbon aerogels of pore volume 0.75ml/g.
Example 4
Take by weighing the 2g Resorcinol with the dissolving of 4g furfural, form A liquid, hexamethylenetetramine is dissolved in forms B liquid in the 20ml Virahol again.At normal temperatures the A drop is added to and forms the organosol performed polymer in the B liquid under the whipped state; pour in the sealed vessel under 75 ℃ of conditions gel into and formed organic alcogel in aging 3-15 days; unlimited sealing is placed on 60 ℃ of dry down organic aerogels that form; this gel is kept 2 hours formation carbon aerogels in 900 ℃ of following protection of inert gas; be the KOH activation 24h of 1:1 with this carbon aerogels and mass ratio again; under protection of inert gas,, reduce to room temperature water and be washed till neutral dry finished product in 750 ℃ of sintering 2 hours.It is 1800m2/g that this method has made specific surface; The carbon aerogels of pore volume 0.95ml/g.
Example 5
Take by weighing the 2g Resorcinol with the dissolving of 4g furfural, form A liquid, hexamethylenetetramine is dissolved in forms B liquid in the 20ml Virahol again.At normal temperatures the A drop is added to and forms the organosol performed polymer in the B liquid under the whipped state; pour in the sealed vessel under 75 ℃ of conditions gel into and formed organic alcogel in aging 3-15 days; unlimited sealing is placed on 60 ℃ of dry down organic aerogels that form; this gel is kept 2 hours formation carbon aerogels in 900 ℃ of following protection of inert gas; be the KOH activation 24h of 1:2 with this carbon aerogels and mass ratio again; under protection of inert gas,, reduce to room temperature water and be washed till neutral dry finished product in 750 ℃ of sintering 2 hours.It is 2000m2/g that this method has made specific surface; The carbon aerogels of pore volume 1.1ml/g.
Example 6
Take by weighing the 2g Resorcinol with the dissolving of 4g furfural, form A liquid, hexamethylenetetramine is dissolved in forms B liquid in the 20ml Virahol again.At normal temperatures the A drop is added to and forms the organosol performed polymer in the B liquid under the whipped state; pour in the sealed vessel under 75 ℃ of conditions gel into and formed organic alcogel in aging 3-15 days; unlimited sealing is placed on 60 ℃ of dry down organic aerogels that form; this gel is kept 2 hours formation carbon aerogels in 900 ℃ of following protection of inert gas; be the KOH activation 24h of 1:3 with this carbon aerogels and mass ratio again; under protection of inert gas,, reduce to room temperature water and be washed till neutral dry finished product in 750 ℃ of sintering 2 hours.It is 2200m2/g that this method has made specific surface; The carbon aerogels of pore volume 1.3ml/g.
Example 7
Take by weighing the 2g Resorcinol with the dissolving of 4g furfural, form A liquid, hexamethylenetetramine is dissolved in forms B liquid in the 20ml Virahol again.At normal temperatures the A drop is added to and forms the organosol performed polymer in the B liquid under the whipped state; pour in the sealed vessel under 75 ℃ of conditions gel into and formed organic alcogel in aging 3-15 days; unlimited sealing is placed on 60 ℃ of dry down organic aerogels that form; this gel is kept 2 hours formation carbon aerogels in 900 ℃ of following protection of inert gas; be the KOH activation 24h of 1:4 with this carbon aerogels and mass ratio again; under protection of inert gas,, reduce to room temperature water and be washed till neutral dry finished product in 750 ℃ of sintering 2 hours.It is 3000m2/g that this method has made specific surface; The carbon aerogels of pore volume 1.5ml/g.
Claims (7)
1. a method for preparing high specific surface carbon aerogel is characterized in that, is undertaken by following step:
(1) Resorcinol that takes by weighing some amount mixes with a certain amount of furfural, forms A liquid.
(2) catalyzer, dispersion agent etc. are formed B liquid with the alcohol dilution.
(3) the B drop is added to forms organic alcosol performed polymer in the A liquid under the whipped state at normal temperatures.
(4) in sealed vessel under 30-90 ℃ of condition gel formed organic alcogel in aging 3-15 days.
(5) sealed vessel is open to the 30-80 ℃ of dry down organic aerogel that forms.
(6) this gel is kept 1-3 hour formation carbon aerogels in 700-1100 ℃ of following protection of inert gas.
(7) highly basic or the strong acid with this carbon aerogels and 1-5 times (weight ratio) activates 1-2 days, is washed to neutral dry.
(8) must high specific surface carbon aerogel under protection of inert gas in 650-900 ℃ of sintering 1-3 hour.
2. alcohol according to claim 1 is characterized in that, employed alcohol is monohydroxy-alcohol, particular methanol, ethanol, Virahol, more preferably ethanol or Virahol.
3. according to claim 1 described between 30-90 ℃ preferred 60-90 ℃ more preferably 70-80 ℃.
4. in gelation process, can not there be or seldom has solvent evaporates according to described in sealed vessel, the referring to of claim 1.
5. highly basic according to claim 1 or strong acid activation can be KOH, NaOH, Na2CO3 or H3PO4, HNO3 or the like.
6. 1-5 according to claim 1 times, preferred 2-5 times, more preferably 2-4 times, most preferably 3-4 times (weight ratio).
7. protection of inert gas according to claim 1 can be, a kind of in all rare gas elementes such as N2, Ar2.
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| CNA2007100509755A CN101468795A (en) | 2007-12-25 | 2007-12-25 | Preparation of high specific surface carbon aerogel |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102826534A (en) * | 2011-06-14 | 2012-12-19 | 北京航空航天大学 | Preparation method of organic aerogel and carbon aerogel |
| CN102874791A (en) * | 2011-07-15 | 2013-01-16 | 同济大学 | Method for preparing hierarchical porous nano carbon materials |
| CN103922328A (en) * | 2014-04-18 | 2014-07-16 | 山东大学 | Method for preparing nitrogenous hierarchical pore three-dimensional graphene by using chitosan |
| CN104627976A (en) * | 2013-11-11 | 2015-05-20 | 天津得瑞丰凯新材料科技有限公司 | Preparation method of meso-porous carbon aerogel with high specific surface area |
| CN105645382A (en) * | 2016-01-12 | 2016-06-08 | 中国工程物理研究院激光聚变研究中心 | Preparation method of wide-spectrum-antireflection-structure carbon aerogel |
| CN106531454A (en) * | 2016-12-29 | 2017-03-22 | 铜陵市胜美达电子制造有限公司 | Ageing-resistant cobaltosic oxide nanowire carbon aerogel composite supercapacitor positive electrode material and preparation method thereof |
| CN106683902A (en) * | 2016-12-29 | 2017-05-17 | 铜陵市胜美达电子制造有限公司 | High-specific-capacity cobaltosic oxide nanowire carbon aerogel hybrid supercapacitor anode material and preparation method thereof |
| CN106829911A (en) * | 2016-09-19 | 2017-06-13 | 广东工业大学 | A kind of porous carbon electrode material and its preparation method and application |
| CN109317063A (en) * | 2018-12-13 | 2019-02-12 | 黑龙江科技大学 | A kind of charcoal-aero gel and preparation method thereof |
| CN109734072A (en) * | 2019-03-11 | 2019-05-10 | 中国科学院合肥物质科学研究院 | A kind of phenolic aldehyde base carbon aerogels material and preparation method thereof |
| CN111540896A (en) * | 2020-05-07 | 2020-08-14 | 七台河万锂泰电材有限公司 | Preparation method of silicon-carbon composite negative electrode material |
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2007
- 2007-12-25 CN CNA2007100509755A patent/CN101468795A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102826534A (en) * | 2011-06-14 | 2012-12-19 | 北京航空航天大学 | Preparation method of organic aerogel and carbon aerogel |
| CN102874791A (en) * | 2011-07-15 | 2013-01-16 | 同济大学 | Method for preparing hierarchical porous nano carbon materials |
| CN104627976A (en) * | 2013-11-11 | 2015-05-20 | 天津得瑞丰凯新材料科技有限公司 | Preparation method of meso-porous carbon aerogel with high specific surface area |
| CN103922328A (en) * | 2014-04-18 | 2014-07-16 | 山东大学 | Method for preparing nitrogenous hierarchical pore three-dimensional graphene by using chitosan |
| CN105645382B (en) * | 2016-01-12 | 2017-06-09 | 中国工程物理研究院激光聚变研究中心 | A kind of preparation method of the carbon aerogels with wide spectrum dimmer reflecting structure |
| CN105645382A (en) * | 2016-01-12 | 2016-06-08 | 中国工程物理研究院激光聚变研究中心 | Preparation method of wide-spectrum-antireflection-structure carbon aerogel |
| CN106829911A (en) * | 2016-09-19 | 2017-06-13 | 广东工业大学 | A kind of porous carbon electrode material and its preparation method and application |
| CN106683902A (en) * | 2016-12-29 | 2017-05-17 | 铜陵市胜美达电子制造有限公司 | High-specific-capacity cobaltosic oxide nanowire carbon aerogel hybrid supercapacitor anode material and preparation method thereof |
| CN106531454A (en) * | 2016-12-29 | 2017-03-22 | 铜陵市胜美达电子制造有限公司 | Ageing-resistant cobaltosic oxide nanowire carbon aerogel composite supercapacitor positive electrode material and preparation method thereof |
| CN109317063A (en) * | 2018-12-13 | 2019-02-12 | 黑龙江科技大学 | A kind of charcoal-aero gel and preparation method thereof |
| CN109734072A (en) * | 2019-03-11 | 2019-05-10 | 中国科学院合肥物质科学研究院 | A kind of phenolic aldehyde base carbon aerogels material and preparation method thereof |
| CN109734072B (en) * | 2019-03-11 | 2022-05-03 | 中国科学院合肥物质科学研究院 | Phenolic-based carbon aerogel material and preparation method thereof |
| CN111540896A (en) * | 2020-05-07 | 2020-08-14 | 七台河万锂泰电材有限公司 | Preparation method of silicon-carbon composite negative electrode material |
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Open date: 20090701 |