CN1480392A - Method for preparing organic aerogel and carbon aerogel by using normal pressure exsiccation - Google Patents
Method for preparing organic aerogel and carbon aerogel by using normal pressure exsiccation Download PDFInfo
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- CN1480392A CN1480392A CNA031398529A CN03139852A CN1480392A CN 1480392 A CN1480392 A CN 1480392A CN A031398529 A CNA031398529 A CN A031398529A CN 03139852 A CN03139852 A CN 03139852A CN 1480392 A CN1480392 A CN 1480392A
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- resorcinol
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- aero gel
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Abstract
A process for preparing the organic aerogel and carbon aerogel by ordinary-pressure drying method includes reaction between resorcin and furaldehyde, in which the hexamethylene tetraamine is used as catalyst and organic reagent (isopropanol) is used as solvent, thermal setting to obtain organic gel, drying or baking to obtain organic aerogel, and charring in inertial gas to obtain carbon aerogel.
Description
Technical field
The present invention relates to the method that a kind of atmosphere pressure desiccation prepares organic aerogel and charcoal-aero gel.
Technical background
Late 1980s, the PekalaR.W. of U.S. Lawrance Livermore National Laboratory prepares RF (resorcinolformaldehyde) organic aerogel first, and charing obtains charcoal-aero gel (carbon aerogel).Charcoal-aero gel is a kind of lightweight nano-porous materials that is linked mutually by spherical nanoparticle, and its porosity is up to 80～98%, typical pore dimension less than 50nm usually, the network particle diameter is about 3～20nm, specific surface area is up to 600～1100m
2g
-1, density is 0.05～0.80g/cm
3Because this unique nanometer network structure, charcoal-aero gel and organic aerogel presoma thereof are with a wide range of applications in the pharmaceutical carrier fields such as [9] of electrode materials [8], artificial creature's histoorgan, medical diagnosis agent and the parenteral admin system of Qie Lunkefu (Cerenkov) detector, specific acoustic resistance coupling material, catalyzer and support of the catalyst, gas filtering material, high efficiency heat insulation material, ultracapacitor, and charcoal-aero gel and organic aerogel thereof also obtain extensive concern in the potential using value of other field.Therefore, under huge industry and commercial benefits driving, charcoal-aero gel and organic aerogel presoma thereof obtain more and more research workers' very big concern.All there is the research group that is engaged in this field for a long time in countries such as the U.S., Germany, Japan, France.At home, units such as Zhongshan University, Dalian University of Technology, Tongji University have also carried out a series of correlative studys.
At present, in order to stop the aerial contraction of organogel, cracked and the block organic aerogel of the organogel structure that is maintained is taked freeze-drying and supercritical drying usually.Freeze-drying can be avoided gas one liquid interface, but can produce at the freezing pt place of solvent the discontinuous density transition district that destroys gel structure and at low temperatures solvent to distil from gel be a slow mass transfer process; And liquid-gas interface disappears under critical condition, surface tension has not existed, do not have the kapillary additional pressure in the gel pore, the original porous network structure of organogel is maintained after drying, thereby obtains to have the block organic aerogel of very high porosities, extremely-low density.Therefore, the supercritical drying drying method generally is considered to the most effective gel drying method.Wherein, with CO
2Supercritical drying is the typical case the most, but makes preparation cycle length consuming time owing to this method needs tediously long exchange of solvent; Subsequently, people have proposed acetone [10], Virahol organic solvent supercritical dryings such as [11] in succession, and these class methods have shortened preparation cycle to a certain extent.Yet, the aerogel product that utilizes supercritical drying to make is extremely expensive, therefore, the someone has proposed with the little big solvent of solvent replacing surface tension of surface tension again, thereby realize the constant pressure and dry [12] of organogel, still, there is the shortcoming of preparation cycle length consuming time equally in solvent replacing, and this method is harsh for the requirement of replacement degree, and this has just increased the difficulty for preparing big block aerogel widely.Therefore how to realize substituting lyophilize and/or supercritical drying process with common drying process (we are referred to as constant pressure and dry), set up the constant pressure and dry new technology and the novel process of a cover aerogel preparation, just become the key that this block extremely-low density nano materials research of promotion is tending towards deeply and moves towards commercialization, industrialization.
Summary of the invention
The object of the present invention is to provide a kind of atmosphere pressure desiccation preparation technology of charcoal-aero gel.This method has gained charcoal-aero gel specific surface area height, and preparation technology is simple, fast, characteristics such as equipment requirements is low, therefore can realize the suitability for industrialized production of charcoal-aero gel.
For achieving the above object, the present invention is a reaction monomers with Resorcinol and furfural, and hexamethylenetetramine is a catalyzer, and organic solvent (being generally Virahol, methyl alcohol or ethanol etc.) is a solvent, in 40 ℃ to the solvent boiling point temperature be heating and curing organogel; Then, directly seasoning or heating, drying get organic aerogel; Afterwards, charing gets the charcoal-aero gel of high-specific surface area in inert atmosphere (as nitrogen, argon gas etc.); Used each material mixture ratio is: the mol ratio of Resorcinol and furfural (R/F) is 0.1～1.0, and the mol ratio of Resorcinol and hexamethylenetetramine (R/H) is 10～100, and the quality of Resorcinol is 0.05～0.5g*cm with the ratio (R/I) of volume of organic solvent
-3
The concrete processing step of the inventive method is:
(1). hexamethylenetetramine is dissolved in organic solvent (Virahol, methyl alcohol or ethanol etc.), Resorcinol is dissolved in furfural, then these two parts of solution are mixed and stir, pour in the reaction flask afterwards and sealing, (be generally 1～10 day) more than 3 days to the temperature between solvent boiling point heating in 40 ℃, obtain organogel;
(2). place the air seasoning (to be generally 2～7 days) more than 3 days the organogel of (1) gained or 40～110 ℃ of heating, dryings (were generally 1～48 hour) more than 5 hours and obtain organic aerogel;
(3). the organic aerogel of (2) gained is placed carbide furnace; rare gas element (being generally purity nitrogen or argon gas)) protection heats down carbonization; carbonization temperature (is generally 600～1100 ℃) more than 600 ℃; carbonization time (was generally 30～180 minutes) more than 60 minutes; naturally cooling cooling afterwards; take out product, obtain charcoal-aero gel.
The prepared charcoal-aero gel of the inventive method contains abundant microporous, mesopore and some macropores, the BET specific surface area up to 550 to 700m
2More than/the g; And preparation technology is simple, quick, equipment requirements is low, can realize the suitability for industrialized production of charcoal-aero gel.
Below the invention will be further described by drawings and Examples.
Description of drawings
Fig. 1 is the SEM figure of the charcoal-aero gel for preparing of the present invention;
Fig. 2 is the TEM figure of the charcoal-aero gel for preparing of the present invention;
Fig. 3 is the nitrogen adsorption isothermal line of some charcoal-aero gels of preparing of the present invention; Wherein the R/F in the prescription of the charcoal-aero gel of WDC60-CA～WDC64-CA is 0.5, and R/I is 0.1g/cm
3, R/H is respectively 25,30,35,40,45.
From Fig. 1～as can be seen shown in Figure 3: the prepared charcoal-aero gel of the present invention contains abundant microporous, mesopore and some macropores, the BET specific surface area up to 550 to 700m
2More than/the g.
Embodiment
Embodiment 1: according to R/F=0.5, R/H=25, R/I=0.1gcm
-3(R/I represents the quality of Resorcinol and the ratio of the volume of Virahol), 0.0509 gram hexamethylenetetramine is dissolved in 10 milliliters Virahol, 1 gram Resorcinol is dissolved in 1.5 milliliters the furfural, then these two parts of solution are mixed and stir, pour in the ampoule afterwards and sealing, reaction obtained organogel in 7 days under 75 ℃; Dry down at 60 ℃ then and obtained organic aerogel in 10 hours; Afterwards, organic aerogel is placed desk-top charring furnace, under the protection of high pure nitrogen, be warming up to 900 ℃ with 5 ℃/minute heating rate from room temperature, constant temperature carbonization 180 minutes, charcoal-aero gel is taken out in cooling cooling naturally.The density that records organic aerogel is 0.226gcm
-3, with theoretical density 0.226gcm
-3Very approaching; The density of charcoal-aero gel is 0.244gcm
-3The BET specific surface area of charcoal-aero gel is 551.28m
2G
-1
Embodiment 2: according to R/F=0.5, R/H=45, R/I=0.1gcm
-30.0283 gram hexamethylenetetramine is dissolved in 10 milliliters Virahol, 1 gram Resorcinol is dissolved in 1.5 milliliters the furfural, then these two parts of solution are mixed and stir, pour in the ampoule afterwards and sealing, in 75 ℃ down reaction obtained organogel in 7 days; Seasoning 3 days and obtain organic aerogel then in 85 ℃ of down about 2 hours of oven dry (or 60 ℃ of directly oven dry 10 hours down); Afterwards, organic aerogel is placed desk-top charring furnace, under the protection of high pure nitrogen, be warming up to 900 ℃ with 5 ℃/minute heating rate from room temperature, constant temperature carbonization 180 minutes, charcoal-aero gel is taken out in cooling cooling naturally.The density that records organic aerogel is 0.239gcm
-3, with theoretical density 0.225gcm
-3Approaching; The density of charcoal-aero gel is 0.282gcm
-3The BET specific surface area of charcoal-aero gel is 660.03m
2G
-1
Embodiment 3: according to R/F=0.5, R/H=50, R/I=0.072g*cm
-30.0254 gram hexamethylenetetramine is dissolved in 13.96 milliliters Virahol, 1 gram Resorcinol is dissolved in 1.5 milliliters the furfural, then these two parts of solution are mixed and stir, pour in the ampoule afterwards and sealing, in 75 ℃ down reaction obtained organogel in 7 days; Directly dry down at 60 ℃ then and obtained organic aerogel in 10 hours; Afterwards, organic aerogel is placed desk-top charring furnace, under the protection of high pure nitrogen, be warming up to 900 ℃ with 5 ℃/minute heating rate from room temperature, constant temperature carbonization 180 minutes, charcoal-aero gel is taken out in cooling cooling naturally.The density that records organic aerogel is 0.238gcm
-3, with theoretical density 0.169gcm
-3Approaching; The density of charcoal-aero gel is 0.223gcm
-3
Embodiment 4: according to R/F=0.5, R/H=50, R/I=0.287 g*cm
-30.0254 gram hexamethylenetetramine is dissolved in 3.49 milliliters Virahol, 1 gram Resorcinol is dissolved in 1.5 milliliters the furfural, then these two parts of solution are mixed and stir, pour in the ampoule afterwards and sealing, in 75 ℃ down reaction obtained organogel in 7 days; Directly dry down at 60 ℃ then and obtained organic aerogel in 10 hours.The density that records organic aerogel is 0.719gcm
-3, with theoretical density 0.475gcm
-3More approaching.
Embodiment 5: according to R/F=0.5, R/H=35, R/I=0.072g*cm
-30.0364 gram hexamethylenetetramine is dissolved in 13.84 milliliters methyl alcohol, 1 gram Resorcinol is dissolved in 1.5 milliliters the furfural, then these two parts of solution are mixed and stir, pour in the ampoule afterwards and sealing, in 50 ℃ down reaction obtained organogel in 7 days; Then seasoning 3 days and 70 ℃ down oven dry obtained organic aerogel in about 2 hours; Afterwards, organic aerogel is placed desk-top charring furnace, under the protection of high pure nitrogen, be warming up to 800 ℃ with 5 ℃/minute heating rate from room temperature, constant temperature carbonization 180 minutes, charcoal-aero gel is taken out in cooling cooling naturally.The density that records organic aerogel is 0.462gcm
-3The density of charcoal-aero gel is 0.422gcm
-3
Embodiment 6: according to R/F=0.5, R/H=35, R/I=0.1gcm
-30.0364 gram hexamethylenetetramine is dissolved in 10 milliliters Virahol, 1 gram Resorcinol is dissolved in 1.5 milliliters the furfural, then these two parts of solution are mixed and stir, pour in the ampoule afterwards and sealing, in 75 ℃ down reaction obtained organogel in 4 days; Directly dry down at 60 ℃ then and obtained organic aerogel in 10 hours.Afterwards, organic aerogel is placed desk-top charring furnace, under the protection of high pure nitrogen, be warming up to 800 ℃ with 5 ℃/minute heating rate from room temperature, constant temperature carbonization 180 minutes, charcoal-aero gel is taken out in cooling cooling naturally.The density that records organic aerogel is 0.260gcm
-3, with theoretical density 0.225gcm
-3Approaching; The density of charcoal-aero gel is 0.270gcm
-3
Embodiment 7: according to R/F=0.5, R/H=35, R/I=0.1gcm
-30.0364 gram hexamethylenetetramine is dissolved in 10 milliliters Virahol, 1 gram Resorcinol is dissolved in 1.5 milliliters the furfural, then these two parts of solution are mixed and stir, pour in the ampoule afterwards and sealing, in 75 ℃ down reaction obtained organogel in 6 days; Directly dry down at 60 ℃ then and obtained organic aerogel in 10 hours.Afterwards, organic aerogel is placed desk-top charring furnace, under the protection of high pure nitrogen, be warming up to 800 ℃ with 5 ℃/minute heating rate from room temperature, constant temperature carbonization 180 minutes, charcoal-aero gel is taken out in cooling cooling naturally.The density that records organic aerogel is 0.253gcm
-3, with theoretical density 0.225gcm
-3Approaching; The density of charcoal-aero gel is 0.268gcm
-3
Embodiment 8: according to R/F=0.5, R/H=35, R/I=0.1gcm
-30.0364 gram hexamethylenetetramine is dissolved in 10 milliliters Virahol, 1 gram Resorcinol is dissolved in 1.5 milliliters the furfural, then these two parts of solution are mixed and stir, pour in the ampoule afterwards and sealing, in 75 ℃ down reaction obtained organogel in 7 days; Directly dry down at 60 ℃ then and obtained organic aerogel in 10 hours.Afterwards, organic aerogel is placed desk-top charring furnace, under the protection of high pure nitrogen, be warming up to 900 ℃ with 5 ℃/minute heating rate from room temperature, constant temperature carbonization 180 minutes, charcoal-aero gel is taken out in cooling cooling naturally.The density that records organic aerogel is 0.238gcm
-3, with theoretical density 0.225gcm
-3Approaching; The density of charcoal-aero gel is 0.227gcm
-3The BET specific surface area of charcoal-aero gel is 678.52m
2G
-1
Embodiment 9: according to R/F=0.5, R/H=30, R/I=0.1gcm
-30.0424 gram hexamethylenetetramine is dissolved in 10 milliliters Virahol, 1 gram Resorcinol is dissolved in 1.5 milliliters the furfural, then these two parts of solution are mixed and stir, pour in the ampoule afterwards and sealing, in 75 ℃ down reaction obtained organogel in 7 days; Dry down at 60 ℃ then and obtained organic aerogel in 10 hours; Afterwards, organic aerogel is placed desk-top charring furnace, under the protection of high pure nitrogen, be warming up to 900 ℃ with 5 ℃/minute heating rate from room temperature, constant temperature carbonization 180 minutes, charcoal-aero gel is taken out in cooling cooling naturally.The density that records organic aerogel is 0.234gcm
-3, with theoretical density 0.226gcm
-3Very approaching; The density of charcoal-aero gel is 0.212gcm
-3The BET specific surface area of charcoal-aero gel is 650.69m
2G
-1
Embodiment 10: according to R/F=0.5, R/H=40, R/I=0.1gcm
-30.0318 gram hexamethylenetetramine is dissolved in 10 milliliters Virahol, 1 gram Resorcinol is dissolved in 1.5 milliliters the furfural, then these two parts of solution are mixed and stir, pour in the ampoule afterwards and sealing, in 75 ℃ down reaction obtained organogel in 7 days; Dry down at 60 ℃ then and obtained organic aerogel in 10 hours; Afterwards, organic aerogel is placed desk-top charring furnace, under the protection of high pure nitrogen, be warming up to 900 ℃ with 5 ℃/minute heating rate from room temperature, constant temperature carbonization 180 minutes, charcoal-aero gel is taken out in cooling cooling naturally.The density that records organic aerogel is 0.218gcm
-3, be slightly less than theoretical density 0.226gcm
-3, but very approaching; The density of charcoal-aero gel is 0.250gcm
-3The BET specific surface area of charcoal-aero gel is 612.32m
2G
-1
Embodiment 11: according to R/F=0.5, R/H=25, R/E=0.2gcm
-3(R/E represents the quality of Resorcinol and the ratio of alcoholic acid volume), 0.0509 gram hexamethylenetetramine is dissolved in 10 milliliters ethanol, 1 gram Resorcinol is dissolved in 1.5 milliliters the furfural, then these two parts of solution are mixed and stir, pour in the ampoule afterwards and sealing, reaction obtained organogel in 7 days under 75 ℃; Dry down at 60 ℃ then and obtained organic aerogel in 10 hours; Afterwards, organic aerogel is placed desk-top charring furnace, under the protection of high pure nitrogen, be warming up to 900 ℃ with 5 ℃/minute heating rate from room temperature, constant temperature carbonization 180 minutes, charcoal-aero gel is taken out in cooling cooling naturally.The density that records organic aerogel is 0.413gcm
-3, be slightly less than theoretical density 0.384gcm
-3, but very approaching; The density of charcoal-aero gel is 0.444gcm
-3The BET specific surface area of organic aerogel is 270.24m
2G
-1, the BET specific surface area of charcoal-aero gel is 545.71m
2G
-1
Embodiment 12: according to R/F=0.5, R/H=25, R/M=0.2gcm
-3(R/M represents the quality of Resorcinol and the ratio of the volume of methyl alcohol), 0.0509 gram hexamethylenetetramine is dissolved in 10 milliliters methyl alcohol, 1 gram Resorcinol is dissolved in 1.5 milliliters the furfural, then these two parts of solution are mixed and stir, pour in the ampoule afterwards and sealing, reaction obtained organogel in 7 days under 75 ℃; Dry down at 60 ℃ then and obtained organic aerogel in 10 hours; Afterwards, organic aerogel is placed desk-top charring furnace, under the protection of high pure nitrogen, be warming up to 900 ℃ with 5 ℃/minute heating rate from room temperature, constant temperature carbonization 180 minutes, charcoal-aero gel is taken out in cooling cooling naturally.The density that records organic aerogel is 0.423gcm
-3, be slightly less than theoretical density 0.384gcm
-3, but very approaching; The density of charcoal-aero gel is 0.458gcm
-3The BET specific surface area of organic aerogel is 236.80m
2G
-1, the BET specific surface area of charcoal-aero gel is 524.75m
2G
-1
Claims (4)
1. an atmosphere pressure desiccation prepares the method for organic aerogel and charcoal-aero gel, is reaction monomers with Resorcinol and furfural, and hexamethylenetetramine is a catalyzer, and organic solvent is a solvent, in 40 ℃ to the solvent boiling point temperature be heating and curing organogel; Then, directly seasoning or heating, drying get organic aerogel; Afterwards, charing gets the charcoal-aero gel of high-specific surface area in inert atmosphere; Used each material mixture ratio is: the mol ratio R/F of Resorcinol and furfural is 0.1～1.0, and the mol ratio R/H of Resorcinol and hexamethylenetetramine is 10～100, and the quality of Resorcinol is 0.05～0.5g*cm with the ratio R/I of volume of organic solvent
-3
2. in accordance with the method for claim 1, it is characterized in that described organic solvent is Virahol, methyl alcohol or ethanol.
3. according to claim 1 or 2 described methods, it is characterized in that concrete processing step is:
(1). hexamethylenetetramine is dissolved in organic solvent, and Resorcinol is dissolved in furfural, then these two parts of solution is mixed and stirs, and pours in the reaction flask afterwards and sealing, in 40 ℃ to the heating of the temperature between the solvent boiling point more than 3 days, obtain organogel;
(2). with the organogel of (1) gained place the air seasoning more than 3 days or 40～110 ℃ of heating, dryings obtain organic aerogel more than 5 hours;
(3). the organic aerogel of (2) gained is placed carbide furnace, heat carbonization under protection of inert gas, carbonization temperature is more than 600 ℃, and carbonization time is more than 60 minutes, and product is taken out in cooling cooling naturally afterwards, obtains charcoal-aero gel.
4. in accordance with the method for claim 3, it is characterized in that step (1) described heat-up time is 1～10 day; The described seasoning time of step (2) is 2～7 days, and the heating, drying time is 1～48 hour; The described carbonization temperature of step (3) is 600～1100 ℃, and carbonization time is 30～180 minutes.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100430312C (en) * | 2006-09-22 | 2008-11-05 | 华东理工大学 | Charcoal aerogel |
| CN102097620A (en) * | 2011-01-13 | 2011-06-15 | 华南师范大学 | Lead-loaded carbon aerogel and preparation method thereof |
| CN102774824A (en) * | 2012-06-11 | 2012-11-14 | 北京化工大学 | Method for preparing graphene crosslinked type organic aerogel and carbon aerogel by normal-pressure drying |
| CN102807357A (en) * | 2012-07-13 | 2012-12-05 | 中国科学院研究生院 | Block aerogel composite material and preparation method thereof |
| CN106013640A (en) * | 2016-05-28 | 2016-10-12 | 湖南细心信息科技有限公司 | Air purification wall cloth |
| CN106560234A (en) * | 2015-10-06 | 2017-04-12 | 河南工业大学 | Method for preparing carbon aerogel by using plant biomorphic material |
| CN107473761A (en) * | 2016-06-08 | 2017-12-15 | 中国科学院金属研究所 | Anti- heat-insulated, integrated charcoal-aero gel/ceramic laminar composite material of carrying of one kind and its preparation method and application |
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| CN108609606A (en) * | 2018-06-25 | 2018-10-02 | 中国人民解放军国防科技大学 | Preparation method of carbon aerogel heat insulation material |
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2003
- 2003-07-18 CN CN 03139852 patent/CN1199854C/en not_active Expired - Fee Related
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100430312C (en) * | 2006-09-22 | 2008-11-05 | 华东理工大学 | Charcoal aerogel |
| CN102097620A (en) * | 2011-01-13 | 2011-06-15 | 华南师范大学 | Lead-loaded carbon aerogel and preparation method thereof |
| CN102774824A (en) * | 2012-06-11 | 2012-11-14 | 北京化工大学 | Method for preparing graphene crosslinked type organic aerogel and carbon aerogel by normal-pressure drying |
| CN102774824B (en) * | 2012-06-11 | 2014-08-20 | 北京化工大学 | Method for preparing graphene crosslinked type organic aerogel and carbon aerogel by normal-pressure drying |
| CN102807357A (en) * | 2012-07-13 | 2012-12-05 | 中国科学院研究生院 | Block aerogel composite material and preparation method thereof |
| CN102807357B (en) * | 2012-07-13 | 2014-04-02 | 中国科学院研究生院 | Block aerogel composite material and preparation method thereof |
| CN106560234B (en) * | 2015-10-06 | 2019-10-25 | 河南工业大学 | A method of state, which is lost, using plant prepares charcoal-aero gel |
| CN106560234A (en) * | 2015-10-06 | 2017-04-12 | 河南工业大学 | Method for preparing carbon aerogel by using plant biomorphic material |
| CN106013640A (en) * | 2016-05-28 | 2016-10-12 | 湖南细心信息科技有限公司 | Air purification wall cloth |
| CN106013640B (en) * | 2016-05-28 | 2018-12-07 | 绍兴艺涵纺织有限公司 | A kind of air purification wall cloth |
| CN107473761A (en) * | 2016-06-08 | 2017-12-15 | 中国科学院金属研究所 | Anti- heat-insulated, integrated charcoal-aero gel/ceramic laminar composite material of carrying of one kind and its preparation method and application |
| CN107473761B (en) * | 2016-06-08 | 2020-07-07 | 中国科学院金属研究所 | Heat-proof and load-bearing integrated carbon aerogel/ceramic layered composite material and preparation method and application thereof |
| CN108039457A (en) * | 2017-11-08 | 2018-05-15 | 西安理工大学 | A kind of preparation method of lithium sulfur battery anode material |
| CN108609606A (en) * | 2018-06-25 | 2018-10-02 | 中国人民解放军国防科技大学 | Preparation method of carbon aerogel heat insulation material |
| CN108609606B (en) * | 2018-06-25 | 2020-03-06 | 中国人民解放军国防科技大学 | Preparation method of carbon aerogel heat insulation material |
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