CN1583555A - Method for preparing carbon gas gel - Google Patents
Method for preparing carbon gas gel Download PDFInfo
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- CN1583555A CN1583555A CN 200410027355 CN200410027355A CN1583555A CN 1583555 A CN1583555 A CN 1583555A CN 200410027355 CN200410027355 CN 200410027355 CN 200410027355 A CN200410027355 A CN 200410027355A CN 1583555 A CN1583555 A CN 1583555A
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Abstract
A process for preparing the organic aerogel and its carbon aerogel includes such steps as reaction between resorcin, formaldehyde, organic surfactant and catalyst in water, thermal solidifying to obtain organic gel, natural cooling or baking to obtain organic aerogel, and charring in inertial gas to obtain carbon aerogel.
Description
Technical field
The present invention relates to the atmosphere pressure desiccation preparation technology of block organic aerogel of a kind of low density and charcoal-aero gel thereof.
Technical background
Because the nano-particle network structure of charcoal-aero gel uniqueness, abundant mesopore, characteristics such as bigger serface and excellent conductive performance, it just is being developed and is being used in electrode, catalyzer and support of the catalyst, gas filtering material, pharmaceutical carrier, infrared ray absorption material and the specific acoustic resistance coupling material of making ultracapacitor, and good market outlook are arranged.So at present, the preparation research of relevant charcoal-aero gel constantly causes people's attention both at home and abroad.Since the eighties in 20th century, Pekala prepared charcoal-aero gel first, existing many preparations, structure and application achievements were delivered.
Yet the problem of charcoal-aero gel existence in preparation is at present seriously restricting its practical application in electrode for capacitors and other fields, also seriously hampers the development of charcoal-aero gel theory and applied research.At present, the charcoal-aero gel technology of comparative maturity is the dry preparation of the CO 2 supercritical technology of preparing of Pekala invention, but this Technology Need experience: " water-sol is synthetic-organic hydrogel-organic solvent exchange-be full of the gel-carbon dioxide exchange of organic solvent-the be full of gel-supercritical drying-organic aerogel-charing-charcoal-aero gel of carbonic acid gas " tediously long like this and complex process, preparation cycle is long, carries out the liquid CO of supercritical drying mass consumption
2, production efficiency is low, and product cost height, the organic solvent of exchange are difficult for reclaiming not environmental protection.Theoretical and the industrial application requirements consideration from synthetic; aspect the preparation of charcoal-aero gel; the technical barrier that people attempt to capture always is exactly to abandon supercritical drying commonly used; and adopt the constant pressure and dry technology to prepare the organogel presoma; could fundamentally simplify the production technique and the production unit of charcoal-aero gel like this, reduce production costs, reduce a large amount of carbonic acid gas and organic solvent emission simultaneously; help protecting environment, thereby promote the mass-producing and the suitability for industrialized production of charcoal-aero gel.
Why the past people will can not prepare the organic aerogel presoma with the constant pressure and dry technology with Supercritical Drying Technology, and its reason is, unsuitable constant pressure and dry can cause the nanoparticle structure of gel to be subsided, and charcoal particulate size and porosity are destroyed.People it is generally acknowledged, cause such result's factor to have two.One can produce huge capillary pressure when being these gel dryings and causes subsiding of granulation mass stack structure; It is more weak that another is that the nanoparticle of these gels piles up formed skeleton.
Summary of the invention
The object of the present invention is to provide the atmosphere pressure desiccation preparation technology of block organic aerogel of a kind of low density and charcoal-aero gel thereof.
For achieving the above object, the present invention is with Resorcinol and formaldehyde (formalin, 37～40wt%) is reaction monomers, organic surface active agent (for example, cetyl trimethylammonium bromide, sodium laurylsulfonate) as emulsifying agent and catalyzer, water is solvent, in be heating and curing between room temperature～100 ℃ hydrogel; 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: Resorcinol (R) is 0.2～1.3 with the mol ratio R/F of formaldehyde (F); The mol ratio R/C of Resorcinol and tensio-active agent (C) is 10～2000; Reactant total concn (RF%) is 10～80wt%.
The concrete processing step of the inventive method is:
(1). Resorcinol, formaldehyde, water and tensio-active agent (catalyzer) are mixed and stir according to predetermined formulation, pour into afterwards in the reaction flask and sealing, (be generally 10 hours～10 days) more than 10 hours in heating between room temperature～100 ℃ and obtain organic hydrogel;
(2). place the air seasoning (to be generally 3～10 days) more than 3 days the organogel of (1) gained or first seasoning is about (was generally 5～24 hours) direct heating oven dry then more than 5 hours and (was generally 1～48 hour) more than 1 hour and obtains organic aerogel.
(3). the organic aerogel of (2) gained is placed carbide furnace, heat carbonization under protection of inert gas, carbonization temperature (is generally 600～1100 ℃) more than 600 ℃; carbonization time (was generally 60～300 ℃) more than 60 minutes; naturally product is taken out in cooling cooling afterwards, obtains charcoal-aero gel.
The invention provides the new way that a hydrogel constant pressure and dry prepares novel charcoal-aero gel.That is, adopt the distribution and the interaction of tensio-active agent emulsion process control monomer and catalyzer, make suitable hydrogel, constant pressure and dry afterwards, charing makes charcoal-aero gel.The gel of this prepared does not shrink (gel particle skeleton collapse phenomenon can not occur) substantially in the constant pressure and dry process, particle size is little, the porosity height, and specific surface area is big.Compared with prior art, technology of the present invention and simple equipments, control is easy, and preparation time shortens, and cost reduces, and helps environmental protection, easier mass-producing and suitability for industrialized production.This is having greatly improved aspect preparation of charcoal-aero gel, plays an important role for the application that promotes charcoal-aero gel.
Principal feature of the present invention is: (1) adopts the water-soluble polymeric monomer; (2) when gel polymerisation, adopt suitable tensio-active agent and control it and the interaction of polymerization single polymerization monomer and catalyzer, thus in the control gelation process nanoparticle size of aerogel precursor body with pile up situation; (3) interaction between the enhanced granule improves gel skeleton intensity, reduces capillary pressure; (4) the constant pressure and dry hydrogel prepares the charcoal-aero gel presoma.
Prepared organic aerogel of the present invention and charcoal-aero gel thereof contain abundant mesopore, micropore and some macropores, and the BET specific surface area is up to 700m
2G
-1, mesopore volume is up to 1.2cm
3G
-1And 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 organic aerogel for preparing of the present invention;
Fig. 2 is the SEM figure of the charcoal-aero gel for preparing of the present invention;
Fig. 3 is some organic aerogels that prepare of the present invention and the nitrogen adsorption isothermal line of charcoal-aero gel thereof; Wherein the prescription of RFA-42, RFA-43 is respectively R/F=0.5, RF%=40wt%, R/C=100,200 (C is a cetyl trimethylammonium bromide), and CA-42 and CA-43 are respectively the charcoal-aero gel that organic aerogel RFA-42 and RFA-43 charing obtain.
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, and the BET specific surface area is up to 700m
2G
-1, mesopore volume is up to 1.2cm
3G
-1, the network particle diameter is about 20～50 nanometers.
Embodiment
Embodiment 1: according to R/F=0.5, R/C=100 (C is a cetyl trimethylammonium bromide), RF%=40wt%, with 1 gram Resorcinol, 1.26 milliliters of formalin (37～40wt%, this paper calculates prescription with 38.5wt%), 0.0331 gram cetyl trimethylammonium bromide and 1.46 ml distilled waters mix and stir, pour in the ampoule afterwards and sealing, reaction obtained organogel in 5 days under 85 ℃; Seasoning half a day, infrared lamp oven dry (about 60 ℃ of drying position) 5 hours in air then, put into the last drying and dewatering of baking oven (110 ℃) 5 hours subsequently, obtain organic aerogel.The density that records organic aerogel is 0.452gcm
-3, with theoretical density 0.449gcm
-3Very approaching; The BET specific surface area is 282m
2G
-1m
2G
-1, mesopore volume 1.1cm
3G
-1, the mesopore aperture is about 18nm.
Embodiment 2: according to R/F=0.5, R/C=200 (C is a sodium laurylsulfonate), RF%=40wt%, 1 gram Resorcinol, 1.26 milliliters of formalins, 0.0124 gram sodium laurylsulfonate and 1.46 ml distilled waters are mixed and stir, pour in the ampoule afterwards and sealing, reaction obtained organogel in 1 day under 85 ℃; Seasoning 1 day in air then, infrared lamp are dried (about 60 ℃ of drying position) 5 hours, were put into the last drying and dewatering of baking oven (110 ℃) 5 hours subsequently, obtain organic aerogel.The density that records organic aerogel is 0.452gcm
-3, with theoretical density 0.448gcm
-3Very approaching.The BET specific surface area is 227m
2G
-1, mesopore volume 0.52cm
3G
-1, mean pore size 10.6nm.
Embodiment 3: according to R/F=0.5, R/C=100 (C is a Tetrabutyl amonium bromide), RF%=40wt%, 1 gram Resorcinol, 1.26 milliliters of formalins, 0.0293 gram Tetrabutyl amonium bromide and 1.46 ml distilled waters are mixed and stir, pour in the ampoule afterwards and sealing, reaction obtained organogel in 5 days under 85 ℃; Seasoning half a day, infrared lamp oven dry (about 60 ℃ of drying position) 5 hours in air then, put into the last drying and dewatering of baking oven (110 ℃) 5 hours subsequently, obtain organic aerogel.The density that records organic aerogel is 0.559gcm
-3, with theoretical density 0.448gcm
-3More approaching.
Embodiment 4: according to R/F=0.5, R/C=200 (C is a cetyl trimethylammonium bromide), RF%=40wt%, 1 gram Resorcinol, 1.26 milliliters of formalins, 0.0165 gram cetyl trimethylammonium bromide and 1.46 ml distilled waters are mixed and stir, pour in the ampoule afterwards and sealing, reaction obtained organogel in 5 days under 85 ℃; Seasoning more than 5 hours in air then, infrared lamp oven dry (about 60 ℃ of drying position) 5 hours, put into the last drying and dewatering of baking oven (110 ℃) 5 hours subsequently; obtain organic aerogel; 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 0.434gcm
-3, with theoretical density 0.447gcm
-3Very approaching, the BET specific surface area is 228m
2G
-1, mesopore volume 0.67cm
3G
-1The density of charcoal-aero gel is 0.504gcm
-3, the charing yield is 49%, the BET specific surface area is 682m
2G
-1, mesopore volume 1.2cm
3G
-1
Embodiment 5: according to R/F=0.5, R/C=1000 (C is a cetyl trimethylammonium bromide), RF%=40wt%, with 1 gram Resorcinol, 1.26 milliliters of formalins, (autogamy of 0.33 milliliter of cetyl trimethylammonium bromide aqueous solution, concentration is 1wt%) and 1.13 ml distilled waters mix and stir, pour in the ampoule afterwards and sealing, reaction obtained organogel in 5 days under 85 ℃; Dry (about 60 ℃ of drying position) 5 hours, put into the last drying and dewatering of baking oven (110 ℃) 5 hours subsequently at infrared lamp then; obtain organic aerogel; 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 0.417gcm
-3, with theoretical density 0.444gcm
-3Very approaching, the BET specific surface area is 54m
2G
-1The density of charcoal-aero gel is 0.388gcm
-3, the charing yield is 45.6%, the BET specific surface area is 777m
2G
-1
Embodiment 6: according to R/F=0.8, R/C=200 (C is a cetyl trimethylammonium bromide), RF%=40wt%, 1 gram Resorcinol, 0.79 milliliter of formalin, 0.0165 gram cetyl trimethylammonium bromide and 1.46 ml distilled waters are mixed and stir, pour in the ampoule afterwards and sealing, reaction obtained organogel in 7 days under 75 ℃; Seasoning more than 5 hours in air then, infrared lamp oven dry (about 60 ℃ of drying position) 5 hours, put into the last drying and dewatering of baking oven (110 ℃) 5 hours subsequently, obtain organic aerogel.The density that records organic aerogel is 0.520gcm
-3, with theoretical density 0.451gcm
-3More approaching.
Embodiment 7: according to R/F=0.5, R/C=200 (C is a cetyl trimethylammonium bromide), RF%=40wt%, 1 gram Resorcinol, 1.26 milliliters of formalins, 0.0165 gram cetyl trimethylammonium bromide and 1.46 ml distilled waters are mixed and stir, pour in the ampoule afterwards and sealing, reaction obtained organogel in 1 day under 75 ℃; Seasoning 1 day in air then, infrared lamp are dried (about 60 ℃ of drying position) 5 hours, were put into the last drying and dewatering of baking oven (110 ℃) 5 hours subsequently, obtain organic aerogel.The density that records organic aerogel is 0.478gcm
-3, with theoretical density 0.447gcm
-3Very approaching.
Embodiment 8: according to R/F=0.5, R/C=200 (C is a cetyl trimethylammonium bromide), RF%=40wt%, 1 gram Resorcinol, 1.26 milliliters of formalins, 0.0165 gram cetyl trimethylammonium bromide and 1.46 ml distilled waters are mixed and stir, pour in the ampoule afterwards and sealing, reaction obtained organogel in 13 days under 75 ℃; Seasoning half a day, infrared lamp oven dry (about 60 ℃ of drying position) 5 hours in air then, put into the last drying and dewatering of baking oven (110 ℃) 5 hours subsequently, obtain organic aerogel.The density that records organic aerogel is 0.474gcm
-3, with theoretical density 0.447gcm
-3Very approaching.
Embodiment 9: according to R/F=0.5, R/C=500 (C is a cetyl trimethylammonium bromide), RF%=30wt%, 1 gram Resorcinol, 1.26 milliliters of formalins, 0.0066 gram cetyl trimethylammonium bromide and 2.73 ml distilled waters are mixed and stir, pour in the ampoule afterwards and sealing, reaction obtained organogel in 5 days under 85 ℃; Seasoning half a day, infrared lamp oven dry (about 60 ℃ of drying position) 5 hours in air then, put into the last drying and dewatering of baking oven (110 ℃) 5 hours subsequently, obtain organic aerogel.The density that records organic aerogel is 0.413gcm
-3, with theoretical density 0.325gcm
-3More approaching.
Embodiment 10: according to R/F=0.5, R/C=500 (C is a cetyl trimethylammonium bromide), RF%=60wt%, 1 gram Resorcinol, 1.26 milliliters of formalins, 0.0066 gram cetyl trimethylammonium bromide and 0.17 ml distilled water are mixed and stir, pour in the ampoule afterwards and sealing, reaction obtained organogel in 5 days under 85 ℃; Seasoning half a day, infrared lamp oven dry (about 60 ℃ of drying position) 5 hours in air then, put into the last drying and dewatering of baking oven (110 ℃) 5 hours subsequently, obtain organic aerogel.The density that records organic aerogel is 0.766gcm
-3, with theoretical density 0.708gcm
-3More approaching.
Claims (5)
1. a method for preparing charcoal-aero gel is a reaction monomers with Resorcinol and formaldehyde, and organic surface active agent is as emulsifying agent and catalyzer, and water is solvent, in be heating and curing between room temperature to 100 ℃ hydrogel; Direct seasoning of this hydrogel or heating, drying are got organic aerogel; The charing in inert atmosphere of this organic aerogel is got required charcoal-aero gel; Used each material mixture ratio is: the mol ratio R/F of Resorcinol and formaldehyde is 0.2～1.3; The mol ratio R/C of Resorcinol and organic surface active agent is 10～2000; Reactant total concn RF% is 10～80wt%.
2. in accordance with the method for claim 1, it is characterized in that described formaldehyde is the formalin of 37～40wt%.
3. in accordance with the method for claim 1, it is characterized in that described organic surface active agent is cetyl trimethylammonium bromide or sodium laurylsulfonate.
4. according to the described method of claim 1,2 or 3, it is characterized in that concrete processing step is:
(1). Resorcinol, formaldehyde, water and organic surface active agent are mixed and stir according to predetermined formulation, pour in the reaction flask afterwards and sealing, more than 10 hours, obtain organic hydrogel in heating between room temperature to 100 ℃;
(2). place the air seasoning more than 3 days organic hydrogel of (1) gained, perhaps first seasoning more than 5 hours then heating, drying obtain organic aerogel more than 1 hour;
(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 cooling cooling naturally obtains charcoal-aero gel afterwards.
5. in accordance with the method for claim 4, it is characterized in that step (1) described heat-up time is 10 hours to 10 days; The seasoning time before the described heating, drying of step (2) is 5 hours to 10 days, and the heating, drying time is 1～48 hour; The described carbonization temperature of step (3) is 600～1100 ℃, and carbonization time is 60～300 minutes.
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| CN100430312C (en) * | 2006-09-22 | 2008-11-05 | 华东理工大学 | Charcoal aerogel |
| CN100450938C (en) * | 2006-04-21 | 2009-01-14 | 中山大学 | Method for preparing globular silver carried organic aerogel and carbon aerogel particle |
| CN102302917A (en) * | 2011-07-18 | 2012-01-04 | 南京工业大学 | Preparation method of bulk C-Al2O3 composite aerogel |
| CN102423668A (en) * | 2011-09-09 | 2012-04-25 | 中国人民解放军国防科学技术大学 | Preparation method of phenolic resin base carbon aerogel |
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| CN100450938C (en) * | 2006-04-21 | 2009-01-14 | 中山大学 | Method for preparing globular silver carried organic aerogel and carbon aerogel particle |
| CN100430312C (en) * | 2006-09-22 | 2008-11-05 | 华东理工大学 | Charcoal aerogel |
| CN102302917A (en) * | 2011-07-18 | 2012-01-04 | 南京工业大学 | Preparation method of bulk C-Al2O3 composite aerogel |
| CN102302917B (en) * | 2011-07-18 | 2013-09-04 | 南京工业大学 | Preparation method of bulk C-Al2O3 composite aerogel |
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| CN102513041A (en) * | 2011-12-26 | 2012-06-27 | 南京工业大学 | Method for preparing high-strength and high-temperature-resistance carbon-supported Al2O3-Al4C3 composite blocky aerogel |
| CN103682379B (en) * | 2012-09-07 | 2016-08-03 | 中国科学院大连化学物理研究所 | A kind of fuel cell metal-doped nitrogenous carbon base catalyst and application thereof |
| CN103682379A (en) * | 2012-09-07 | 2014-03-26 | 中国科学院大连化学物理研究所 | Metal-doped nitrogen-containing carbon-based catalyst of fuel cell and application thereof |
| CN104755419A (en) * | 2012-10-17 | 2015-07-01 | 哈金森公司 | Thermally insulating composition for organic monolithic gel, use thereof and process for preparing same |
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| CN112358586A (en) * | 2020-11-10 | 2021-02-12 | 中钢集团马鞍山矿山研究总院股份有限公司 | Low-cost preparation method of carbon aerogel precursor |
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