CN102515143A - Nano-grade porous aerogel and preparation method thereof - Google Patents
Nano-grade porous aerogel and preparation method thereof Download PDFInfo
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- CN102515143A CN102515143A CN2011104377605A CN201110437760A CN102515143A CN 102515143 A CN102515143 A CN 102515143A CN 2011104377605 A CN2011104377605 A CN 2011104377605A CN 201110437760 A CN201110437760 A CN 201110437760A CN 102515143 A CN102515143 A CN 102515143A
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Abstract
The invention provides nano-grade porous aerogel and a preparation method thereof. The method comprises steps of organic wet gel preparing, solvent replacing, normal-pressure drying, and high-temperature carbonizing. With the method, the prepared nano-grade porous aerogel has parameters of: a pore size distribution of 1-2nm, a specific surface area of 850-900m<2>/g, a porosity of 81-89%, a density of 280-325mg/cm<3>, and an electrical resistivity of 0.045-0.06ohm*mm. The method provided by the invention is advantaged in that: with the method for preparing the nano-grade porous aerogel, the prepared nano-grade porous aerogel is characterized by high specific surface area, high porosity, high density, and low electrical resistivity. The aerogel can be widely applied in fields of super-capacitor electrodes, catalysts, catalyst carriers, gas absorption, and the like. The aerogel has a good market prospect. The preparation process is simple, convenient, and easy to operate. The production period is short, the requirement on equipment is low, and the aerogel and the method are environment friendly.
Description
Technical field
The present invention relates to a kind of carbon aerogels, especially relate to a kind of nanoporous carbon aerogels and preparation method thereof.
Background technology
Carbon aerogels is a kind of novel nano porous carbon material with crosslinked shape structure that is generated through the solid phase carburizing reagent by organic aerogel; It is unique gas gel with electroconductibility and chemicalstability; Its variable density scope is wide, Adjustable structure, and porosity reaches 80%-99.8%; The aperture is general＜50nm, and specific surface area is up to 400-1000m
2/ g.The material of this special construction is with a wide range of applications.1987, U.S. Pekala was a raw material with Resorcinol-formaldehyde first, and through sol-gel process, pickling is aging under the base catalysis condition, and supercritical drying and carbonization get organic aerogel and carbon aerogels, and this indicates the beginning of organic aerogel research.Between the more than ten years subsequently, various countries investigators such as the U.S., Japan, Germany, France show great interest to this research topic, and are in the ascendant about the research of gas gel, and existing at home and abroad multinomial preparation about carbon aerogels, application achievements are delivered.
At present comparatively sophisticated carbon aerogels preparation method is that the U.S. Patent number that the people invented such as Pekala is US19890406009; US19880199404; But this preparation method need pass through tediously long and complicated preparation cycle; The dry technology of preparing of the CO 2 supercritical of taking has increased production cost greatly, and not environmental protection, has restricted the industrialization production of carbon aerogels and application widely comprehensively.By patent " carbon-gas gel powder and preparation method thereof " Chinese patent of people such as Wang Zhaoyang invention number is CN200610021241.X; Adopted the ethanol supercritical drying equally; And adopt the low temperature ultrasonic technique, it is low fundamentally not solve production efficiency, the restraining factors that cost is too high.And the patent " a kind of method for preparing carbon aerogels " of Zhu Zhen equality people invention, Chinese patent number be CN01120419.2, because introducing is heated blast process and made and exist unsafe factor in the preparation process in preparation technology.
Summary of the invention
The problem that the present invention will solve provides a kind of preparation cycle weak point, saving cost, safety and environmental protection, specific surface area height; Porosity is high; Density is low; Resistivity is low, can be widely used in the nanoporous carbon aerogels in fields such as electrode of super capacitor, catalyzer and support of the catalyst, gas adsorption and preparation method thereof.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: a kind of preparation method of nanoporous carbon aerogels comprises the steps:
1) organic wet gel preparation: with reactant Resorcinol and formaldehyde, be 1/2 mixed, add the de-ionized water as solvent again with mol ratio; Being made into mass percent and being 30% reaction solution, is that the sodium carbonate solution of 0.05mol/L is a catalyzer with the volumetric molar concentration, after stirring; Sealing is inserted in the baking oven, in the time of 30 ℃, handles 1 day respectively; Handled 1 day in the time of 50 ℃, handled 3 days in the time of 90 ℃, make Resorcinol-formaldehyde wet gel at last;
2) solvent replacing: the Resorcinol-formaldehyde wet gel of step 1) preparation is immersed in carries out solvent replacing in the acetone; Whenever changed an acetone during this time at a distance from 24 hours; Replace 2 times-5 times, treat that acetone volatilizees fully naturally after, promptly make Resorcinol-formaldehyde organic aerogel;
3) constant pressure and dry: at normal temperatures and pressures, promptly temperature is at 20-30 ℃, and a standard atmosphere is depressed and carried out drying, let acetone volatilize naturally clean after, promptly make exsiccant Resorcinol-formaldehyde organic aerogel;
4) high temperature cabonization: at normal temperatures, promptly temperature is under 20-30 ℃, with the exsiccant Resorcinol-formaldehyde organic aerogel of the step 3) preparation silica tube of packing into; Be placed in the High Temperature Furnaces Heating Apparatus; In stove, feeding earlier 30-50 minute nitrogen, in the whole process of charing is that the speed of 20ml/min-60ml/min constantly feeds inertia protection gas with speed, be warmed up to 1045-1055 ℃ after constant temperature 4-6 hour; Slowly be cooled to normal temperature again, promptly make the nanoporous carbon aerogels of black.
Said step 2) to thoroughly replace water and other impurity in Resorcinol-formaldehyde wet gel.
Said step 4) fed nitrogen earlier before feeding inertia protection gas purpose is to prevent exsiccant Resorcinol-formaldehyde organic aerogel oxidation for the air in the emptying silica tube.
Said inertia protection gas is any one in helium, neon, argon gas, krypton gas, xenon or the radon gas.
Preferably, in order to reach better effect, said step 4) feeds 30 minutes nitrogen earlier in stove.
Preferably, in order to reach better effect, constant temperature was 4 hours after said step 4) was warmed up to 1050 ℃.
Said nanoporous carbon aerogels makes according to aforesaid method, and it possesses following parameter:
Pore size distribution 1nm-2nm, specific surface area 850m
2/ g-900m
2/ g, porosity 81%-89%, density 280mg/cm
3-325mg/cm
3, resistivity 0.045 Ω mm-0.06 Ω mm.
Advantage and positively effect that the present invention has are: owing to adopt technique scheme, the present invention is a raw material with Resorcinol and formaldehyde, and yellow soda ash is catalyzer, adopts sol-gel method to prepare organic wet gel; Aging wet gel under suitable temperature control; Through solvent replacing, preparation organic aerogel under normal temperature and pressure conditions; Through suitable charring process, the carbon aerogels that the preparation pore space structure is not damaged basically through the method for preparing the nanoporous carbon aerogels provided by the present invention, has the specific surface area height; Porosity is high, and density is low, and resistivity is low; Can be widely used in fields such as electrode of super capacitor, catalyzer and support of the catalyst, gas adsorption, good market outlook are arranged, its preparation process is simple, convenient, easy to operate; With short production cycle, equipment requirements is low, environmental friendliness.
Description of drawings
Fig. 1 is the SEM figure of nanoporous carbon aerogels of the present invention, 10000 times of figure of magnification
Fig. 2 is the graph of pore diameter distribution that the BJH method of the prepared nanoporous carbon aerogels of the present invention is calculated
Fig. 3 is the graph of pore diameter distribution that the DFT method of the prepared nanoporous carbon aerogels of the present invention is calculated
Embodiment
Below in conjunction with specific embodiment nanoporous carbon aerogels of the present invention and preparation method thereof is described further.
Embodiment one
1) organic wet gel preparation: with reactant Resorcinol and formaldehyde, be 1/2 mixed, add the de-ionized water as solvent again with mol ratio; Being made into mass percent and being 30% reaction solution, is that the sodium carbonate solution of 0.05mol/L is a catalyzer with the volumetric molar concentration, after stirring; Sealing is inserted in the baking oven, in the time of 30 ℃, handles 1 day respectively; Handled 1 day in the time of 50 ℃, handled 3 days in the time of 90 ℃, make Resorcinol-formaldehyde wet gel at last;
2) solvent replacing: the Resorcinol-formaldehyde wet gel of step 1) preparation is immersed in carries out solvent replacing in the acetone, during whenever changed an acetone at a distance from 24 hours, replace 3 times, treat acetone volatilize naturally complete after, promptly make Resorcinol-formaldehyde organic aerogel;
3) constant pressure and dry: at normal temperatures and pressures, promptly temperature is at 20-30 ℃, and a standard atmosphere is depressed and carried out drying, let acetone volatilize naturally clean after, promptly make exsiccant Resorcinol-formaldehyde organic aerogel;
4) high temperature cabonization: at normal temperatures, promptly temperature is under 20-30 ℃, with the exsiccant Resorcinol-formaldehyde organic aerogel of the step 3) preparation silica tube of packing into; Be placed in the High Temperature Furnaces Heating Apparatus; In stove, feeding earlier 30 minutes nitrogen, in the whole process of charing is that the speed of 25ml/min constantly feeds helium with speed, be warmed up to 1050 ℃ after constant temperature 4 hours; Slowly be cooled to normal temperature again, promptly make the nanoporous carbon aerogels of black.
Prepared nanoporous carbon aerogels, aperture are concentrated and are distributed in 1.4nm, even structure and stable, specific surface area 865.1m
2/ g, porosity 83.89%, density 306mg/cm
3, resistivity 0.055 Ω mm.
Embodiment 2
1) organic wet gel preparation: with reactant Resorcinol and formaldehyde, be 1/2 mixed, add the de-ionized water as solvent again with mol ratio; Being made into mass percent and being 32% reaction solution, is that the sodium carbonate solution of 0.05mol/L is a catalyzer with the volumetric molar concentration, after stirring; Sealing is inserted in the baking oven, in the time of 30 ℃, handles 1 day respectively; Handled 1 day in the time of 50 ℃, handled 3 days in the time of 90 ℃, make Resorcinol-formaldehyde wet gel at last;
2) solvent replacing: the Resorcinol-formaldehyde wet gel of step 1) preparation is immersed in carries out solvent replacing in the acetone, during whenever changed an acetone at a distance from 24 hours, replace 4 times, treat acetone volatilize naturally complete after, promptly make Resorcinol-formaldehyde organic aerogel;
3) constant pressure and dry: at normal temperatures and pressures, promptly temperature is at 20-30 ℃, and a standard atmosphere is depressed and carried out drying, let acetone volatilize naturally clean after, promptly make exsiccant Resorcinol-formaldehyde organic aerogel;
4) high temperature cabonization: at normal temperatures, promptly temperature is under 20-30 ℃, with the exsiccant Resorcinol-formaldehyde organic aerogel of the step 3) preparation silica tube of packing into; Be placed in the High Temperature Furnaces Heating Apparatus; In stove, feeding earlier 40 minutes nitrogen, in the whole process of charing is that the speed of 35ml/min constantly feeds neon with speed, be warmed up to 1052 ℃ after constant temperature 5 hours; Slowly be cooled to normal temperature again, promptly make the nanoporous carbon aerogels of black.
Prepared nanoporous carbon aerogels, aperture are concentrated and are distributed in 1.2nm, even structure and stable, specific surface area 860.1m
2/ g, porosity 82.89%, density 320mg/cm
3, resistivity 0.051 Ω mm.
Embodiment 3
1) organic wet gel preparation: with reactant Resorcinol and formaldehyde, be 1/2 mixed, add the de-ionized water as solvent again with mol ratio; Being made into mass percent and being 33% reaction solution, is that the sodium carbonate solution of 0.05mol/L is a catalyzer with the volumetric molar concentration, after stirring; Sealing is inserted in the baking oven, in the time of 30 ℃, handles 1 day respectively; Handled 1 day in the time of 50 ℃, handled 3 days in the time of 90 ℃, make Resorcinol-formaldehyde wet gel at last;
2) solvent replacing: the Resorcinol-formaldehyde wet gel of step 1) preparation is immersed in carries out solvent replacing in the acetone, during whenever changed an acetone at a distance from 24 hours, replace 5 times, treat acetone volatilize naturally complete after, promptly make Resorcinol-formaldehyde organic aerogel;
3) constant pressure and dry: at normal temperatures and pressures, promptly temperature is at 20-30 ℃, and a standard atmosphere is depressed and carried out drying, let acetone volatilize naturally clean after, promptly make exsiccant Resorcinol-formaldehyde organic aerogel;
4) high temperature cabonization: at normal temperatures, promptly temperature is under 20-30 ℃, with the exsiccant Resorcinol-formaldehyde organic aerogel of the step 3) preparation silica tube of packing into; Be placed in the High Temperature Furnaces Heating Apparatus; In stove, feeding earlier 40 minutes nitrogen, in the whole process of charing is that the speed of 35ml/min constantly feeds argon gas with speed, be warmed up to 1055 ℃ after constant temperature 6 hours; Slowly be cooled to normal temperature again, promptly make the nanoporous carbon aerogels of black.
Prepared nanoporous carbon aerogels, aperture are concentrated and are distributed in 1.2nm, even structure and stable, specific surface area 858.1m
2/ g, porosity 81.69%, density 325mg/cm
3, resistivity 0.045 Ω mm.
More than three embodiment of the present invention are specified, but said content is merely preferred embodiment of the present invention, can not be considered to be used to limit practical range of the present invention.All equalizations of doing according to application range of the present invention change and improve etc., all should still belong within the patent covering scope of the present invention.
Claims (5)
1. the preparation method of a nanoporous carbon aerogels is characterized in that: comprise the steps:
1) organic wet gel preparation: with reactant Resorcinol and formaldehyde, be 1/2 mixed, add the de-ionized water as solvent again with mol ratio; Being made into the reaction solution that mass percent is 30%-33%, is that the sodium carbonate solution of 0.05mol/L is a catalyzer with the volumetric molar concentration, after stirring; Sealing is inserted in the baking oven, in the time of 30 ℃, handles 1 day respectively; Handled 1 day in the time of 50 ℃, handled 3 days in the time of 90 ℃, make Resorcinol-formaldehyde wet gel at last;
2) solvent replacing: the Resorcinol-formaldehyde wet gel of step 1) preparation is immersed in carries out solvent replacing in the acetone; Whenever changed an acetone during this time at a distance from 24 hours; Replace 2 times-5 times, treat that acetone volatilizees fully naturally after, promptly make Resorcinol-formaldehyde organic aerogel;
3) constant pressure and dry: carry out drying at normal temperatures and pressures, let acetone volatilize naturally clean after, promptly make exsiccant Resorcinol-formaldehyde organic aerogel;
4) high temperature cabonization: at normal temperatures; With the exsiccant Resorcinol-formaldehyde organic aerogel of the step 3) preparation silica tube of packing into, be placed in the High Temperature Furnaces Heating Apparatus, in stove, feed 30-50 minute nitrogen earlier; The speed that with speed is 20ml/min-60ml/min in the whole process of charing constantly feeds inertia protection gas; Constant temperature 4-6 is individual hour after being warmed up to 1045-1055 ℃, slowly is cooled to normal temperature again, promptly makes the nanoporous carbon aerogels of black.
2. the preparation method of nanoporous carbon aerogels according to claim 1 is characterized in that: said inertia protection gas is any one in helium, neon, argon gas, krypton gas, xenon or the radon gas.
3. the preparation method of nanoporous carbon aerogels according to claim 1 is characterized in that: said step 4) feeds 30 minutes nitrogen earlier in stove.
4. the preparation method of nanoporous carbon aerogels according to claim 1 is characterized in that: constant temperature was 4 hours after said step 4) was warmed up to 1050 ℃.
5. a nanoporous carbon aerogels is characterized in that: prepare according to each described method of claim 1-4.
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103058171A (en) * | 2013-01-07 | 2013-04-24 | 航天材料及工艺研究所 | Preparation method of filled high-heat-conduction foamy carbon material for energy storage |
| CN103551091A (en) * | 2013-11-25 | 2014-02-05 | 北京化工大学 | Method for drying aerogel |
| CN103933900A (en) * | 2014-04-22 | 2014-07-23 | 中国工程物理研究院激光聚变研究中心 | Method for preparing resorcinol-formaldehyde aerogel |
| CN104549142A (en) * | 2013-10-11 | 2015-04-29 | 天津得瑞丰凯新材料科技有限公司 | Nanometer porous carbon aerogel dry-wet balance preparation and preparation method thereof |
| CN106044740A (en) * | 2016-05-25 | 2016-10-26 | 天津晨祥丰凯新材料科技有限公司 | Porous carbon nanomaterial and preparation method therefor |
| CN106542517A (en) * | 2016-12-06 | 2017-03-29 | 绵阳泛博新材料科技有限公司 | The preparation method of carbon aerogels |
| CN106976864A (en) * | 2017-05-22 | 2017-07-25 | 河北省科学院能源研究所 | A kind of micropore carbon aerogels and preparation method thereof |
| CN107473199A (en) * | 2016-06-08 | 2017-12-15 | 中国科学院金属研究所 | A kind of high intensity large scale bulk charcoal-aero gel and its preparation method and application |
| CN107761124A (en) * | 2017-10-23 | 2018-03-06 | 大连理工大学 | A kind of preparation method and application for carrying silver-colored carbon aerogels |
| CN108440899A (en) * | 2018-03-26 | 2018-08-24 | 中国科学技术大学 | Phenolic resin aerogel and carbon aerogels material with Nanofiber Network structure and preparation method thereof |
| CN108975300A (en) * | 2017-06-02 | 2018-12-11 | 中国科学院金属研究所 | High-intensitive large scale bulk charcoal-aero gel and its preparation method and application |
| CN109289814A (en) * | 2018-10-16 | 2019-02-01 | 大连工业大学 | It is a kind of for adsorbing the magnetic carbon aerogels and preparation method thereof of antibiotic in waste water |
| CN109786120A (en) * | 2019-01-25 | 2019-05-21 | 内蒙古科技大学 | Utilize the method for ionic liquid preparation metal/carbon aeroge composite nano materials |
| CN110170322A (en) * | 2019-06-21 | 2019-08-27 | 天津大学 | A kind of preparation method for the platinum/carbon aerogel catalyst loading atom level noble metal |
| CN111498828A (en) * | 2020-04-15 | 2020-08-07 | 贵州梅岭电源有限公司 | Method for preparing carbon aerogel by utilizing normal-pressure drying |
| CN113429182A (en) * | 2021-06-23 | 2021-09-24 | 武汉纺织大学 | Carbon aerogel cement brick and preparation method thereof |
-
2011
- 2011-12-23 CN CN2011104377605A patent/CN102515143A/en active Pending
Non-Patent Citations (1)
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| 沈军等: "纳米多孔碳气凝胶的储氢性能", 《强激光与粒子束》 * |
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| CN103058171A (en) * | 2013-01-07 | 2013-04-24 | 航天材料及工艺研究所 | Preparation method of filled high-heat-conduction foamy carbon material for energy storage |
| CN103058171B (en) * | 2013-01-07 | 2014-11-19 | 航天材料及工艺研究所 | Preparation method of filled high-heat-conduction foamy carbon material for energy storage |
| CN104549142A (en) * | 2013-10-11 | 2015-04-29 | 天津得瑞丰凯新材料科技有限公司 | Nanometer porous carbon aerogel dry-wet balance preparation and preparation method thereof |
| CN103551091A (en) * | 2013-11-25 | 2014-02-05 | 北京化工大学 | Method for drying aerogel |
| CN103933900A (en) * | 2014-04-22 | 2014-07-23 | 中国工程物理研究院激光聚变研究中心 | Method for preparing resorcinol-formaldehyde aerogel |
| CN106044740A (en) * | 2016-05-25 | 2016-10-26 | 天津晨祥丰凯新材料科技有限公司 | Porous carbon nanomaterial and preparation method therefor |
| CN107473199A (en) * | 2016-06-08 | 2017-12-15 | 中国科学院金属研究所 | A kind of high intensity large scale bulk charcoal-aero gel and its preparation method and application |
| CN106542517A (en) * | 2016-12-06 | 2017-03-29 | 绵阳泛博新材料科技有限公司 | The preparation method of carbon aerogels |
| CN106976864A (en) * | 2017-05-22 | 2017-07-25 | 河北省科学院能源研究所 | A kind of micropore carbon aerogels and preparation method thereof |
| CN108975300A (en) * | 2017-06-02 | 2018-12-11 | 中国科学院金属研究所 | High-intensitive large scale bulk charcoal-aero gel and its preparation method and application |
| CN107761124A (en) * | 2017-10-23 | 2018-03-06 | 大连理工大学 | A kind of preparation method and application for carrying silver-colored carbon aerogels |
| CN107761124B (en) * | 2017-10-23 | 2019-06-07 | 大连理工大学 | A kind of preparation method and application carrying silver-colored carbon aerogels |
| CN108440899A (en) * | 2018-03-26 | 2018-08-24 | 中国科学技术大学 | Phenolic resin aerogel and carbon aerogels material with Nanofiber Network structure and preparation method thereof |
| CN109289814A (en) * | 2018-10-16 | 2019-02-01 | 大连工业大学 | It is a kind of for adsorbing the magnetic carbon aerogels and preparation method thereof of antibiotic in waste water |
| CN109289814B (en) * | 2018-10-16 | 2021-08-27 | 大连工业大学 | Magnetic carbon aerogel for adsorbing antibiotics in wastewater and preparation method thereof |
| CN109786120A (en) * | 2019-01-25 | 2019-05-21 | 内蒙古科技大学 | Utilize the method for ionic liquid preparation metal/carbon aeroge composite nano materials |
| CN110170322A (en) * | 2019-06-21 | 2019-08-27 | 天津大学 | A kind of preparation method for the platinum/carbon aerogel catalyst loading atom level noble metal |
| CN111498828A (en) * | 2020-04-15 | 2020-08-07 | 贵州梅岭电源有限公司 | Method for preparing carbon aerogel by utilizing normal-pressure drying |
| CN113429182A (en) * | 2021-06-23 | 2021-09-24 | 武汉纺织大学 | Carbon aerogel cement brick and preparation method thereof |
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Application publication date: 20120627 |