CN102557022A - Preparation method of graphene conductive foam - Google Patents
Preparation method of graphene conductive foam Download PDFInfo
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- CN102557022A CN102557022A CN2012100529285A CN201210052928A CN102557022A CN 102557022 A CN102557022 A CN 102557022A CN 2012100529285 A CN2012100529285 A CN 2012100529285A CN 201210052928 A CN201210052928 A CN 201210052928A CN 102557022 A CN102557022 A CN 102557022A
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Abstract
The invention relates to a preparation method of graphene conductive foam. The method comprises the following steps: adding a graphite sheet into concentrated sulfuric acid containing sodium nitrate, adding potassium permanganate and preserving heat at the temperature of between 35 and 40 DEG C for 60 to 90 minutes; adding water under magnetic stirring and preserving heat at the temperature of between 85 and 95 DEG C for 60 to 90 minutes; adding hydrogen peroxide with the mass content of 30 percent, stirring, filtering, dispersing for twice, centrifugally separating and ultrasonically separating to obtain oxidized graphene; and dispersing foam into water containing the oxidized graphene, coating the oxidized graphene on the surface of the foam, taking out the foam, soaking into aqueous solution containing a reducing agent and performing reducing reaction to obtain the conductive foam with the surface coated with a graphene conductive layer. By the method, the conductive foam is obtained by adsorbing the graphene conductive film to the surface of the foam. The prepared conductive foam has the advantages of low density, high conductivity, large specific surface area and low cost.
Description
Technical field
The invention belongs to the material technology field, be specifically related to a kind of graphene conductive foamy preparation method.
Background technology
Conductive foam is the conductive solid material that a kind of inside is uniform-distribution with a large amount of connections or disconnected bubble, is used for antistatic, electromagnetic shielding, air-sensitive or fields such as voltage sensitive sensor, sewage purification.The preparation method that conductive foam is commonly used be in the polymkeric substance filled conductive material carbon black after the foam process preparation.
Graphene is a plane bidimensional monoatomic layer carbon material, is to find the hardest nano material at present, and the electronic mobility of Graphene reaches 10 under the room temperature
6Cm
2V
-1s
-1, resistivity about 10
-6Ω cm also is the minimum material of resistivity.These performances of Graphene have guaranteed to have lower density and the conductivity of Geng Gao by the foam of Graphene preparation than regular foam material.Chemical Vapor deposition process can prepare the small size grapheme foam, but receives preparing method's restriction, and grapheme foam can't volume production.
Summary of the invention
The purpose of this invention is to provide a kind of graphene conductive foamy preparation method, this method utilizes the Graphene of high conductivity and common insulating foams material compound, realizes low density, the preparation of high conductivity graphene conductive foamy.
The inventive method is that starting material adopt chemical oxidization method with the flake graphite; Be prepared into the graphene oxide material; Graphene oxide is coated in foam surfaces such as urethane, PS or Vilaterm through padding technology; Graphene oxide with the polyethylene surface is reduced into Graphene then, obtains the graphene coated conductive foams of foam surface such as urethane.
The concrete steps of the inventive method are:
Step (1). SODIUMNITRATE is added in the vitriol oil as reaction solution, and the mass content of SODIUMNITRATE is 1~2 ﹪ in the reaction solution; Then graphite flake is added in the reaction solution, the mass ratio of graphite flake and reaction solution is 1:80~100;
Step (2). add potassium permanganate in the reaction solution, be incubated 60~90 minutes after temperature rises to 35~40 ℃; Add the graphite flake of potassium permanganate and adding mass ratio be 6~10:1;
Step (3). the magnetic agitation limit is carried out on the reaction solution limit add entry, be incubated 60~90 minutes after temperature rises to 85~95 ℃; Add the graphite flake of water and adding mass ratio be 350~400:1;
Step (4). add the ydrogen peroxide 50 of mass content 30%, stir 5~10 minutes after-filtration; Add the graphite flake of ydrogen peroxide 50 and adding mass ratio be 5~6:1;
Step (5). water disperses filtration product, carries out a spinning with whizzer with 1000~2000 rev/mins speed then;
Step (6). the product that a spinning goes out is used water-dispersion once more, carry out secondary centrifuging with whizzer with 8000~10000 rev/mins speed then and separate;
Step (7). add entry in the secondary centrifuging separated products, and separate, obtain graphene oxide with ultrasonic echography;
Step (8). foam is immersed in the water that is dispersed with graphene oxide of step (7) acquisition, graphene oxide is coated in foam surface with padding technology; Add foam and graphite flake mass ratio be 1~20:1;
Described foam is polyurethane foam, polystyrene foam, polyethylene, polyvinyl chloride foam or polypropylene foam;
Step (9). there is the foam of graphene oxide to pull back the immersion in the aqueous solution that contains reductive agent out surface-coated and carries out reduction reaction, obtain the conductive foam of surface-coated graphene conductive layer; Wherein the mass ratio of contained reductive agent and graphite flake is 2~10:1 in the aqueous solution.
Described reductive agent is hydrazine, dimethylhydrazine, Peng Qinghuana, lithium aluminium hydride, hydroiodic acid HI or Hydrogen bromide.
The inventive method obtains conductive foam through foam surface absorption graphene conductive film, and the conductive foam of preparation has the advantage that density is low, specific conductivity is high, specific surface area is big, cost is low.The conductive layer Graphene of foam surface does not come off through the water repetitive scrubbing, can recirculation use through cleaning after using as the filtering material for core of environmental protection equipment pollutent.That tradition gas sensor complex manufacturing technology, difficulty require is high, surrounding environment is required harshly to compare with existing sensors, plays a significant role in gas detection and environment detection and can overcome above-mentioned shortcoming with the novel gas sensor of grapheme foam material prepn.The graphene conductive foam mechanical intensity and the good springiness of the inventive method preparation, resistance will produce considerable change under external force such as extruding, bending, can be used to prepare novel vibrating transmitter or the like.
Embodiment
Embodiment 1.
Step (1). 10 gram SODIUMNITRATE are added in the vitriol oil of 990 grams, 98 ﹪ as reaction solution, then 10 gram graphite flakes are added in the reaction solutions;
Step (2). slowly add 60 gram potassium permanganate in the reaction solution, insulation was 90 minutes after temperature rose to 35 ℃;
Step (3). the magnetic agitation limit is carried out on the reaction solution limit add 4 premium on currency, insulation was 90 minutes after temperature rose to 85 ℃;
Step (4). add the ydrogen peroxide 50 of 50 gram mass content 30%, stir 10 minutes after-filtration;
Step (5). water disperses filtration product, carries out a spinning with whizzer with 1000 rev/mins speed then;
Step (6). the product that a spinning goes out is used water-dispersion once more, carry out secondary centrifuging with whizzer with 10000 rev/mins speed then and separate;
Step (7). add entry in the secondary centrifuging separated products, and separate, obtain graphene oxide with ultrasonic echography;
Step (8). 200 gram polyurethane foams immersions are dispersed with in the water of graphene oxide, graphene oxide are coated in foam surface with padding technology;
Step (9). after having the polyurethane foam of graphene oxide to pull out the surface-coated, immerse in the aqueous solution that contains 20 gram dimethylhydrazines and carry out reduction reaction, obtain the conductive foam of surface-coated graphene conductive layer.
Embodiment 2.
Step (1). 15 gram SODIUMNITRATE are added in the vitriol oil of 785 grams, 98 ﹪ as reaction solution, then 10 gram graphite flakes are added in the reaction solutions;
Step (2). slowly add 70 gram potassium permanganate in the reaction solution, insulation was 70 minutes after temperature rose to 37 ℃;
Step (3). the magnetic agitation limit is carried out on the reaction solution limit add 3.5 premium on currency, insulation was 75 minutes after temperature rose to 90 ℃;
Step (4). add the ydrogen peroxide 50 of 60 gram mass content 30%, stir 5 minutes after-filtration;
Step (5). water disperses filtration product, carries out a spinning with whizzer with 1500 rev/mins speed then;
Step (6). the product that a spinning goes out is used water-dispersion once more, carry out secondary centrifuging with whizzer with 5000 rev/mins speed then and separate;
Step (7). add entry in the secondary centrifuging separated products, and separate, obtain graphene oxide with ultrasonic echography;
Step (8). 100 gram polystyrene foams immersions are dispersed with in the water of graphene oxide, graphene oxide are coated in foam surface with padding technology;
Step (9). after having the polystyrene foam of graphene oxide to pull out the surface-coated, immerse in the aqueous solution that contains 100 gram Peng Qinghuanas and carry out reduction reaction, obtain the conductive foam of surface-coated graphene conductive layer.
Embodiment 3.
Step (1). 18 gram SODIUMNITRATE are added in the vitriol oil of 882 grams, 98 ﹪ as reaction solution, then 10 gram graphite flakes are added in the reaction solutions;
Step (2). slowly add 80 gram potassium permanganate in the reaction solution, insulation was 60 minutes after temperature rose to 40 ℃;
Step (3). the magnetic agitation limit is carried out on the reaction solution limit add 3.8 premium on currency, insulation was 60 minutes after temperature rose to 95 ℃;
Step (4). add the ydrogen peroxide 50 of 55 gram mass content 30%, stir 8 minutes after-filtration;
Step (5). water disperses filtration product, carries out a spinning with whizzer with 2000 rev/mins speed then;
Step (6). the product that a spinning goes out is used water-dispersion once more, carry out secondary centrifuging with whizzer with 8000 rev/mins speed then and separate;
Step (7). add entry in the secondary centrifuging separated products, and separate, obtain graphene oxide with ultrasonic echography;
Step (8). 10 gram polyethylenes immersions are dispersed with in the water of graphene oxide, graphene oxide are coated in foam surface with padding technology;
Step (9). after having the polyethylene of graphene oxide to pull out the surface-coated, immerse in the aqueous solution that contains 50 gram hydrazines and carry out reduction reaction, obtain the conductive foam of surface-coated graphene conductive layer.
Embodiment 4.
Step (1). 15 gram SODIUMNITRATE are added in the vitriol oil of 985 grams, 98 ﹪ as reaction solution, then 10 gram graphite flakes are added in the reaction solutions;
Step (2). slowly add 90 gram potassium permanganate in the reaction solution, insulation was 75 minutes after temperature rose to 35 ℃;
Step (3). the magnetic agitation limit is carried out on the reaction solution limit add 3.6 premium on currency, insulation was 75 minutes after temperature rose to 88 ℃;
Step (4). add the ydrogen peroxide 50 of 57 gram mass content 30%, stir 6 minutes after-filtration;
Step (5). water disperses filtration product, carries out a spinning with whizzer with 1200 rev/mins speed then;
Step (6). the product that a spinning goes out is used water-dispersion once more, carry out secondary centrifuging with whizzer with 10000 rev/mins speed then and separate;
Step (7). add entry in the secondary centrifuging separated products, and separate, obtain graphene oxide with ultrasonic echography;
Step (8). 50 gram polypropylene foams immersions are dispersed with in the water of graphene oxide, graphene oxide are coated in foam surface with padding technology;
Step (9). after having the polypropylene foam of graphene oxide to pull out the surface-coated, immerse in the aqueous solution that contains 40 gram hydroiodic acid HIs and carry out reduction reaction, obtain the conductive foam of surface-coated graphene conductive layer.
Embodiment 5.
Step (1). 10 gram SODIUMNITRATE are added in the vitriol oil of 790 grams, 98 ﹪ as reaction solution, then 10 gram graphite flakes are added in the reaction solutions;
Step (2). slowly add 70 gram potassium permanganate in the reaction solution, insulation was 70 minutes after temperature rose to 40 ℃;
Step (3). the magnetic agitation limit is carried out on the reaction solution limit add 3.9 premium on currency, insulation was 70 minutes after temperature rose to 92 ℃;
Step (4). add the ydrogen peroxide 50 of 52 gram mass content 30%, stir 9 minutes after-filtration;
Step (5). water disperses filtration product, carries out a spinning with whizzer with 2000 rev/mins speed then;
Step (6). the product that a spinning goes out is used water-dispersion once more, carry out secondary centrifuging with whizzer with 5000 rev/mins speed then and separate;
Step (7). add entry in the secondary centrifuging separated products, and separate, obtain graphene oxide with ultrasonic echography;
Step (8). 150 gram polyvinyl chloride foams immersions are dispersed with in the water of graphene oxide, graphene oxide are coated in foam surface with padding technology;
Step (9). after having the polyvinyl chloride foam of graphene oxide to pull out the surface-coated, immerse to contain in the hydrobromic aqueous solution of 80 grams and carries out reduction reaction, obtain the conductive foam of surface-coated graphene conductive layer.
Embodiment 6.
Step (1). 10 gram SODIUMNITRATE are added in the vitriol oil of 890 grams, 98 ﹪ as reaction solution, then 10 gram graphite flakes are added in the reaction solutions;
Step (2). slowly add 100 gram potassium permanganate in the reaction solution, insulation was 80 minutes after temperature rose to 35 ℃;
Step (3). the magnetic agitation limit is carried out on the reaction solution limit add 3.7 premium on currency, insulation was 80 minutes after temperature rose to 85 ℃;
Step (4). add the ydrogen peroxide 50 of 55 gram mass content 30%, stir 7 minutes after-filtration;
Step (5). water disperses filtration product, carries out a spinning with whizzer with 1800 rev/mins speed then;
Step (6). the product that a spinning goes out is used water-dispersion once more, carry out secondary centrifuging with whizzer with 3000 rev/mins speed then and separate;
Step (7). add entry in the secondary centrifuging separated products, and separate, obtain graphene oxide with ultrasonic echography;
Step (8). 20 gram polyurethane foams immersions are dispersed with in the water of graphene oxide, graphene oxide are coated in foam surface with padding technology;
Step (9). after having the polyurethane foam of graphene oxide to pull out the surface-coated, immerse in the aqueous solution that contains 30 gram lithium aluminium hydride and carry out reduction reaction, obtain the conductive foam of surface-coated graphene conductive layer.
Claims (3)
1. graphene conductive foamy preparation method is characterized in that the concrete steps of this method are:
Step (1). SODIUMNITRATE is added in the vitriol oil as reaction solution, and the mass content of SODIUMNITRATE is 1~2 ﹪ in the reaction solution; Graphite flake is added in the reaction solution, the mass ratio of graphite flake and reaction solution is 1:80~100 again;
Step (2). add potassium permanganate in the reaction solution, be incubated 60~90 minutes after temperature rises to 35~40 ℃; Add the graphite flake of potassium permanganate and adding mass ratio be 6~10:1;
Step (3). the magnetic agitation limit is carried out on the reaction solution limit add entry, be incubated 60~90 minutes after temperature rises to 85~95 ℃; Add the graphite flake of water and adding mass ratio be 350~400:1;
Step (4). add the ydrogen peroxide 50 of mass content 30%, stir 5~10 minutes after-filtration; Add the graphite flake of ydrogen peroxide 50 and adding mass ratio be 5~6:1;
Step (5). water disperses filtration product, carries out a spinning with whizzer with 1000~2000 rev/mins speed then;
Step (6). the product that a spinning goes out is used water-dispersion once more, carry out secondary centrifuging with whizzer with 8000~10000 rev/mins speed then and separate;
Step (7). add entry in the secondary centrifuging separated products, and separate, obtain graphene oxide with ultrasonic echography;
Step (8). the foam immersion is dispersed with in the water of graphene oxide, graphene oxide is coated in foam surface with padding technology; Add foam and graphite flake mass ratio be 1~20:1;
Step (9). there is the foam of graphene oxide to pull back the immersion in the aqueous solution that contains reductive agent out surface-coated and carries out reduction reaction, obtain the conductive foam of surface-coated graphene conductive layer; Wherein the mass ratio of contained reductive agent and graphite flake is 2~10:1 in the aqueous solution.
2. graphene conductive foamy preparation method as claimed in claim 1 is characterized in that: the foam described in the step (8) is polyurethane foam, polystyrene foam, polyethylene, polyvinyl chloride foam or polypropylene foam.
3. graphene conductive foamy preparation method as claimed in claim 1 is characterized in that: the reductive agent described in the step (9) is hydrazine, dimethylhydrazine, Peng Qinghuana, lithium aluminium hydride, hydroiodic acid HI or Hydrogen bromide.
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CN103332686A (en) * | 2013-07-12 | 2013-10-02 | 中国科学院新疆理化技术研究所 | Preparation method of three-dimensional graphene-based foam material |
CN103342827A (en) * | 2013-06-28 | 2013-10-09 | 上海大学 | Preparation method of hydrophobic/lipophilic polyurethane sponge |
CN103663414A (en) * | 2012-09-03 | 2014-03-26 | 国家纳米科学中心 | Preparation method of graphene sponge |
CN103663433A (en) * | 2012-09-26 | 2014-03-26 | 海洋王照明科技股份有限公司 | Graphene as well as preparation method and application thereof |
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CN101029456A (en) * | 2007-03-06 | 2007-09-05 | 天津工业大学 | Non-woven elastic substrate and its production |
WO2009073324A2 (en) * | 2007-11-29 | 2009-06-11 | Invista Technologies S.A.R.L. | High-loft nonwoven including stabilizer or binder |
CN101250817A (en) * | 2008-03-14 | 2008-08-27 | 福建鑫华股份有限公司 | Stephanoporate springiness nonwoven material backing material and manufacturing method thereof |
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CN104661959A (en) * | 2012-08-23 | 2015-05-27 | 莫纳什大学 | Graphene-based materials |
CN103663414A (en) * | 2012-09-03 | 2014-03-26 | 国家纳米科学中心 | Preparation method of graphene sponge |
CN103663433A (en) * | 2012-09-26 | 2014-03-26 | 海洋王照明科技股份有限公司 | Graphene as well as preparation method and application thereof |
CN103342827A (en) * | 2013-06-28 | 2013-10-09 | 上海大学 | Preparation method of hydrophobic/lipophilic polyurethane sponge |
CN103332686A (en) * | 2013-07-12 | 2013-10-02 | 中国科学院新疆理化技术研究所 | Preparation method of three-dimensional graphene-based foam material |
CN103723709A (en) * | 2013-11-22 | 2014-04-16 | 盐城纳新天地新材料科技有限公司 | Preparation method of aqueous single-layer graphene solution |
CN103723710A (en) * | 2013-11-22 | 2014-04-16 | 盐城纳新天地新材料科技有限公司 | Preparation method of single-layer graphene pyridine solution |
CN104807861B (en) * | 2015-04-09 | 2017-05-24 | 山东师范大学 | Preparation method of spongy graphene-based stretchable gas sensor |
CN104807861A (en) * | 2015-04-09 | 2015-07-29 | 山东师范大学 | Preparation method of spongy graphene-based stretchable gas sensor |
CN105387927A (en) * | 2015-11-23 | 2016-03-09 | 南京邮电大学 | Novel flexible vibration sensor |
CN105600777A (en) * | 2016-01-29 | 2016-05-25 | 北京理工大学 | Preparation method of polystyrene modified three-dimensional graphene foam |
CN106257275B (en) * | 2016-06-21 | 2019-08-20 | 杭州师范大学 | A kind of open celled polymeric gas sensitive and the preparation method and application thereof |
CN106257275A (en) * | 2016-06-21 | 2016-12-28 | 杭州师范大学 | A kind of open celled polymeric gas sensitive and preparation method and application |
CN106243378A (en) * | 2016-07-14 | 2016-12-21 | 温州乐发教育科技有限公司 | A kind of graphene conductive foam and preparation method thereof |
CN106432671A (en) * | 2016-09-21 | 2017-02-22 | 江苏盖姆纳米材料科技有限公司 | Preparation method of carbon-base sponge and foam material |
CN107522895A (en) * | 2017-08-08 | 2017-12-29 | 东南大学 | A kind of gentle method for preparing graphene polyurethane sponge composite |
US11760056B2 (en) * | 2018-12-05 | 2023-09-19 | Battelle Memorial Institute | Flexible foam resistive heaters and methods of making flexible resistive heaters |
CN111086979A (en) * | 2019-12-16 | 2020-05-01 | 北京航空航天大学 | Compressible carbon black/wood derived carbon sponge and preparation method thereof |
CN111086979B (en) * | 2019-12-16 | 2021-11-12 | 北京航空航天大学 | Compressible carbon black/wood derived carbon sponge and preparation method thereof |
CN112969356A (en) * | 2021-01-19 | 2021-06-15 | 西安理工大学 | Preparation method of polyurethane/graphene nanosheet/sponge composite material |
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