CN107649078A - A kind of graphene composite material aeroge and preparation method - Google Patents
A kind of graphene composite material aeroge and preparation method Download PDFInfo
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- CN107649078A CN107649078A CN201711034292.0A CN201711034292A CN107649078A CN 107649078 A CN107649078 A CN 107649078A CN 201711034292 A CN201711034292 A CN 201711034292A CN 107649078 A CN107649078 A CN 107649078A
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- composite material
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- aeroge
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0052—Preparation of gels
- B01J13/0065—Preparation of gels containing an organic phase
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of graphene composite material aeroge and preparation method.Preparation process of the present invention is that catalyst and nano material are scattered in a solvent, then it is mixed to get mixed liquor with resorcinol and formaldehyde, graphite oxide obtains graphene oxide dispersion by supersound process in deionized water, it is mixed with mixed liquor, continuous poriferous foam material is soaked into mixed liquor again, taken out after continuous poriferous foam material is full of mixed liquor, it is carbonized by being put into after freeze-drying in the high temperature carbonization furnace of inert gas atmosphere, graphene composite material aeroge is prepared after cooling.Present invention process environmental protection is simple, and cost is low, and obtained graphene composite aerogel has the characteristics that dispersion stabilization is high, specific surface area is high, porosity is big, pore-size distribution is wide and conducts electricity very well.
Description
Technical field
The present invention relates to the technical field in nano material, more particularly to a kind of graphene composite material aeroge and preparation
Method.
Background technology
Graphene is the first two dimensional crystal material truly, and the further investigation to graphene receives many sections
Learn the concern of researcher.On graphenic surface, the migration rate of carrier is far above the migration rate in conventional conductor so that
Graphene shows the electrical conductivity of superelevation.At room temperature, the Conductivity Ratio copper of graphene has been higher by two orders of magnitude.
Graphene aerogel is a kind of three-dimensional net structure graphene macroform of internal connection, inherits the good of graphene
Good chemical stability and superior catalytic performance, while also possess higher specific surface area and electric conductivity.Graphene aerogel by
It is widely used in its superior performance and unique structure in fields such as catalysis, energy storage, absorption and conductions.Graphene airsetting
Glue is raw material usually using resorcinol and formaldehyde in preparation process, and organogel is obtained under catalyst action, by with
Supercritical drying and carbonization process afterwards obtains graphene aerogel.
The content of the invention
The shortcomings that it is an object of the invention to overcome prior art, propose a kind of graphene composite material aeroge.
It is another object of the present invention to propose a kind of preparation method of graphene composite material aeroge.
The purpose of the present invention is achieved through the following technical solutions：
A kind of graphene composite material aeroge includes following components：
Resorcinol 50-150 parts
Formaldehyde 80-200 parts
Nano material 0.1-1 parts
Catalyst 0.05-0.15 parts
Graphene 100-300 parts
Described nano material includes the one or more in nano-sized carbon, nano-silicon, nano-metal particle.Preferably nano-silicon.
Described catalyst is phenpromethamine.
A kind of preparation method of graphene composite material aeroge comprises the following steps：
S1, a certain amount of catalyst and nano material are added to the dispersed 3-7h of water；
S2, resorcinol and formaldehyde are added to S1 mixing by a certain percentage, obtain mixed liquor；
S3, graphene oxide is ultrasonically treated in deionized water, ultrasonic time 0.5-2h, ultrasonic power 2500-
3500W,
Obtain the graphene oxide dispersion that concentration is 0.1-5mg/mL；Optimum condition is：Ultrasonic time is 1h, and ultrasonic power is
3000W。
S4, graphene oxide dispersion will be obtained it is scattered in S2 mixed liquor, reacts 1-5h at 80-100 DEG C；
S5, continuous poriferous foam material is soaked into the solution obtained by S4, treats that continuous poriferous foam material is full of the solution
After take out, obtain xerogel by what gel seal was freeze-dried.
S6, by xerogel as in the high-temperature atmosphere furnace of inert gas, at high temperature carbonization a period of time obtain graphene
Composite aeroge.
Described continuous poriferous foam material is High load-bearing foam.
Described inert gas is nitrogen or argon gas.Preferably nitrogen.
Reaction temperature in described S6 is 800-1500 DEG C, carbonization time 3-7h.
The graphene composite material aeroge is applied to lithium battery, by the way that graphene composite material aeroge is ground,
It is prepared into cathode of lithium battery.
The present invention has advantages below：Nano material is added in the solution of resorcinol-formaldehyde, makes the stone easily reunited
Black alkene is dispersed, has higher dispersion stabilization；The lithium cell cathode material being made into, with the negative of traditional lithium battery
Pole material is compared, and has higher capacity and stability；Using High load-bearing foam, the material of its soft quality, the stronger intensity of pressure
With it compared with high carrying so that the specific surface area for the obtained graphene composite aerogel that is finally carbonized is high, porosity is big, aperture point
Cloth is wide.Exchange of solvent is not needed, reduces energy resource consumption, while reduces the environmental pollution brought by exchange of solvent.
Embodiment
In order to which technical characteristic, purpose and the effect of the present invention is more clearly understood, now to the specific reality of the present invention
The mode of applying illustrates.
Embodiment 1
0.05 part of catalyst and 0.01 part of nano material are added to the dispersed 3-7h of water；Then add 50 parts of resorcinols and
80 parts of formaldehyde are well mixed, and obtain mixed liquor；Graphene oxide is ultrasonically treated in deionized water, ultrasonic time 1h, surpassed
Acoustical power is 3000W, obtains the graphene oxide dispersion that concentration is 0.1mg/mL；Graphene oxide dispersion will be obtained to disperse
In above-mentioned mixed liquor, 1-5h is reacted at 80-100 DEG C；High load-bearing foam is soaked into solution obtained above, treated
High load-bearing foam takes out after being full of the solution, and be sealed against being freeze-dried obtains xerogel.By xerogel as nitrogen
In the high-temperature atmosphere furnace of gas gas, carbonization 3-7h obtains graphene composite material aeroge at 800-1500 DEG C of high temperature.
Embodiment 2
0.07 part of catalyst and 0.02 part of nano material are added to the dispersed 3-7h of water；Then add 70 parts of resorcinols and
110 parts of formaldehyde are well mixed, and obtain mixed liquor；Graphene oxide is ultrasonically treated in deionized water, ultrasonic time 1h, surpassed
Acoustical power is 3000W, obtains the graphene oxide dispersion that concentration is 0.3mg/mL；Graphene oxide dispersion will be obtained to disperse
In above-mentioned mixed liquor, 1-5h is reacted at 80-100 DEG C；High load-bearing foam is soaked into solution obtained above, treated
High load-bearing foam takes out after being full of the solution, and be sealed against being freeze-dried obtains xerogel.By xerogel as nitrogen
In the high-temperature atmosphere furnace of gas gas, carbonization 3-7h obtains graphene composite material aeroge at 800-1500 DEG C of high temperature.
Embodiment 3
0.10 part of catalyst and 0.04 part of nano material are added to the dispersed 3-7h of water；Then add 90 parts of resorcinols and
140 parts of formaldehyde are well mixed, and obtain mixed liquor；Graphene oxide is ultrasonically treated in deionized water, ultrasonic time 1h, surpassed
Acoustical power is 3000W, obtains the graphene oxide dispersion that concentration is 0.6mg/mL；Graphene oxide dispersion will be obtained to disperse
In above-mentioned mixed liquor, 1-5h is reacted at 80-100 DEG C；High load-bearing foam is soaked into solution obtained above, treats height
Carrying foam takes out after being full of the solution, and be sealed against being freeze-dried obtains xerogel.By xerogel as nitrogen
In the high-temperature atmosphere furnace of gas, carbonization 3-7h obtains graphene composite material aeroge at 800-1500 DEG C of high temperature.
Embodiment 4
0.12 part of catalyst and 0.06 part of nano material are added to the dispersed 3-7h of water；Then 110 parts of resorcinols are added
It is well mixed with 170 parts of formaldehyde, obtains mixed liquor；Graphene oxide is ultrasonically treated in deionized water, ultrasonic time 1h,
Ultrasonic power is 3000W, obtains the graphene oxide dispersion that concentration is 1mg/mL；Graphene oxide dispersion will be obtained to disperse
In above-mentioned mixed liquor, 1-5h is reacted at 80-100 DEG C；High load-bearing foam is soaked into solution obtained above, treated
High load-bearing foam takes out after being full of the solution, and be sealed against being freeze-dried obtains xerogel.By xerogel as nitrogen
In the high-temperature atmosphere furnace of gas gas, carbonization 3-7h obtains graphene composite material aeroge at 800-1500 DEG C of high temperature.
Embodiment 5
0.15 part of catalyst and 0.08 part of nano material are added to the dispersed 3-7h of water；Then 130 parts of resorcinols are added
It is well mixed with 200 parts of formaldehyde, obtains mixed liquor；Graphene oxide is ultrasonically treated in deionized water, ultrasonic time 1h,
Ultrasonic power is 3000W, obtains the graphene oxide dispersion that concentration is 1.3mg/mL；Graphene oxide dispersion point will be obtained
Dissipate in above-mentioned mixed liquor, react 1-5h at 80-100 DEG C；High load-bearing foam is soaked into solution obtained above, treated
High load-bearing foam takes out after being full of the solution, and be sealed against being freeze-dried obtains xerogel.By xerogel as nitrogen
In the high-temperature atmosphere furnace of gas gas, carbonization 3-7h obtains graphene composite material aeroge at 800-1500 DEG C of high temperature.
Embodiment 6
0.15 part of catalyst and 0.10 part of nano material are added to the dispersed 3-7h of water；Then 150 parts of resorcinols are added
It is well mixed with 200 formaldehyde, obtains mixed liquor；Graphene oxide is ultrasonically treated in deionized water, ultrasonic time 1h, surpassed
Acoustical power is 3000W, obtains the graphene oxide dispersion that concentration is 1.5mg/mL；Graphene oxide dispersion will be obtained to disperse
In above-mentioned mixed liquor, 1-5h is reacted at 80-100 DEG C；High load-bearing foam is soaked into solution obtained above, treated
High load-bearing foam takes out after being full of the solution, and be sealed against being freeze-dried obtains xerogel.By xerogel as nitrogen
In the high-temperature atmosphere furnace of gas gas, carbonization 3-7h obtains graphene composite material aeroge at 800-1500 DEG C of high temperature.
It should be noted that for foregoing each embodiment of the method, in order to be briefly described, therefore it is all expressed as to a system
The combination of actions of row, but those skilled in the art should know, the application is not limited by described sequence of movement, because
For according to the application, certain some step can use other orders or carry out simultaneously.Secondly, those skilled in the art also should
Know, embodiment described in this description belongs to preferred embodiment, involved action and unit not necessarily this Shen
Please be necessary.
In the above-described embodiments, the description to each embodiment all emphasizes particularly on different fields, and is not described in some embodiment
Part, may refer to the associated description of other embodiment.
Claims (9)
- A kind of 1. graphene composite material aeroge, it is characterised in that：Include following components by weight：Resorcinol 50-150 Part；Formaldehyde 80-200 parts；Nano material 0.1-1 parts；Catalyst 0.05-0.15 parts；Graphene 100-300 parts.
- A kind of 2. graphene composite material aeroge according to claim 1, it is characterised in that：Described nano material bag Include the one or more in nano-sized carbon, nano-silicon, nano-metal particle.
- A kind of 3. graphene composite material aeroge according to claim 1, it is characterised in that：Described catalyst is two Methylphenethylamine.
- A kind of 4. preparation method of graphene composite material aeroge, it is characterised in that：Comprise the following steps：S1, a certain amount of catalyst and nano material are added to the dispersed 3-7h of water；S2, resorcinol and formaldehyde are added to S1 mixing by a certain percentage, obtain mixed liquor；S3, graphene oxide is ultrasonically treated in deionized water, ultrasonic time 0.5-2h, ultrasonic power 2500- 3500W,Obtain the graphene oxide dispersion that concentration is 0.1-5mg/mL；S4, graphene oxide dispersion will be obtained it is scattered in S2 mixed liquor, reacts 1-5h at 80-100 DEG C；S5, continuous poriferous foam material is soaked into the solution obtained by S4, treats that continuous poriferous foam material is full of the solution After take out, obtain xerogel by what gel seal was freeze-driedS6, by xerogel as in the high-temperature atmosphere furnace of inert gas, at high temperature carbonization a period of time it is compound to obtain graphene Material aeroge.
- A kind of 5. preparation method of graphene composite material aeroge according to claim 4, it is characterised in that：Described Ultrasonic time is 1h, ultrasonic power 3000W.
- A kind of 6. preparation method of graphene composite material aeroge according to claim 4, it is characterised in that：Described Continuous poriferous foam material is High load-bearing foam.
- A kind of 7. preparation method of graphene composite material aeroge according to claim 4, it is characterised in that：Described Inert gas is nitrogen or argon gas.
- A kind of 8. preparation method of graphene composite material aeroge according to claim 4, it is characterised in that：Described Reaction temperature in S6 is 800-1500 DEG C, carbonization time 3-7h.
- A kind of 9. preparation method of graphene composite material aeroge according to claim 4, it is characterised in that：The stone Black alkene composite aeroge is applied to lithium battery, by the way that graphene composite material aeroge is ground, is prepared into lithium battery and bears Pole.
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| CN201711034292.0A CN107649078A (en) | 2017-10-30 | 2017-10-30 | A kind of graphene composite material aeroge and preparation method |
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| CN201711034292.0A CN107649078A (en) | 2017-10-30 | 2017-10-30 | A kind of graphene composite material aeroge and preparation method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111793346A (en) * | 2020-07-25 | 2020-10-20 | 方彭 | Graphene aerogel composite material and preparation method thereof |
| CN112691676A (en) * | 2021-02-01 | 2021-04-23 | 河南师范大学 | Zn-doped alpha-Fe2O3Preparation method of/graphene aerogel composite catalyst, oxidation system and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103274384A (en) * | 2013-04-24 | 2013-09-04 | 中科院广州化学有限公司 | Graphene oxide reinforced carbon aerogel material, and preparation method and application thereof |
| CN104993138A (en) * | 2015-05-21 | 2015-10-21 | 湖南元素密码石墨烯研究院（有限合伙） | Preparation method and application of graphene composite material aerogel |
| CN106565267A (en) * | 2016-11-01 | 2017-04-19 | 天津晨祥丰凯新材料科技有限公司 | Preparation method for carbon aerogel composite material |
-
2017
- 2017-10-30 CN CN201711034292.0A patent/CN107649078A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103274384A (en) * | 2013-04-24 | 2013-09-04 | 中科院广州化学有限公司 | Graphene oxide reinforced carbon aerogel material, and preparation method and application thereof |
| CN104993138A (en) * | 2015-05-21 | 2015-10-21 | 湖南元素密码石墨烯研究院（有限合伙） | Preparation method and application of graphene composite material aerogel |
| CN106565267A (en) * | 2016-11-01 | 2017-04-19 | 天津晨祥丰凯新材料科技有限公司 | Preparation method for carbon aerogel composite material |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111793346A (en) * | 2020-07-25 | 2020-10-20 | 方彭 | Graphene aerogel composite material and preparation method thereof |
| CN112691676A (en) * | 2021-02-01 | 2021-04-23 | 河南师范大学 | Zn-doped alpha-Fe2O3Preparation method of/graphene aerogel composite catalyst, oxidation system and application thereof |
| CN112691676B (en) * | 2021-02-01 | 2024-03-01 | 河南师范大学 | Zn doped alpha-Fe 2 O 3 Preparation method of graphene aerogel composite catalyst, and oxidation system and application thereof |
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Application publication date: 20180202 |