CN105964193B - A kind of preparation method of graphene oxide-alumina composite aeroge - Google Patents
A kind of preparation method of graphene oxide-alumina composite aeroge Download PDFInfo
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- CN105964193B CN105964193B CN201610260244.2A CN201610260244A CN105964193B CN 105964193 B CN105964193 B CN 105964193B CN 201610260244 A CN201610260244 A CN 201610260244A CN 105964193 B CN105964193 B CN 105964193B
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- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
Abstract
The invention discloses a kind of preparation methods of graphene oxide alumina composite aeroge, include the following steps：Graphene oxide is taken, is added in dispersion solvent, ultrasound 1h, is detached with low speed centrifuge in instrument is cleaned by ultrasonic, and the precipitation for filtering out lower floor takes upper solution；Solution is taken, the pH of solution is adjusted with weak aqua ammonia and dilute hydrochloric acid, Aluminium chloride hexahydrate is added, is reacted；It treats to react to finish in step 2 to be cooled to room temperature, magnetic agitation 0.5h, then mixed solution is transferred in polytetrafluoro water heating kettle, 12h is kept at 180 DEG C, it treats that reaction kettle is down to room temperature, cylindric product is taken out, washed with alcohol, wash each two to three times, by product in freeze drier dry 12h to get to graphene oxide alumina aerogels composite material.Ultralight composite material prepared by the method for the present invention possesses abundant pore passage structure, and can give full play to the good electric conductivity of graphene, gathers around and has broad application prospects.
Description
Technical field
The present invention relates to organic and inorganic oxide composite aerogel preparation field, specifically a kind of graphene oxide-oxidations
The preparation method of aluminium composite aerogel.
Background technology
Aeroge is that a kind of inside for mutually assembling composition with nanometer scale ultramicro powder is low full of gaseous state decentralized medium
Density cellular solid material, porosity may be up to 98.9%.It is presently found, and most light solid material, has in the world
The title of " solid-state cigarette ".Aeroge remove with nano material fundamental property, also with high porosity, low heat transfer coefficient, low-density,
Low electrical conductivity, in a low voice low refraction coefficient, many good characteristics such as spread speed, in fireclay insulating refractory, catalyst and catalysis
Agent carrier, silencing and damping material, novel high-energy particle detector, the cleanser of gas and water, special glass presoma etc.
With boundless application prospect.Wherein graphene aerogel has light weight, intensity height, high-specific surface area, thermal stability
The advantages that good and conductivity is high.The graphene of three-dimensional structure is in ultracapacitor, oily sorbing material and catalyst carrier etc.
Aspect has huge potential use.
Aluminium oxide (Al2O3), alumina is industrially commonly called as, is a kind of sizable chemical article of dosage.It has mechanical strength
Greatly, the advantages that thermal stability is good and cheap and easy to get is a kind of very important industrial chemicals, therefore can be widely used in
The fields such as structure and function ceramics, medicine, environmental protection, adsorbent, catalyst and catalyst carrier.However be prepared at this stage
Aluminium oxide is easily reunited, specific surface area is small, if therefore the dispersibility that effective method improves aluminium oxide can be found, will be to aluminium oxide
The performances such as adsoption catalysis generate active influence, this has great meaning to improving its commercial Application.
Invention content
Easily reunite the present invention is directed to being directed to the aluminium oxide prepared at this stage, specific surface area it is small, layered graphite oxide alkene is three-dimensional
The problem of block difficulty is molded proposes the preparation method of graphene oxide-alumina composite aeroge a kind of, so as to obtain with
Aluminium oxide and graphene oxide advantage and the new material for improving its inherent shortcoming.
To achieve the above object, the technical solution adopted by the present invention is：
A kind of preparation method of graphene oxide-alumina composite aeroge, includes the following steps：
Step 1: taking graphene oxide, it is added in dispersion solvent, ultrasound 1h, uses low-speed centrifugal in instrument is cleaned by ultrasonic
Machine detaches, and the precipitation for filtering out lower floor takes upper solution；
Step 2: the solution that step 1 is taken to obtain, the pH of solution is adjusted with weak aqua ammonia and dilute hydrochloric acid, adds six hydration chlorine
Change aluminium, reacted；
Step 3: treating to react to finish in step 2 to be cooled to room temperature, then mixed solution is transferred to poly- by magnetic agitation 0.5h
In tetrafluoro water heating kettle, 12h is kept at 180 DEG C, treats that reaction kettle is down to room temperature, cylindric product is taken out, washed, washed respectively with alcohol
Two to three times, by product in freeze drier dry 12h to get to graphene oxide-alumina aerogels composite material.
Further, in step 1, the graphene oxide is prepared by being modified Hummer methods, the specific steps are：According to matter
Amount is than being 2:1 takes natural flake graphite and sodium nitrate to be added in the concentrated sulfuric acid, and 2h is stirred under condition of ice bath, which is pre- oxygen
The change stage；After pre-oxidation, potassium permanganate is slowly added to, wherein, the mass ratio of potassium permanganate and natural flake graphite is 3：
1, and the reaction was continued the 2h under condition of ice bath, the stage are the low-temp reaction stage；Ice bath is removed, above-mentioned reactant is transferred to 35
In DEG C water-bath, the reaction was continued 1h, which is the medium temperature stage of reaction；Deionized water is slowly added into above-mentioned reaction system, with
After be warming up to 98 DEG C, and react 30min at such a temperature, the stage be the pyroreaction stage；After the pyroreaction stage, add
Enter deionized water and hydrogen peroxide, and stir 1h, reaction terminates；After prepared by graphite oxide, by way of centrifuge washing
Remove foreign ion therein；After washing, obtained graphite oxide slurry is subjected to forced air drying under the conditions of 60 DEG C,
It is spare.
Further, in step 1, the mass volume ratio of graphene oxide and dispersion solvent is 0.3:100~0.2:50g/
mL。
Further, in step 1, dispersion solvent is distilled water.
Further, in step 1, the ultrasonic power for being cleaned by ultrasonic instrument is 180W.
Further, in step 1, the rotating speed of low speed centrifuge is 4000rpm/min.
Further, in step 2, the volume mass ratio of step 1 acquired solution and Aluminium chloride hexahydrate is 50:1.2~
50:2.4。
Further, in step 2, the pH of solution is adjusted to 1-12.
Further, in step 2, reaction temperature is 50-100 DEG C.
Further, in step 2, reaction time 0.5h-10h.
The beneficial effects of the invention are as follows：The preparation method of graphene oxide provided by the invention-alumina composite aeroge,
It is modified using graphene oxide, by the way that Aluminium chloride hexahydrate is scattered in graphene oxide solution, using a step hydro-thermal
Synthesis obtains product, and aluminium oxide has dispersibility well, and this composite material has abundant pore structure, while has graphite
The superior electrical conductivity energy of alkene can be used as catalyst and catalyst carrier, sorbing material etc., there is higher actual application value.
Description of the drawings
The scanning electron microscope (SEM) photograph that it is dried composite aerogel prepared by embodiment that Fig. 1, which is,.
Specific embodiment
The present invention is done with reference to embodiment and is further explained.The following example is merely to illustrate the present invention, but
It is not used to limit the practical range of the present invention.
The preparation method of a kind of graphene oxide-alumina composite aeroge, using graphene oxide as raw material ultrasonic disperse
In a solvent, it adds a certain amount of Aluminium chloride hexahydrate and is stirred at reflux certain time at a set temperature, finally use hydro-thermal method
Synthesis obtains cylindric wet gel, is freeze-dried after alcohol is washed, washed and obtains ultralight graphene oxide-alumina composite gas
Gel specifically comprises the following steps：
Step 1: taking the graphene oxide prepared by modified Hummer methods, it is added in dispersion solvent, in 180W ultrasound work(
Ultrasound 1h in the ultrasonic cleaning instrument of rate is detached with low speed centrifuge in the case where rotating speed is 1000-8000rpm/min, filtering
The precipitation for falling down layer takes upper solution；
Wherein, graphene oxide and the mass volume ratio of dispersion solvent are 0.3:100~0.2:50g/mL.
Step 2: the solution that step 1 is taken to obtain, the pH to 1-12 of solution is adjusted with weak aqua ammonia and dilute hydrochloric acid, adds six
Aluminium chlorohydrate reacts 0.5h-10h in 50-100 DEG C；
Wherein, the volume mass of step 1 acquired solution and Aluminium chloride hexahydrate ratio is 50:1.2~50:2.4.
Step 3: treating to react to finish in step 2 to be cooled to room temperature, then mixed solution is transferred to poly- by magnetic agitation 0.5h
In tetrafluoro water heating kettle, 12h is kept at 180 DEG C, treats that reaction kettle is down to room temperature, cylindric product is taken out, washed with alcohol, wash two
To three times, by product in freeze drier dry 12h to get to graphene oxide-alumina aerogels composite material.
Graphene oxide used in the present invention is prepared using modified Hummer methods, and preparation method is as follows：
The preparation of graphene oxide：It weighs 5g natural flake graphites and 2.5g sodium nitrate is added in the 130ml concentrated sulfuric acids,
2h is stirred under condition of ice bath, which is pre-oxidizing the stage；After pre-oxidation, the potassium permanganate of 15g is slowly added to, and in ice
The reaction was continued under the conditions of bath 2h, the stage are the low-temp reaction stage；Ice bath is removed, above-mentioned reactant is transferred to 35 DEG C of water-baths
In, the reaction was continued 1h, the stage is the medium temperature stage of reaction；230mL deionized waters are slowly added into above-mentioned reaction system, then
98 DEG C are warming up to, and reacts 30min at such a temperature, which is the pyroreaction stage；After the pyroreaction stage, add in
400ml deionized waters and 10ml hydrogen peroxide, and 1h is stirred, reaction terminates.After prepared by graphite oxide, pass through centrifuge washing
Mode remove foreign ion therein, such as potassium ion, manganese ion and sulfate ion.After washing, by obtained by
Graphite oxide slurry forced air drying is carried out under the conditions of 60 DEG C, it is spare.
Embodiment 1
Step 1: taking 0.3g graphite oxides, it is added in 100ml distilled water, in the ultrasonic cleaning instrument of 180W ultrasonic powers
Middle ultrasound 1h, is detached, the precipitation for filtering out lower floor takes upper solution with low speed centrifuge；
Step 2: taking the solution in 50ml step 1, the pH that solution is adjusted with weak aqua ammonia is 7.5, adds 2.4143g six
Aluminium chlorohydrate reacts 4h at 80 DEG C；
Step 3: treating to react to finish in step 2 to be cooled to room temperature, mixed solution is transferred to polytetrafluoro by magnetic agitation 0.5h
In water heating kettle, 12h is kept at 180 DEG C, treats that reaction kettle is down to room temperature, cylindric product is taken out, washed with alcohol, washed each two and arrive
Three times, by product in freeze drier dry 12h to get to graphene oxide-alumina aerogels composite material.
Embodiment 2
Step 1: taking 0.2g graphite oxides, it is added in 50ml water, it is ultrasonic in the ultrasonic cleaning instrument of 180W ultrasonic powers
1h is detached with low speed centrifuge, and the precipitation for filtering out lower floor takes upper solution；
Step 2: taking the solution in 50ml step 1, the pH that solution is adjusted with weak aqua ammonia is 6, adds six water of 1.2072g
Aluminium chloride is closed, reacts 5h at 100 DEG C；
Step 3: treating to react to finish in step 2 to be cooled to room temperature, mixed solution is transferred to polytetrafluoro by magnetic agitation 0.5h
In water heating kettle, 12h is kept at 180 DEG C, treats that reaction kettle is down to room temperature, cylindric product is taken out, washed with alcohol, washed each two and arrive
Three times, by product in freeze drier dry 12h to get to graphene oxide-alumina aerogels composite material.
Embodiment 3
Step 1: taking 0.25g graphite oxides, it is added in 75ml distilled water, in the ultrasonic cleaning instrument of 180W ultrasonic powers
Middle ultrasound 1h, is detached, the precipitation for filtering out lower floor takes upper solution with low speed centrifuge；
Step 2: taking the solution in 50ml step 1, the pH that solution is adjusted with weak aqua ammonia is 2, adds six water of 1.8107g
Aluminium chloride is closed, reacts 8h at 60 DEG C；
Step 3: treating to react to finish in step 2 to be cooled to room temperature, mixed solution is transferred to polytetrafluoro by magnetic agitation 0.5h
In water heating kettle, 12h is kept at 180 DEG C, treats that reaction kettle is down to room temperature, cylindric product is taken out, washed with alcohol, washed each two and arrive
Three times, by product in freeze drier dry 12h to get to graphene oxide-alumina aerogels composite material.
Embodiment 4
Step 1: taking 0.3g graphite oxides, it is added in 100ml distilled water, in the ultrasonic cleaning instrument of 180W ultrasonic powers
Middle ultrasound 1h, is detached, the precipitation for filtering out lower floor takes upper solution with low speed centrifuge；
Step 2: taking the solution in 50ml step 1, the pH that solution is adjusted with weak aqua ammonia is 6, adds six water of 1.2072g
Aluminium chloride is closed, reacts 7h at 70 DEG C；
Step 3: treating to react to finish in step 2 to be cooled to room temperature, mixed solution is transferred to polytetrafluoro by magnetic agitation 0.5h
In water heating kettle, 12h is kept at 180 DEG C, treats that reaction kettle is down to room temperature, cylindric product is taken out, washed with alcohol, washed each two and arrive
Three times, by product in freeze drier dry 12h to get to graphene oxide-alumina aerogels composite material.
Embodiment 5
Step 1: taking 0.25g graphite oxides, it is added in 80ml distilled water, in the ultrasonic cleaning instrument of 180W ultrasonic powers
Middle ultrasound 1h, is detached, the precipitation for filtering out lower floor takes upper solution with low speed centrifuge；
Step 2: taking the solution in 50ml step 1, the pH that solution is adjusted with weak aqua ammonia is 5, adds six water of 1.2072g
Aluminium chloride is closed, reacts 3h at 90 DEG C；
Step 3: treating to react to finish in step 2 to be cooled to room temperature, mixed solution is transferred to polytetrafluoro by magnetic agitation 0.5h
In water heating kettle, 12h is kept at 180 DEG C, treats that reaction kettle is down to room temperature, cylindric product is taken out, washed with alcohol, washed each two and arrive
Three times, by product in freeze drier dry 12h to get to graphene oxide-alumina aerogels composite material.
Fig. 1 is the scanning electron microscope (SEM) photograph of dried composite aerogel prepared by embodiment, as seen from the figure graphite oxide
Alkene piece is mutually accumulated to form three-dimensional network structure, and three-dimensional tufted aluminium oxide is dispersed in graphene oxide on piece, illustrates
Such preparation method can effectively prepare the aluminium oxide of good dispersion.
The above is only the preferred embodiment of the present invention, it should be pointed out that：For the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of preparation method of graphene oxide-alumina composite aeroge, it is characterised in that：Include the following steps：
Step 1: taking graphene oxide, it is added in dispersion solvent, the ultrasound 1h in instrument is cleaned by ultrasonic, with low speed centrifuge point
From the precipitation for filtering out lower floor takes upper solution；
Step 2: the solution that step 1 is taken to obtain, the pH of solution is adjusted with weak aqua ammonia and dilute hydrochloric acid, adds six chloride hydrates
Aluminium is reacted；
Step 3: treating to react to finish in step 2 to be cooled to room temperature, then mixed solution is transferred to polytetrafluoro by magnetic agitation 0.5h
In water heating kettle, 12h is kept at 180 DEG C, treats that reaction kettle is down to room temperature, cylindric product is taken out, washed with alcohol, washed each two and arrive
Three times, by product in freeze drier dry 12h to get to graphene oxide-alumina aerogels composite material；
In step 1, the graphene oxide is prepared by being modified Hummer methods, the specific steps are：It is 2 according to mass ratio:1 takes day
Right crystalline flake graphite and sodium nitrate are added in the concentrated sulfuric acid, and 2h is stirred under condition of ice bath, which is pre-oxidizing the stage；Pre-oxidation
After, potassium permanganate is slowly added to, wherein, the mass ratio of potassium permanganate and natural flake graphite is 3：1, and in condition of ice bath
Lower the reaction was continued 2h, which is the low-temp reaction stage；Ice bath is removed, above-mentioned reactant is transferred in 35 DEG C of water-baths, is continued
1h is reacted, which is the medium temperature stage of reaction；Deionized water is slowly added into above-mentioned reaction system, then raises temperature to 98 DEG C,
And 30min is reacted at such a temperature, which is the pyroreaction stage；After the pyroreaction stage, add in deionized water with
And hydrogen peroxide, and 1 h is stirred, reaction terminates；After prepared by graphite oxide, removed by way of centrifuge washing therein miscellaneous
Matter ion；After washing, obtained graphite oxide slurry is subjected to forced air drying under the conditions of 60 DEG C, it is spare.
2. the preparation method of graphene oxide according to claim 1-alumina composite aeroge, it is characterised in that：Step
In rapid one, the mass volume ratio of graphene oxide and dispersion solvent is 0.3:100~0.2:50g/mL.
3. the preparation method of graphene oxide according to claim 1 or 2-alumina composite aeroge, it is characterised in that：
In step 1, dispersion solvent is distilled water.
4. the preparation method of graphene oxide according to claim 1-alumina composite aeroge, it is characterised in that：Step
In rapid one, the ultrasonic power for being cleaned by ultrasonic instrument is 180 W.
5. the preparation method of graphene oxide according to claim 1-alumina composite aeroge, it is characterised in that：Step
In rapid one, the rotating speed of low speed centrifuge is 1000-8000rpm/min.
6. the preparation method of graphene oxide according to claim 1-alumina composite aeroge, it is characterised in that：Step
In rapid two, the volume mass ratio of step 1 acquired solution and Aluminium chloride hexahydrate is 50:1.2~50:2.4.
7. the preparation method of graphene oxide according to claim 1-alumina composite aeroge, it is characterised in that：Step
In rapid two, the pH of solution is adjusted to 1-12.
8. the preparation method of graphene oxide according to claim 1-alumina composite aeroge, it is characterised in that：Step
In rapid two, reaction temperature is 50-100 DEG C.
9. the preparation method of graphene oxide according to claim 1-alumina composite aeroge, it is characterised in that：Step
In rapid two, reaction time 0.5h-10h.
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| CN106634863A (en) * | 2016-12-30 | 2017-05-10 | 深圳市大族元亨光电股份有限公司 | Graphene based silica gel heat-conductive gasket and preparation method thereof |
| CN107324454B (en) * | 2017-07-07 | 2020-12-15 | 重庆三峡学院 | Copper ion-loaded graphene aerogel electrode material and preparation method thereof |
| CN108746580A (en) * | 2018-04-04 | 2018-11-06 | 北京石墨烯技术研究院有限公司 | A kind of dispersing method of graphene oxide in metal powder |
| CN110918010B (en) * | 2019-12-06 | 2022-02-01 | 石家庄铁道大学 | Preparation method of sepiolite-graphene composite aerogel |
| CN111097387B (en) * | 2020-01-19 | 2023-04-07 | 闽江师范高等专科学校 | Preparation of COF-1/GONs composite material and application thereof in detection of o-hydroxy phytohormones |
| CN111154368A (en) * | 2020-02-28 | 2020-05-15 | 厦门红彩化工有限公司 | Coating and preparation method thereof |
| CN111346632B (en) * | 2020-04-27 | 2023-12-15 | 山西恒投环保节能科技有限公司 | Catalyst composition for improving thermal efficiency of boiler and reducing emission of nitrogen oxides |
| CN113351201A (en) * | 2021-06-04 | 2021-09-07 | 武汉氢能与燃料电池产业技术研究院有限公司 | Thin film catalyst, precious metal/graphene composite thin film, and preparation method and application thereof |
| CN114956834A (en) * | 2022-06-14 | 2022-08-30 | 天津城建大学 | Reinforced graphene composite aerogel and preparation method thereof |
| CN115161790A (en) * | 2022-07-12 | 2022-10-11 | 凯盛家纺股份有限公司 | Preparation method of light and warm aerogel modified fiber |
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| CN101941693B (en) * | 2010-08-25 | 2012-07-25 | 北京理工大学 | Graphene aerogel and preparation method thereof |
| US9208919B2 (en) * | 2012-02-03 | 2015-12-08 | Massachusetts Institute Of Technology | Aerogels and methods of making same |
| CN102941042B (en) * | 2012-10-25 | 2016-03-09 | 北京理工大学 | A kind of Graphene/metal oxide hybrid aeroge, preparation method and application thereof |
| CN103157410A (en) * | 2013-03-13 | 2013-06-19 | 中国科学院化学研究所 | Aerogel preparation method |
| CN103977815A (en) * | 2014-05-22 | 2014-08-13 | 天津大学 | Catalyst carrying Pt-Ni alloy on silicon oxide-graphene, and preparation and application of catalyst |
| CN104250005B (en) * | 2014-09-11 | 2016-07-06 | 中国科学院上海应用物理研究所 | A kind of graphene aerogel and its preparation method and application |
| CN105271212B (en) * | 2015-11-30 | 2018-01-16 | 航天特种材料及工艺技术研究所 | A kind of graphene aerogel material and preparation method thereof |
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