CN105964193A - Method for preparing graphene oxide-alumina composite aerogel - Google Patents
Method for preparing graphene oxide-alumina composite aerogel Download PDFInfo
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- CN105964193A CN105964193A CN201610260244.2A CN201610260244A CN105964193A CN 105964193 A CN105964193 A CN 105964193A CN 201610260244 A CN201610260244 A CN 201610260244A CN 105964193 A CN105964193 A CN 105964193A
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- 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
- B01J13/0091—Preparation of aerogels, e.g. xerogels
Abstract
The invention discloses a method for preparing a graphene oxide-alumina composite aerogel, wherein the method comprises the following steps: taking graphene oxide, adding the graphene oxide into a dispersing solvent, carrying out ultrasonic treatment for 1 h in an ultrasonic cleaning instrument, separating with a low speed centrifuge, filtering out a lower precipitate, and taking an upper solution; taking the solution, adjusting the pH of the solution with dilute ammonia water and dilute hydrochloric acid, then adding aluminum chloride hexahydrate, and carrying out a reaction; and after the reaction in the second step is finished, cooling to room temperature, carrying out magnetic stirring for 0.5 h, then transferring the mixed solution into a polytetrafluoroethylene hydrothermal kettle, keeping for 12 h at the temperature of 180 DEG C, after the reaction kettle is cooled to room temperature, taking out a cylindrical product, washing the cylindrical product with alcohol and water for two to three times respectively, and drying the product for 12 h in a freeze dryer, to obtain the graphene oxide-alumina aerogel composite material. The ultra-light composite material prepared by the method has rich pore passage structure, can give full play to the excellent electrical conductivity of graphene, and has wide application prospect.
Description
Technical field
The present invention relates to organic and inorganic oxide composite aerogel preparation field, specifically a kind of oxidation stone
The preparation method of ink alkene-alumina composite aeroge.
Background technology
Aeroge is a kind of mutually to assemble the inside of composition with nanometer scale ultramicro powder and be full of gaseous state dispersion
The low density porous property solid material of medium, porosity may be up to 98.9%.It has now been found that, generation
Solid material the lightest in boundary, has the title of " solid-state cigarette ".Aeroge is except having the basic of nano material
Character, also have high porosity, low heat transfer coefficient, low-density, low electrical conductivity, low coefficient of refraction,
Many good characteristics such as low acoustic propagation velocity, fireclay insulating refractory, catalyst and catalyst carrier,
Silencing and damping material, novel high-energy particle detector, gas and water purification agent, special glass forerunner
The aspects such as body have boundless application prospect.Wherein graphene aerogel has light weight, intensity
Height, high-specific surface area, Heat stability is good and conductivity advantages of higher.The Graphene of three dimensional structure exists
Ultracapacitor, the oil aspect such as adsorbing material and catalyst carrier have huge potential use.
Aluminium oxide (Al2O3), industrial it is commonly called as alumina, is a kind of sizable chemical article of consumption.Its tool
Have that mechanical strength is big, Heat stability is good and the advantage such as cheap and easy to get, be a kind of very important industrial chemicals,
Therefore, it is possible to be widely used in 26S Proteasome Structure and Function pottery, medicine, environmental protection, adsorbent, catalyst
With fields such as catalyst carriers.But the aluminium oxide that present stage prepares easily is reunited, specific surface area is little,
If effective method therefore can be found to improve the dispersibility of aluminium oxide, by the adsoption catalysis etc. to aluminium oxide
Performance produces active influence, and this has great meaning to improving its commercial Application.
Summary of the invention
It is contemplated that the aluminium oxide prepared for present stage is easily reunited, specific surface area is little, stratiform aoxidizes
The problem of Graphene three-dimensional block difficulty molding, proposes a kind of graphene oxide-alumina composite aeroge
Preparation method, thus obtain with aluminium oxide and graphene oxide advantage and improve its inherent shortcoming
New material.
For achieving the above object, the technical solution used in the present invention is:
The preparation method of a kind of graphene oxide-alumina composite aeroge, comprises the steps:
Step one, take graphene oxide, join in dispersion solvent, ultrasonic 1h in ultrasonic cleaning instrument,
Separating with low speed centrifuge, the precipitation filtering out lower floor takes upper solution；
Step 2, take the solution that step one obtains, regulate the pH of solution with weak ammonia and dilute hydrochloric acid, then
Add Aluminium chloride hexahydrate, react；
Step 3, treat step 2 is reacted the complete room temperature that is cooled to, magnetic agitation 0.5h, then will be mixed
Close solution and proceed in polytetrafluoro water heating kettle, keep 12h, question response still to be down to room temperature at 180 DEG C, will
Cylindric product takes out, and washes with alcohol, washes each two to three times, is dried by product in freezer dryer
12h, i.e. obtains graphene oxide-alumina aerogels composite.
Further, in step one, described graphene oxide is prepared by modified Hummer method, specifically walks
Suddenly it is: be that 2:1 takes natural flake graphite and sodium nitrate is added in concentrated sulphuric acid, at ice according to mass ratio
Stirring 2h under the conditions of bath, this stage is the pre-oxidation stage；After pre-oxidation, it is slowly added to permanganic acid
Potassium, wherein, potassium permanganate is 3:1 with the mass ratio of natural flake graphite, and continues under condition of ice bath
Continuous reaction 2h, this stage is the low-temp reaction stage；Remove ice bath, above-mentioned reactant is transferred to 35 DEG C
In water-bath, continuing reaction 1h, this stage is the middle temperature stage of reaction；Slowly add in above-mentioned reaction system
Entering deionized water, then raise temperature to 98 DEG C, and react 30min at such a temperature, this stage is high temperature
The stage of reaction；After the pyroreaction stage terminates, add deionized water and hydrogen peroxide, and stir 1h,
Reaction terminates；Graphite oxide preparation after, remove by the way of centrifuge washing impurity therein from
Son；After washing, obtained graphite oxide slurry is carried out forced air drying under the conditions of 60 DEG C,
Standby.
Further, in step one, graphene oxide with dispersion solvent mass volume ratio be 0.3:100～
0.2:50g/mL。
Further, in step one, dispersion solvent is distilled water.
Further, in step one, the ultrasonic power of ultrasonic cleaning instrument is 180W.
Further, in step one, the rotating speed of low speed centrifuge is 4000rpm/min.
Further, in step 2, step one gained solution with the volume mass ratio of Aluminium chloride hexahydrate is
50:1.2～50:2.4.
Further, in step 2, the pH regulator of solution to 1-12.
Further, in step 2, reaction temperature is 50-100 DEG C.
Further, in step 2, the response time is 0.5h-10h.
The invention has the beneficial effects as follows: graphene oxide-alumina composite aeroge that the present invention provides
Preparation method, uses graphene oxide to be modified, by Aluminium chloride hexahydrate is scattered in oxidation stone
In ink alkene solution, using a step Hydrothermal Synthesis to obtain product, aluminium oxide has good dispersibility, this
Plant composite and there is abundant pore structure, there is the superior electrical conductivity energy of Graphene simultaneously, can conduct
Catalyst and catalyst carrier, adsorbing material etc., have higher actual application value.
Accompanying drawing explanation
Fig. 1 is to be the scanning electron microscope (SEM) photograph of dried composite aerogel prepared by embodiment.
Detailed description of the invention
Below in conjunction with embodiment the present invention done and further explain.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, with graphene oxide as raw material
Ultrasonic disperse in a solvent, adds a certain amount of Aluminium chloride hexahydrate and is stirred at reflux at a set temperature
Certain time, finally obtain cylindric wet gel with water heat transfer, wash through alcohol, wash after freezing
It is dried to obtain ultralight graphene oxide-alumina composite aeroge, specifically includes following steps:
Step one, take the graphene oxide prepared by modified Hummer method, join in dispersion solvent,
Ultrasonic 1h in the ultrasonic cleaning instrument of 180W ultrasonic power, with low speed centrifuge at rotating speed be
Separating in the case of 1000-8000rpm/min, the precipitation filtering out lower floor takes upper solution；
Wherein, graphene oxide is 0.3:100～0.2:50g/mL with the mass volume ratio of dispersion solvent.
Step 2, take the solution that step one obtains, regulate the pH of solution extremely with weak ammonia and dilute hydrochloric acid
1-12, adds Aluminium chloride hexahydrate, reacts 0.5h-10h in 50-100 DEG C；
Wherein, the volume mass of step one gained solution and Aluminium chloride hexahydrate than for 50:1.2～
50:2.4。
Step 3, treat step 2 is reacted the complete room temperature that is cooled to, magnetic agitation 0.5h, then will be mixed
Close solution and proceed in polytetrafluoro water heating kettle, keep 12h, question response still to be down to room temperature at 180 DEG C, will
Cylindric product takes out, and washes with alcohol, washes two to three times, and product is dried in freezer dryer 12h,
I.e. obtain graphene oxide-alumina aerogels composite.
Graphene oxide used in the present invention is to use modified Hummer method to prepare, and it is prepared
Method is as follows:
The preparation of graphene oxide: weigh 5g natural flake graphite and 130ml is added in 2.5g sodium nitrate to
In concentrated sulphuric acid, stirring 2h under condition of ice bath, this stage is the pre-oxidation stage；After pre-oxidation, slow
The slow potassium permanganate adding 15g, and under condition of ice bath, continue reaction 2h, this stage is low-temp reaction
Stage；Removing ice bath, be transferred to by above-mentioned reactant in 35 DEG C of water-baths, continue reaction 1h, this stage is
The middle temperature stage of reaction；In above-mentioned reaction system, it is slowly added to 230mL deionized water, then raises temperature to
98 DEG C, and react 30min at such a temperature, this stage is the pyroreaction stage；The pyroreaction stage ties
Shu Hou, adds 400ml deionized water and 10ml hydrogen peroxide, and stirs 1h, and reaction terminates.Oxygen
Graphite preparation after, remove by the way of centrifuge washing foreign ion therein, such as potassium from
Son, manganese ion and sulfate ion.After washing, by obtained graphite oxide slurry at 60 DEG C
Under the conditions of carry out forced air drying, standby.
Embodiment 1
Step one, take 0.3g graphite oxide, join in 100ml distilled water, in the ultrasonic merit of 180W
Ultrasonic 1h in the ultrasonic cleaning instrument of rate, separates with low speed centrifuge, and the precipitation filtering out lower floor takes upper strata
Solution；
Step 2, the solution taken in 50ml step one, be 7.5 with the pH of weak ammonia regulation solution, then
Add 2.4143g Aluminium chloride hexahydrate, at 80 DEG C, react 4h；
Step 3, treat step 2 is reacted the complete room temperature that is cooled to, magnetic agitation 0.5h, will mix molten
Liquid proceeds in polytetrafluoro water heating kettle, keeps 12h at 180 DEG C, and room temperature is down to by question response still, by cylinder
Shape product takes out, and washes with alcohol, washes each two to three times, and product is dried in freezer dryer 12h,
I.e. obtain graphene oxide-alumina aerogels composite.
Embodiment 2
Step one, take 0.2g graphite oxide, join in 50ml water, super at 180W ultrasonic power
Ultrasonic 1h in sound cleaning device, separates with low speed centrifuge, and the precipitation filtering out lower floor takes upper solution；
Step 2, the solution taken in 50ml step one, be 6 with the pH of weak ammonia regulation solution, then add
Enter 1.2072g Aluminium chloride hexahydrate, at 100 DEG C, react 5h；
Step 3, treat step 2 is reacted the complete room temperature that is cooled to, magnetic agitation 0.5h, will mix molten
Liquid proceeds in polytetrafluoro water heating kettle, keeps 12h at 180 DEG C, and room temperature is down to by question response still, by cylinder
Shape product takes out, and washes with alcohol, washes each two to three times, and product is dried in freezer dryer 12h,
I.e. obtain graphene oxide-alumina aerogels composite.
Embodiment 3
Step one, take 0.25g graphite oxide, join in 75ml distilled water, in the ultrasonic merit of 180W
Ultrasonic 1h in the ultrasonic cleaning instrument of rate, separates with low speed centrifuge, and the precipitation filtering out lower floor takes upper strata
Solution；
Step 2, the solution taken in 50ml step one, be 2 with the pH of weak ammonia regulation solution, then add
Enter 1.8107g Aluminium chloride hexahydrate, at 60 DEG C, react 8h；
Step 3, treat step 2 is reacted the complete room temperature that is cooled to, magnetic agitation 0.5h, will mix molten
Liquid proceeds in polytetrafluoro water heating kettle, keeps 12h at 180 DEG C, and room temperature is down to by question response still, by cylinder
Shape product takes out, and washes with alcohol, washes each two to three times, and product is dried in freezer dryer 12h,
I.e. obtain graphene oxide-alumina aerogels composite.
Embodiment 4
Step one, take 0.3g graphite oxide, join in 100ml distilled water, in the ultrasonic merit of 180W
Ultrasonic 1h in the ultrasonic cleaning instrument of rate, separates with low speed centrifuge, and the precipitation filtering out lower floor takes upper strata
Solution；
Step 2, the solution taken in 50ml step one, be 6 with the pH of weak ammonia regulation solution, then add
Enter 1.2072g Aluminium chloride hexahydrate, at 70 DEG C, react 7h；
Step 3, treat step 2 is reacted the complete room temperature that is cooled to, magnetic agitation 0.5h, will mix molten
Liquid proceeds in polytetrafluoro water heating kettle, keeps 12h at 180 DEG C, and room temperature is down to by question response still, by cylinder
Shape product takes out, and washes with alcohol, washes each two to three times, and product is dried in freezer dryer 12h,
I.e. obtain graphene oxide-alumina aerogels composite.
Embodiment 5
Step one, take 0.25g graphite oxide, join in 80ml distilled water, in the ultrasonic merit of 180W
Ultrasonic 1h in the ultrasonic cleaning instrument of rate, separates with low speed centrifuge, and the precipitation filtering out lower floor takes upper strata
Solution；
Step 2, the solution taken in 50ml step one, be 5 with the pH of weak ammonia regulation solution, then add
Enter 1.2072g Aluminium chloride hexahydrate, at 90 DEG C, react 3h；
Step 3, treat step 2 is reacted the complete room temperature that is cooled to, magnetic agitation 0.5h, will mix molten
Liquid proceeds in polytetrafluoro water heating kettle, keeps 12h at 180 DEG C, and room temperature is down to by question response still, by cylinder
Shape product takes out, and washes with alcohol, washes each two to three times, and product is dried in freezer dryer 12h,
I.e. obtain graphene oxide-alumina aerogels composite.
Fig. 1 is the scanning electron microscope (SEM) photograph of dried composite aerogel prepared by embodiment, as seen from the figure
Graphene oxide sheet is mutually piled up and is formed three-dimensional network structure, and three-dimensional tufted aluminium oxide is dispersed in
On graphene oxide sheet, illustrate that this kind of 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 art
For those of ordinary skill, under the premise without departing from the principles of the invention, it is also possible to make some improvement
And retouching, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (10)
1. the preparation method of graphene oxide-alumina composite aeroge, it is characterised in that: comprise the steps:
Step one, take graphene oxide, join in dispersion solvent, ultrasonic 1h in ultrasonic cleaning instrument, separate with low speed centrifuge, the precipitation filtering out lower floor takes upper solution；
Step 2, take the solution that step one obtains, regulate the pH of solution with weak ammonia and dilute hydrochloric acid, add Aluminium chloride hexahydrate, react；
Step 3, treat that reacting complete in step 2 is cooled to room temperature, magnetic agitation 0.5h, then mixed solution is proceeded in polytetrafluoro water heating kettle, 12h is kept at 180 DEG C, room temperature is down to by question response still, is taken out by cylindric product, washes with alcohol, washes each two to three times, product is dried in freezer dryer 12h, i.e. obtains graphene oxide-alumina aerogels composite.
2.According to claimThe preparation method of the graphene oxide described in 1-alumina composite aeroge, it is characterized in that: in step one, described graphene oxide is prepared by modified Hummer method, concretely comprise the following steps: be that 2:1 takes natural flake graphite and sodium nitrate is added in concentrated sulphuric acid according to mass ratio, stirring 2h under condition of ice bath, this stage is the pre-oxidation stage；After pre-oxidation, being slowly added to potassium permanganate, wherein, potassium permanganate is 3:1 with the mass ratio of natural flake graphite, and continues reaction 2h under condition of ice bath, and this stage is the low-temp reaction stage；Removing ice bath, be transferred to by above-mentioned reactant in 35 DEG C of water-baths, continue reaction 1h, this stage is the middle temperature stage of reaction；Being slowly added to deionized water in above-mentioned reaction system, then raise temperature to 98 DEG C, and react 30min at such a temperature, this stage is the pyroreaction stage；After the pyroreaction stage terminates, adding deionized water and hydrogen peroxide, and stir 1 h, reaction terminates；After graphite oxide preparation, by the way of centrifuge washing, remove foreign ion therein；After washing, obtained graphite oxide slurry is carried out under the conditions of 60 DEG C forced air drying, standby.
3.According to claimThe preparation method of the graphene oxide described in 1-alumina composite aeroge, it is characterised in that: in step one, graphene oxide is 0.3:100～0.2:50g/mL with the mass volume ratio of dispersion solvent.
4.According to claimThe preparation method of the graphene oxide described in 1 or 3-alumina composite aeroge, it is characterised in that: in step one, dispersion solvent is distilled water.
5.According to claimThe preparation method of the graphene oxide described in 1-alumina composite aeroge, it is characterised in that: in step one, the ultrasonic power of ultrasonic cleaning instrument is 180 W.
6.According to claimThe preparation method of the graphene oxide described in 1-alumina composite aeroge, it is characterised in that: in step one, the rotating speed of low speed centrifuge is 1000-8000rpm/min.
7.According to claimThe preparation method of the graphene oxide described in 1-alumina composite aeroge, it is characterised in that: in step 2, the volume mass of step one gained solution and Aluminium chloride hexahydrate is than for 50:1.2～50:2.4.
8.According to claimThe preparation method of the graphene oxide described in 1-alumina composite aeroge, it is characterised in that: in step 2, the pH regulator of solution to 1-12.
9.According to claimThe preparation method of the graphene oxide described in 1-alumina composite aeroge, it is characterised in that: in step 2, reaction temperature is 50-100 DEG C.
10.According to claimThe preparation method of the graphene oxide described in 1-alumina composite aeroge, it is characterised in that: in step 2, the response time is 0.5h-10h.
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| CN107324454A (en) * | 2017-07-07 | 2017-11-07 | 重庆三峡学院 | A kind of graphene aerogel electrode material for loading copper ion and preparation method thereof |
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| CN111097387A (en) * | 2020-01-19 | 2020-05-05 | 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 |
| 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 |
| CN111346632A (en) * | 2020-04-27 | 2020-06-30 | 山西恒投环保节能科技有限公司 | Catalyst composition for improving boiler thermal efficiency and reducing nitrogen oxide emission |
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