CN107235744A - A kind of preparation method of graphene aerosil - Google Patents
A kind of preparation method of graphene aerosil Download PDFInfo
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- CN107235744A CN107235744A CN201710407812.1A CN201710407812A CN107235744A CN 107235744 A CN107235744 A CN 107235744A CN 201710407812 A CN201710407812 A CN 201710407812A CN 107235744 A CN107235744 A CN 107235744A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/0045—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by a process involving the formation of a sol or a gel, e.g. sol-gel or precipitation processes
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/02—Macromolecular compounds
- C04B26/28—Polysaccharides or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/20—Mortars, concrete or artificial stone characterised by specific physical values for the density
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
Abstract
The present invention proposes a kind of preparation method of graphene aerosil, and composite aerogel is mainly made up of aerosil, graphene aerogel and chitosan.The method being related in the present invention, the characteristics of make use of the low thermal conductivity of aerosil, the low-density and high intensity of graphene aerogel and the cementation characteristic of chitosan, the mode for employing freeze-drying prepare graphene-enhancing silica aerogel material.A process for preparing composite good thermal and insulating performance and mechanical property are all kept under middle cryogenic conditions, significantly improve single SiO2The problem of fragility of aeroge big poor mechanical property；Density is relatively low, up to 96mg/cm3；Technique is simple, workable, cost is relatively low, and with SiO2The characteristic of two kinds of materials of aeroge and graphene aerogel.
Description
Technical field
The present invention relates to a kind of NEW TYPE OF COMPOSITE aerogel heat-insulating material and preparation method thereof, and in particular to and a kind of graphene-
The preparation method of aerosil.
Background technology
Aerosil is a kind of ultralight porous with three-dimensional net structure by decentralized medium of gas
Condensed state matter.Aerosil has the advantages that big chemical property stabilization, specific surface area, low-density and high porosity,
Therefore aeroge is active in the fields such as heat-insulating sound-insulating, adsoption catalysis always.In heat-insulation and heat-preservation field, current most study is
Aerosil.It is the key that aeroge is difficult to expansion application but aerosil poor mechanical property, fragility are big
Problem.People mainly solve this problem by two ways：(1) by adding polymer after reaction in-situ or immersion
Into the skeleton of SiO2 aeroges；(2) by being strengthened Ludox and fiber composite or Nano filling is added to airsetting
Strengthened in the nanostructured of glue.
Graphene aerogel has the microstructure of aeroge, at the same have lower density, higher mechanical strength and
Opacity, and the opacity of graphene can reduce conduct radiation, therefore graphene aerogel is expected to turn into a kind of new
The heat-insulating heat-preserving material of type.It is usually using graphene oxide solution as raw material, with electronation to obtain graphene aerogel
Method be the easiest and efficient mode.
Patent CN104826582A obtains the composite with adsorption capacity using graphene and the compound of silica.
Its preparation method is, in the mixing of graphene oxide solution, the NaOH aqueous solution and silicon source, to be added drop-wise to cetyl front three successively afterwards
In bromide aqueous ammonium, room temperature ageing adds after reducing agent, is placed in 70-100 DEG C of baking oven and collects 1-10h, obtain water-setting
Glue, resulting reaction product is washed, and dries 12-24h in vacuum drier -70~-90 DEG C, you can not removed
The graphene of template-aerosil, template is removed, and obtains graphene-meso-porous titanium dioxide silica aerogel.
Patent CN105217640A proposes a kind of preparation method of graphene oxide/SiO 2 hybrid aeroge, its
Preparation method is：Silicon dioxide gel and graphene oxide dispersion are first prepared respectively, are mixed and are obtained hybridized hydrogel, with
The freezing by liquid nitrogen and the freezing processing of freeze drier, obtain graphene oxide/SiO 2 hybrid aeroge afterwards.The party
Method cleverly controls refrigerating process, first pass through under liquid nitrogen environment by liquid/gas interface transform be gas/solid interface, so as to
The curved liquid surface in hole is avoided, the influence of capillary force is eliminated as far as possible.
Patent CN104860304A discloses a kind of silica with great specific surface area hydridization graphene aerogel and its preparation side
Method.By the mixing of Ludox and graphene oxide dispersion, the minimum silica nano particle of reacted generation particle diameter is dried
Afterwards so as to obtain silica with great specific surface area hydridization graphene aerogel.
The content of the invention
Technical problem：The problem of present invention solves aerosil fragility big poor mechanical property, and utilize graphite
The low-density and agglomeration property of alkene aeroge are good, prepare composite aerogel heat-barrier material.
Technical scheme：A kind of preparation method of graphene-aerosil of the present invention comprises the following steps：
The preparation of step 1. graphite oxide：In ice-water bath, the concentrated sulfuric acid is poured into reaction vessel, then by natural stone
The sodium nitrate of ink pours into ultrasonic agitation；Potassium permanganate is slowly added into reaction vessel again, continues to stir；Reaction vessel is turned
Move on in another water-bath, be warming up to 25-45 DEG C, distilled water is slowly added into reaction vessel, after be transferred in high temperature oil bath
Continue to stir, be eventually adding distilled water and 10%-40% oxydol H2O2, final mixture is in glassy yellow, product with 1%~
Final product is placed in 50-100 DEG C of vacuum drying chamber and dried to close to neutrality by 10% hydrochloric acid and distilled water centrifuge washing
12-24h, the sepia sheet output of gained is exactly graphite oxide GO；
Step 2, preparation graphene oxide solution：The graphite oxide GO for taking step 1 to obtain is dissolved in deionized water, is carried out
More than ultrasonic disperse 30min, centrifuges away unstripped graphite oxide and impurity, obtains the uniform graphite oxide of yellowish-brown
Alkene solution；
The preparation of step 3, graphene：Ethylenediamine is dissolved in deionized water in beaker, magnetic agitation for a period of time after, will
Described graphene oxide solution is added dropwise in ethylenediamine solution dropwise, is kept stirring for, and baking oven is placed in after mixed solution is sealed
In, gained black colloid is designated as redox graphene rGO；
The preparation of step 4, silicon dioxide gel：Silicon source, water and ethanol are taken successively respectively in container, keeps magnetic force to stir
Mix, salt acid for adjusting pH is added dropwise and reaches 2-5, is stood after stirring；N is then added dropwise, N-dimethylformamide and ammoniacal liquor regulation pH reach
To 6-7, now solution becomes sticking silicon dioxide gel；
The preparation of step 5, chitosan solution：Acetum is measured with graduated cylinder and is made into acetum with deionized water, then
Take chitosan stirring and dissolving in acetum, obtain chitosan solution；
The preparation of step 6, graphene-silica mixed sols：RGO that step 3, step 4, step 5 are respectively obtained,
Silicon dioxide gel, chitosan solution mixing and magnetic agitation, obtain mixed sols, are kept stirring for, N, N dimethyl is added dropwise to it
Formamide and ammoniacal liquor, stand, and wait gel；
The preparation of step 7, graphene-aerosil：The gel that step 6 is obtained is placed in low temperature refrigerator in advance
It is cold, 24-48h then is freeze-dried with freeze drier, vacuum drying oven drying is finally placed in, obtains graphene-silica gas
Gel.
Wherein：
Ultrasonic disperse frequency described in step 2 is 20-60KHZ, and ultrasonic power is 100W, the rotating speed of described centrifugation
For 1000-3000r/min.
The consumption of ethylenediamine described in step 3 is relevant with graphene oxide solution volume, ethylenediamine volume and graphite oxide
The volume ratio of alkene solution is 1：(300-800).
Silicon source, water and ethanol described in step 4, its mol ratio are silicon source：Deionized water：Ethanol=1:(2-6):(4-
9), mixing speed control is 500r/min-2500r/min.
The silicon source and the mol ratio of ammoniacal liquor being added dropwise in step 4 are 1：(10-3-1.5×10-3)。
Chitosan described in step 5, the quality of the chitosan and the mass ratio of graphene oxide are (1-8)：1.
In step 6, described magnetic stirring speed control is 500r/min-1500r/min.
In step 7, pre-coo time is 1-3h, and drying temperature is 60 DEG C -100 DEG C.
Beneficial effect：The present invention has the advantages that with other preparation methods：
1st, with low cost using different raw materials as silicon source, preparation process eliminates cumbersome during constant pressure and dry
Surface be modified and solvent displacement etc. operation, saved the time, improved efficiency.
2nd, the graphene for preparing of the present invention-aerosil it is blockiness good, mechanical property is good, and with relatively low
Thermal conductivity factor, can be with as little as 0.037W/ (mK), density as little as 96mg/cm3。
3rd, the skeleton structure of aerogel composite is good, and with micron-sized aperture, be expected to catalyst carrier,
Adsorb with separating, the field such as high temperature insulating is widely used.
Brief description of the drawings
Fig. 1 is graphene-the SEM figures of aerosil.
Fig. 2 is graphene-the stress-strain diagram of aerosil.
Fig. 3 is graphene-aerosil thermal conductivity is with graphene changes of contents figure.
Embodiment
Graphene is provided below-the embodiment of silica aerogel material, as further to the present invention
Describe in detail.
Embodiment 1
A. the synthesis of graphite oxide
In ice-water bath, 21ml 98% concentrated sulfuric acid is poured into flask, then by 1g native graphites, 0.5g nitre
Sour sodium pours into ultrasonic agitation 45min in 250ml round-bottomed flask；Magnetic agitation 30min, the potassium permanganate for weighing 3g is slowly added to
Into flask, continue to stir 45min.Flask is transferred in another water-bath, 35 DEG C are warming up to, continues to stir 30min, measures
23ml distilled water is slowly added into flask, after be transferred in 98 DEG C of oil bath continue stir 15min, be eventually adding 140ml
Distilled water and 20mL 30% hydrogen peroxide.Final mixture is in glassy yellow.Product 500mL 5% hydrochloric acid and distilled water
Centrifuge washing is neutral to approaching.Final product is placed in 60 DEG C of vacuum drying chambers and dries 24h, the sepia sheet production of gained
Thing is exactly graphite oxide GO.
The preparation of b graphene oxide solutions
Take 60mg graphite oxides to grind, be dissolved in 10ml deionized waters, after ultrasonic disperse 30min, centrifugal treating is removed
Impurity, obtains the filemot graphene oxide solution of homogeneous.
C. the preparation of graphene
40 μ L ethylenediamine is dissolved in deionized water in beaker, after magnetic agitation 10min, by ready graphite oxide
Alkene solution is added dropwise in ethylenediamine solution dropwise, is kept stirring for 30min.It is 75 DEG C of baking ovens that temperature is placed in after mixed solution is sealed
Middle 6h, obtains black colloid for rGO.
D. the preparation of silicon dioxide gel
20.8g silicon sources, 7.2g water and 32.2g ethanol are weighed successively respectively in beaker, magnetic agitation 30min, drop is kept
Plus appropriate hydrochloric acid regulation pH reaches 3, is kept stirring for after 30min standing 8h；1mlN, N-dimethylformamide and 0.5ml is then added dropwise
Ammoniacal liquor (0.3mol/L) regulation pH, which reaches, obtains 6, obtains colloidal sol.
The preparation of e chitosan solutions
The acetum and deionized water that 2ml is measured with graduated cylinder are made into 100ml2% acetums, then weigh 2g shell
Glycan stirring and dissolving obtains 100ml chitosan solutions in 2% acetum.
F. graphene-the preparation of silica mixed sols
The graphene colloid being previously obtained, silicon dioxide gel, 10ml chitosan solutions are mixed and magnetic agitation
20min, obtains mixed sols.20min is kept stirring for, 1mlN, N-dimethylformamide and 1ml ammoniacal liquor is added dropwise to it, is stood
10min, waits gel.
G. graphene-the preparation of aerosil
Gel obtained in the previous step is placed in precooling 2h in low temperature refrigerator, precooling temperature is -40 DEG C, then with freeze-drying
Machine is freeze-dried 48h, and the vacuum drying oven for being finally placed in 60 DEG C dries 2h, obtains graphene-aerosil.
Embodiment 2
A. the synthesis of graphite oxide
In ice-water bath, 22ml 98% concentrated sulfuric acid is poured into flask, then by 1g native graphites, 0.5g nitre
Sour sodium pours into ultrasonic agitation 50min in 250ml round-bottomed flask；Magnetic agitation 45min, the potassium permanganate for weighing 3g is slowly added to
Into flask, continue to stir 60min.Flask is transferred in another water-bath, 35 DEG C are warming up to, continues to stir 35min, measures
25ml distilled water is slowly added into flask, after be transferred in 98 DEG C of oil bath continue stir 15min, be eventually adding 140ml
Distilled water and 20mL 30% hydrogen peroxide, product is with 500mL 3% watery hydrochloric acid and distilled water centrifuge washing in
Property.Final product is placed in 60 DEG C of vacuum drying chambers and dries 24h, the sepia sheet output of gained is exactly graphite oxide
GO。
The preparation of b graphene oxide solutions
Take 120mg graphite oxides to grind, be dissolved in 12ml deionized waters, after ultrasonic disperse 45min, centrifugal treating is removed
Impurity, obtains the filemot graphene oxide solution of homogeneous.
C. the preparation of graphene
25 μ L ethylenediamine is dissolved in deionized water in beaker, after magnetic agitation 10min, by ready graphite oxide
Alkene solution is added dropwise in ethylenediamine solution dropwise, is kept stirring for 45min.It is 85 DEG C of baking ovens that temperature is placed in after mixed solution is sealed
Middle 4h, obtains black colloid for rGO.
D. the preparation of silicon dioxide gel
20.8g silicon sources, 7.2g water and 32.2g ethanol are weighed successively respectively in beaker, magnetic agitation 40min, drop is kept
Plus appropriate hydrochloric acid regulation pH reaches 3.5, is kept stirring for after 40min standing 9h；Then be added dropwise 1mlN, N-dimethylformamide and
0.5ml ammoniacal liquor (0.3mol/L) regulation pH, which reaches, obtains 6.5, obtains colloidal sol.
The preparation of e chitosan solutions
The acetum and deionized water that 2ml is measured with graduated cylinder are made into 100ml2% acetums, then weigh 2g shell
Glycan stirring and dissolving obtains 100ml chitosan solutions in 2% acetum.
F. graphene-the preparation of silica mixed sols
The graphene colloid being previously obtained, silicon dioxide gel, 10ml chitosan solutions are mixed and magnetic agitation
20min, obtains mixed sols.30min is kept stirring for, 0.5mlN, N-dimethylformamide and 0.5ml ammoniacal liquor is added dropwise to it, is stood
10min, waits gel.
G. graphene-the preparation of aerosil
Gel obtained in the previous step is placed in precooling 3h in low temperature refrigerator, precooling temperature is -35 DEG C, then with freeze-drying
Machine is freeze-dried 48h, and the vacuum drying oven for being finally placed in 70 DEG C dries 2h, obtains graphene-aerosil.
Embodiment 3
A. the synthesis of graphite oxide
In ice-water bath, 21ml 98% concentrated sulfuric acid is poured into flask, then by 1g native graphites, 0.5g nitre
Sour sodium pours into ultrasonic agitation 45min in 250ml round-bottomed flask；Magnetic agitation 30min, the potassium permanganate for weighing 3g is slowly added to
Into flask, continue to stir 45min-60min.Flask is transferred in another water-bath, 35 DEG C are warming up to, continues to stir 30min,
The distilled water for measuring 23ml is slowly added into flask, after be transferred in 98 DEG C of oil bath continue stir 15min, be eventually adding
140ml distilled water and 20mL30% hydrogen peroxide.Final mixture is in glassy yellow.Hydrochloric acid and steaming of the product with 500mL 5%
Distilled water centrifuge washing is neutral to approaching.Final product is placed in 60 DEG C of vacuum drying chambers and dries 24h, the brown color chips of gained
Shape product is exactly graphite oxide GO.
The preparation of b graphene oxide solutions
Take 180mg graphite oxides to grind, be dissolved in 15ml deionized waters, after ultrasonic disperse 40min, centrifugal treating is removed
Impurity, obtains the filemot graphene oxide solution of homogeneous.
C. the preparation of graphene
A small amount of ethylenediamine is dissolved in deionized water in beaker, after magnetic agitation 10min, by ready graphite oxide
Alkene solution is added dropwise in ethylenediamine solution dropwise, is kept stirring for 30min.It is 85 DEG C of baking ovens that temperature is placed in after mixed solution is sealed
Middle 5h, obtains black graphene colloid.
D. the preparation of silicon dioxide gel
20.8g silicon sources, 7.2g water and 32.2g ethanol are weighed successively respectively in beaker, magnetic agitation 30min, drop is kept
Plus appropriate hydrochloric acid regulation pH reaches 3.5, is kept stirring for after 50min standing 10h；Then be added dropwise 1mlN, N-dimethylformamide and
0.6ml ammoniacal liquor (0.3mol/L) regulation pH, which reaches, obtains 6, obtains colloidal sol.
The preparation of e chitosan solutions
The acetum and deionized water that 2ml is measured with graduated cylinder are made into 100ml2% acetums, then weigh 2g shell
Glycan stirring and dissolving obtains 100ml chitosan solutions in 2% acetum.
F. graphene-the preparation of silica mixed sols
The graphene colloid being previously obtained, silicon dioxide gel, 10ml chitosan solutions are mixed and magnetic agitation
30min, obtains mixed sols.30min is kept stirring for, 1mlN, N-dimethylformamide and 1.5ml ammoniacal liquor is added dropwise to it, one is stood
The section time, wait gel.
G. graphene-the preparation of aerosil
Gel obtained in the previous step is placed in precooling 3h in low temperature refrigerator, precooling temperature is -40 DEG C, then with freeze-drying
Machine is freeze-dried 48h, and the vacuum drying oven for being finally placed in 90 DEG C dries 3h, obtains graphene-aerosil.
Embodiment 4
A. the synthesis of graphite oxide
In ice-water bath, 21ml 98% concentrated sulfuric acid is poured into flask, then by 1g native graphites, 0.5g nitre
Sour sodium pours into ultrasonic agitation 45min in 250ml round-bottomed flask；Magnetic agitation 30min, the potassium permanganate for weighing 3g is slowly added to
Into flask, continue to stir 45min-60min.Flask is transferred in another water-bath, 35 DEG C are warming up to, continues to stir 30min,
The distilled water for measuring 23ml is slowly added into flask, after be transferred in 98 DEG C of oil bath continue stir 15min, be eventually adding
140ml distilled water and 20mL30% hydrogen peroxide.Final mixture is in glassy yellow.Hydrochloric acid and steaming of the product with 500mL 5%
Distilled water centrifuge washing is neutral to approaching.Final product is placed in 60 DEG C of vacuum drying chambers and dries 24h, the brown color chips of gained
Shape product is exactly graphite oxide GO.
The preparation of b graphene oxide solutions
Take 240mg graphite oxides to grind, be dissolved in 20ml deionized waters, after ultrasonic disperse 45min, centrifugal treating is removed
Impurity, obtains the filemot graphene oxide solution of homogeneous.
C. the preparation of graphene
A small amount of ethylenediamine is dissolved in deionized water in beaker, after magnetic agitation 20min, by ready graphite oxide
Alkene solution is added dropwise in ethylenediamine solution dropwise, is kept stirring for 45min.It is 95 DEG C of baking ovens that temperature is placed in after mixed solution is sealed
Middle 3h, obtains black graphene colloid.
D. the preparation of silicon dioxide gel
20.8g silicon sources, 7.2g water and 32.2g ethanol are weighed successively respectively in beaker, magnetic agitation 35min, drop is kept
Plus appropriate hydrochloric acid regulation pH reaches 3, is kept stirring for after 30min standing 8h；1mlN, N-dimethylformamide and 0.7ml is then added dropwise
Ammoniacal liquor (0.3mol/L) regulation pH, which reaches, obtains 6.5, obtains colloidal sol.
The preparation of e chitosan solutions
The acetum and deionized water that 2ml is measured with graduated cylinder are made into 100ml2% acetums, then weigh 2g shell
Glycan stirring and dissolving obtains 100ml chitosan solutions in 2% acetum.
F. graphene-the preparation of silica mixed sols
The graphene colloid being previously obtained, silicon dioxide gel, 10ml chitosan solutions are mixed and magnetic agitation
30min, obtains mixed sols.30min is kept stirring for, 1mlN, N-dimethylformamide and 1.5ml ammoniacal liquor is added dropwise to it, one is stood
The section time, wait gel.
G. graphene-the preparation of aerosil
Gel obtained in the previous step is placed in precooling 3h in low temperature refrigerator, precooling temperature is -35 DEG C, then with freeze-drying
Machine is freeze-dried 48h, and the vacuum drying oven for being finally placed in 80 DEG C dries 2h, obtains graphene-aerosil.Work as oxidation
When graphene volume is 120mg, graphene is measured-the thermal conductivity factor of aerosil is 0.037W/ (mK), now
The compression strength measured is 0.45MPa, significantly larger than aerosil compression strength.
Claims (8)
1. a kind of preparation method of graphene-aerosil, it is characterised in that the preparation method comprises the following steps：
The preparation of step 1. graphite oxide：In ice-water bath, the concentrated sulfuric acid is poured into reaction vessel, then by native graphite
Sodium nitrate pours into ultrasonic agitation；Potassium permanganate is slowly added into reaction vessel again, continues to stir；Reaction vessel is transferred to
In another water-bath, be warming up to 25-45 DEG C, distilled water be slowly added into reaction vessel, after to be transferred to high temperature oil bath relaying continuous
Stirring, is eventually adding distilled water and 10%-40% oxydol H2O2, final mixture is in glassy yellow, and product is with 1%~10%
Hydrochloric acid and distilled water centrifuge washing to close to neutrality, by final product be placed in 50-100 DEG C of vacuum drying chamber dry 12-
24h, the sepia sheet output of gained is exactly graphite oxide GO；
Step 2, preparation graphene oxide solution：The graphite oxide GO for taking step 1 to obtain is dissolved in deionized water, carries out ultrasound
Scattered more than 30min, centrifuges away unstripped graphite oxide and impurity, obtains the uniform graphene oxide of yellowish-brown molten
Liquid；
The preparation of step 3, graphene：Ethylenediamine is dissolved in deionized water in beaker, magnetic agitation for a period of time after, will be described
Graphene oxide solution be added dropwise to dropwise in ethylenediamine solution, be kept stirring for, be placed in after mixed solution is sealed in baking oven, institute
Obtain black colloid and be designated as redox graphene rGO；
The preparation of step 4, silicon dioxide gel：Silicon source, water and ethanol are taken successively respectively in container, magnetic agitation, drop is kept
Plus salt acid for adjusting pH reaches 2-5, stood after stirring；N is then added dropwise, N-dimethylformamide and ammoniacal liquor regulation pH reach and obtain 6-
7, now solution become sticking silicon dioxide gel；
The preparation of step 5, chitosan solution：Acetum is measured with graduated cylinder and is made into acetum with deionized water, shell is then taken
Glycan stirring and dissolving obtains chitosan solution in acetum；
The preparation of step 6, graphene-silica mixed sols：RGO, the dioxy that step 3, step 4, step 5 are respectively obtained
SiClx colloidal sol, chitosan solution mixing and magnetic agitation, obtain mixed sols, are kept stirring for, N, N dimethyl formyl is added dropwise to it
Amine and ammoniacal liquor, stand, and wait gel；
The preparation of step 7, graphene-aerosil：The gel that step 6 is obtained is placed in precooling in low temperature refrigerator, with
24-48h is freeze-dried with freeze drier afterwards, vacuum drying oven drying is finally placed in, obtains graphene-aerosil.
2. the preparation method of graphene-aerosil according to claim 1, it is characterised in that institute in step 2
Ultrasonic disperse frequency is stated for 20-60KHZ, ultrasonic power is 100W, the rotating speed of described centrifugation is 1000-3000r/min.
3. the preparation method of graphene-aerosil as claimed in claim 1, it is characterised in that described in step 3
The consumption of ethylenediamine is relevant with graphene oxide solution volume, and the volume ratio of ethylenediamine volume and graphene oxide solution is 1：
(300-800)。
4. the preparation method of graphene-aerosil as claimed in claim 1, it is characterised in that described in step 4
Silicon source, water and ethanol, its mol ratio be silicon source：Deionized water：Ethanol=1:(2-6):(4-9), mixing speed control be
500r/min-2500r/min。
5. the preparation method of graphene-aerosil as claimed in claim 1, it is characterised in that dripped in step 4
Plus silicon source and ammoniacal liquor mol ratio be 1：(10-3-1.5×10-3)。
6. the preparation method of graphene-aerosil as claimed in claim 1, it is characterised in that described in step 5
Chitosan, the quality of the chitosan and the mass ratio of graphene oxide are (1-8)：1.
7. the preparation method of graphene-aerosil as claimed in claim 1, it is characterised in that described in step 6
Magnetic stirring speed control be 500r/min-1500r/min.
8. the preparation method of graphene-aerosil as claimed in claim 1, it is characterised in that in step 7, precooling
Time is 1-3h, and drying temperature is 60 DEG C -100 DEG C.
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| CN108083262A (en) * | 2018-02-01 | 2018-05-29 | 济南大学 | A kind of preparation method of redox graphene-silica block aeroge |
| CN108325507A (en) * | 2018-03-30 | 2018-07-27 | 江苏大学 | A kind of mesoporous silicon fiml of graphene oxide doped and its preparation method and application |
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