CN108275678B - Graphene oxide/ionic liquid nanocomposite and preparation method thereof - Google Patents
Graphene oxide/ionic liquid nanocomposite and preparation method thereof Download PDFInfo
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- CN108275678B CN108275678B CN201711456297.2A CN201711456297A CN108275678B CN 108275678 B CN108275678 B CN 108275678B CN 201711456297 A CN201711456297 A CN 201711456297A CN 108275678 B CN108275678 B CN 108275678B
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Abstract
The invention provides a graphene oxide/ionic liquid nanocomposite and a preparation method thereof. The preparation method can enable graphene oxide and ionic liquid to achieve nanoscale uniform compounding, and can realize the preparation of the liquid, non-flowing soft solid and hard solid graphene oxide/ionic liquid composite material, and the method can endow the composite material with various plastic deformation capabilities by regulating and controlling the mass ratio of the two components and the transverse dimension of graphene oxide lamella, and has strong processability and wide application prospect.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to a graphene oxide/ionic liquid nanocomposite and a preparation method thereof, and belongs to the technical field of composite material preparation.
[ background of the invention ]
The graphene oxide is an intermediate product of graphene prepared by graphite through a redox method, the transverse size of the graphene oxide is in the range of tens of nanometers to hundreds of micrometers, the graphene oxide with different sizes has different performances and application fields, the surface of the graphene oxide has rich oxygen-containing groups, the graphene oxide can be well dispersed in water, the graphene oxide has incomparable excellent solution processing performance and chemical reaction activity, and the graphene oxide has obvious advantages in the aspects of preparation, processing and application of graphene-based materials. The ionic liquid is a substance which is completely composed of anions and cations and is in a liquid state at room temperature. Ionic liquids are diverse in variety, not only excellent green solvents (no vapor pressure, non-volatile, easy to separate, easy to recycle, and good in biocompatibility), but also multifunctional. Due to the unique properties of the graphene oxide and the ionic liquid, the graphene oxide/ionic liquid composite material has great application potential in the aspects of processing, modification, application and the like of graphene-based materials.
At present, there is a related technology for preparing a composite material by mixing an ionic liquid and graphene oxide, for example, chinese patent No. CN 103102514B discloses grinding an ionic liquid and graphene oxide powder to prepare a composite material, and then modifying natural rubber with the composite material to achieve a good modification effect. However, the solid grinding method can destroy the size of the graphene oxide, and has the problems of uneven mixing and dispersion and narrow adjustable range of the mixture ratio of the two components. The Chinese patent with patent number CN 101985354A uniformly mixes graphene oxide aqueous dispersion and amino ionic liquid, then carries out ultrasonic heating reaction, and finally carries out filtration, washing and drying to obtain the ionic liquid modified graphene oxide material. In the method, the ionic liquid is limited to the amino ionic liquid, other acidic ionic liquids are difficult to be uniformly mixed with the graphene oxide, and the size of the graphene oxide is seriously damaged due to the ultrasonic treatment in the preparation process; the prepared material is powder of a small amount of ionic liquid modified graphene oxide, a large amount of ionic liquid is washed away, and the plasticity and the forming and processing capability are poor. In conclusion, no method can simultaneously achieve the requirements of nanoscale uniform compounding, graphene oxide size maintenance and ionic liquid diversity for the graphene oxide/ionic liquid composite material, and no method can be simultaneously suitable for preparing flowable liquid and non-flowable soft solid and hard solid graphene oxide/ionic liquid nanocomposite materials.
[ summary of the invention ]
[ problem to be solved ]
All reported methods can not simultaneously meet the requirements of nano-scale uniform compounding of two components of graphene oxide/ionic liquid, variety diversity of ionic liquid and preparation of various aggregation-state graphene oxide/ionic liquid nanocomposite materials. The invention aims to provide a method for preparing a graphene oxide/ionic liquid composite material, which solves the problems and prepares a graphene oxide/ionic liquid nanocomposite material with extremely high processing performance.
[ solution ]
The preparation method provided by the invention comprises the following steps: firstly, the invention discloses a method for the auxiliary dispersion of an alkaline compound, which is used for uniformly mixing an acidic ionic liquid and a graphene oxide aqueous dispersion, wherein the method can achieve nanoscale uniform compounding when two components are mixed, then water in the mixed solution is removed by rotary evaporation, the graphene oxide and the ionic liquid are ensured to be uniformly compounded, and finally, the nano composite material is obtained by completely drying.
The specific process steps of the invention are as follows:
step (1): preparing graphene oxide aqueous dispersion. The transverse size of the graphene oxide is 0.01-200 microns; the concentration range of the graphene oxide aqueous dispersion is 0.001-20 mg per ml.
Step (2): the ionic liquid is diluted by adding distilled water. The ionic liquid concentration is between 0.001 and 2000 milligrams per milliliter.
And (3): and (3) adding an alkaline compound into the ionic liquid aqueous solution obtained in the step (2) to adjust the ionic liquid aqueous solution to be alkaline, wherein the pH value ranges from 8 to 14.
And (4): and (3) mixing the graphene oxide aqueous dispersion obtained in the step (1) and the ionic liquid aqueous solution obtained in the step (3) and uniformly stirring, wherein a violent mixing mode is not used, and the size of the graphene oxide is kept.
And (5): and (4) heating and evaporating to remove water in the mixed solution obtained in the step (4), and finally completely drying to obtain the graphene oxide/ionic liquid nano composite material.
In the step (1), the preparation method of graphene oxide in the step one is not limited, and all methods are within the range. Preferably, a modified hummer's method is used.
In the step (3), the alkaline compound comprises one or more of ammonia water, sodium hydroxide, potassium hydroxide, calcium hydroxide, sodium carbonate and sodium bicarbonate. Preferably, ammonia is used as the auxiliary dispersant.
In the step (4), the stirring mode is one or more of a stirring paddle, a magnetic rotor and an oscillation method, the stirring rotating speed is not more than 800 revolutions per minute, and the oscillation frequency is not more than 20 Hz. Preferably, the rotor is used for slow stirring, and the stirring speed is 10-500 rpm.
In the step (5), the temperature of the reduced pressure rotary distillation is not higher than 60 ℃, and preferably, the distillation temperature is between 40 and 60 ℃; the drying method comprises one or more of natural evaporation, heating drying and vacuum drying, preferably, the vacuum drying method is adopted, and the drying temperature is 30-60 ℃.
The ionic liquid described herein is one or more of amino ionic liquids or acidic ionic liquids such as 1-aminoethyl-3-methylimidazolium hexafluorophosphate [ H2NC2MIM ] PF6, 1- (3-propylamino) -3-butylimidazolium tetrafluoroborate aPbim BF4, tetrabutylphosphonium glycinate P444Gly, tetrabutylphosphonium alanate P444Ala, sulfonate 1-methyl-3-allylimidazolium ionic liquid, [ Bmim ] + [ H2PO4] -phosphate 1-methyl-3-allylimidazolium ionic liquid, [ Hmim ] + [ HSO4] -sulfonate methylimidazolium ionic liquid, [ Hmim ] + [ H2PO4] - [ Hmim ] + [ HSO4] -phosphate methylimidazolium ionic liquid at room temperature.
The graphene oxide/ionic liquid nanocomposite prepared by the method is characterized in that: in the composite material, graphene oxide and ionic liquid are uniformly compounded in a nanometer scale, and the mass ratio of the graphene oxide to the ionic liquid is 9999: 1-1: 9999, the lateral dimension of the graphene oxide is 0.01-200 microns. The mass ratio is preferably 999: 1-1: 999, more preferably 99: 1-1: 99.
a method for complexing graphene oxide with an ionic liquid at an arbitrary ratio without destroying the size of the graphene oxide, characterized in that in the method, an alkaline compound is added to an ionic liquid aqueous solution to adjust the pH value to 8-14, and then the graphene oxide is complexed with the alkaline compound.
Wherein the pH value of the ionic liquid aqueous solution is adjusted to 8-14 by adding an alkaline compound, more preferably the pH value is 9-12, and still more preferably the pH value is 10-11.
[ advantageous effects ]
Due to the adoption of the technical scheme, the invention has the following advantages:
1. the graphene oxide and the acidic ionic liquid can be uniformly mixed in an alkaline water phase, and two components in the prepared graphene oxide/ionic liquid nano composite material are uniformly compounded in a nanometer level.
2. The size of the graphene oxide in the prepared graphene oxide/ionic liquid nanocomposite is hardly influenced in the preparation process, and the controllability is realized. Because the graphene oxide aqueous dispersion and the acidic ionic liquid are mixed to agglomerate and flocculate, in order to enable the graphene oxide aqueous dispersion and the acidic ionic liquid to be uniformly compounded, the prior art at least comprises a powerful mixing mode of ultrasound, strong shearing and grinding, graphene lamellar layers can be damaged to different degrees in the preparation process, and the size of the graphene lamellar layers is reduced.
3. The material state and rheological property of the prepared graphene oxide/ionic liquid nanocomposite material can be regulated and controlled in a wide range, the material state can be from a flowing liquid state to a non-flowing soft solid state and a non-flowing hard solid state, and the composite material has various plastic deformation capacities and extremely high processability.
4. The preparation method of the graphene oxide/ionic liquid nanocomposite is simple and easy to operate, high in expandability, economical and environment-friendly.
5. The provided graphene oxide/ionic liquid nanocomposite can be used as a precursor for assembling a functional material and a graphene-based material, and has unique advantages and wide application prospects.
[ description of the drawings ]
Fig. 1 is evidence that the acidic ionic liquid and the graphene oxide aqueous dispersion in the invention can be uniformly dispersed by adjusting the PH with alkali. The blend on the left of the figure was not PH adjusted and significant flocculation occurred (comparative example 1); the right side is the blended solution with alkali to adjust pH, no flocculation and uniform mixing (example 8).
Fig. 2 is a photograph showing that graphene oxide is uniformly and stably dispersed in an alkaline liquid phase at a mass ratio of graphene oxide/ionic liquid of 0.0001 and 10000 (examples 5 and 6), and it is approximately demonstrated that graphene oxide and an acidic ionic liquid can be uniformly mixed in water at an arbitrary ratio by using an alkaline compound-assisted dispersion method.
Fig. 3 is XRD spectra of graphene oxide/ionic liquid composites (examples 1, 7, 8, 9, and 10) with various ratios, and no aggregation peak of graphene oxide appears in all XRD spectra, which indicates that graphene oxide is in a single-layer dispersion state in the composite, that is, the graphene oxide layers in nanometer are uniformly dispersed, and graphene oxide and ionic liquid are uniformly mixed in nanometer.
Fig. 4 is an AFM image of different sizes of graphene oxide prepared (examples 1, 2, 3).
Fig. 5 is SEM images of graphene oxide/ionic liquid composites (examples 1, 2, 3) prepared from graphene oxide of different sizes. The method can well ensure that the size of the graphene oxide is not damaged.
Fig. 6 shows that the graphene oxide/ionic liquid composite pasty material prepared by the method (examples 1, 7 and 8) has extremely strong processability and can be easily processed into various shapes.
[ detailed description ] embodiments
The invention will now be further described with reference to the following examples, which are intended to be illustrative only and not to limit the scope of the invention.
Example 1.
Using 32-mesh crystalline flake graphite with the purity of 99.5% as a raw material, preparing graphene oxide with the average size of about 15 microns by an improved Hummer's chemical method, preparing 10 milligrams per milliliter of Graphene Oxide (GO) aqueous dispersion, adding 5 milliliters of GO aqueous dispersion into a round-bottomed flask, adding 45 milliliters of deionized water, and preparing the concentration of the GO aqueous dispersion into 1 milligram per milliliter; taking 1 ml of ionic liquid (1-allyl-3-methylimidazolium chloride), adding 49 ml of water to dilute the ionic liquid, adding sodium hydroxide powder into an ionic liquid aqueous solution, slowly stirring for dissolving, and adjusting the pH value to 9; mixing the prepared graphene oxide aqueous dispersion and the ionic liquid solution, and uniformly stirring by using a stirring paddle at the rotating speed of 200 revolutions per minute; and (3) carrying out reduced pressure rotary distillation on the mixed solution at the distillation temperature of 40-60 ℃ for about 2-5 hours when the proportion of the graphene oxide/the ionic liquid is 50 mg per ml, taking out the prepared composite material, and carrying out vacuum drying at the temperature of 60 ℃ for 24 hours to obtain the graphene oxide/ionic liquid nanocomposite.
Example 2.
The process flow is the same as that of example 1, except that 32-mesh crystalline flake graphite is replaced by 325-mesh crystalline flake graphite, and graphene oxide with the average size of about 8 microns is prepared.
Example 3.
The process flow is the same as example 1, except that 32-mesh crystalline flake graphite is changed into 12000-mesh crystalline flake graphite, and graphene oxide with the average size of about 2 microns is prepared.
Example 4.
The procedure was as in example 1, except that the sodium hydroxide powder was replaced with aqueous ammonia and the pH was adjusted to 10.
Example 5.
The process flow is the same as example 1, except that 0.1 ml of prepared GO water dispersion is taken, the mass of GO is 0.1 mg, the GO is added into 25 ml of ionic liquid water solution with the concentration of 40 mg per ml, the mass of the ionic liquid is 1000 mg, and the mass ratio of graphene oxide/ionic liquid is 0.0001.
Example 6.
The process flow is the same as example 1, except that 20 ml of prepared GO water dispersion is taken, the GO with the mass of 20 mg is added into 0.1 ml of ionic liquid water solution with the concentration of 0.02 mg per ml, the mass of the ionic liquid is 0.002 mg, and the mass ratio of graphene oxide/ionic liquid is 10000.
Example 7.
The process flow is the same as example 1, except that 10 ml of the GO aqueous dispersion is added into a round-bottom flask, 90 ml of deionized water is added, the concentration of the GO aqueous dispersion is prepared into 1 mg/ml, and the ratio of the obtained graphene oxide/the ionic liquid is 100 mg/ml.
Example 8.
The process flow is the same as example 1, except that 20 ml of the GO aqueous dispersion is added into a round-bottom flask, 180 ml of deionized water is added, the concentration of the GO aqueous dispersion is prepared into 1 mg/ml, and the ratio of the obtained graphene oxide/the ionic liquid is 200 mg/ml.
Example 9.
The process flow is the same as example 1, except that 40 ml of GO aqueous dispersion is added into a round-bottom flask, 360 ml of deionized water is added, the concentration of GO aqueous dispersion is prepared into 1 mg/ml, and the ratio of graphene oxide/ionic liquid is 400 mg/ml.
Example 10.
The process flow was the same as in example 1 except that 2 ml of ionic liquid (1-allyl-3-methylimidazolium chloride) was taken and 98 ml of water was added to dilute the ionic liquid to obtain graphene oxide/ionic liquid in a ratio of 25 mg per ml.
Example 11.
The process flow is the same as in example 1, and the ionic liquid used is 1-ethyl-3-methylimidazolium tetrafluoroborate.
Comparative example 1.
The procedure was as in example 1, except that the pH adjustment step with sodium hydroxide powder was not included. Obvious flocculation phenomenon appears after the aqueous dispersion of the graphene oxide and the ionic liquid aqueous solution are mixed.
Claims (6)
1. A preparation method of a graphene oxide/ionic liquid nanocomposite is characterized by comprising the following steps: firstly, adding an alkaline compound into an ionic liquid aqueous solution, and adjusting the pH value of the ionic liquid aqueous solution to 8-14; mixing the graphene oxide with the graphene oxide aqueous dispersion; removing water in the mixed solution to obtain the graphene oxide/ionic liquid nanocomposite; the method specifically comprises the following steps:
the method comprises the following steps: preparing graphene oxide aqueous dispersion, wherein the concentration range of the graphene oxide aqueous dispersion is 0.001-20 mg per milliliter;
step two: preparing an ionic liquid aqueous solution with the concentration range of 0.001-2000 mg per ml;
step three: adding an alkaline compound into the ionic liquid aqueous solution to adjust the ionic liquid aqueous solution to be alkaline, wherein the pH value ranges from 8 to 14;
step four: uniformly mixing the graphene oxide aqueous dispersion with the alkaline ionic liquid aqueous solution obtained in the previous step, wherein the mass ratio of the graphene oxide to the ionic liquid is 9999: 1-1: 9999;
step five: and removing unnecessary water in the mixed solution by rotary evaporation or other drying methods to obtain the graphene oxide/ionic liquid nanocomposite.
2. The method according to claim 1, wherein the lateral dimension of the graphene oxide in the first step is 0.01 to 200 μm.
3. The method according to claim 1, wherein the ionic liquid in the second step is one or more of room temperature hydrophilic ionic liquid amino ionic liquid or acidic ionic liquid.
4. The method according to claim 1, wherein the ionic liquid in the second step is: 1-aminoethyl-3-methylimidazolium hexafluorophosphate, 1- (3-propylamino) -3-butylimidazolium tetrafluoroborate, tetrabutylphosphonium glycinate, tetrabutylphosphonium alanate, sulfonate 1-methyl-3-allylimidazole ionic liquid, [ Bmim ]]+[H2PO4]-Phosphate radical 1-methyl-3-allylimidazole ionic liquid, [ Hmim]+[HSO4]-Sulfonate methylimidazole ionic liquid, [ Hmim ]]+[H2PO4]-[Hmim]+[HSO4]-One or more of phosphate methyl imidazole ionic liquids.
5. The preparation method according to claim 1, wherein the alkaline compound in step three comprises one or more of ammonia, sodium hydroxide, potassium hydroxide, calcium hydroxide, sodium carbonate and sodium bicarbonate; and adding an alkaline compound to adjust the pH value of the ionic liquid aqueous solution to 9-12.
6. The preparation method according to claim 1, wherein the method for uniformly mixing in the fourth step is a gentle stirring manner of mechanical disturbance and oscillation, and does not include a violent dispersion method of ultrasound and high-speed shearing.
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