CN104071778A - Graphene dispersion liquid and method for preparing graphene material power - Google Patents
Graphene dispersion liquid and method for preparing graphene material power Download PDFInfo
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- CN104071778A CN104071778A CN201410277206.9A CN201410277206A CN104071778A CN 104071778 A CN104071778 A CN 104071778A CN 201410277206 A CN201410277206 A CN 201410277206A CN 104071778 A CN104071778 A CN 104071778A
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Abstract
The invention provides a graphene dispersion liquid which comprises an organic solvent and a graphene material dispersed in the organic solvent, wherein the graphene dispersion liquid is prepared by virtue of the following steps: S1, providing a graphene water-based slurry which comprises the graphene material and water; S2, adding the organic solvent once or multiple times into the graphene water-based slurry in an accumulated manner to obtain a mixed slurry, wherein the organic solvent and the water can form an azeotropic system; S3, heating the mixed slurry till all moistures in the mixed slurry are removed, so as to obtain the graphene dispersion liquid. The invention further provides a method for preparing graphene material power by using the graphene dispersion liquid.
Description
Technical field
The present invention relates to grapheme material technical field, relate in particular to and be a kind ofly convenient to dry graphene dispersing solution and utilize this graphene dispersing solution to prepare the method for grapheme material powder.
Background technology
The two-dimensional material that Graphene (Graphene) is a kind of individual layer sheet structure consisting of carbon atom, only have a carbon atom thickness.Graphene has all shown excellent performance aspect a lot, such as Graphene is almost completely transparent, only absorbs 2.3% light, and its light transmission is very good; The thermal conductivity of Graphene, up to 5300W/mK, is greater than carbon nanotube and diamond; Electronic mobility under Graphene normal temperature surpasses 15000cm
2/ Vs, is greater than CNT (carbon nano-tube) and silicon crystal; The resistivity of Graphene only has 10
-6Ω cm, lower than copper or silver, be the material of current resistivity minimum; In addition Graphene is also the thinnest the hardest current material.Graphene is prepared into the application that powder is more conducive to Graphene, as grapheme material powder can be used as high molecular additive, improves high molecular electric property and mechanical strength, grapheme material powder has broad application prospects.
At present, can adopt several different methods to prepare grapheme material powder, as mechanically peel method, oxidation-reduction method, crystal epitaxy method, chemical Vapor deposition process, organic synthesis method with peel off carbon nanotube method etc.In these methods, oxidation-reduction method is prepared the with low cost of grapheme material powder and is easily realized, and is the best approach of preparing grapheme material powder.Yet, while preparing grapheme material powder by this kind of method, all can introduce water as solvent or the carrier of redox reaction, thereby form the Graphene water paste being formed by water and grapheme material, and then need to be dried described Graphene water paste to obtain grapheme material powder.
But in actual applications, described Graphene water paste is difficult to convection drying, while adopting the dry Graphene water paste of direct-fired mode, thereby grapheme material wherein there will be the grapheme material powder that hardens or reunite and can not obtain grapheme material powder or can not get can industrialization utilizing, thereby affect the commercial application of grapheme material powder.
Summary of the invention
In view of this, the object of the present invention is to provide a kind ofly, to solve, be convenient to dry graphene dispersing solution and utilize this graphene dispersing solution to prepare the method for grapheme material powder, to address the above problem.
A kind of graphene dispersing solution, it comprises organic solvent and is dispersed in the grapheme material in this organic solvent, this graphene dispersing solution is prepared from as follows: step 1: a kind of Graphene water paste is provided, and this Graphene water paste comprises grapheme material and water; Step 2: accumulative total once or repeatedly adds organic solvent to obtain mixed slurry in described Graphene water paste, and described organic solvent can form azeotropic system with water; Step 3: heat described mixed slurry until remove all moisture in this mixed slurry, obtain described graphene dispersing solution.
In described Graphene water paste, the mass concentration of described Graphene is 0.1%～5%.
The surface tension of described organic solvent is less than 72.8mN/m, and specific heat capacity is less than 4.2*10
3burnt/kilogram degree Celsius.
The surface tension of described organic solvent is less than 50mN/m, and specific heat capacity is less than 1*10
3burnt/kilogram degree Celsius.
Described organic solvent is a kind of or combination in benzene,toluene,xylene, n-propyl alcohol, Virahol, propyl carbinol, isopropylcarbinol, primary isoamyl alcohol, Pentyl alcohol, acetonitrile, vinyl cyanide.
While defining described organic solvent and water formation azeotropic system, in azeotropic cut out, the mass ratio of organic solvent and water is R, and, in described step 2, the organic solvent that accumulative total one or many adds in described Graphene water paste and the ratio of water are greater than R.
A kind of graphene dispersing solution, it comprises organic solvent and is dispersed in the grapheme material in this organic solvent, this graphene dispersing solution is prepared from as follows: step 1: a kind of Graphene water paste is provided, and this Graphene water paste comprises grapheme material and water; Step 2: add organic solvent to obtain mixed slurry in described Graphene water paste, described organic solvent can form azeotropic system with water; Step 3: heat described mixed slurry to evaporate the moisture in this mixed slurry, and remain on and have organic solvent exist in heat-processed in this mixed slurry, when the moisture in described mixed slurry is all removed, obtain described graphene dispersing solution.
A kind of graphene dispersing solution, this graphene dispersing solution comprises grapheme material and organic solvent, and this graphene dispersing solution is can form with water the organic solvent of azeotropic system by adding in Graphene water paste, and by heating, Heating temperature is more than or equal to the azeotropic temperature of azeotropic system, utilize the water in organic solvent displacement Graphene water paste, until remove the water in Graphene water paste completely, obtain.
The described graphene dispersing solution of use is prepared a method for grapheme material powder, and it comprises the steps: described graphene dispersing solution direct drying, until the organic solvent in this graphene dispersing solution is removed completely, thereby obtains described graphene powder.
The mode of described heat drying comprises that direct drying, spraying are dried with regard to granulating and drying.
The temperature of described heat drying is more than or equal to the azeotropic temperature of azeotropic system.
With respect to prior art, the invention provides a kind of graphene dispersing solution that convection drying forms of being convenient to.This graphene dispersing solution in the preparation, the organic solvent that utilization can form binary azeotropic system with water is by displacing the moisture in Graphene slurry, and moisture is removed in heating completely, Heating temperature is more than or equal to the azeotropic temperature of azeotropic system, if Heating temperature is lower than azeotropic temperature, separation efficiency is low, length consuming time, consume energy high.Obtain being dispersed in the grapheme material in organic solvent.Therefore because this graphene dispersing solution is not moisture, can convection drying remove organic solvent and obtain without reunions of hardening, dispersed good Graphene powder.Owing to having adopted, can form with water the organic solvent of azeotropic system, can make is on the one hand that moisture in Graphene water paste is removed under the condition lower than pure water boiling point, shortens time of drying, reduces energy consumption for drying; After replacing by organic solvent on the other hand, obtain being dispersed in the graphene dispersing solution in organic solvent, this graphene dispersing solution is carried out follow-up when dry, due to organic solvent specific surface tension and specific heat capacity little compared with water, both can shorten time of drying, reduce energy consumption, and can solve preferably again grapheme material incident agglomeration traits in drying process simultaneously; Moreover, after the moisture in mixed solvent is removed in heating, obtain being tentatively dispersed in the Graphene slurry in organic solvent, this system is carried out to ultrasonic dispersion, can also obtain the graphene dispersing solution of good dispersity.Technical scheme provided by the invention has successfully solved Industrialization prepared by graphene dispersing solution and grapheme material powder.
Accompanying drawing explanation
Fig. 1 is scanning electron microscope (SEM) figure of the grapheme material powder that obtains of the embodiment of the present invention 1.
Embodiment
Be below specific embodiments of the invention by reference to the accompanying drawings, technical scheme of the present invention is further described, but the present invention be not limited to these embodiment.
A kind of graphene dispersing solution that embodiment of the present invention provides, it comprises organic solvent and is dispersed in the grapheme material in this organic solvent.This graphene dispersing solution is can form with water the organic solvent of azeotropic system by adding in Graphene water paste, and the water water that also heating is removed in Graphene water paste completely of replacing in Graphene water paste by organic solvent obtains.Particularly, its preparation method can comprise the steps:
Step 1: a kind of Graphene water paste is provided, and this Graphene water paste comprises grapheme material and water.So-called Graphene water paste, this slurry is comprised of grapheme material and water substantially, and preferably, the mass concentration of described Graphene is 0.1%～5%.If concentration is greater than 5%, the grapheme material in described Graphene water-based material is easily reunited; And if concentration is lower than 0.1%, the too high levels in Graphene water-based material, can remove part water until concentration rises to 0.1% by direct heating.That is when the mass concentration of the Graphene in Graphene water paste is 0.1%～5%, it is just better dispersed, does not have again unnecessary water.
The structure of described grapheme material is not limit, and it comprises the derivative of graphene nanometer sheet, Graphene micron film, graphene nanobelt, few layer graphene (2-5 layer), multi-layer graphene (2-9 layer), graphene quantum dot, chemical modification Graphene (graphene oxide, redox graphene) and these Graphene class materials).The definition of described grapheme material can be referring to document " All in the graphene family – A recommended nomenclature for two-dimensional carbon materials ".Described grapheme material can also be selected from thickness≤20nm, more preferably, and the material of thickness≤10nm.In the present embodiment, the thickness of this grapheme material preferably≤3nm, grapheme material is thinner, snappiness is better, more easily processing.Described grapheme material preparation method do not limit, adopt Graphene product well known to those skilled in the art or with conventional preparation method preparation.The Graphene product that the preferred Ningbo of grapheme material of the present invention Mo Xi Science and Technology Ltd. provides.Grapheme material can be selected from the grapheme material that graphene oxide that chemical oxidization method prepared as any one method in Brodie method, Hummers method or Staudenmaier method makes through thermal expansion.Also can select the grapheme material that mechanically peel, liquid phase are peeled off or prepared by electrochemical stripping.Same the present invention also can use graphene oxide or other grapheme materials through chemical modification.
The preparation method of graphene oxide water paste is as follows: graphite oxide is according to known Hummers method, Brodie method and Staudenmaier method and the preparation of improving one's methods thereof.Graphite oxide washing prepared by aforesaid method is purified and is removed foreign ion, and thin up is configured to through ultrasonic peeling off, obtain the graphene oxide water paste that massfraction is 0.1～5wt% again after water paste that massfraction is 0.1～5wt%.
The set out preparation method of Graphene water paste of preparation of compound between graphite layers is as follows: compound between graphite layers is prepared according to known synthetic method.The compound between graphite layers of preparation is peeled off and obtained expanded graphite worm through microwave, high-temperature expansion, then expanded graphite worm is dispersed in water through ultrasonic and is peeled off, shear the Graphene water paste that the dispersion lift-off technologies such as dispersion are prepared into desired concn.
The preparation method of the watersoluble plumbago alkene slurry that electrochemical process is peeled off is as follows: electrochemical stripping Graphene obtains being scattered in the Graphene mixture in ionogen according to known electrochemical stripping technology, this Graphene mixture washing is purified, the Graphene slurry presoma that is configured to desired concn obtains Graphene water paste after ultrasonic dispersion.
Step 2: accumulative total once or repeatedly adds organic solvent to obtain mixed slurry in described Graphene water paste, and described organic solvent can form azeotropic system with water.Be that described organic solvent can disposablely join in described mixed slurry, also can join several times in described Graphene water paste.Select disposable adding, operate easier, but when adding Hot swapping the larger container of needs.And select to add several times, operation steps is relatively many, but does not need larger container, and can reduce material cost, and the organic solvent that for example can be evaporated by recovery joins Graphene water paste again.While defining described organic solvent and water formation azeotropic system, in azeotropic cut out, the mass ratio of organic solvent and water is R, and, in described step 2, the organic solvent that accumulative total one or many adds in described Graphene water paste and the ratio of water are greater than R.Thereby guarantee in heat-processed have organic solvent to exist, to prevent grapheme material reunion always.
The classification of described organic solvent is not limit, as long as can form azeotropic system with water.Azeotropic system, refer to, when the homogeneous phase solution of two or more heterogeneities mixes, under fixing pressure, only has a boiling point, and now this mixture is called azeotropic system.Preferably, described organic solvent is a kind of or combination in benzene,toluene,xylene, n-propyl alcohol, Virahol, propyl carbinol, isopropylcarbinol, primary isoamyl alcohol, Pentyl alcohol, acetonitrile, vinyl cyanide.Conventionally, the surface tension of described organic solvent is less than 72.8mN/m, and preferably, the surface tension of described organic solvent is less than or equal to 50mN/m, and the surface tension of described organic solvent is less, and the grapheme material in graphene dispersing solution is more not easy to produce reunites.The specific heat capacity of described organic solvent is less than 4.2*10
3burnt/kilogram degree Celsius, preferably, described specific heat capacity is less than or equal to 1*10
3burnt/kilogram degree Celsius, specific heat capacity is less, graphene dispersing solution needed energy in drying process is fewer.
Step 3: heat described mixed slurry until remove all moisture in this mixed slurry, obtain described graphene dispersing solution.Understandable, for forming graphene dispersing solution, in the process of the described mixed slurry of heating, need to keep has organic solvent to exist in mixed slurry always, and the moisture in described mixed slurry is all removed, and can obtain described graphene dispersing solution.Be appreciated that due to the azeotropic temperature of the azeotropic system boiling point lower than water and organic solvent, so Heating temperature can remain near azeotropic temperature.Preferably, described Heating temperature can be more than or equal to azeotropic temperature.In the present invention, the azeotropic temperature of azeotropic system used and azeotropic table 1 composed as follows shows:
| Azeotrope | Organic solvent boiling point (℃) | Form (w/w) | Azeotropic temperature (℃) |
| Benzene/water | 80.4 | 91.2/8.8 | 69.2 |
| Toluene/water | 110.5 | 80/20 | 85.0 |
| Dimethylbenzene/water | 137-140.5 | 62.5/37.5 | 92.0 |
| N-propanol/water | 97.2 | 71.2/18.8 | 87.7 |
| Isopropanol/water | 82.4 | 87.9/12.1 | 80.4 |
| N-butanol/water | 117.7 | 62.5/37.5 | 92.2 |
| Isobutanol/water | 108.4 | 69.8/30.2 | 89.9 |
| Primary isoamyl alcohol/water | 131.0 | 50.4/49.6 | 95.1 |
| Pentyl alcohol/water | 138.3 | 55.3/44.7 | 95.4 |
| Acetonitrile/water | 81.5 | 85.8/14.2 | 76.0 |
| Vinyl cyanide/water | 78.0 | 87/13 | 70.0 |
Described graphene dispersing solution, in preparation process, also comprises the step of the graphene dispersing solution in step 3 being carried out to ultrasonic wave dispersion, thereby makes the dispersiveness of grapheme material in graphene dispersing solution better.
Embodiment of the present invention also discloses a kind of preparation method of grapheme material powder, and it comprises the steps:
By described graphene dispersing solution direct drying, until the organic solvent in this graphene dispersing solution is removed completely, thereby obtain described grapheme material powder.The mode of described heat drying comprises that direct drying, spraying are dried with regard to granulating and drying.Being appreciated that by the prepared grapheme material powder of method of the present invention, is to obtain being dried under graphene dispersing solution direct heating, grapheme material in this grapheme material powder is better dispersed, and cost is low, easy and simple to handle, be convenient to commercial application.
With respect to prior art, the invention provides a kind of graphene dispersing solution that convection drying forms of being convenient to.In the preparation, the organic solvent that utilization can form binary azeotropic system with water is by displacing the moisture in Graphene slurry for this graphene dispersing solution, and heating removes moisture completely, obtains being dispersed in the grapheme material in organic solvent.Therefore because this graphene dispersing solution is not moisture, can convection drying remove organic solvent and obtain without reunions of hardening, dispersed good Graphene powder.Owing to having adopted, can form with water the organic solvent of azeotropic system, can make is on the one hand that moisture in Graphene water paste is removed under the condition lower than pure water boiling point, shortens time of drying, reduces energy consumption for drying; After replacing by organic solvent on the other hand, obtain being dispersed in the graphene dispersing solution in organic solvent, this graphene dispersing solution is carried out follow-up when dry, due to organic solvent specific surface tension and specific heat capacity little compared with water, both can shorten time of drying, reduce energy consumption, and can solve preferably again grapheme material incident agglomeration traits in drying process simultaneously; Moreover, after the moisture in mixed solvent is removed in heating, obtain being tentatively dispersed in the Graphene slurry in organic solvent, this system is carried out to ultrasonic dispersion, can also obtain the graphene dispersing solution of good dispersity.Technical scheme provided by the invention has successfully solved Industrialization prepared by graphene dispersing solution and grapheme material powder.
For further describing the present invention, the graphene dispersing solution for providing with described embodiment below, the preparation method of grapheme material powder, the specific embodiment under different parameters:
Embodiment 1
Getting 1Kg mass concentration is 0.1% Graphene water paste, according to Graphene water paste and organic solvent mass ratio, is that 1:5 takes 5Kg toluene and joins in above-mentioned Graphene water paste, mixes and is mixed with intermediate pulp; This intermediate pulp is being more than or equal to heat drying under the condition of azeotropic temperature, after moisture eliminates, is obtaining being tentatively scattered in the Graphene slurry in organic solvent toluene, this Graphene slurry is being carried out to ultrasonic peeling off, obtaining scattered graphene dispersing solution.To heat drying under 120 ℃ of conditions of this graphene dispersing solution, to solvent, all remove, obtain grapheme material powder.
Embodiment 2
Getting 1Kg mass concentration is 5% Graphene water paste, according to Graphene water paste and organic solvent mass ratio, is that 1:4 takes 4Kg toluene and joins in above-mentioned Graphene water paste, mixes and is mixed with intermediate pulp; This intermediate pulp is being more than or equal to heat drying under the condition of azeotropic temperature, after moisture eliminates, is obtaining being tentatively scattered in the Graphene slurry in organic solvent toluene, this Graphene slurry is being carried out to ultrasonic peeling off, obtaining scattered graphene dispersing solution.To heat drying under 120 ℃ of conditions of this graphene dispersing solution, to solvent, all remove, obtain grapheme material powder.
Embodiment 3
Getting 1Kg mass concentration is 1% Graphene water paste, according to Graphene water paste and organic solvent mass ratio, is that 1:7 takes 7Kg toluene and joins in above-mentioned Graphene water paste, mixes and is mixed with intermediate pulp; Dry in 220 ℃ of condition sprayings to this intermediate pulp, obtain grapheme material powder.
Embodiment 4
Getting 1Kg mass concentration is 0.5% Graphene water paste, according to Graphene water paste and organic solvent mass ratio, is that 1:2 takes 2Kg propyl carbinol and joins in above-mentioned Graphene water paste, mixes and is mixed with intermediate pulp; This intermediate pulp is being more than or equal to heat drying under the condition of azeotropic temperature, after moisture eliminates, is obtaining being tentatively scattered in the Graphene slurry in organic solvent propyl carbinol, this Graphene slurry is being carried out to ultrasonic peeling off, obtaining scattered graphene dispersing solution.
Embodiment 5
Getting 1Kg mass concentration is 1.5% Graphene water paste, according to Graphene water paste and organic solvent mass ratio, is that 1:2 takes 2Kg propyl carbinol and joins in above-mentioned Graphene water paste, mixes and is mixed with intermediate pulp; This intermediate pulp is being more than or equal to heat drying under the condition of azeotropic temperature, after moisture eliminates, is obtaining being tentatively scattered in the Graphene slurry in organic solvent propyl carbinol, this Graphene slurry is being carried out to ultrasonic peeling off, obtaining scattered graphene dispersing solution.To this graphene dispersing solution heat drying, to solvent, all remove, obtain grapheme material powder.
Embodiment 6
Getting 1Kg mass concentration is 5% Graphene water paste, according to Graphene water paste and organic solvent mass ratio, is that 1:2 takes 2Kg propyl carbinol and joins in above-mentioned Graphene water paste, mixes and is mixed with intermediate pulp; This intermediate pulp is being more than or equal to heat drying under the condition of azeotropic temperature, after moisture eliminates, is obtaining being tentatively scattered in the Graphene slurry in organic solvent propyl carbinol, this Graphene slurry is being carried out to ultrasonic peeling off, obtaining scattered graphene dispersing solution.To this graphene dispersing solution heat drying, to solvent, all remove, obtain grapheme material powder.
Embodiment 7
Getting 1Kg mass concentration is 0.1% Graphene water paste, according to Graphene water paste and organic solvent mass ratio, is that 1:2 takes 2Kg dimethylbenzene and joins in above-mentioned Graphene water paste, mixes and is mixed with intermediate pulp; This intermediate pulp is being more than or equal to heat drying under the condition of azeotropic temperature, after moisture eliminates, is obtaining being tentatively scattered in the Graphene slurry in organic solvent dimethylbenzene, this Graphene slurry is being carried out to ultrasonic peeling off, obtaining scattered graphene dispersing solution.
Embodiment 8
Getting 1Kg mass concentration is 5% Graphene water paste, according to Graphene water paste and organic solvent mass ratio, is that 1:5 takes 5Kg dimethylbenzene and joins in above-mentioned Graphene water paste, mixes and is mixed with intermediate pulp; This intermediate pulp is being more than or equal to heat drying under the condition of azeotropic temperature, after moisture eliminates, is obtaining being tentatively scattered in the Graphene slurry in organic solvent dimethylbenzene, this Graphene slurry is being carried out to ultrasonic peeling off, obtaining scattered graphene dispersing solution.To this graphene dispersing solution heat drying, to solvent, all remove, obtain grapheme material powder.
Embodiment 9
Getting 1Kg mass concentration is 1% Graphene water paste, according to Graphene water paste and organic solvent mass ratio, is that 1:3 takes 3Kg dimethylbenzene and joins in above-mentioned Graphene water paste, mixes and is mixed with intermediate pulp; This intermediate pulp is sprayed under 220 ℃ of conditions dry, obtain grapheme material powder.
Embodiment 10
Getting 1Kg mass concentration is 0.1% Graphene water paste, according to Graphene water paste and organic solvent mass ratio, is that 1:1.5 takes 1.5Kg primary isoamyl alcohol and joins in above-mentioned Graphene water paste, mixes and is mixed with intermediate pulp; This intermediate pulp is being more than or equal to heat drying under the condition of azeotropic temperature, after moisture eliminates, is obtaining being tentatively scattered in the Graphene slurry in organic solvent primary isoamyl alcohol, this Graphene slurry is being carried out to ultrasonic peeling off, obtaining scattered graphene dispersing solution.
Embodiment 11
Getting 1Kg mass concentration is 5% Graphene water paste, according to Graphene water paste and organic solvent mass ratio, is that 1:2 takes 2Kg primary isoamyl alcohol and joins in above-mentioned Graphene water paste, mixes and is mixed with intermediate pulp; This intermediate pulp is being more than or equal to heat drying under the condition of azeotropic temperature, after moisture eliminates, is obtaining being tentatively scattered in the Graphene slurry in organic solvent primary isoamyl alcohol, this Graphene slurry is being carried out to ultrasonic peeling off, obtaining scattered graphene dispersing solution.To this graphene dispersing solution heat drying, to solvent, all remove, obtain grapheme material powder.
Embodiment 12
Getting 1Kg mass concentration is 1% Graphene water paste, according to Graphene water paste and organic solvent mass ratio, is that 1:2 takes 2Kg Virahol and joins in above-mentioned Graphene water paste, mixes and is mixed with intermediate pulp; This intermediate pulp is sprayed under 200 ℃ of conditions dry, obtain grapheme material powder.
Embodiment 13
Getting 1Kg mass concentration is 0.1% Graphene water paste, according to Graphene water paste and organic solvent mass ratio, is that 1:9 takes 9Kg Virahol and joins in above-mentioned Graphene water paste, mixes and is mixed with intermediate pulp; This intermediate pulp is being more than or equal to heat drying under the condition of azeotropic temperature, after moisture eliminates, is obtaining being tentatively scattered in the Graphene slurry in organic solvent Virahol, this Graphene slurry is being carried out to ultrasonic peeling off, obtaining scattered graphene dispersing solution.
Embodiment 14
Getting 1Kg mass concentration is 5% Graphene water paste, according to Graphene water paste and organic solvent mass ratio, is that 1:8 takes 8Kg n-propyl alcohol and joins in above-mentioned Graphene water paste, mixes and is mixed with intermediate pulp; This intermediate pulp is being more than or equal to heat drying under the condition of azeotropic temperature, after moisture eliminates, is obtaining being tentatively scattered in the Graphene slurry in organic solvent n-propyl alcohol, this Graphene slurry is being carried out to ultrasonic peeling off, obtaining scattered graphene dispersing solution.To this graphene dispersing solution heat drying, to solvent, all remove, obtain grapheme material powder.
Embodiment 15
Getting 1Kg mass concentration is 1% Graphene water paste, according to Graphene water paste and organic solvent mass ratio, is that 1:9 takes 9Kg n-propyl alcohol and joins in above-mentioned Graphene water paste, mixes and is mixed with intermediate pulp; This intermediate pulp is being more than or equal to heat drying under the condition of azeotropic temperature, after moisture eliminates, is obtaining being tentatively scattered in the Graphene slurry in organic solvent n-propyl alcohol, this Graphene slurry is being carried out to ultrasonic peeling off, obtaining scattered graphene dispersing solution.This graphene dispersing solution is sprayed under 200 ℃ of conditions dry, obtain grapheme material powder.
Embodiment 16
Getting 1Kg mass concentration is 5% Graphene water paste, according to Graphene water paste and organic solvent mass ratio, is that 1:8 takes 8Kg vinyl cyanide and joins in above-mentioned Graphene water paste, mixes and is mixed with intermediate pulp; This intermediate pulp is being more than or equal to heat drying under the condition of azeotropic temperature, after moisture eliminates, is obtaining being tentatively scattered in the Graphene slurry in organic solvent vinyl cyanide, this Graphene slurry is being carried out to ultrasonic peeling off, obtaining scattered graphene dispersing solution.To this graphene dispersing solution heat drying, to solvent, all remove, obtain grapheme material powder.
Embodiment 17
Getting 1Kg mass concentration is 0.1% Graphene water paste, according to Graphene water paste and organic solvent mass ratio, is that 1:8 takes 8Kg vinyl cyanide and joins in above-mentioned Graphene water paste, mixes and is mixed with intermediate pulp; This intermediate pulp is being more than or equal to heat drying under the condition of azeotropic temperature, after moisture eliminates, is obtaining being tentatively scattered in the Graphene slurry in organic solvent vinyl cyanide, this Graphene slurry is being carried out to ultrasonic peeling off, obtaining scattered graphene dispersing solution.
Embodiment 18
Getting 1Kg mass concentration is 1% Graphene water paste, according to Graphene water paste and organic solvent mass ratio, is that 1:8 takes 8Kg vinyl cyanide and joins in above-mentioned Graphene water paste, mixes and is mixed with intermediate pulp; This intermediate pulp is sprayed under 200 ℃ of conditions dry, obtain grapheme material powder.
The explanation of above embodiment is just for helping to understand method of the present invention and core concept thereof.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of the claims in the present invention.To the multiple modification of these embodiment, be apparent for those skilled in the art, General Principle as defined herein can realize in other embodiments in the situation that not departing from the spirit or scope of the present invention.Therefore, the present invention will can not be restricted to these embodiment shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (10)
1. a graphene dispersing solution, is characterized in that, it comprises organic solvent and be dispersed in the grapheme material in this organic solvent, and this graphene dispersing solution is prepared from as follows:
Step 1: a kind of Graphene water paste is provided, and this Graphene water paste comprises grapheme material and water;
Step 2: accumulative total once or repeatedly adds organic solvent to obtain mixed slurry in described Graphene water paste, and described organic solvent can form azeotropic system with water;
Step 3: heat described mixed slurry until remove all moisture in this mixed slurry, obtain described graphene dispersing solution.
2. a graphene dispersing solution as claimed in claim 1, is characterized in that, in described Graphene water paste, the mass concentration of described Graphene is 0.1%～5%.
3. a graphene dispersing solution as claimed in claim 1, is characterized in that, described organic solvent is a kind of or combination in benzene,toluene,xylene, n-propyl alcohol, Virahol, propyl carbinol, isopropylcarbinol, primary isoamyl alcohol, Pentyl alcohol, acetonitrile, vinyl cyanide.
4. a graphene dispersing solution as claimed in claim 1, it is characterized in that, while defining described organic solvent and water formation azeotropic system, in azeotropic cut out, the mass ratio of organic solvent and water is R,, in described step 2, the organic solvent that accumulative total one or many adds in described Graphene water paste and the ratio of water are greater than R.
5. a graphene dispersing solution, it is characterized in that, this graphene dispersing solution comprises grapheme material and organic solvent, and this graphene dispersing solution is can form with water the organic solvent of azeotropic system by adding in Graphene water paste, and by heating, Heating temperature is more than or equal to the azeotropic temperature of azeotropic system, utilizes the water in organic solvent displacement Graphene water paste, until remove the water in Graphene water paste completely, obtains.
6. with the graphene dispersing solution described in claim 1-5, prepare a method for grapheme material powder, it comprises the steps:
By described graphene dispersing solution heat drying, until the organic solvent in this graphene dispersing solution is removed completely, thereby obtain described graphene powder.
7. a method of preparing grapheme material powder as claimed in claim 6, is characterized in that, the mode of described heat drying is direct drying.
8. a method of preparing grapheme material powder as claimed in claim 6, is characterized in that, the mode of described heat drying comprises that spraying is dried or granulating and drying.
9. a method of preparing grapheme material powder as claimed in claim 6, is characterized in that, the temperature of described heat drying is more than or equal to the azeotropic temperature of azeotropic system.
10. a method of preparing grapheme material powder as claimed in claim 6, it is characterized in that, described organic solvent is a kind of or combination in benzene,toluene,xylene, n-propyl alcohol, Virahol, propyl carbinol, isopropylcarbinol, primary isoamyl alcohol, Pentyl alcohol, acetonitrile, vinyl cyanide.
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| CN106006611A (en) * | 2016-05-18 | 2016-10-12 | 中国科学院山西煤炭化学研究所 | Method for efficiently preparing graphene oxide organic solution |
| CN106115676A (en) * | 2016-06-28 | 2016-11-16 | 常州第六元素材料科技股份有限公司 | A kind of Graphene organic ink and preparation method thereof |
| CN108028366A (en) * | 2015-09-18 | 2018-05-11 | 东丽株式会社 | The manufacture method of graphene/dispersion in organic solvent and its manufacture method and lithium ion battery electrode |
| CN109971233A (en) * | 2019-04-10 | 2019-07-05 | 常州第六元素材料科技股份有限公司 | Graphene with high specific surface aggregation and preparation method thereof, graphene static conductive coating and preparation method thereof |
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| CN110256109A (en) * | 2019-06-18 | 2019-09-20 | 宁波墨西科技有限公司 | A kind of graphene antistatic lithium based concrete sealing solidifying agent and preparation method thereof |
| CN110299450A (en) * | 2018-03-23 | 2019-10-01 | 中国科学院物理研究所 | A kind of flexible, porous carbon is to electrode preparation method and Ca-Ti ore type solar battery |
| CN110364731A (en) * | 2018-04-09 | 2019-10-22 | 北京航空航天大学 | A kind of graphene conductive slurry |
| CN112945997A (en) * | 2021-02-01 | 2021-06-11 | 天津艾克凯胜石墨烯科技有限公司 | Sample preparation method for aqueous graphene slurry before scanning electron microscope |
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| CN106006611A (en) * | 2016-05-18 | 2016-10-12 | 中国科学院山西煤炭化学研究所 | Method for efficiently preparing graphene oxide organic solution |
| CN106115676A (en) * | 2016-06-28 | 2016-11-16 | 常州第六元素材料科技股份有限公司 | A kind of Graphene organic ink and preparation method thereof |
| CN110299450B (en) * | 2018-03-23 | 2021-03-26 | 中国科学院物理研究所 | Preparation method of flexible porous carbon counter electrode and perovskite type solar cell |
| CN110299450A (en) * | 2018-03-23 | 2019-10-01 | 中国科学院物理研究所 | A kind of flexible, porous carbon is to electrode preparation method and Ca-Ti ore type solar battery |
| CN110364731A (en) * | 2018-04-09 | 2019-10-22 | 北京航空航天大学 | A kind of graphene conductive slurry |
| CN110028828A (en) * | 2019-04-03 | 2019-07-19 | 常州第六元素材料科技股份有限公司 | The graphene composite dry powder and preparation method of high solids content, epoxy zinc-enriched paint and preparation method |
| CN110028828B (en) * | 2019-04-03 | 2021-12-14 | 常州第六元素材料科技股份有限公司 | High-solid-content graphene composite dry powder and preparation method thereof, epoxy zinc-rich coating and preparation method thereof |
| CN109971233A (en) * | 2019-04-10 | 2019-07-05 | 常州第六元素材料科技股份有限公司 | Graphene with high specific surface aggregation and preparation method thereof, graphene static conductive coating and preparation method thereof |
| CN110006956A (en) * | 2019-05-13 | 2019-07-12 | 宁波杉元石墨烯科技有限公司 | A kind of test method of graphene slurry resistivity |
| CN110256109A (en) * | 2019-06-18 | 2019-09-20 | 宁波墨西科技有限公司 | A kind of graphene antistatic lithium based concrete sealing solidifying agent and preparation method thereof |
| CN112945997A (en) * | 2021-02-01 | 2021-06-11 | 天津艾克凯胜石墨烯科技有限公司 | Sample preparation method for aqueous graphene slurry before scanning electron microscope |
| CN113956720A (en) * | 2021-11-26 | 2022-01-21 | 重庆石墨烯研究院有限公司 | Preparation method of flexible conductive film |
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