CN109052372A - A method of carbon nano tube dispersion liquid is prepared by solid phase removing - Google Patents
A method of carbon nano tube dispersion liquid is prepared by solid phase removing Download PDFInfo
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- CN109052372A CN109052372A CN201811321937.3A CN201811321937A CN109052372A CN 109052372 A CN109052372 A CN 109052372A CN 201811321937 A CN201811321937 A CN 201811321937A CN 109052372 A CN109052372 A CN 109052372A
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- C01B32/15—Nano-sized carbon materials
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Abstract
A kind of method preparing carbon nano tube dispersion liquid by solid phase removing disclosed by the invention, comprising the following steps: carbon nanotube and solid phase dispersion agent are uniformly mixed, mixture is obtained；Carbon nanotube powder by mixture ball-milling treatment, after obtaining solid phase removing；Carbon nanotube powder after solid-phase ball milling is distributed in solvent, carbon nano tube dispersion liquid is obtained；Any solvent is not used in the present invention in stripping process, carbon nanotube powder can storing for a long time, after removing is prepared by solid phase removing, it can long-term preservation with solid phase form, it realizes on-demand, furthermore, carbon nanotube powder after removing can be dispersed in water by jiggling, convenient for following process and application.
Description
Technical field
The present invention relates to the field of dispersions of carbon nanotube, and in particular to a kind of to remove preparation carbon nanotube dispersion by solid phase
The method of liquid.
Background technique
The one-dimension tube material that carbon nanotube is made of sp2 carbon atom, according to the difference of tube wall, carbon nanotube can be divided into
Single-walled carbon nanotube and multi-walled carbon nanotube.Carbon nanotube is due to good conjugacy, big draw ratio and high ratio table
The architectural characteristics such as area, electricity, optics, mechanics, in terms of show excellent performance, to be widely used in
The fields such as composite material, supercapacitor, feds, absorbing material.However, due to π-π phase interaction strong between tube wall
With and difference dissolubility, carbon nanotube usually exists in the form of aggregate (on microcosmic), and not soluble in water and various common
Organic solvent, to strongly limit it in the application of the above numerous areas.Therefore, carbon nanotube boundling, preparation are efficiently removed
The carbon nanotube of solvable (or dispersible), and then formed by way of solution processing (such as spin coating, printing, drop film), to pushing away
Application into carbon nanotube in various fields is of great significance.
The method of the solubilized modification of carbon nanotube can be divided into covalent modification and non-covalent modification two major classes.Covalent modification is usual
It is that logical peracid treatment makes the side wall of carbon nanotube or both ends generate active site, so as to the access of subsequent soluble structural units；Or
The tube wall of person's carbon nanotube directly carries out cycloaddition reaction with certain specific bioactive molecules (such as nitrogen base, amino acid).It is non-total
Valence modification is then by utilizing π-π interaction or Van der Waals between soluble dispersant molecule and carbon nanotube side-wall
The solubilising of power realization carbon nanotube.Covalent modification can destroy the integrality of carbon nanotube conjugated structure, to influence its performance.It is non-
Covalent modification can realize the solubilized of carbon nanotube while not destroying carbon nanotube conjugated structure integrality, thus become
The hot spot of recent researches.
The dispersing agent reported at present has conjugation small molecule, polymer, biomolecule, ionic surfactant (such as gallbladder
Sour sodium, neopelex) etc..The above dispersing agent mostly passes through ultrasound when being used for dispersing Nano carbon tubes in the liquid phase
And it realizes, the finally obtained dispersion liquid for carbon nanotube.However, due to the unique structure feature of carbon nanotube itself, it is different
There are strong π-π interactions between carbon tube wall, cause the carbon nanotube in liquid phase easily to occur slowly to assemble, settle, no
Conducive to long-time preservation and subsequent processed and applied.Therefore, a kind of non-covalent modification, dispersible carbon nanotube powders are developed
End, with solid phase form for a long time save, need using when be scattered in solvent, realize it is used as needed, to promote carbon nanotube exist
The application in each field has great significance.
Summary of the invention
To solve the above problems, the present invention provides a kind of method for preparing carbon nano tube dispersion liquid by solid phase removing.Its
In, solid phase removes obtained carbon nanotube powder, can with solid phase form can long-term preservation, avoid the slow aggregation in liquid phase
With sedimentation.In addition, the carbon nanotube after removing, can be dispersed in water, to realize used as needed by jiggling.
The technical solution that the present invention solves is to provide a kind of method for preparing carbon nano tube dispersion liquid by solid phase removing,
Characterized by comprising the following steps:
(1) carbon nanotube and solid phase dispersion agent are uniformly mixed, obtains mixture；
(2) mixture solid-phase ball milling is handled, the carbon nanotube powder after obtaining solid phase removing；
(3) carbon nanotube powder after solid-phase ball milling is distributed in solvent, obtains carbon nano tube dispersion liquid.
Preferably, further comprising the steps of: carbon nano tube dispersion liquid being centrifuged, the poor a small amount of aggregation of dispersibility is removed
Body.
Preferably, the carbon nanotube of the powdery is single wall or multi-walled carbon nanotube.
Preferably, the dispersing agent is sodium taurocholate, hexahydroxy triphenylene, tannic acid, dodecyl sodium sulfate, deoxycholic acid
One kind of sodium.
Preferably, the ball milling includes: the powder that medication spoon will be affixed on tank skin and cover after every ball milling 0.5-1 hours
It scrapes, uniformly to mix, improves grinding efficiency.In addition, discontinuity ball milling also can guarantee ball milling system temperature will not it is obvious on
It rises.The above process recycles n times, wherein 1≤N≤15.
Preferably, the diameter of the mill ball in the ball milling is 2~16 millimeters.
Preferably, the mass ratio of the carbon nanotube of the solid phase dispersion agent and powdery is >=1:2.
Preferably, the solvent is the organic solvents such as water or n,N-Dimethylformamide, tetrahydrofuran.
It is worth noting that, the present invention prepares soluble carbon nanotube powder by ball-milling method realization solid phase removing,
In mechanical milling process, carbon nanotube agglomerate is gradually stripped under the action of mill ball shearing force, and length shortens, simultaneously as
In the presence of between carbon nanotube tube wall π-π or Van der Waals force interaction, dispersant molecule is gradually inserted carbon nanotube collection
Shu Zhong, and interaction occurs with carbon nanotube and forms compound, further speed up the removing of carbon nanotube boundling.
Be not used any solvent in stripping process, thus the carbon nanotube powder after removing will not passage at any time and weigh
New aggregation is realized on-demand so as to save for a long time.In addition, the carbon nanotube after removing, it both can be by ultrasound to its point
It dissipates, it can also be by jiggling dispersion, principle are as follows: carbon nanotube occurs noncovalent interaction with solvable dispersant molecule and formed
Compound realizes the effective solubilization of carbon nanotube while guaranteeing carbon nanotube conjugated structure integrality, i.e., by gently
Rocking uniformly to be scattered in solvent, eliminate ultrasonic disperse technique, convenient and efficient.Dispersion liquid can be processed by solution
The mode of (such as spin coating, printing, drop film) forms, and simplifies pre-processing process when materials'use, for after carbon nanotube
Continuous application, processing provide convenience.
In addition, the carbon nanotube powder after ball milling removing, can quantitatively weigh, and can be real by controlling the additional amount of solvent
It now to the control of dispersion liquid concentration, avoids in liquid phase ultrasonic disperse, dispersion liquid concentration is low, concentration is uncontrollable and is not suitable for
The problem of long-time storage.
Compared with prior art, any solvent is not used in the present invention in stripping process, and preparing by solid phase removing can
Carbon nanotube powder storing for a long time, after removing.The powder is led to by rocking can preferably be scattered in solvent manually
Cross the dosage for changing powder and solvent, can easily obtain that concentration is high and regulatable carbon nano tube dispersion liquid, realize with take with
With while, facilitate following process and application.
Detailed description of the invention
Fig. 1 is carbon nano tube dispersion liquid picture prepared by 1(of embodiment of the present invention Fig. 1 a) and 2 (Fig. 1 b).
Fig. 2 is scanning transmission electron microscope (STEM) figure of carbon nano tube dispersion liquid prepared by the embodiment of the present invention 1
Piece.
Specific embodiment
Following is a specific embodiment of the present invention in conjunction with the accompanying drawings, technical scheme of the present invention will be further described,
However, the present invention is not limited to these examples.
To solve the above-mentioned problems, the main thought of the embodiment of the present invention is:
The embodiment of the present invention provides a kind of method for preparing carbon nano tube dispersion liquid by solid phase removing, and the method includes as follows
Step:
Carbon nanotube and dispersant are uniformly obtained into mixture, the dispersing agent is selected from sodium taurocholate, hexahydroxy triphenylene, list
Peaceful acid, dodecyl sodium sulfate, NaTDC；The carbon nanotube is to pass through different approaches (such as arc discharge method, high pressure
Carbon monoxide method etc.) preparation single wall or multi-walled carbon nanotube.
At room temperature, the carbon nanotube powder by the mixture ball milling, after being removed.Carbon nanometer after ball milling
Pipe, can be preferably dispersed in water, to obtain stable carbon nano tube dispersion liquid by rocking manually.In addition, by from
The heart can remove a small amount of aggregation that dispersibility is slightly worse in dispersion liquid.
In mechanical milling process, carbon nanotube agglomerate is gradually stripped under the action of mill ball shearing force, and length shortens.
Simultaneously as in the presence of between carbon nanotube tube wall π-π or Van der Waals force interact, dispersant molecule is gradually inserted carbon
In nanotube boundling, the removing of carbon nanotube boundling is further speeded up.Due to avoiding the use of solvent, Gu the single wall after removing
Carbon nanotube powder will not passage at any time and reassemble, thus can save, realize on-demand for a long time.
The ball milling includes: after every ball milling 0.5-1 hours, and medication spoon scrapes the powder being affixed on tank skin and cover, with
Just uniformly mixing, improves grinding efficiency.In addition, discontinuity ball milling also can guarantee that ball milling system temperature will not obviously rise；It is above-mentioned
Process recycles n times, wherein 1≤N≤15, the diameter of the mill ball in the ball milling is 2~16 millimeters.
The milling apparatus such as planetary ball mill can be selected in the ball milling, and carbon nanotube and dispersant are uniformly added afterwards
In milling apparatus, the diameter of mill ball therein may be selected to be 2~16 millimeters.In addition, by using large-scale ball mill, it can
Preparative-scale is magnified, realizes magnanimity production.
Dispersing agent described in the embodiment of the present invention and the mass ratio of powdery carbon nanotube are chosen as >=1:2, and ball milling speed can
Selection revolving speed is 100~500 rpm.The ball milling total time can be chosen for 1~8 hour.It should be noted that dispersing agent
Feed ratio, ball milling speed and time between carbon nanotube, by carbon nanotube dispersion effect (yield) and length generate compared with
Big influence can select suitable preparation condition according to practical use.
Carbon nanotube powder after ball milling removing has fabulous dispersibility, can be uniformly scattered in by jiggling
In water, eliminate ultrasonic disperse technique, simplify pre-processing process when materials'use, be carbon nanotube subsequent applications,
Processing provides convenience.In addition, the carbon nanotube powder after ball milling removing, can quantitatively weigh, and control solvent can be passed through
Additional amount realizes the control to dispersion liquid concentration.This is effectively prevented in liquid phase ultrasonic disperse, and dispersion liquid concentration is low, concentration is difficult to
The problem of control and unsuitable long-time storage.
In order to which above and other purpose, feature and the advantage of the present invention can be clearer and more comprehensible, several implementations are cited below particularly
Example, to illustrate the method for the invention.
Embodiment 1
Under 25 DEG C of environment temperatures, single wall that 52.5 mg sodium taurocholates and 7.5 mg are prepared by high pressure carbon monoxide method (HiPco)
Carbon nanometer tube material is placed in the ball grinder that volume is 150 ml, and then 2 diameters of addition are 16 millimeters and 8 diameters are 10 millis
The mill ball of rice, tightens cover, and ball milling is ground 0.5 hour under the revolving speed of 150 rpm.Stop ball milling and medication spoon will be affixed on tank skin
It is scraped with the powder on cover, uniformly to mix, improves grinding efficiency.After continuing ball milling 0.5 hour, powder is taken out, i.e.,
Soluble carbon nanotube can be obtained.The carbon nanotube powder of this solid phase modification, due to not introducing any solvent, when can be long
Between save, realize it is on-demand.By jiggling, the carbon nanotube powder that solid phase is modified can be dispersed in water.Dispersion
Liquid is centrifuged 1 hour under the centrifugal force of 23797g, the slightly worse carbon nanotube of dispersibility can be removed, to obtain well dispersed
Dispersion liquid, as shown in Figure 1a, dispersion liquid are finally in black, it was demonstrated that have a considerable amount of carbon nanotubes evenly dispersed in water；It is right
Scanning transmission electron microscope (STEM) picture answered is as shown in Figure 2.
Embodiment 2
Under 25 DEG C of environment temperatures, 52.5 mg sodium taurocholates and 7.5 mg are prepared by arc discharge method (Arc-discharge)
Single-walled carbon nanotube raw material is placed in the ball grinder that volume is 150 ml, and then 2 diameters of addition are 16 millimeters and 8 diameters are
10 millimeters of mill ball, tightens cover, ball milling 0.5 hour under the revolving speed of 150 rpm.Stop ball milling and medication spoon will be affixed on tank
Powder on wall and cover scrapes, and uniformly to mix, improves grinding efficiency.After continuing grinding 0.5 hour, powder is taken out,
Soluble carbon nanotube can be obtained.The carbon nanotube powder of this solid phase modification, due to not introducing any solvent, Ke Yichang
Time saves, and realizes on-demand.By jiggling, the carbon nanotube powder that solid phase is modified can be dispersed in water.Point
Dispersion liquid is centrifuged 1 hour under the centrifugal force of 23797g, the slightly worse carbon nanotube of dispersibility can be removed, to obtain well dispersed
Dispersion liquid, as shown in Figure 1 b.
Embodiment 3
Under 20 DEG C of environment temperatures, 20 mg sodium taurocholates and 10 mg carbon nanometer tube materials are placed in the grinding pot that volume is 150 ml
In, the mill ball that 2 diameters are 16 millimeters and 8 diameters are 10 millimeters is then added, cover is tightened, in the revolving speed of 200 rpm
Lower ball milling 0.5 hour.Stop ball milling and medication spoon scrapes the powder being affixed on tank skin and cover, uniformly to mix, improves
Grinding efficiency.It repeats the above process, until milling time reaches 2 hours.Powder is taken out, soluble carbon nanometer can be obtained
Pipe.The carbon nanotube powder of this solid phase modification can save for a long time due to not introducing any solvent, realize on-demand.
By jiggling, the carbon nanotube powder that solid phase is modified can be dispersed in water.Dispersion liquid is under the centrifugal force of 23797g
Centrifugation 1 hour can remove the slightly worse carbon nanotube of dispersibility, to obtain well dispersed dispersion liquid.
Embodiment 4
Under 25 DEG C of environment temperatures, 10 mg tannic acid and 20 mg carbon nanometer tube materials are placed in the ball milling that volume is 150 ml
In tank, the mill ball that 2 diameters are 16 millimeters and 8 diameters are 10 millimeters is then added, tightens cover, in turning for 300 rpm
Speed is ball milling 0.5 hour lower.And medication spoon scrapes the powder being affixed on tank skin and cover, uniformly to mix, improves ball milling effect
Rate.It repeats the above process, until Ball-milling Time reaches 2 hours.Powder is taken out, soluble single can be obtained
Pipe.This solid phase modification single pipe powder can be saved for a long time due to not introducing any solvent, realize with
With taking.By jiggling, the single pipe powder that solid phase is modified can be dispersed in water.Dispersion liquid is 1028g's
It is centrifuged 0.5 hour under centrifugal force, the slightly worse carbon nanotube of dispersibility can be removed, to obtain well dispersed dispersion liquid.
Embodiment 5
Under 30 DEG C of environment temperatures, 30 mg sodium taurocholates and 10mg carbon nanotube are placed in the ball grinder that volume is 150 ml,
Then the mill ball that 2 diameters are 16 millimeters and 8 diameters are 10 millimeters is added, tightens cover, the ball under the revolving speed of 100 rpm
Mill 0.5 hour.And medication spoon scrapes the powder being affixed on tank skin and cover, uniformly to mix, improves grinding efficiency.It repeats
The above process, until Ball-milling Time reaches 4 hours.Powder is taken out, soluble single-walled carbon nanotube can be obtained.This solid phase
The single pipe powder of modification can save for a long time due to not introducing any solvent, realize on-demand.Pass through
It jiggles, the single pipe powder that solid phase is modified can be dispersed in water.Dispersion liquid is under the centrifugal force of 23797g
Centrifugation 0.5 hour can remove the slightly worse carbon nanotube of dispersibility, to obtain well dispersed dispersion liquid.
Embodiment 6
Under 25 DEG C of environment temperatures, 100 mg sodium taurocholates and 5 mg carbon nanometer tube materials are placed in the ball grinder that volume is 150 ml
In, the mill ball that 2 diameters are 16 millimeters and 8 diameters are 10 millimeters is then added, cover is tightened, under the revolving speed of 150rpm
Ball milling 0.5 hour.Stop ball milling and medication spoon scrapes the powder being affixed on tank skin and cover, uniformly to mix, improves ball
Grind efficiency.It repeats the above process, until Ball-milling Time reaches 8 hours.Powder is taken out, soluble single wall carbon can be obtained and receive
Mitron.This solid phase modification single pipe powder can be saved for a long time due to not introducing any solvent, realize with
With with taking.By jiggling, the single pipe powder that solid phase is modified can be dispersed in water.Dispersion liquid is in 1028g
Centrifugal force under be centrifuged 1 hour, the slightly worse carbon nanotube of dispersibility can be removed, to obtain well dispersed dispersion liquid.
Embodiment 7
Under 15 DEG C of environment temperatures, 50 mg, 2,3,6,7,10,11- hexahydroxy triphenylene and 5mg carbon nanometer tube material are placed in
Volume is that the mill ball that 2 diameters are 16 millimeters and 8 diameters are 10 millimeters is then added, tightens in the ball grinder of 150 ml
Cover, ball milling 0.5 hour under the revolving speed of 250 rpm.Stop ball milling and medication spoon scrapes the powder being affixed on tank skin and cover
Under, uniformly to mix, improve grinding efficiency.It repeats the above process, until Ball-milling Time reaches 4 hours.Powder is taken out, i.e.,
Soluble single-walled carbon nanotube can be obtained.The single pipe powder of this solid phase modification, due to not introducing any solvent,
It can save, realize on-demand for a long time.By jiggling, the single pipe powder that can modify solid phase disperses
In N,N-dimethylformamide.Dispersion liquid is centrifuged 1 hour under the centrifugal force of 1028g, can be removed the slightly worse carbon of dispersibility and be received
Mitron, to obtain well dispersed dispersion liquid.
Embodiment 8
Under 35 DEG C of environment temperatures, 75 tannic acid and 5mg carbon nanometer tube material are placed in the ball grinder that volume is 150 ml, so
The mill ball that 2 diameters are 16 millimeters and 8 diameters are 10 millimeters is added afterwards, tightens cover, the ball milling under the revolving speed of 200 rpm
0.5 hour.Stop ball milling and medication spoon scrapes the powder being affixed on tank skin and cover, uniformly to mix, improves ball milling effect
Rate.It repeats the above process, until Ball-milling Time reaches 6 hours.Powder is taken out, soluble single can be obtained
Pipe.This solid phase modification single pipe powder can be saved for a long time due to not introducing any solvent, realize with
With taking.By jiggling, the single pipe powder that solid phase is modified can be dispersed in water.Dispersion liquid is in 23797g
Centrifugal force under be centrifuged 1 hour, the slightly worse carbon nanotube of dispersibility can be removed, to obtain well dispersed dispersion liquid.More than
It is not directed to place, is suitable for the prior art.
Specific embodiment described herein is only an example for the spirit of the invention.The neck of technology belonging to the present invention
The technical staff in domain can make various modifications or additions to the described embodiments or replace by a similar method
In generation, however, it does not deviate from the spirit of the invention or beyond the scope of the appended claims.
Claims (8)
1. a kind of method for preparing carbon nano tube dispersion liquid by solid phase removing, which comprises the following steps:
Carbon nanotube and solid phase dispersion agent are uniformly mixed, mixture is obtained；
Carbon nanotube powder by mixture ball-milling treatment, after obtaining solid phase removing；
Carbon nanotube powder after solid-phase ball milling is distributed in solvent, carbon nano tube dispersion liquid is obtained.
2. a kind of method for preparing carbon nano tube dispersion liquid by solid phase removing according to claim 1, which is characterized in that
It is further comprising the steps of: carbon nano tube dispersion liquid being centrifuged, the poor a small amount of aggregation of dispersibility is removed.
3. a kind of method for preparing carbon nano tube dispersion liquid by solid phase removing according to claim 1, which is characterized in that
The carbon nanotube is single wall or multi-walled carbon nanotube；
A kind of method preparing carbon nano tube dispersion liquid by solid phase removing according to claim 1, which is characterized in that institute
State one kind that dispersing agent is sodium taurocholate, hexahydroxy triphenylene, tannic acid, dodecyl sodium sulfate, NaTDC.
4. a kind of method for preparing carbon nano tube dispersion liquid by solid phase removing according to claim 1, which is characterized in that
The ball milling includes: after every ball milling 0.5-1 hours, and medication spoon scrapes the powder being affixed on tank skin and cover, uniformly to mix
It closes, improves grinding efficiency.
5. in addition, discontinuity ball milling also can guarantee that ball milling system temperature will not obviously rise；The above process recycles n times, wherein 1≤
N≤15。
6. a kind of method for preparing carbon nano tube dispersion liquid by solid phase removing according to claim 1, which is characterized in that
The diameter of mill ball in the ball milling is 2~16 millimeters.
7. a kind of method for preparing carbon nano tube dispersion liquid by solid phase removing according to claim 1, which is characterized in that
Mass ratio >=1:2 of the solid phase dispersion agent and carbon nanotube.
8. a kind of method for preparing carbon nano tube dispersion liquid by solid phase removing according to claim 1, which is characterized in that
The solvent is the organic solvents such as water or n,N-Dimethylformamide, tetrahydrofuran.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110591641A (en) * | 2019-01-25 | 2019-12-20 | 陕西科技大学 | Fe2O3@ MXene composite powder and preparation method thereof |
| CN114538419A (en) * | 2020-11-26 | 2022-05-27 | 江苏天奈科技股份有限公司 | Preparation method and equipment of dispersible carbon nanotube powder |
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| CN1374250A (en) * | 2002-04-19 | 2002-10-16 | 清华大学 | Method of utilizing external force to crush, wash and purify slender carbon nanotube |
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| CN1374250A (en) * | 2002-04-19 | 2002-10-16 | 清华大学 | Method of utilizing external force to crush, wash and purify slender carbon nanotube |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110591641A (en) * | 2019-01-25 | 2019-12-20 | 陕西科技大学 | Fe2O3@ MXene composite powder and preparation method thereof |
| CN114538419A (en) * | 2020-11-26 | 2022-05-27 | 江苏天奈科技股份有限公司 | Preparation method and equipment of dispersible carbon nanotube powder |
| CN114538419B (en) * | 2020-11-26 | 2023-08-18 | 江苏天奈科技股份有限公司 | Preparation method and equipment of dispersible carbon nano tube powder |
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