CN105885474A - Preparation method of carbon black-electrostatically adsorbed carbon nano tube conductive filler - Google Patents
Preparation method of carbon black-electrostatically adsorbed carbon nano tube conductive filler Download PDFInfo
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- CN105885474A CN105885474A CN201510420102.3A CN201510420102A CN105885474A CN 105885474 A CN105885474 A CN 105885474A CN 201510420102 A CN201510420102 A CN 201510420102A CN 105885474 A CN105885474 A CN 105885474A
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Abstract
The invention discloses a preparation method of a carbon black-electrostatically adsorbed carbon nano tube conductive filler, and belongs to the technical field of conductive material preparation. The technical problems that in the prior art, the cost is high, and a carbon nano tube is large in specific surface area and difficult to disperse are solved. The preparation method sequentially comprises the following three steps of 1 pretreating, wherein the surface of the carbon nano tube is coated with a layer of a cationic surfactant; 2 electrostatic adsorbing, wherein carbon black is electrostatically adsorbed on carbon nano tube prefabricated powder; 3 standing, filtering and drying. The carbon black-electrostatically adsorbed carbon nano tube conductive filler is obtained.
Description
Technical field
The invention belongs to conductive material preparing technical field, relate to a kind of carbon black Electrostatic Absorption carbon nanotube conducting
The preparation method of filler.
Background technology
Carbon atom on Sheet Graphite has a unpaired electron to be located normal on the P track of synusia, has
Well electric conductivity.CNT can regard Graphene curling as, so CNT and stone
Ink equally has good electric conductivity, and the electric conductivity of CNT depends on that graphite linings curls into pipe
The diameter of shape and helical angle.The electric conductivity of CNT between conductor and semi-conducting material, and with
(the energy gap width of CNT can change from zero to equal with silicon materials for n, difference m) helix parameter.
SWCN and the less multi-walled carbon nano-tubes of tube wall can show Quantum Teleportation.
Although CNT has the electric conductivity of excellence, but CNT is applied less in actual product,
The most relatively costly due to it, on the other hand big due to its specific surface area, it is difficult to dispersion.On solving
State problem, have people that carbon black is wrapped in carbon nano tube surface, thus reduce cost, to a certain degree promote
Dispersion.Such as: the Chinese patent of Application No. 200710048028.2 discloses a kind of CNT/granule
The preparation method of shape carbon complex, first carries out pickling with to CNT, removes unnecessary catalyst, with
After CNT is mixed with carbon black, obtain end product after drying.The method is by CNT and carbon
Black it is simply mixed, and both of which is electronegative, it is impossible to really combine.The most such as: application number
Be 200410040704.8 Chinese patent application disclose the preparation side of a kind of carbon containing nano tube conductive powder
Method, uses chemical vapour deposition technique directly to grow CNT on inorganic particle so that both have had very
Good combination, but the method preparation condition is harsh, is not suitable for large-scale batch production.Therefore the most still
So lack a kind of efficient, economic method preparing CNT/carbon black compounded mix.
Summary of the invention
The technical problem to be solved is just to provide a kind of carbon black Electrostatic Absorption carbon nanotube conducting filler
Preparation method, good dispersion, low cost, it is adaptable to industrialized mass production.
For solving above-mentioned technical problem, the present invention adopts the following technical scheme that a kind of carbon black Electrostatic Absorption carbon is received
The preparation method of mitron conductive filler, comprises the following steps successively:
Step one, pretreatment: first CNT and the first solvent are mixed, add cation surface activating
Agent, stirs, make carbon nano tube surface wrap up one layer of cationic surfactant, be then passed through filter,
It is dried, obtains the prefabricated powder body of CNT；
Step 2, Electrostatic Absorption: the prefabricated powder body of CNT step one obtained is dissolved in the second solvent,
And be slowly stirred, it is slowly added carbon black, makes carbon black Electrostatic Absorption on the prefabricated powder body of CNT, obtain
To composite solution；
Step 3, standing: composite solution step 2 obtained stands, until after being layered, passing through
Filter, be dried, obtain carbon black Electrostatic Absorption carbon nanotube conducting filler product.
CNT is first disperseed by the present invention with the first solvent, after forming carbon nano tube suspension, passes through
Wrapping up one layer of cationic surfactant in carbon nano tube surface, cationic surfactant molecule is in carbon nanometer
After ionizing in pipe suspension, the hydrophilic group being connected with lipophilic group is positively charged, then carries out carbon black electrostatic suction
Attached, stable carbon black Electrostatic Absorption carbon nanotube systems can be obtained, and due to cationic surfactant
Existence, Electrostatic Absorption process can be quickly completed between carbon black and CNT, be then passed through stand, filter
With i.e. can get carbon black Electrostatic Absorption carbon nanotube conducting filler product after drying.Dispersibility significantly improves, and inhales
Additive process can carry out rapidly and be properly completed, and output capacity is high.It addition, cationic surfactant is in the later stage
Need not remove, itself there is suitable electric conductivity, be conducive to improving carbon black Electrostatic Absorption CNT and lead
The electric conductivity that electricity filler product is overall.
Preferably, in described step one, the first solvent is deionized water, DMF, N-first
Any one or two or more compositions in base ketopyrrolidine.
Preferably, in described step one, cationic surfactant is fatty amine salt, ethanolamine salt, poly-second
Any one or two kinds in the many amine salt of alkene, quaternary ammonium salt, imidazoline, morpholine guanidine, triazine derivative with
On compositions.
Preferably, in described step one, the quality of the cationic surfactant of addition is the matter of CNT
The 5～20% of amount.
Preferably, in described step one, after CNT and the mixing of the first solvent, put into ultrasonic disperse equipment
Ultrasonic disperse 5～25min.Ultrasonic disperse equipment energy rapid dispersion CNT, forms the suspension of CNT
Liquid, and can guarantee that suspension has good stability.
Preferably, in described step 2, the second solvent is deionized water, DMF, N-first
Any one or two or more compositions in base ketopyrrolidine.
Preferably, in described step 2, the quality of the carbon black of addition is the 0.7～1.5 of the quality of CNT
Times.On the one hand carbon black promotes the dispersion effect of CNT, on the other hand reduces material cost, carbon black
Quality can account for carbon black Electrostatic Absorption carbon nanotube conducting filler product gross mass 50～70%, cost
Can be dropped by nearly half.
Preferably, in described step 2, mixing speed is 100～200r/min.
Preferably, in described step 3, time of repose is 30～120min.
Compared with prior art, the invention have the advantage that CNT and carbon black are combined by employing Electrostatic Absorption
Together, while electric conductivity both playing, material structure will not be produced and destroy；The addition of carbon black,
On the one hand promote the dispersion effect of CNT, on the other hand reduce material cost；By add sun from
Sub-surface activating agent, can promote the Electrostatic Absorption between CNT and carbon black more quickly and up hill and dale to carry out,
And be conducive to improving overall electric conductivity；Preparation method equipment needed thereby cost is relatively low, easy to operate, system
The standby cycle is shorter, and whole process is environment friendly and pollution-free, it is adaptable to industrialized mass production.
Accompanying drawing explanation
The invention will be further described with detailed description of the invention below in conjunction with the accompanying drawings:
Fig. 1 is the preparation method embodiment 1 of the present invention a kind of carbon black Electrostatic Absorption carbon nanotube conducting filler
Process chart.
Detailed description of the invention
As it is shown in figure 1, be the preparation method reality of the present invention a kind of carbon black Electrostatic Absorption carbon nanotube conducting filler
Execute example 1, comprise the following steps successively:
Step one, pretreatment: first mixed with 1000ml deionized water by 2g CNT, put into ultrasonic point
After being casually arranged with standby ultrasonic disperse 15min, add 0.2g cetyl trimethylammonium bromide, stir, make
Carbon nano tube surface one layer of cationic surfactant of parcel, is then passed through filtering, being dried, obtains carbon nanometer
Manage prefabricated powder body；
Step 2, Electrostatic Absorption: the prefabricated powder body of CNT step one obtained is dissolved in other 1000ml
In deionized water, and being slowly stirred, mixing speed is 150r/min, is slowly added 3g carbon black, makes carbon
Black Electrostatic Absorption, on the prefabricated powder body of CNT, obtains composite solution；
Step 3, standing: composite solution step 2 obtained stands, after time of repose is 90min, warp
Filter, be dried, obtain carbon black Electrostatic Absorption carbon nanotube conducting filler product.
The preparation method embodiment 2 of the present invention a kind of carbon black Electrostatic Absorption carbon nanotube conducting filler, according to enforcement
Prepared by the step of example 1, be with the difference of embodiment 1: the cetyl trimethyl bromination in step one
The addition of ammonium is 0.1g.
The preparation method embodiment 3 of the present invention a kind of carbon black Electrostatic Absorption carbon nanotube conducting filler, according to enforcement
Prepared by the step of example 1, be with the difference of embodiment 1: the cetyl trimethyl bromination in step one
The addition of ammonium is 0.3g.
The preparation method embodiment 4 of the present invention a kind of carbon black Electrostatic Absorption carbon nanotube conducting filler, according to enforcement
Prepared by the step of example 1, be with the difference of embodiment 1: the cetyl trimethyl bromination in step one
The addition of ammonium is 0.4g.
The preparation method embodiment 5 of the present invention a kind of carbon black Electrostatic Absorption carbon nanotube conducting filler, according to enforcement
Prepared by the step of example 1, be with the difference of embodiment 1: adding of CNT in step 2 and carbon black
Dosage is respectively 1g and 4g.
The preparation method embodiment 6 of the present invention a kind of carbon black Electrostatic Absorption carbon nanotube conducting filler, according to enforcement
Prepared by the step of example 1, be with the difference of embodiment 1: adding of CNT in step 2 and carbon black
Dosage is respectively 3g and 2g.
The preparation method embodiment 7 of the present invention a kind of carbon black Electrostatic Absorption carbon nanotube conducting filler, according to enforcement
Prepared by the step of example 1, be with the difference of embodiment 1: adding of CNT in step 2 and carbon black
Dosage is respectively 4g and 1g.
The preparation method embodiment 8 of the present invention a kind of carbon black Electrostatic Absorption carbon nanotube conducting filler, according to enforcement
Prepared by the step of example 1, be with the difference of embodiment 1: the time of repose in step 3 is 30min.
The preparation method embodiment 9 of the present invention a kind of carbon black Electrostatic Absorption carbon nanotube conducting filler, according to enforcement
Prepared by the step of example 1, be with the difference of embodiment 1: the time of repose in step 3 is 60min.
The preparation method embodiment 10 of the present invention a kind of carbon black Electrostatic Absorption carbon nanotube conducting filler, according to reality
Prepared by the step executing example 1, be with the difference of embodiment 1: the time of repose in step 3 is 120min.
Performance detects: the carbon black Electrostatic Absorption carbon nanometer preparation method embodiment 1～10 of the present invention prepared
Pipe conductive filler product, is modified making epoxy resin-base composite material to epoxy resin, then leads
Electric performance test, and contrast with the epoxide resin material of non-modified, result is as shown in table 1:
Table 1
| Resistivity/Ω cm |
| Embodiment 1 | 6.5×10-4 |
| Embodiment 2 | 8.8×101 |
| Embodiment 3 | 2.6×10-2 |
| Embodiment 4 | 4.5×10-3 |
| Embodiment 5 | 9.1×10-2 |
| Embodiment 6 | 1.2×10-1 |
| Embodiment 7 | 3.7×10-3 |
| Embodiment 8 | 3.1×10-1 |
| Embodiment 9 | 4.8×10-3 |
| Embodiment 10 | 9.7×10-3 |
| Comparative example | 1.0×1013 |
Illustrate: use the carbon black Electrostatic Absorption carbon nanotube conducting filler product that the present invention prepares, to asphalt mixtures modified by epoxy resin
Fat is modified making epoxy resin-base composite material, and its resistivity is 10-4～101Ω cm, well below not
The epoxide resin material being modified, illustrates that its electric conductivity is substantially better than the epoxide resin material of non-modified.
Meanwhile, the proportioning of addition, CNT and carbon black, standing to cetyl trimethylammonium bromide respectively
Time is adjusted, and by contrast experiment, the parameters impact on product characteristics is described.Find by contrast,
The resistivity using the composite obtained by the technological parameter in embodiment 1 can reach 6.5 × 10-4
Ω cm, is superior to other each embodiments.Meanwhile, carbon black proportion account for nearly 50%, carbon black relative to
CNT cost is almost negligible, and the most raw-material cost can reduce half, it is seen then that implement
Example 1 is comparatively ideal technical scheme.
Additionally, cationic surfactant can also select fatty amine salt, ethanolamine salt, polyethylene polyamines salt,
Any one or two or more compositions in quaternary ammonium salt, imidazoline, morpholine guanidine, triazine derivative,
Above-mentioned is to carry out comparative illustration as a example by cetyl trimethylammonium bromide, it is not limited to cetyl three
Methyl bromide ammonium is as cationic surfactant.
The foregoing is only the specific embodiment of the present invention, but the technical characteristic of the present invention be not limited thereto,
Any those skilled in the art is in the field of the invention, and change or the modification made all are contained in the present invention
The scope of the claims among.
Claims (9)
1. the preparation method of a carbon black Electrostatic Absorption carbon nanotube conducting filler, it is characterised in that: include successively with
Lower step:
Step one, pretreatment: first CNT and the first solvent are mixed, add cationic surfactant,
Stir, make carbon nano tube surface wrap up one layer of cationic surfactant, be then passed through filtering, being dried,
Obtain the prefabricated powder body of CNT；
Step 2, Electrostatic Absorption: the prefabricated powder body of CNT step one obtained is dissolved in the second solvent, and
It is slowly stirred, is slowly added carbon black, make carbon black Electrostatic Absorption on the prefabricated powder body of CNT, obtain
Composite solution；
Step 3, standing: composite solution step 2 obtained stands, until after being layered, through filtering,
It is dried, obtains carbon black Electrostatic Absorption carbon nanotube conducting filler product.
The preparation method of a kind of carbon black Electrostatic Absorption carbon nanotube conducting filler the most as claimed in claim 1, it is special
Levying and be: in described step one, the first solvent is deionized water, DMF, N-methyl
Any one or two or more compositions in ketopyrrolidine.
The preparation method of a kind of carbon black Electrostatic Absorption carbon nanotube conducting filler the most as claimed in claim 1, it is special
Levying and be: in described step one, cationic surfactant is fatty amine salt, ethanolamine salt, polyethylene
Any one or two kinds in many amine salt, quaternary ammonium salt, imidazoline, morpholine guanidine, triazine derivative with
On compositions.
The preparation method of a kind of carbon black Electrostatic Absorption carbon nanotube conducting filler the most as claimed in claim 1, it is special
Levying and be: in described step one, the quality of the cationic surfactant of addition is the quality of CNT
5～20%.
The preparation method of a kind of carbon black Electrostatic Absorption carbon nanotube conducting filler the most as claimed in claim 1, it is special
Levy and be: in described step one, after CNT and the mixing of the first solvent, put into ultrasonic disperse equipment and surpass
Sound dispersion 5～25min.
The preparation method of a kind of carbon black Electrostatic Absorption carbon nanotube conducting filler the most as claimed in claim 1, it is special
Levying and be: in described step 2, the second solvent is deionized water, DMF, N-methyl
Any one or two or more compositions in ketopyrrolidine.
The preparation method of a kind of carbon black Electrostatic Absorption carbon nanotube conducting filler the most as claimed in claim 1, it is special
Levying and be: in described step 2, the quality of the carbon black of addition is 0.7～1.5 times of the quality of CNT.
The preparation method of a kind of carbon black Electrostatic Absorption carbon nanotube conducting filler the most as claimed in claim 1, it is special
Levying and be: in described step 2, mixing speed is 100～200r/min.
The preparation method of a kind of carbon black Electrostatic Absorption carbon nanotube conducting filler the most as claimed in claim 1, it is special
Levying and be: in described step 3, time of repose is 30～120min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107416795A (en) * | 2017-09-06 | 2017-12-01 | 张永霞 | A kind of preparation method of conductive carbon nanotube tube material |
| CN108948529A (en) * | 2018-07-06 | 2018-12-07 | 佛山市高明区爪和新材料科技有限公司 | A kind of preparation method of composite conductive plastic |
| KR20190120532A (en) * | 2018-04-16 | 2019-10-24 | 오씨아이 주식회사 | Apparatus for manufacturing carbon black |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007144322A1 (en) * | 2006-06-14 | 2007-12-21 | Basf Se | Method for producing electrically conductive surfaces on a carrier |
| CN102151529A (en) * | 2011-02-11 | 2011-08-17 | 许昌学院 | Phenolic resin coated carbon nanotube composite material and chemical preparation method thereof |
| CN102321398A (en) * | 2011-09-02 | 2012-01-18 | 广东工业大学 | A kind of preparation method of carbon black enveloped carbon nanometer tube heat conductive filler |
-
2015
- 2015-07-16 CN CN201510420102.3A patent/CN105885474B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007144322A1 (en) * | 2006-06-14 | 2007-12-21 | Basf Se | Method for producing electrically conductive surfaces on a carrier |
| CN102151529A (en) * | 2011-02-11 | 2011-08-17 | 许昌学院 | Phenolic resin coated carbon nanotube composite material and chemical preparation method thereof |
| CN102321398A (en) * | 2011-09-02 | 2012-01-18 | 广东工业大学 | A kind of preparation method of carbon black enveloped carbon nanometer tube heat conductive filler |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107416795A (en) * | 2017-09-06 | 2017-12-01 | 张永霞 | A kind of preparation method of conductive carbon nanotube tube material |
| KR20190120532A (en) * | 2018-04-16 | 2019-10-24 | 오씨아이 주식회사 | Apparatus for manufacturing carbon black |
| KR102587771B1 (en) | 2018-04-16 | 2023-10-12 | 오씨아이 주식회사 | Apparatus for manufacturing carbon black |
| CN108948529A (en) * | 2018-07-06 | 2018-12-07 | 佛山市高明区爪和新材料科技有限公司 | A kind of preparation method of composite conductive plastic |
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