CN106128556A - A kind of preparation method of high dispersive type oil system carbon nanotube conducting slurry - Google Patents
A kind of preparation method of high dispersive type oil system carbon nanotube conducting slurry Download PDFInfo
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- CN106128556A CN106128556A CN201610514307.2A CN201610514307A CN106128556A CN 106128556 A CN106128556 A CN 106128556A CN 201610514307 A CN201610514307 A CN 201610514307A CN 106128556 A CN106128556 A CN 106128556A
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- carbon nanotube
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
Abstract
The invention discloses the preparation method of a kind of high dispersive type oil system carbon nanotube conducting slurry, described method is: CNT is carried out high-speed stirred, dispersant is dissolved in liquid in the carbon nanotube dust being sprayed in stirring by the way of spraying simultaneously, carbon nano tube surface is activated, the activated carbon nanotube obtained;Activated carbon nanotube mixes with organic resin, organic solvent B, antisettling agent, defoamer, through ultrasonic or sand milling technique mix homogeneously, prepares high dispersive type oil system carbon nanotube conducting slurry.Prepared by the present invention high dispersive type oil system carbon nanotube conducting slurry electric conductivity is good, and antistatic property is good, and dispersibility is good, can preserve for a long time.
Description
One, technical field
The present invention relates to the preparation method of a kind of high dispersive type oil system carbon nanotube conducting slurry.
Two, background technology
Electrically-conducting paint is to be applied on the macromolecular material of high resistivity, is allowed to have conduction electric current and eliminating accumulation electrostatic charge
The sapecial coating of ability, can be coated on surface or the inside of any shape substrate.Electrically-conducting paint can be divided by composition and electrical conduction mechanism
It is two big classes: structural type (also known as Intrinsical) electrically-conducting paint and compound (also known as addition type) electrically-conducting paint.Intrinsically conducting is coated with
The conductive material of material is high polymer self.The conductive material of addition type electrically-conducting paint is the conducting objects added in insulation high polymer
Matter (metal, graphite etc.), utilizes the electric action of conductive materials, makes high polymer have electric conductivity.
It is compound-type conducting coating that current practice obtains more, and it utilizes conductive filler to realize conduction, its
Electrical conduction mechanism is more complicated, contacts with each other formation continuous network chain than more consistent view mainly conductive filler at present, carrier
Can move on network chain, so that coated conductive.Electrically-conducting paint be mainly used for antistatic (ESD), electromagnetic wave shielding (EMI)
With as electric heating body, the class that wherein antistatic coating is most widely used in being current all electrically-conducting paints.Conductive filler
It is the important component part of addition type electrically-conducting paint, is also the emphasis of the required research of electrically-conducting paint, can serve as leading of electrically-conducting paint
Electric material is usually metal system filler, and the shape of metal particle, consumption, stability, skin effect etc. all can affect leading of coating
Electrical property. in general, the coating selecting flake or dendritic metal to fill is better than the coatings conductive property that ball-type metal is filled.
Just can form space conductive network when the consumption of conductive filler reaches critical concentration, the electric conductivity of coating just can significantly improve. and right
Some oxidizable metals (such as Cu) must add corresponding antioxidant in coating.In addition to make conductive filler and matrix
Resin should have certain affinity and wettability, also needs to add certain dispersant and coupling agent etc..But the dispersibility of filler
Can not be very good, otherwise make interparticle connection first separate out with base material polymer and carry out simultaneously, form even-textured film, electricity
Conductance declines.It addition, conventional conductive filler also include carbon system filler, burning system filler and compound be filler.
CNT since being found for 1991, and between the short more than ten years, the carbonaceous tube of this nano-scale is just
Cause the broad interest of the scientific circles such as global physics, chemistry and material.Special construction and excellence due to CNT
Mechanics, electrical and optical performance and its potential industrial value so that it is be increasingly becoming the ambits such as chemistry, physics and material
Study hotspot.Owing to CNT has good electric conductivity, have again bigger draw ratio simultaneously, thus be well suited for leading
Electricity filler, relative to other metallic particles and graphite granule, just can form conductive net, and its density compares metal by little amount
Granule is much smaller, is difficult to the coagulation because of the effect of gravity.
But, owing to CNT is a kind of high degree of polarization, ganoid inorganic macromolecule compound, surface defect
Less, lack active group, between CNT, there is stronger Van der Waals force and its huge specific surface area, the highest length simultaneously
Footpath ratio, causes in the ordinary course of things, and CNT is easily wound around reunion bunchy.CNT game performance to be played makes it extensively should
With, the dispersion how solving CNT is critical problem.At present, the method for dispersing Nano carbon tubes has grinding and stirring, high energy
The washing of ball milling, ultrasonic Treatment, strong acid and strong base, interpolation surfactant, growth in situ synthesis, multiple method integrated treatment etc..
Three, summary of the invention
The invention provides a kind of high dispersive type oil system carbon nanotube conducting slurry, by preprocessed for CNT modification
After, add in organic solvent as conductive filler, thus prepare high dispersive type oil system carbon nanotube conducting slurry.
The technical solution used in the present invention is:
The preparation method of a kind of high dispersive type oil system carbon nanotube conducting slurry, said method comprising the steps of:
(1) oiliness dispersant is dissolved in organic solvent A, obtains dispersant solution, then by dispersant solution by height
Pressure spray process sprays in the CNT of high-speed stirred, after high-speed stirred mixing, prepares activated carbon nanotube;
(2) activated carbon nanotube mixes with organic resin, organic solvent B, antisettling agent, defoamer, through ultrasonic or sand milling
Technique mix homogeneously, prepares described high dispersive type oil system carbon nanotube conducting slurry;
In described step (1), described CNT, oiliness dispersant, the mass fraction ratio of organic solvent A are 85~95:
0.1~5:5~10.
Described oiliness dispersant is polyvinylpyrrolidone, polyvinyl alcohol, Triton X-100, alkyl phenol epoxy
One or more mixture in oxide condensate emulsifying agent, Kynoar.
Described organic solvent A or organic solvent B each stand alone as N,N-dimethylformamide, N-Methyl pyrrolidone, two
One or both in methylformamide, dimethyl sulfoxide, chloroform, petroleum ether, ethyl acetate, butyl acetate, acetone, Ketohexamethylene
Above mixture.
Described CNT is one or both the mixture in multi-walled carbon nano-tubes, SWCN, the most
Wall carbon nano tube.
In described method, organic solvent A and organic solvent B are for distinguishing the organic solvent used in different step, A, B
Not there is chemical sense.
In described step (2), organic resin, activated carbon nanotube, organic solvent B, antisettling agent, the mass parts of defoamer
Number is 10~60 mass parts, 5~40 mass parts, 20~70 mass parts, 0.01~10 mass parts, 0.01~10 mass parts, preferably
It is 20~40 mass parts, 10~40 mass parts, 30~60 mass parts, 0.1~5 mass parts, 0.1~5 mass parts.
Described organic resin selected from epoxy resin, polyurethane resin, polyester resin, acrylic resin, silicone resin or
In one or more mixture in polyether polyol resin, preferably epoxy resin, acrylic resin, polyester resin
Any one or two or more mixture.Described organic resin is commercially available.
In described step (2), described antisettling agent is organically-modified boron-moisten soil, polyamide anti-settling wax slurry, gas phase two
One or more mixing in silicon oxide, can be purchased from the modest chemistry of moral, Degussa company and ROCKWOOD company etc..
Described defoamer has relatively low surface tension and high surfaces activity, can suppress or eliminate adding at ultrasonic or sand milling
The foam produced in liquid during work, described defoamer is preferably mineral oil, polysiloxane polyether copolymer, polyethers chemical combination
One or more mixing in thing, modified organic silicon mixture.BYK-065 defoamer, BYK-such as the production of BYK company
The TEGO-940 defoamer that 066N defoamer, TEGO company produce, the EFKA-2022 defoamer etc. that EFKA company produces.
In described step (1), described high-pressure spraying method is that dispersant solution passes through the high-pressure spray device shape with spraying
Formula sprays into the CNT of high-speed stirred, and described high-pressure spray device can use high-pressure spraying machine, will dispersion by high-pressure hydraulic pump
Agent solution becomes spray form to spray in material through high-pressure nozzle.Described high-pressure spraying machine still belongs to the first time for CNT pretreatment.
Dispersant solution is atomized by high-pressure spraying method, obtains a large amount of fine droplet after atomization, significantly increases solution and CNT
Contact area, beneficially carbon nanotube particulate are coated with by auxiliary agent, strengthen its dispersibility.
In described high-pressure spraying method, spray rate is generally 10~100ml/min;
Atomized particle size is 0.1~1um.
In described step (1), the rotating speed of described high-speed stirred is 300~1500 turns/min.
The time of described high-speed stirred mixing is generally 1 minute~1 hour, preferably 5~40 minutes.
The present invention carries out high-speed stirred to CNT, to its surface pretreatment, dispersant is dissolved in liquid simultaneously
In sprayed in the carbon nanotube dust in stirring by the way of spraying so that carbon nano tube surface activates, and is divided simultaneously
Powder uniform wet, causes to be formed between CNT and repels, and improves CNT dispersibility in a solvent, and can be simultaneously
Improve the bulk density of CNT, to obtain optimal dispersion effect and good processability.
The present invention is by preprocessed for CNT modified, then by activated carbon nanotube and organic resin, organic solvent, anti-
Sedimentation agent, defoamer etc. mix, and are mixed uniformly by ultrasonic, sand milling technique, prepare high efficiency dispersion type oil system carbon nanometer
Pipe electrocondution slurry.The electrocondution slurry prepared reduces the reunion degree of CNT so that it is be preferably scattered in solvent, shape
Reticulate structure, improve its conductive capability, greatly reduce the sedimentation velocity of CNT simultaneously, extend product preservation and
In the use cycle, the good dispersion of slurry, storage stability is outstanding.
The present invention provides high dispersive type oil system carbon nanotube conducting slurry can be applied as electromagnetic screen coating, antistatic
Coating, electrically-conducting paint.
Four, detailed description of the invention
With specific embodiment, technical scheme is described further below, but the protection content of the present invention is not
It is limited to this.
Embodiment 1~16
According to the form below 1 takes each raw material, is dissolved in organic solvent by oiliness dispersant, obtains dispersant solution, then will dispersion
Agent solution sprays into the CNT of high-speed stirred (diameter 1~30nm, length 1~100 μm, bulk density by high-pressure spraying method
In 0.02g/mL), technological parameter is as shown in table 1, after high-speed stirred mixing, prepares activated carbon nanotube;
Table 1
The performance test results such as table 2 below of the activated carbon nanotube prepared
Table 2
Dispersibility experiment detection by the following method: the activated carbon nanotube 10mg that embodiment 1~16 prepares is separately added into
10mL prepares in this solvent (seeing table 1) used by activated carbon nanotube, and ultrasonic disperse 30 minutes obtains suspension, stands, goes out
When being the most substantially layered, the record time is the holding time, and acquired results refers to table 2.Holding time is the longest, shows that its dispersibility is more
Good.The most pretreated CNT cannot form stable suspension.
Above-mentioned test result indicate that, after pretreatment, the bulk density of CNT improve about 10 times (untreated
The bulk density of CNT is about 0.02g/mL), dispersibility is all significantly increased.
Embodiment 17~32
Activated carbon nanotube prepared by embodiment 1~16 is mixed with organic resin, organic solvent, antisettling agent, defoamer
Close, through ultrasonic or sand milling technique mix homogeneously, prepare described high dispersive type oil system carbon nanotube conducting slurry;Each raw material dosage is shown in
Table 3.Embodiment 17~24 uses ultrasonic technique, and embodiment 25~32 uses sand milling technique.
Solid content and the performance data of the high dispersive type oil system carbon nanotube conducting slurry prepared are as shown in table 4.Its
Middle storage stability (1 year) detects according to standard " GB6753.3 ".
High dispersive type oil system carbon nanotube conducting pulp spraying embodiment 17~32 prepared is applied in PET base material, according to
The sheet resistance of " GB/T1410-2006 solid insulating material specific insulation and surface resistivity test method " testing coating
Rate, result is as shown in table 4.
Table 3
Table 4
Embodiment data show, the antistatic of the preparation of prepared by the present invention high dispersive type oil system carbon nanotube conducting slurry
The surface resistivity of coating is preferable, and surface resistivity is 106~108About Ω, antistatic property is good, and used anti-quiet
The consumption of the antistatic additive of the amount ratio prior art same performance to be reached of electricity agent (i.e. CNT) to significantly reduce.Dispersion
Property is excellent, and long-term preservability can show outstanding.
Claims (10)
1. the preparation method of a high dispersive type oil system carbon nanotube conducting slurry, it is characterised in that described method includes following step
Rapid:
(1) oiliness dispersant is dissolved in organic solvent A, obtains dispersant solution, then dispersant solution is passed through high pressure spray
Pouring method sprays in the CNT of high-speed stirred, after high-speed stirred mixing, prepares activated carbon nanotube;
(2) activated carbon nanotube mixes with organic resin, organic solvent B, antisettling agent, defoamer, through ultrasonic or sand milling technique
Mix homogeneously, prepares described high dispersive type oil system carbon nanotube conducting slurry.
2. the method for claim 1, it is characterised in that in described step (1), described CNT, oiliness dispersant,
The mass fraction ratio of organic solvent A is 85~95:0.1~5:5~10.
3. the method for claim 1, it is characterised in that in described step (1), described oiliness dispersant is polyethylene pyrrole
In pyrrolidone, polyvinyl alcohol, Triton X-100, alkyl phenol ethylene oxide condensation substance emulsifying agent, Kynoar
One or more mixture.
4. the method for claim 1, it is characterised in that described organic solvent A or organic solvent B each stand alone as N, N-
Dimethylformamide, N-Methyl pyrrolidone, dimethylformamide, dimethyl sulfoxide, chloroform, petroleum ether, ethyl acetate, acetic acid
One or more mixture in butyl ester, acetone, Ketohexamethylene.
5. the method for claim 1, it is characterised in that in described step (2), described organic resin, activated carbon nanometer
Pipe, organic solvent B, antisettling agent, the mass fraction of defoamer are 10~60 mass parts, 5~40 mass parts, 20~70 mass
Part, 0.01~10 mass parts, 0.01~10 mass parts.
6. the method for claim 1, it is characterised in that in described step (2), described organic resin, activated carbon nanometer
Pipe, organic solvent B, antisettling agent, the mass fraction of defoamer are 20~40 mass parts, 10~40 mass parts, 30~60 mass
Part, 0.1~5 mass parts, 0.1~5 mass parts.
7. the method for claim 1, it is characterised in that in described step (2), described organic resin selected from epoxy resin,
In polyurethane resin, polyester resin, acrylic resin, silicone resin or polyether polyol resin one or more
Mixture.
8. the method for claim 1, it is characterised in that in described step (2), described antisettling agent is organically-modified
Boron-moisten soil, polyamide anti-settling wax slurry, one or more mixing in aerosil.
9. the method for claim 1, it is characterised in that in described step (2), described defoamer is mineral oil, poly-silica
One or more mixing in alkane copolyether, polyether compound, modified organic silicon mixture.
10. the method for claim 1, it is characterised in that described CNT is multi-walled carbon nano-tubes, single
One or both mixture in pipe.
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Cited By (5)
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CN107482220A (en) * | 2017-06-23 | 2017-12-15 | 深圳市德方纳米科技股份有限公司 | A kind of lithium ion battery conductive carbon pastes and its preparation method and application |
CN108986985A (en) * | 2018-06-07 | 2018-12-11 | 太仓萃励新能源科技有限公司 | A kind of production method of waterborne conductive slurry |
CN111450771A (en) * | 2020-04-01 | 2020-07-28 | 中国石油天然气股份有限公司 | Multifunctional integrated Pickering particle emulsifier and preparation method thereof |
CN115073979A (en) * | 2022-05-27 | 2022-09-20 | 广东安拓普聚合物科技有限公司 | Preparation method of antistatic cable and cable prepared by preparation method |
CN115417400A (en) * | 2022-09-15 | 2022-12-02 | 明光科迪新材料有限公司 | Preparation of carbon nano tube dispersion liquid for antistatic fiber coating |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN107482220A (en) * | 2017-06-23 | 2017-12-15 | 深圳市德方纳米科技股份有限公司 | A kind of lithium ion battery conductive carbon pastes and its preparation method and application |
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CN111450771A (en) * | 2020-04-01 | 2020-07-28 | 中国石油天然气股份有限公司 | Multifunctional integrated Pickering particle emulsifier and preparation method thereof |
CN115073979A (en) * | 2022-05-27 | 2022-09-20 | 广东安拓普聚合物科技有限公司 | Preparation method of antistatic cable and cable prepared by preparation method |
CN115417400A (en) * | 2022-09-15 | 2022-12-02 | 明光科迪新材料有限公司 | Preparation of carbon nano tube dispersion liquid for antistatic fiber coating |
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