CN104844820B - A kind of carbon nanotube conducting master batch and its preparation method and application - Google Patents
A kind of carbon nanotube conducting master batch and its preparation method and application Download PDFInfo
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- CN104844820B CN104844820B CN201510200400.1A CN201510200400A CN104844820B CN 104844820 B CN104844820 B CN 104844820B CN 201510200400 A CN201510200400 A CN 201510200400A CN 104844820 B CN104844820 B CN 104844820B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 43
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 43
- 239000004594 Masterbatch (MB) Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000003960 organic solvent Substances 0.000 claims abstract description 12
- 239000000654 additive Substances 0.000 claims abstract description 11
- 230000000996 additive effect Effects 0.000 claims abstract description 11
- 238000013019 agitation Methods 0.000 claims abstract description 7
- 239000012141 concentrate Substances 0.000 claims abstract description 3
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- 239000000463 material Substances 0.000 claims description 28
- 239000004743 Polypropylene Substances 0.000 claims description 9
- -1 polypropylene Polymers 0.000 claims description 8
- 239000004793 Polystyrene Substances 0.000 claims description 7
- 229920001707 polybutylene terephthalate Polymers 0.000 claims description 7
- 229920002292 Nylon 6 Polymers 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- UAUDZVJPLUQNMU-KTKRTIGZSA-N erucamide Chemical compound CCCCCCCC\C=C/CCCCCCCCCCCC(N)=O UAUDZVJPLUQNMU-KTKRTIGZSA-N 0.000 claims description 5
- GTDHYNXLIKNVTJ-UHFFFAOYSA-N n-(1-hydroxy-2-methylpropan-2-yl)octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NC(C)(C)CO GTDHYNXLIKNVTJ-UHFFFAOYSA-N 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- FATBGEAMYMYZAF-KTKRTIGZSA-N oleamide Chemical compound CCCCCCCC\C=C/CCCCCCCC(N)=O FATBGEAMYMYZAF-KTKRTIGZSA-N 0.000 claims description 4
- FATBGEAMYMYZAF-UHFFFAOYSA-N oleicacidamide-heptaglycolether Natural products CCCCCCCCC=CCCCCCCCC(N)=O FATBGEAMYMYZAF-UHFFFAOYSA-N 0.000 claims description 4
- 229920000573 polyethylene Polymers 0.000 claims description 4
- 229920002223 polystyrene Polymers 0.000 claims description 4
- 239000004698 Polyethylene Substances 0.000 claims description 3
- 229920000642 polymer Polymers 0.000 claims description 3
- 229920001155 polypropylene Polymers 0.000 claims description 3
- 239000002861 polymer material Substances 0.000 claims description 2
- TXQVDVNAKHFQPP-UHFFFAOYSA-N [3-hydroxy-2,2-bis(hydroxymethyl)propyl] octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(CO)(CO)CO TXQVDVNAKHFQPP-UHFFFAOYSA-N 0.000 claims 1
- 238000009413 insulation Methods 0.000 abstract description 10
- 238000005191 phase separation Methods 0.000 abstract description 5
- 239000004033 plastic Substances 0.000 abstract description 3
- 229920003023 plastic Polymers 0.000 abstract description 3
- 239000002216 antistatic agent Substances 0.000 description 16
- 238000000034 method Methods 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- 238000002156 mixing Methods 0.000 description 5
- WSEFPKKOUNRCAJ-UHFFFAOYSA-N 2,2-bis(hydroxymethyl)propane-1,3-diol;octadecanoic acid Chemical compound OCC(CO)(CO)CO.CCCCCCCCCCCCCCCCCC(O)=O WSEFPKKOUNRCAJ-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 229920005669 high impact polystyrene Polymers 0.000 description 3
- 239000004797 high-impact polystyrene Substances 0.000 description 3
- 230000004931 aggregating effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 238000005461 lubrication Methods 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229920000426 Microplastic Polymers 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000002305 electric material Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000005453 pelletization Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Abstract
The present invention relates to plastic master batch preparing technical field, specifically disclose a kind of carbon nanotube conducting master batch and its preparation method and application.The preparation method of described carbon nanotube conducting master batch, comprises the steps of: antistatic additive is dissolved and obtains solution A in organic solvent by S1.；S2. CNT is put into organic solvent for ultrasonic dispersion, add solution A ultrasonic under mechanical agitation, concentrate removing organic solvent and obtain paste；S3. paste is added heat fusing, then by melted paste through freely falling body drippage, cool down and i.e. obtain described carbon nanotube conducting master batch.Described carbon nanotube conducting master batch has the specific insulation of excellence, can form the high-effective conductive network of rotation joint phase separation structure in the application.
Description
Technical field
The present invention relates to plastic master batch preparing technical field, be specifically related to a kind of carbon nanotube conducting master batch and preparation side thereof
Method and application.
Background technology
Macromolecular material obtains large-scale application in various fields such as national defence, military project, electronic products at present.But it is most of high
Molecular material has higher specific insulation, and owing to macromolecular material self-resistance rate is high, electrostatic is difficult to remove and cause amassing
Tired voltage is very big, and production and use process to plastic cause the biggest negative effect.Such as electrostatic can make in air
Dust be adsorbed on goods and affect its outward appearance, reduce its commercial value, and for example goods static electricity during printing can make ink or fuel
Attachment inequality easily comes off, and electrostatic can produce electric discharge phenomena for another example, so cause click to catch fire, the accident such as smashed district.Electrostatic
It is also possible to damage the serviceability of product, such as the envelope assembly and disassembly behavior etc. of electronic chip.Reduce this kind of electrostatic at present most effective
Method be in macromolecular material interpolation conductive agglomerate.
The existing method preparing conductive agglomerate is through twin screw by antistatic additive such as the material with carbon elements such as CNT and polyethylene
Extruder or banbury melt blending prepare.CNT cannot be had by the preparation method at existing this conductive agglomerate
Effect dispersion, CNT is mutual aggregating state (as shown in Figure 1), it is necessary to make that each aggregate is close to each other could form conductive mesh
Network conducts electricity.The result causing final application is that wanting to arrive certain specific insulation must increase CNT consumption.Due to
CNT is the most expensive, increases CNT consumption thus the cost of material can be caused to increase.On the other hand CNT is increased
Consumption can cause its material property applied to decline.Therefore, develop and a kind of there is excellent specific insulation, apply in reality
In can form the conductive agglomerate of high-effective conductive network there is good market prospect.
Summary of the invention
The technical problem to be solved is, in order to overcome conductive agglomerate in prior art can not form high-effective conductive
The technical problem that network, electric conductivity are the best, it is provided that a kind of carbon nanotube conducting master batch.
Above-mentioned technical problem to be solved by this invention is achieved by the following technical programs:
The preparation method of a kind of carbon nanotube conducting master batch, it is characterised in that comprise the steps of:
S1. antistatic additive is dissolved and obtain solution A in organic solvent；
S2. CNT is put into organic solvent for ultrasonic dispersion, add solution A ultrasonic under mechanical agitation, concentrate
Remove organic solvent and obtain paste；
S3. paste is added heat fusing, then by melted paste through freely falling body drippage, cool down i.e. obtain described
Carbon nanotube conducting master batch；
Antistatic additive described in S1 is in oleamide, erucyl amide, stearmide and tetramethylolmethane stearate
One or more.
The selected oleamide of the present invention, erucyl amide, stearmide and tetramethylolmethane stearate etc. are amorphous, have
Dispersion, lubrication and the organic material of certain antistatic property, be mixed with conductive agglomerate with CNT under solution state, this
CNT can effectively be scatter by method, forms the high-effective conductive network of rotation joint phase separation structure in the middle of reality application
(as shown in Figure 2).Effectively prevent CNT in prior art to disperse not open, the situation forming aggregating state occurs.Permissible
It is greatly saved CNT usage amount, industrial production cost is greatly lowered.
Preferably, the antistatic additive described in S1 is 1 ~ 2:1 ~ 2 with the weight consumption ratio of the CNT in S2.
Most preferably, the weight consumption of the antistatic additive described in S1 and the CNT in S2 is than for 1:1.
Preferably, the organic solvent described in S1 and S2 is ethanol.
Preferably, the ultrasonic disperse described in S2, its jitter time is 1 ~ 3h.
Preferably, the paste described in S2 contains the CNT of 30 ~ 70% weight.
Most preferably, the paste described in S2 contains the CNT of 50% weight.
Preferably, the particle diameter preparing carbon nanotube conducting master batch in S3 is 2 ~ 4mm.
Most preferably, the particle diameter preparing carbon nanotube conducting master batch in S3 is 3mm.
The present invention provides a kind of carbon nanotube conducting master batch prepared by above-mentioned preparation method.
The application in forming rotation joint Phase Separating Morphology high-effective conductive network of the described carbon nanotube conducting master batch.
Preferably, described application, is to be blended with melt polymer material by carbon nanotube conducting master batch, is shape after cooling
Cheng Xuanjie Phase Separating Morphology high-effective conductive network.
Preferably, described macromolecular material is polypropylene material (PP), polythene material (PE), polystyrene material
(PS), ABS polymer (ABS), impact resistant polystyrene material (HIPS), polyamide 6 material
Material (PA6) or polybutylene terephthalate (PBT) material (PBT).
Relative to prior art, there is advantages that
(1) present invention uses the mode of solution blending to prepare carbon nanotube conducting master batch, has overturned existing melt blended
Mode prepares carbon nanotube conducting master batch so that under the consumption using same carbon nano-tube material, specific insulation ratio is existing
Technology prepares little 5 ~ 6 orders of magnitude of specific insulation of conductive agglomerate；
(2) CNT is first disperseed in organic solvent, be subsequently adding antistatic additive, can effectively prevent after removing solvent
The reunion again of CNT, by melted rear tear drop, makes the granule close with plastic pellet size, it is simple to when applying subsequently
The situation that mixing is uneven occurs, uses after convenient mixing；
(3) with acid amide, erucyl amide, these are amorphous for stearmide or tetramethylolmethane stearate, have dispersion,
Lubrication and the organic material of certain antistatic property, can make CNT form rotation joint phase separation structure in application subsequently
High-effective conductive network；Rather than as tradition master batch, it is necessary in whole matrix, conducting particles forms overlap joint close to each other
After conductive network, just conduction (typically to reach 106, need the CNT of more than 8%), so can be less with expensive CNT
(CNT of about 4% is only needed i.e. to can reach 102Conductive effect), reach identical conductive effect, greatly reduce into
This.
Accompanying drawing explanation
Fig. 1 is the aggregate conduction close to each other schematic diagram that traditional carbon nanotube conducting master batch is formed.
Fig. 2 is the fully dispersed high-effective conductive network conduction signal forming rotation joint phase separation structure of CNT of the present invention
Figure.
Fig. 3 is the carbon nanomaterial scatter diagram in anti-static material PP described in embodiment 5.
Detailed description of the invention
The present invention is explained further below in conjunction with specific embodiment, but the present invention is not done any type of limit by embodiment
Fixed.
Embodiment 1
S1. 200g oleamide is dissolved in 1L ethanol and obtains solution A；
S2. 200g CNT is put into ultrasonic disperse 1h in 4L ethanol, adds solution A ultrasonic under mechanical agitation,
Concentrating under reduced pressure removes ethanol must be containing the paste of 50% wt carbon nanotube；
S3. paste is added heat fusing, then melted paste is dripped through freely falling body, drops on cold metal plate
Cool down to obtain the carbon nanotube conducting master batch of particle diameter about 3mm.
Embodiment 2
S1. 200g erucyl amide is dissolved in 1L ethanol and obtains solution A；
S2. 200g CNT is put into ultrasonic disperse 1h in 4L ethanol, adds solution A ultrasonic under mechanical agitation,
Concentrating under reduced pressure removes ethanol must be containing the paste of 50% wt carbon nanotube；
S3. paste is added heat fusing, then melted paste is dripped through freely falling body, drops on cold metal plate
Cool down to obtain the carbon nanotube conducting master batch of particle diameter about 3mm.
Embodiment 3
S1. 200g stearmide is dissolved in 1L ethanol and obtains solution A；
S2. 200g CNT is put into ultrasonic disperse 1h in 4L ethanol, adds solution A ultrasonic under mechanical agitation,
Concentrating under reduced pressure removes ethanol must be containing the paste of 50% wt carbon nanotube；
S3. paste is added heat fusing, then melted paste is dripped through freely falling body, drops on cold metal plate
Cool down to obtain the carbon nanotube conducting master batch of particle diameter about 3mm.
Embodiment 4
S1. 200g tetramethylolmethane stearate is dissolved in 1L ethanol and obtains solution A；
S2. 200g CNT is put into ultrasonic disperse 1h in 4L ethanol, adds solution A ultrasonic under mechanical agitation,
Concentrating under reduced pressure removes ethanol must be containing the paste of 50% wt carbon nanotube；
S3. paste is added heat fusing, then melted paste is dripped through freely falling body, drops on cold metal plate
Cool down to obtain the carbon nanotube conducting master batch of particle diameter about 3mm.
The preparation of embodiment 5 anti-static material PP
The carbon nanotube conducting master batch that 800g embodiment 1 is prepared and 9200g polypropylene material (PP) material molten
It is blended, after double screw extruder extrusion cooling, forms the anti-static material PP with rotation joint Phase Separating Morphology high-effective conductive network
(wherein the content of carbon nanotubes is 4%).
Embodiment 6
With reference to the preparation method of embodiment 5, prepare anti-static material PE, antistatic material that content of carbon nanotubes is 4% respectively
Material PS, anti-static material ABS, anti-static material HIPS, anti-static material PA6, anti-static material PBT.
The preparation of comparative example 1 conventional carbon nanotube conductive master batch
With traditional melting, by 200g polyethylene with 200g CNT through banbury melt blending, then through single spiral shell
Bar extruder extruding pelletization obtains the conventional carbon nanotube conductive master batch containing 50% wt carbon nanotube that particle diameter is about 3mm.
Comparative example 2
The conventional carbon nanotube conductive master batch prepared by comparative example 1, with reference to preparation method and the polymer of embodiment 5
Material molten is blended, and prepares, after double screw extruder extrusion cooling, the anti-static material that content of carbon nanotubes is 4% respectively
PP, anti-static material PE, anti-static material PS, anti-static material ABS, anti-static material HIPS, anti-static material PA6, anti-quiet
Electric material PBT.
Embodiment 7 specific insulation and material properties test
The method of testing of specific insulation: use EST121 type numeral ultra-high resistance, micro current instrument, according to GB/
T1410-2006 tests, sample diameter 82mm, and thick 2mm, each sample is surveyed five groups, taken its meansigma methods.
As can be seen from Table 1, the carbon nanotube conducting master batch that the present invention prepares has good specific insulation, than
The resistivity of the carbon nanotube conducting master batch that traditional method prepares is low 6 orders of magnitude.Data from table 2 and table 3 can
To find out, the anti-static material that the carbon nanotube conducting master batch present invention prepared prepares, described CNT
Conductive agglomerate can form the high-effective conductive network of rotation joint phase separation structure wherein so that its specific insulation ratio uses tradition side
The resistivity of the carbon nanotube conducting master batch that method prepares is low 5 ~ 6 orders of magnitude, performance is greatly improved.
Claims (10)
1. the preparation method of a carbon nanotube conducting master batch, it is characterised in that comprise the steps of:
S1. antistatic additive is dissolved and obtain solution A in organic solvent；
S2. CNT is put into organic solvent for ultrasonic dispersion, add solution A ultrasonic under mechanical agitation, concentrate and remove
Organic solvent obtains paste；
S3. paste is added heat fusing, then by melted paste through freely falling body drippage, cool down and i.e. obtain described carbon and receive
Mitron conductive agglomerate；
Wherein, the antistatic additive described in S1 is in oleamide, erucyl amide, stearmide and pentaerythritol stearate
One or more.
Preparation method the most according to claim 1, it is characterised in that the antistatic additive described in S1 and the carbon nanometer in S2
The weight consumption ratio of pipe is 1 ~ 2:1 ~ 2.
Preparation method the most according to claim 1, it is characterised in that the antistatic additive described in S1 and the carbon nanometer in S2
The weight consumption of pipe is than for 1:1.
Preparation method the most according to claim 1, it is characterised in that the organic solvent described in S1 and S2 is ethanol.
Preparation method the most according to claim 1, it is characterised in that the ultrasonic disperse described in S2, its jitter time is 1
~3h。
Preparation method the most according to claim 1, it is characterised in that containing 30 ~ 70% weight in the paste described in S2
CNT.
7. the carbon nanotube conducting master batch prepared by claim 1 ~ 6 any one preparation method.
8. the application in forming rotation joint Phase Separating Morphology high-effective conductive network of the carbon nanotube conducting master batch described in claim 7.
Application the most according to claim 8, it is characterised in that by carbon nanotube conducting master batch with melt polymer material altogether
Mixed, i.e. form rotation joint Phase Separating Morphology high-effective conductive network after cooling.
Application the most according to claim 8, it is characterised in that described macromolecular material is polypropylene material, polyethylene
Material, polystyrene material, ABS polymer, impact resistant polystyrene material, polyamide 6
Material or polybutylene terephthalate (PBT) material.
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| CN110862667B (en) * | 2019-12-05 | 2022-07-22 | 江西省纳米技术研究院 | Easy-to-disperse high-content master batch and preparation method and application thereof |
| CN110982257B (en) * | 2019-12-23 | 2022-10-11 | 江西省纳米技术研究院 | High-strength nylon 6 composite material and preparation method thereof |
| CN115612211A (en) * | 2022-09-29 | 2023-01-17 | 江阴市龙山合成材料有限公司 | Conductive polypropylene composite material and preparation method thereof |
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| US8961834B2 (en) * | 2011-03-23 | 2015-02-24 | Sabic Global Technologies B.V. | Carbon nanotube masterbatch, preparation thereof, and use in forming electrically conductive thermoplastic composition |
| CN102675893B (en) * | 2012-06-04 | 2014-07-02 | 西南交通大学 | Method for preparing polymer-based conducting composite material by melt blending |
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Date of cancellation: 20230919 Granted publication date: 20161116 Pledgee: Bank of Guangzhou Co.,Ltd. Guangzhou South China sub branch Pledgor: GUANGZHOU RUNFENG TECHNOLOGY Co.,Ltd. Registration number: Y2022980012275 |
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Denomination of invention: A carbon nanotube conductive masterbatch and its preparation method and application Effective date of registration: 20230922 Granted publication date: 20161116 Pledgee: Bank of Guangzhou Co.,Ltd. Guangzhou South China sub branch Pledgor: GUANGZHOU RUNFENG TECHNOLOGY Co.,Ltd. Registration number: Y2023980058404 |
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