CN106167611A - A kind of PC/ carbon nanotube conducting master batch - Google Patents
A kind of PC/ carbon nanotube conducting master batch Download PDFInfo
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention discloses a kind of PC/ carbon nanotube conducting master batch, including the raw material of following weight portion: PC polymeric matrix material 70~95 mass parts, Activated Carbon Nanotubes 0.01~30 mass parts;Described Activated Carbon Nanotubes is that CNT carries out high-speed stirred, is dissolved in liquid by dispersant in the carbon nanotube dust being sprayed in stirring by the way of spraying so that carbon nano tube surface activates, the Activated Carbon Nanotubes obtained simultaneously.The present invention, by preprocessed for CNT modified, add to PC material matrix as conductive filler, thus prepares PC/ carbon nanotube conducting master batch.PC/ carbon nanotube conducting master batch can be used for preparing antistatic article, and antistatic property is excellent.
Description
One, technical field
The present invention relates to a kind of PC/ carbon nanotube conducting master batch and preparation technology thereof.
Two, background technology
Merlon (PC) is a kind of noncrystal engineering material, has and particularly preferred anti-fills hit intensity, heat stability, gloss
Degree, suppression bacteria characteristic, flame-retarding characteristic and resistance tocrocking.
Owing to its electrical insulating property is excellent, therefore its goods are extremely suitable to make industry insulant, this be due to its sheet resistance or
The reason that specific insulation is higher.But in numerous applications, when because of friction, peeling off or sensing process can make PC product surface produce
Raw and accumulation electrostatic charge, these characteristics can cause serious potential danger, such as dust suction, shocks by electricity, discharges and even burn and explode.For
Avoiding this kind of danger, carrying out antistatic modified to it is industrial conventional effective ways, it is intended that reduce frosting
The generation of electrostatic charge and accumulation.
Traditional antistatic PC is material modified generally adds antistatic additive, metal dust or carbon system implant, thus makes
For going out antistatic PC goods, eliminate its surface electrostatic lotus produced during producing, using.
The advantage of antistatic additive filled-type product is that color articles is unrestricted, and wherein low molecule type antistatic additive is to product
Performance impact is little, and its surface resistivity is 1010-1013Ω.But the electrical property of low molecule antistatic additive filled-type product can be with
The passage of time and gradually lose.
Carbon system implant is mainly conductive black, graphite and carbon fiber, and the specific insulation of manufactured goods is 102-109Ω·
cm.The most carbon black filled is main flow, and why carbon black filled type conducting polymer is widely adopted, and the first is because of conductive black
Price is the cheapest;It two is because white carbon black and can have bigger choice according to different electric conductivity demands, its manufactured goods
Resistance value can be 102-109Change in broad range between Ω;Its three be electric conductivity persistently, stable;Therefore it is the most anti-
Electrostatic material.
Metal system conductive agglomerate is roughly divided into and forms the method for conductive layer at frosting and be mixed into by electroconductive stuffing
Plastics are made the method two kinds of conductive plastics.Different screen methods is respectively arranged with its pluses and minuses and the scope of application, and application in the past is relatively
Many is zinc spraying plating and electrically-conducting paint method.
But, use carbon system or metal based material the highest as consumption required during implant, this not only makes to gather
Laminate material characteristic inherently is a greater impact, and the mechanical property of composite and processing characteristics are become
Difference.
CNT relies on the one-dimensional nano structure of its uniqueness and excellent electric property, and extremely low consumption can make polymerization
The electric conductivity of thing material obtains the biggest raising, and can be effectively improved the mechanical property of composite, becomes a kind of excellent
Conductive modified agent.
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 simultaneously
Draw ratio, causes in the ordinary course of things, and CNT is easily wound around reunion bunchy.CNT game performance to be played makes it extensive
Application, the dispersion how solving CNT is critical problem.At present, the method for dispersing Nano carbon tubes have grinding with stirring,
The washing of high-energy ball milling, ultrasonic Treatment, strong acid and strong base, interpolation surfactant, growth in situ synthesis, multiple method integrated treatment
Deng.
Three, summary of the invention
The invention provides a kind of PC/ carbon nanotube conducting master batch, CNT is preprocessed modified, fills out as conduction
Fill agent to add to PC material matrix, thus prepare the PC/ carbon nanotube conducting master batch that electric conductivity is good.
The technical solution used in the present invention is:
A kind of PC/ carbon nanotube conducting master batch, described PC/ carbon nanotube conducting master batch includes the raw material of following weight portion:
PC polymeric matrix material 70~95 mass parts, Activated Carbon Nanotubes 0.01~30 mass parts
Described Activated Carbon Nanotubes prepares by the following method:
Dispersant A is dissolved in solvent, obtains dispersant solution, then dispersant solution is sprayed into by high-pressure spraying method
In the CNT of high-speed stirred, after high-speed stirred mixing, prepare Activated Carbon Nanotubes.
Described CNT, dispersant A, the mass fraction ratio of solvent are 85~95:0.1~5:5~10.
Further, described raw material can also include that auxiliary agent, the formula of described raw material are: PC polymeric matrix material 70~95
Mass parts, Activated Carbon Nanotubes 0.01~30 mass parts, auxiliary agent 0.1~20 mass parts;
Described auxiliary agent is one or more the mixing in dispersant B, coupling agent, antioxidant, lubricant, preferably institute
State auxiliary agent be one or more mixing with dispersant B, more preferably auxiliary agent in coupling agent, antioxidant, lubricant be idol
One or both in connection agent, antioxidant are with dispersant B, the mixing of lubricant.
Further, the formula of preferred feedstock is: PC polymeric matrix material, Activated Carbon Nanotubes, the mass parts of dispersant B
Number is 70~95 mass parts, 0.01~30 mass parts, 0.1~10 mass parts.
Further, the formula of preferred feedstock is: PC polymeric matrix material, Activated Carbon Nanotubes, dispersant B, coupling agent
Mass fraction be 70~95 mass parts, 0.01~30 mass parts, 0.1~10 mass parts, 0.01~5 mass parts.
Further, the formula of preferred feedstock is: PC polymeric matrix material, Activated Carbon Nanotubes, dispersant B, antioxidant
Mass fraction be 70~95 mass parts, 0.01~30 mass parts, 0.1~10 mass parts, 0.01~2 mass parts.
Further, the formula of preferred feedstock is: PC polymeric matrix material, Activated Carbon Nanotubes, dispersant B, lubricant
Mass fraction be 70~95 mass parts, 0.01~30 mass parts, 0.1~10 mass parts, 0.01~10 mass parts.
Further, the formula of preferred feedstock is: PC polymeric matrix material, Activated Carbon Nanotubes, dispersant B, coupling agent,
The mass fraction of antioxidant be 70~95 mass parts, 0.01~30 mass parts, 0.1~10 mass parts, 0.01~5 mass parts,
0.01~2 mass parts.
Further, the formula of preferred feedstock is: PC polymeric matrix material, Activated Carbon Nanotubes, dispersant B, coupling agent,
The mass fraction of lubricant be 70~95 mass parts, 0.01~30 mass parts, 0.1~10 mass parts, 0.01~5 mass parts,
0.01~10 mass parts, wherein dispersant B, coupling agent, total mass fraction of lubricant are 0.2~20 mass parts.
Further, the formula of preferred feedstock is: PC polymeric matrix material, Activated Carbon Nanotubes, dispersant B, antioxidant,
The mass fraction of lubricant be 70~95 mass parts, 0.01~30 mass parts, 0.1~10 mass parts, 0.01~2 mass parts,
0.01~10 mass parts, wherein dispersant B, antioxidant, total mass fraction of lubricant are 0.2~20 mass parts.
Further, the formula of preferred feedstock is: PC polymeric matrix material, Activated Carbon Nanotubes, dispersant B, coupling
Agent, antioxidant, the mass fraction of lubricant be 70~95 mass parts, 0.01~30 mass parts, 0.1~10 mass parts, 0.01~5
Mass parts, 0.01~2 mass parts, 0.01~10 mass parts, wherein total matter of dispersant B, coupling agent, antioxidant, lubricant
Amount number is 0.2~20 mass parts.
Further, the formula of preferred feedstock is: PC polymeric matrix material, Activated Carbon Nanotubes, dispersant B, coupling
Agent, antioxidant, the mass fraction of lubricant are 70~95 mass parts, 0.1~30 mass parts, 1~10 mass parts, 0.01~3 matter
Amount part, 0.01~2 mass parts, 0.01~3 mass parts.
Further, the formula of preferred feedstock is: PC polymeric matrix material, Activated Carbon Nanotubes, dispersant B, coupling
Agent, antioxidant, the mass fraction of lubricant are 70~95 mass parts, 1~30 mass parts, 1~10 mass parts, 0.01~3 mass
Part, 0.01~2 mass parts, 0.01~3 mass parts.
In described method, dispersant A and dispersant B are for distinguishing the dispersant used in different step, and A, B do not have
Chemical sense.
Described dispersant A and dispersant B each stand alone as dodecylbenzene sodium sulfonate, polyvinylpyrrolidone, polyethylene
Alcohol, xanthan gum, sodium lauryl sulphate, Triton X-100, sodium carboxymethyl cellulose, Dihexadecylphosphate, Ah
Draw primary glue, cetyl trimethylammonium bromide, alkyl phenol ethylene oxide condensation substance emulsifying agent, cetyl trimethyl sodium bromide,
One or more mixture in Kynoar.
Described solvent be water, N,N-dimethylformamide, N-Methyl pyrrolidone, n-butyl alcohol, chloroform, dehydrated alcohol, third
One or more mixture in ketone, petroleum ether, ethyl acetate, butyl acetate;
Described CNT, dispersant A, the mass fraction ratio of solvent are 85~95:0.1~5:5~10.
Described CNT is one or both the mixture in multi-walled carbon nano-tubes, SWCN, the most
Wall carbon nano tube.
Described PC polymeric matrix material is particle or pulverulent material, and PC polymer pulverulent material, average particle are preferably used
Footpath be 0.5 μm to the melt index of 5mm, preferably PC polymeric matrix material be 2-100g/10min, preferably 10-30g/10min,
It is beneficial to CNT dispersion in PC matrix.
Described coupling agent is one or more the mixture in titante coupling agent, silane coupling agent;Institute
Stating titante coupling agent can be isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate esters, isopropyl three (dioctyl phosphoric acid
Acyloxy) titanate esters, isopropyl two oleic acid acyloxy (dioctyl phosphoric acid acyloxy) titanate esters, monoalkoxy unsaturated fatty acid
One or more mixture in titanate esters or Di(dioctylpyrophosphato) ethylene titanate;Described silane is even
Connection agent can use KH550, one or more the mixture in KH560, KH570, KH792, DL602, DL171;
Described antioxidant is preferably 1098,168,1010,1076, DLTP, one or more in MB, 164,264
Mixture.
Described auxiliary agent is one or more the mixing in dispersant B, coupling agent, antioxidant, lubricant, preferably institute
State auxiliary agent be one or more mixing with dispersant B, more preferably auxiliary agent in coupling agent, antioxidant, lubricant be idol
One or both in connection agent, antioxidant are with dispersant B, the mixing of lubricant.
Described PC/ carbon nanotube conducting master batch can prepare by the following method: after each raw material stirring of prescription amount being mixed
Prepare through double screw extruder extruding pelletization.
The processing technique of described double screw extruder is screw speed 100~1000r/min, and extrusion temperature is 260-290
℃。
Described double screw extruder melt extrudes pelletize, and pelletize mode has multiple, optional water cooling bracing pelletizing, air-cooled tie rod
Pelletizing, die face are earnestly, cut under water.The method being well known to those skilled in the art.
High-pressure spraying method used when preparing Activated Carbon Nanotubes is that dispersant solution is passed through high-pressure spray device with spray
The form of mist sprays into the CNT of high-speed stirred, and described high-pressure spray device can use high-pressure spraying machine, pass through high-pressure hydraulic pump
Spray form is become to spray in material through high-pressure nozzle dispersant solution.Described high-pressure spraying machine still belongs to for CNT pretreatment
First.Dispersant solution is atomized by high-pressure spraying method, obtains a large amount of fine droplet after atomization, significantly increases solution and carbon nanometer
The contact area of pipe, 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
When preparing Activated Carbon Nanotubes, the rotating speed of described high-speed stirred is 300~1500 turns/min.
The time of described high-speed stirred mixing is generally 0~1 hour, preferably 5~40 minutes.
The present invention carries out high-speed stirred to CNT, to its surface pretreatment, simultaneously by dispersant, surface activity
The auxiliary agents such as agent are dissolved in liquid in the carbon nanotube dust being sprayed in stirring by the way of spraying so that CNT table
Face activation, simultaneously by the material uniform wet such as dispersant, surfactant, causes to be formed between CNT and repels, and can be same
The bulk density of Shi Tigao CNT, to obtain optimal dispersion effect and good processability.
The present invention, by preprocessed for CNT modified, adds to PC material matrix as conductive filler, thus
Prepare PC/ carbon nanotube conducting master batch.Compared with traditional antistatic modified material of PC, reaching same electric conductivity condition
Under, the Activated Carbon Nanotubes implant consumption that the present invention uses can reduce by more than 5 times, therefore can make PC characteristic inherently
Hardly suffer from impact, and the mechanical property and processing characteristics impact on composite is relatively low, also assures that antistatic simultaneously
The persistency of performance.Therefore, the PC conductive agglomerate that the present invention provides can expand the range of PC antistatic article, improves system
The service life of product.
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 solvent by dispersant, obtains dispersant solution, is then led to by dispersant solution
Cross high pressure spray process and spray into the CNT (diameter 1~30nm, length 1~100 μm, bulk density 0.02g/mL) of high-speed stirred
In, technological parameter is as shown in table 1, after high-speed stirred mixing, prepares Activated Carbon Nanotubes;
Table 1
The performance test results such as table 2 below of the Activated Carbon Nanotubes prepared
Table 2
Dispersibility experiment detection by the following method: the Activated Carbon Nanotubes 10mg that embodiment 1~16 prepares is separately added into
10mL prepares in the solvent (seeing table 1) used by this Activated Carbon Nanotubes, 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 Nanotubes prepared by embodiment 1~16 and PC polymer pulverulent material (mean diameter 100 μm~2mm)
Stirring and evenly mixing, consumption is shown in Table 3, and then the auxiliary agent with table 4 mixes, and melt extrudes through double screw extruder, stretches, cooling and dicing system
Obtain PC/ carbon nanotube conducting master batch;The processing technique of double screw extruder is screw speed 200r/min, and extrusion temperature is 280
℃。
The content of carbon nanotubes of the PC/ carbon nanotube conducting master batch prepared is as shown in table 5.
The content of carbon nanotubes of conductive agglomerate of embodiment 17,21,24 preparation more than 10%, the conduction of these high-loads
Master batch is conducive to production and sales.When subsequent production is applied can by the conductive agglomerate of high content of carbon nanotubes again with PC matrix material
Material and the mixing of other auxiliary agent, prepare antistatic article.
Concrete, PC/ carbon nanotube conducting master batch prepared by embodiment 17~32 is mixed with PC base material according to the formula of table 5
Close, and add the auxiliary agents such as flow ability modifying agent, thermal oxidation stabilizer, antifriction liniment, prepare antistatic film through biaxial tension, according to
The sheet resistance of " GB/T1410-2006 solid insulating material specific insulation and surface resistivity test method " testing film
Rate, result is as shown in table 5.
Table 3
Table 4
Table 5
In table 5, thermal oxidation stabilizer is 1098, and flow ability modifying agent is erucyl amide, and antifriction liniment is nano-calcium carbonate.
Embodiment data show, the surface resistivity of antistatic article prepared by conductive agglomerate prepared by the present invention is preferable,
In the case of content of carbon nanotubes 2~4wt.%, surface resistivity is 103~106About Ω, antistatic property is good.
Claims (10)
1. a PC/ carbon nanotube conducting master batch, it is characterised in that described PC/ carbon nanotube conducting master batch includes following weight portion
Raw material:
PC polymeric matrix material 70~95 mass parts, Activated Carbon Nanotubes 0.01~30 mass parts
Described Activated Carbon Nanotubes prepares by the following method:
Dispersant A is dissolved in solvent, obtains dispersant solution, then dispersant solution is sprayed at a high speed by high-pressure spraying method
In the CNT of stirring, after high-speed stirred mixing, prepare Activated Carbon Nanotubes.
2. PC/ carbon nanotube conducting master batch as claimed in claim 1, it is characterised in that described raw material also includes auxiliary agent, described
The formula of raw material is: PC polymeric matrix material 70~95 mass parts, Activated Carbon Nanotubes 0.01~30 mass parts, auxiliary agent 0.1
~20 mass parts;
Described auxiliary agent is one or more the mixing in dispersant B, coupling agent, antioxidant, lubricant.
3. PC/ carbon nanotube conducting master batch as claimed in claim 1, it is characterised in that described CNT, dispersant A, molten
The mass fraction ratio of agent is 85~95:0.1~5:5~10.
4. PC/ carbon nanotube conducting master batch as claimed in claim 2, it is characterised in that described dispersant A and dispersant B are each
Stand alone as dodecylbenzene sodium sulfonate, polyvinylpyrrolidone, polyvinyl alcohol, xanthan gum, sodium lauryl sulphate, Polyethylene Glycol
Octyl phenyl ether, sodium carboxymethyl cellulose, Dihexadecylphosphate, arabic gum, cetyl trimethylammonium bromide, alkyl phenol
One or more mixing in ethylene oxide condensate emulsifying agent, cetyl trimethyl sodium bromide, Kynoar
Thing.
5. PC/ carbon nanotube conducting master batch as claimed in claim 1, it is characterised in that described solvent is water, N, N-dimethyl
In Methanamide, N-Methyl pyrrolidone, n-butyl alcohol, chloroform, dehydrated alcohol, acetone, petroleum ether, ethyl acetate, butyl acetate
One or more mixture.
6. PC/ carbon nanotube conducting master batch as claimed in claim 2, it is characterised in that the formula of described raw material be following it
One:
Formula (one) PC polymeric matrix material, Activated Carbon Nanotubes, the mass fraction of dispersant B be 70~95 mass parts,
0.01~30 mass parts, 0.1~10 mass parts;
Formula (two) PC polymeric matrix material, Activated Carbon Nanotubes, dispersant B, the mass fraction of coupling agent are 70~95 matter
Amount part, 0.01~30 mass parts, 0.1~10 mass parts, 0.01~5 mass parts;
Formula (three) PC polymeric matrix material, Activated Carbon Nanotubes, dispersant B, the mass fraction of antioxidant are 70~95 matter
Amount part, 0.01~30 mass parts, 0.1~10 mass parts, 0.01~2 mass parts;
Formula (four) PC polymeric matrix material, Activated Carbon Nanotubes, dispersant B, the mass fraction of lubricant are 70~95 matter
Amount part, 0.01~30 mass parts, 0.1~10 mass parts, 0.01~10 mass parts;
Formula (five) PC polymeric matrix material, Activated Carbon Nanotubes, dispersant B, coupling agent, the mass fraction of antioxidant are 70
~95 mass parts, 0.01~30 mass parts, 0.1~10 mass parts, 0.01~5 mass parts, 0.01~2 mass parts;
Formula (six) PC polymeric matrix material, Activated Carbon Nanotubes, dispersant B, coupling agent, the mass fraction of lubricant are 70
~95 mass parts, 0.01~30 mass parts, 0.1~10 mass parts, 0.01~5 mass parts, 0.01~10 mass parts, wherein disperse
Agent B, coupling agent, total mass fraction of lubricant are 0.2~20 mass parts;
Formula (seven) PC polymeric matrix material, Activated Carbon Nanotubes, dispersant B, antioxidant, the mass fraction of lubricant are 70
~95 mass parts, 0.01~30 mass parts, 0.1~10 mass parts, 0.01~2 mass parts, 0.01~10 mass parts, wherein disperse
Agent B, antioxidant, total mass fraction of lubricant are 0.2~20 mass parts;
Formula (eight) PC polymeric matrix material, Activated Carbon Nanotubes, dispersant B, coupling agent, antioxidant, the quality of lubricant
Number be 70~95 mass parts, 0.01~30 mass parts, 0.1~10 mass parts, 0.01~5 mass parts, 0.01~2 mass parts,
0.01~10 mass parts, wherein dispersant B, coupling agent, antioxidant, total mass fraction of lubricant are 0.2~20 mass parts.
7. PC/ carbon nanotube conducting master batch as claimed in claim 2, it is characterised in that described coupling agent is titanate ester coupling
One or more mixture in agent, silane coupling agent.
8. PC/ carbon nanotube conducting master batch as claimed in claim 2, it is characterised in that described antioxidant is 1098,168,
1010,1076, one or more the mixture in DLTP, MB, 164,264.
9. PC/ carbon nanotube conducting master batch as claimed in claim 2, it is characterised in that described lubricant be PE wax, montanin wax,
One or more mixing in silicone powder, stearic acid, oleic acid, calcium stearate, ethylene bis stearic acid amide, erucyl amide
Thing..
10. the application in preparing antistatic article of the PC/ carbon nanotube conducting master batch as described in one of claim 1~9.
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Cited By (2)
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CN112143200A (en) * | 2020-09-25 | 2020-12-29 | 上海雅承塑胶制品有限公司 | Polycarbonate plastic and processing technology thereof |
CN114316558A (en) * | 2021-12-20 | 2022-04-12 | 杨劲光 | Carbon nano tube concentrated composition and preparation method and application thereof |
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