CN108129794A - Styrene polymer base conductive agglomerate based on carbon nanotube and graphene compound system and preparation method thereof - Google Patents
Styrene polymer base conductive agglomerate based on carbon nanotube and graphene compound system and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of styrene polymer base conductive agglomerates based on carbon nanotube and graphene compound system and preparation method thereof；Carbon nanotube and graphene are dispersed in respectively in volatile atent solvent first, sonicated device processing 1h respectively, then the dispersion liquid handled well is proportionally stirred with raw material in homogenizer, then after being mixed at room temperature according to a certain percentage with compatilizer, melting extrusion is carried out by twin-screw, is prepared into conductive agglomerate.Conductivity of composite material prepared by the present invention can be excellent, is easy to add, and the fields such as can be widely applied to be molded, squeeze out and be modified.
Description
Technical field
The invention belongs to the field of polymers, and in particular to a kind of benzene second of the compound system based on carbon nanotube and graphene
Alkene polymer base conductive agglomerate and preparation method thereof.
Background technology
ABS resins are a kind of resins haveing excellent performance, have excellent impact resistance, heat resistance, dimensional stability and
Excellent dyeability is widely used in fields such as electric, household electrical appliances, automobiles, suitable for various processing
Technique.But plastics are typically all what is insulated, with the development of society and the progress of science and technology, the application range of plastics is increasingly
Extensively, the requirement of people is also higher and higher, and the electrostatic charge that insulating properties can cause surface of plastic products to accumulate can not be released, into
And electrostatic pressure is formed, the dirts such as dust are easily adsorbed, after electrostatic potential reaches a certain level, static discharge can be generated（ESD）With
Shock phenomenon.Especially in electronics industry, various precision instruments and precision electronic element can be damaged even due to electrostatic breakdown
It scraps, in addition, in the industrial and mining enterprises of some contact inflammable and explosive substances, if static discharge cannot be protected effectively, can produce
Raw more serious consequence, may be with regard to the life of entail dangers to field worker once there is accident, and causes great economic loss.Separately
On the one hand, with the development of modern electronics industry, Electromagnetic Interference（EMI）And radio frequency interference（RFI）Become new " environment dirt
Dye " problem, the micro-current between precise electronic component are highly susceptible to the influence of such complex electromagnetic environment, generate malfunction
The failures such as work, image obstacle.
Then how people improves the antistatic property of plastics if beginning one's study.There are mainly two types of methods at present, and one kind is poly-
The conjunction stage introduces conjugated structure, forms conductive path, and improves electrostatic dissipation；It is another then be it is compound with conductive auxiliary agent, i.e.,
Prepare compound anti-static plastic.Conductive auxiliary agent has inorganic and organic structure.Organic conductive agent and plastics it is excellent in compatibility,
But after some shortcomings, such as 1000 h exposed in air of the polyacetylene of I2 doping, antistatic rate can decline one
A order of magnitude, and after the polyphenylacetylene of I2 doping exposes 250 h in air, antistatic property is lost substantially.Inorganic conductive helps
Agent generally by dispersion obtain in the plastic conduction, anti-static composite material, at present widely be used in communication eventually
In the equipment such as end, computer, automobile telephone, cashing machine；But there are a fatal defects, i.e. bad dispersibility, particularly nano junction
The carbon nanotube and graphene of structure.The novel nano-material most strong as presently found electrical and thermal conductivity performance, mixes in plastics
Enter a small amount of carbon nanotube and graphene, theoretically plastics can be made to have good antistatic property；But carbon material is due to surface
Between inertia and lamella there is very strong Van der Waals force, therefore disperse extremely difficult.How carbon is effectively disperseed in the composite
Material becomes a hot spot of antistatic or even conductive material research, and there is no effective solutions to this for the prior art.
Invention content
The purpose of the present invention is exactly the above problem in order to be directed in anti-static composite material in the prior art, it is difficult to be met
The demand of requirements at the higher level occasion and the demand of stability, and propose a kind of simply and effectively based on carbon nanotube and graphene compounding
Styrene polymer base conductive agglomerate of system and preparation method thereof, carbon nanotube and graphene are formed runs through structure through/half,
Obtained conduction, anti-static composite material have many advantages, such as that performance is stable, processing technology is simple controllable, safe.
The purpose of the present invention is what is be achieved through the following technical solutions：
A kind of styrene polymer base conductive agglomerate based on carbon nanotube and graphene compound system, percentage,
The raw material being made up of is prepared：
Styrene polymer 86~94%；
Carbon nanotube 0.2~1%；
Graphene 1~5%；
Compatilizer 0.5~2%；
Dispersant 4~8%.
The present invention also provides a kind of above-mentioned styrene polymer bases based on carbon nanotube and graphene compound system to lead
The preparation method of goddess of lightning's grain, includes the following steps：
（1）Carbon nanotube and graphene are scattered in respectively in inertia easy volatile solvent, 10~30min of stirring at normal temperature obtains carbon
Nanotube suspension, graphene suspension；
（2）By the carbon nano tube suspension, graphene suspension, the ultrasonic processing apparatus through 400W~800W handles 1h respectively,
Obtain carbon nano tube dispersion liquid, graphene dispersing solution；
（3）The carbon nano tube dispersion liquid, graphene dispersing solution and dispersant are stirred, obtain disperse materials；The stirring
Rotating speed be 1300~2000 revs/min；
（4）After the disperse materials are mixed with compatilizer, by twin-screw melting extrusion, obtain based on carbon nanotube and graphene
The styrene polymer base conductive agglomerate of compound system；Processing temperature during the twin-screw melting extrusion is 190~230 DEG C,
Rotating speed is 100~400rpm.
In above-mentioned technical proposal, the compatilizer is aromatic ethenyl compound, acrylonitrile and Glycidyl methacrylate
The terpolymer that glyceride (GMA) copolymerization obtains.
Preferably, the compatilizer is styrene-acrylonitrile-glycidyl methacrylate terpolymer, i.e. ST-
AN-GMA terpolymers；It is further preferred that the styrene-acrylonitrile-glycidyl methacrylate ternary polymerization
In object, styrene, acrylonitrile, glycidyl methacrylate mass percent be respectively 75%, 25%, 5%；The benzene second
Alkene-acrylonitrile-methacylate ethylene oxidic ester terpolymer number-average molecular weight is 75000~82000.
In above-mentioned technical proposal, the dispersant for aromatic ethenyl compound, acrylonitrile compolymer obtain it is random altogether
Polymers.
Preferably, the dispersant is styrene-acrylonitrile copolymer, i.e. ST-AN copolymers；It is further preferred that institute
State in styrene-acrylonitrile copolymer, styrene, acrylonitrile mass percent be respectively 75%, 25%；The styrene-the third
The number-average molecular weight of alkene lonitrile copolymer is 18000~21000.
Preferably, the terpolymer is 5~15g/10min in the melt index (MI) of 235 DEG C/2.16kg；It is described random
Copolymer is 40~100 g/10min in the melt index (MI) of 190 DEG C/5kg.
In above-mentioned technical proposal, the average diameter of the carbon nanotube<20nm, average length are 1~20 μm, average parietal layer
Number<15.
In above-mentioned technical proposal, the mean wall number of plies of the graphene<15.
In above-mentioned technical proposal, the styrene polymer is ABS and/or ASA.
In above-mentioned technical proposal, the draw ratio of the double screw extruder is more than 40, preferably double spiral shells of more than 52 draw ratio
Bar extruder.
In styrene polymer base conductive agglomerate disclosed by the invention based on carbon nanotube and graphene compound system, carbon
The P of carbon atom electronically forms large-scale delocalized pi-bond on nanotube, and conjugation is notable, and carbon nanotube has good anti-quiet
Electrical property, while antistatic property is related with the helical angle of caliber and tube wall, the present invention, which limits parameter, has good antistatic property
Energy；Graphene is a kind of cellular flat film formed by carbon atom with sp2 hybrid forms, and wherein single-layer graphene only has one
The quasi- two-dimensional material of a atomic layer level thickness has very good intensity, flexible, conductive, heat conduction, optical characteristics, so as to prepare
Obtained conductivity of composite material can be excellent, easily manufactured, is easy to add, can be widely applied to be molded, squeeze out and be modified
Field, be all widely used space in fields such as physics, materialogy, electronic information, computer, aerospaces.
The prior art is compared, and the present invention has following advantageous effect：
1. the preparation of the styrene polymer base conductive agglomerate disclosed by the invention based on carbon nanotube and graphene compound system
It is by Vltrasonic device, carbon nanotube and graphene progress is effectively pre-dispersed in method, reduce the model moral between nanostructured
Hua Li, and surface is activated, so as to ensure that carbon nanomaterial has good dispersibility during melting extrusion.
2. the styrene polymer base conductive agglomerate disclosed by the invention based on carbon nanotube and graphene compound system
In, the random copolymer reactivity with compatibilized effect is high, has thermodynamic compatibility, functional group's energy with styrene polymer
General polymer rank with molecular weight, thus during subsequent technique with polymer co-extrusion good thermal stability.
3. the styrene polymer base conductive agglomerate disclosed by the invention based on carbon nanotube and graphene compound system
Preparation method is easy to use, and there is no secondary pollution, the preparation for highly effective antistatic agglomerate provides a kind of applicable method.
Specific embodiment
With reference to specific embodiment, the present invention is described in detail.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill to this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection domain.
The raw material of the master batch of embodiment and comparative example is formed referring to table 1.
Wherein, the average diameter of the carbon nanotube<20nm, 1-20 μm of average length, the mean wall number of plies<15.
Wherein, the graphene mean wall number of plies<15.
Wherein, in the ST-AN-GMA terpolymers, ST contents are 70 wt%, and AN contents are 25 wt%, GMA
Content be 5 wt%, number average molecular weight 80000；In the ST-AN copolymers, ST contents are 75wt%, and AN contents are 25
Wt%, number-average molecular weight molecular weight 20000.The mass percent of copolymer each unit is calculated according to CPC.The ST-AN-
GMA terpolymers are 5~15g/10min in the melt index (MI) of 235 DEG C/2.16kg；The ST-AN copolymers 190 DEG C/
The melt index (MI) of 5kg is 40~100 g/10min.
Preparation method includes the following steps：
（1）Carbon nanotube and graphene are scattered in respectively in inertia easy volatile solvent butanone, 10~30min of stirring at normal temperature is obtained
To carbon nano tube suspension, graphene suspension；
（2）Carbon nano tube dispersion liquid, graphite are obtained by the carbon nano tube suspension, graphene suspension are sonicated respectively
Alkene dispersion liquid；The parameter of supersound process is referring to table 2；
（3）The carbon nano tube dispersion liquid, graphene dispersing solution and dispersant are stirred, obtain disperse materials；The stirring
Rotating speed for parameter referring to table 2；
（4）After the disperse materials are mixed with compatilizer, by twin-screw melting extrusion, obtain based on carbon nanotube and graphene
The styrene polymer base conductive agglomerate of compound system；Processing temperature during the twin-screw melting extrusion is 190~230 DEG C,
Rotating speed is referring to table 2, the draw ratio 55 of double screw extruder.
1 conductive agglomerate formula of table, mass ratio
2 processing parameter of table
Technique effect
The master batch sample that above-described embodiment and comparative example manufacture and ABS are mixed with conductive material, ensure that end article is conductive
Carbon material content 1%, afterwards with compression molding instrument tabletting, 220 DEG C of pelletizing temperature, 30 seconds, then the test of progress sheet resistance, was tied
Fruit is as shown in table 3, and according to extrusion observation be granulated stability, be divided into, preferably, generally, it is poor, according to multi-point sampler piece
The electric conductivity observation stability of material.
3 performance comparison of table
As shown in Table 3, the present invention uses the combination of carbon material and compatilizer, and technique according to the invention, can just obtain
It is excellent to obtain electric conductivity, processes stable styrene polymer conductive agglomerate.The too high levels of compatilizer too low can cause
Electrical property reduces, and the too high levels of carbon material, although electric conductivity is preferable, processing stability is poor, and the too low then conductive effect of content
Fruit is poor；Meanwhile the sheet material that 6 master batch of Example is prepared, quadrangle and centre respectively take one piece of sample, test shows resistance,
Fluctuation is in the same order of magnitude；The sheet material that 2 master batch of comparative example is taken to be prepared, quadrangle and centre respectively take one piece of sample, test
Show resistance, fluctuation reaches the 3-4 order of magnitude.
In conclusion one kind provided by the present invention is simple and effective, the compound system based on carbon nanotube and graphene
Conductive agglomerate of styrene polymer base material and preparation method thereof can obtain the conductive agglomerate with superior electrical conductivity energy, add
It is apt fixed, using simple.
There are many concrete application approach of the present invention, and the above is only the preferred embodiment of the present invention.More than it should be pointed out that
Embodiment is merely to illustrate the present invention, and the protection domain being not intended to restrict the invention.For the common skill of the art
For art personnel, without departing from the principle of the present invention, several improvement can also be made, these improvement also should be regarded as this hair
Bright protection domain.
Claims (10)
1. a kind of styrene polymer base conductive agglomerate based on carbon nanotube and graphene compound system, weight percent
Meter, the raw material being made up of are prepared：
Styrene polymer 86~94%；
Carbon nanotube 0.2~1%；
Graphene 1~5%；
Compatilizer 0.5~2%；
Dispersant 4~8%；
The compatilizer is the ternary that aromatic ethenyl compound, acrylonitrile and glycidyl methacrylate are copolymerized
Copolymer；The number-average molecular weight of the terpolymer is 50000~90000；In the terpolymer, methacrylic acid contracting
The mass percent of water glyceride is 5wt%~20wt%；
The random copolymer that the dispersant is aromatic ethenyl compound, acrylonitrile compolymer obtains；The random copolymer
Number-average molecular weight be 10000~30000.
2. the styrene polymer base conductive agglomerate based on carbon nanotube and graphene compound system as described in claim 1,
It is characterized in that, the average diameter of the carbon nanotube<20nm, average length are 1~20 μm, the mean wall number of plies<15.
3. the styrene polymer base conductive agglomerate based on carbon nanotube and graphene compound system as described in claim 1,
It is characterized in that, the mean wall number of plies of the graphene<15.
4. the styrene polymer base conductive agglomerate based on carbon nanotube and graphene compound system as described in claim 1,
It is characterized in that, the styrene polymer is ABS and/or ASA.
5. the styrene polymer base conductive agglomerate based on carbon nanotube and graphene compound system as described in claim 1,
It is characterized in that, the terpolymer is 5~15g/10min in the melt index (MI) of 235 DEG C/2.16kg；The random copolymer
It is 40~100 g/10min in the melt index (MI) of 190 DEG C/5kg.
6. the styrene polymer base conductive agglomerate based on carbon nanotube and graphene compound system as described in claim 1,
It is characterized in that, the compatilizer is styrene-acrylonitrile-glycidyl methacrylate terpolymer；The styrene-
In acrylonitrile-methacylate ethylene oxidic ester terpolymer, styrene, acrylonitrile, glycidyl methacrylate
Mass percent is respectively 75%, 25%, 5%；The styrene-acrylonitrile-glycidyl methacrylate terpolymer number
Average molecular weight is 75000~82000.
7. the styrene polymer base conductive agglomerate based on carbon nanotube and graphene compound system as described in claim 1,
It is characterized in that, the dispersant is styrene-acrylonitrile copolymer；In the styrene-acrylonitrile copolymer, styrene, third
The mass percent of alkene nitrile is respectively 75%, 25%；The number-average molecular weight of the styrene-acrylonitrile copolymer for 18000~
21000。
8. the preparation of the styrene polymer base conductive agglomerate based on carbon nanotube and graphene compound system described in claim 1
Method, which is characterized in that include the following steps：
（1）Carbon nanotube and graphene are scattered in respectively in inertia easy volatile solvent, 10~30min of stirring at normal temperature obtains carbon
Nanotube suspension, graphene suspension；
（2）By the carbon nano tube suspension, graphene suspension, the ultrasonic processing apparatus through 400W~800W handles 1h respectively,
Obtain carbon nano tube dispersion liquid, graphene dispersing solution；
（3）The carbon nano tube dispersion liquid, graphene dispersing solution and dispersant are stirred, obtain disperse materials；The stirring
Rotating speed be 1300~2000 revs/min；
（4）After the disperse materials are mixed with compatilizer, by twin-screw melting extrusion, obtain based on carbon nanotube and graphene
The styrene polymer base conductive agglomerate of compound system；Processing temperature during the twin-screw melting extrusion is 190~230 DEG C,
Rotating speed is 100~400rpm.
9. styrene polymer base conductive agglomerate according to claim 8 based on carbon nanotube and graphene compound system
Preparation method, which is characterized in that the draw ratio of the double screw extruder is more than 40.
10. the styrene polymer base conductive agglomerate based on carbon nanotube and graphene compound system described in claim 1 is being made
Application in standby conductive material.
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