CN108129794B - Styrene polymer-based conductive master batch based on carbon nanotube and graphene compound system and preparation method thereof - Google Patents
Styrene polymer-based conductive master batch based on carbon nanotube and graphene compound system and preparation method thereof Download PDFInfo
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Abstract
The invention provides a styrene polymer-based conductive master batch based on a carbon nano tube and graphene compound system and a preparation method thereof; firstly, respectively and uniformly dispersing carbon nano tubes and graphene in a volatile inert solvent, respectively treating for 1h by an ultrasonic treatment device, then stirring the treated dispersion liquid and the raw materials in a high-speed stirrer according to a certain proportion, mixing the dispersion liquid and a compatilizer at room temperature according to a certain proportion, and then carrying out melt extrusion through a double screw to prepare the conductive master batch. The composite material prepared by the invention has excellent conductivity, is easy to add, and can be widely applied to the fields of injection molding, extrusion, modification and the like.
Description
Technical Field
The invention belongs to the field of macromolecules, and particularly relates to a styrene polymer-based conductive master batch based on a compounding system of a carbon nano tube and graphene and a preparation method thereof.
Background
The ABS resin is a resin with excellent performance, has excellent impact resistance, heat resistance, dimensional stability and dyeing property, is widely applied to the fields of electronics, electrics, household appliances, automobiles and the like, and is suitable for various processing technologies. However, plastics are generally insulated, and with the development of society and the progress of science and technology, the application range of plastics is wider and wider, and the requirements of people are higher and higher, and the insulation can cause that static charges accumulated on the surface of a plastic product can not be released, so that static voltage is formed, dirt such as dust and the like can be easily adsorbed, and after the static voltage reaches a certain degree, electrostatic discharge (ESD) and electric shock phenomena can be generated. In particular, in the electronic industry, various precision instruments and precision electronic components are damaged or even scrapped due to electrostatic breakdown, and in some industrial and mining enterprises contacting flammable and explosive substances, electrostatic discharge can have more serious consequences if the electrostatic discharge cannot be effectively protected, and the life of field workers can be endangered once an accident occurs, and serious economic loss is caused. On the other hand, with the development of modern electronic industry, electromagnetic interference (EMI) and Radio Frequency Interference (RFI) become new "environmental pollution" problems, and micro-current between precision electronic components is easily affected by such a complicated electromagnetic environment, resulting in malfunctions, image obstruction, and the like.
Therefore, studies have been made on how to improve the antistatic property of plastics. At present, two methods are mainly used, one is a polymerization stage, a conjugated structure is introduced to form a conductive path, so that the static dissipation is improved; and the other is compounded with conductive auxiliary agent to prepare the composite antistatic plastic. The conductive assistant has inorganic and organic structures. The organic conductive agent has excellent compatibility with plastics, but has some disadvantages, such as that the antistatic rate of iodine-doped polyacetylene is reduced by an order of magnitude after being exposed to air for 1000 hours, and the iodine-doped polyphenylacetylene is substantially lost antistatic property after being exposed to air for 250 hours. The inorganic conductive additive is generally a conductive and antistatic composite material obtained by dispersing in plastic, and is widely used on communication terminals, computers, automobile telephones, cash registers and other equipment at present; but has a fatal disadvantage of poor dispersion, particularly, nano-structured carbon nanotubes and graphene. As a novel nano material with the strongest electric conduction and heat conduction performance discovered at present, a small amount of carbon nano tubes and graphene are doped into the plastic, so that the plastic theoretically has good antistatic property; however, carbon materials are extremely difficult to disperse due to surface inertness and strong van der waals forces between sheets. How to effectively disperse carbon materials in composite materials becomes a hot spot for researching antistatic and even conductive materials, and the prior art has no effective solution for the problem.
Disclosure of Invention
The invention aims to solve the problems in the antistatic composite material in the prior art and solve the problem that the requirements of occasions with higher requirements and the requirements of stability are difficult to meet, and provides a simple and effective styrene polymer-based conductive master batch based on a carbon nano tube and graphene compounding system and a preparation method thereof.
The purpose of the invention is realized by the following technical scheme:
a styrene polymer-based conductive master batch based on a carbon nanotube and graphene compound system is prepared from the following raw materials in percentage by weight:
86-94% of styrene polymer;
0.2-1% of carbon nano tube;
1-5% of graphene;
0.5-2% of a compatilizer;
4-8% of a dispersing agent.
The invention also provides a preparation method of the styrene polymer-based conductive master batch based on the carbon nanotube and graphene compound system, which comprises the following steps:
(1) respectively dispersing carbon nanotubes and graphene in an inert volatile solvent, and stirring at normal temperature for 10-30 min to obtain a carbon nanotube suspension and a graphene suspension;
(2) respectively treating the carbon nano tube suspension and the graphene suspension for 1 hour by using a 400-800W ultrasonic treatment device to obtain a carbon nano tube dispersion liquid and a graphene dispersion liquid;
(3) mixing and stirring the carbon nanotube dispersion liquid, the graphene dispersion liquid and a dispersing agent to obtain a dispersing material; the stirring speed is 1300-2000 rpm;
(4) mixing the dispersing material with a compatilizer, and then carrying out melt extrusion through a double screw to obtain styrene polymer-based conductive master batch based on a carbon nano tube and graphene compound system; the processing temperature of the twin-screw melt extrusion is 190-230 ℃, and the rotating speed is 100-400 rpm.
In the technical scheme, the compatilizer is a terpolymer obtained by copolymerizing an aromatic vinyl compound, acrylonitrile and Glycidyl Methacrylate (GMA).
Preferably, the compatibilizer is a styrene-acrylonitrile-glycidyl methacrylate terpolymer, i.e., AN ST-AN-GMA terpolymer; more preferably, in the styrene-acrylonitrile-glycidyl methacrylate terpolymer, the mass percentages of styrene, acrylonitrile and glycidyl methacrylate are respectively 75%, 25% and 5%; the number average molecular weight of the styrene-acrylonitrile-glycidyl methacrylate terpolymer is 75000-82000.
In the technical scheme, the dispersing agent is a random copolymer obtained by copolymerizing aromatic vinyl compounds and acrylonitrile.
Preferably, the dispersant is a styrene-acrylonitrile copolymer, i.e., AN ST-AN copolymer; more preferably, in the styrene-acrylonitrile copolymer, the mass percentages of styrene and acrylonitrile are 75% and 25%, respectively; the number average molecular weight of the styrene-acrylonitrile copolymer is 18000-21000.
Preferably, the melt index of the terpolymer at 235 ℃/2.16kg is 5-15 g/10 min; the melt index of the random copolymer at 190 ℃/5kg is 40-100 g/10 min.
In the technical scheme, the average diameter of the carbon nano tube is less than 20nm, the average length of the carbon nano tube is 1-20 mu m, and the average number of wall layers is less than 15.
In the above technical solution, the average number of wall layers of the graphene is less than 15.
In the above technical scheme, the styrene polymer is ABS and/or ASA.
In the technical scheme, the length-diameter ratio of the double-screw extruder is more than 40, and preferably the length-diameter ratio of the double-screw extruder is more than 52.
In the styrene polymer-based conductive master batch based on the carbon nano tube and graphene compound system, P electrons of carbon atoms on the carbon nano tube form a large-range delocalized pi bond, the conjugation effect is obvious, the carbon nano tube has good antistatic performance, and meanwhile, the antistatic performance is related to the tube diameter and the helix angle of the tube wall, and the limited parameters of the invention have good antistatic performance; graphene is a honeycomb-shaped planar thin film formed by carbon atoms in an sp2 hybridization mode, wherein a single-layer graphene is a quasi-two-dimensional material with the thickness of only one atomic layer, and the quasi-two-dimensional thin film has very good strength, flexibility, electric conduction, heat conduction and optical characteristics, so that the prepared composite material has excellent electric conductivity, is convenient to manufacture and easy to add, can be widely applied to the fields of injection molding, extrusion, modification and the like, and has wide application space in the fields of physics, materials science, electronic information, computers, aerospace and the like.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the preparation method of the styrene polymer-based conductive master batch based on the carbon nano tube and graphene compound system, the carbon nano tube and graphene are effectively pre-dispersed through an ultrasonic device, so that van der Waals force among nano structures is weakened, and the surface is activated, so that the carbon nano material is ensured to have good dispersibility in the melting and extruding process.
2. In the styrene polymer-based conductive master batch based on the carbon nano tube and graphene compound system, the random copolymer with the compatibilization effect has high reaction activity and thermodynamic compatibility with styrene polymers, and the functional group and the molecular weight are in the level of common polymers, so that the styrene polymer-based conductive master batch has good thermal stability in co-extrusion with the polymers in the subsequent process.
3. The preparation method of the styrene polymer-based conductive master batch based on the carbon nano tube and graphene compounding system, disclosed by the invention, is convenient to use, does not have secondary pollution, and provides an applicable method for preparing the efficient antistatic master batch.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
The raw material composition of the master batches of examples and comparative examples is shown in table 1.
Wherein the carbon nanotubes have an average diameter of less than 20nm, an average length of 1-20 μm, and an average number of wall layers of less than 15.
Wherein the average number of graphene wall layers is < 15.
Wherein in the ST-AN-GMA terpolymer, the ST content is 70 wt%, the AN content is 25 wt%, the GMA content is 5 wt%, and the data molecular weight is 80000; in the ST-AN copolymer, the ST content is 75 wt%, the AN content is 25 wt%, and the number average molecular weight is 20000. The mass percentages of the individual units of the copolymers are calculated on the basis of CPC. The melt index of the ST-AN-GMA terpolymer at 235 ℃/2.16kg is 5-15 g/10 min; the melt index of the ST-AN copolymer at 190 ℃/5kg is 40-100 g/10 min.
The preparation method comprises the following steps:
(1) respectively dispersing carbon nanotubes and graphene in an inert volatile solvent butanone, and stirring at normal temperature for 10-30 min to obtain a carbon nanotube suspension and a graphene suspension;
(2) respectively carrying out ultrasonic treatment on the carbon nanotube suspension and the graphene suspension to obtain a carbon nanotube dispersion liquid and a graphene dispersion liquid; see table 2 for parameters of sonication;
(3) mixing and stirring the carbon nanotube dispersion liquid, the graphene dispersion liquid and a dispersing agent to obtain a dispersing material; the rotating speed of the stirring is taken as a parameter and is referred to a table 2;
(4) mixing the dispersing material with a compatilizer, and then carrying out melt extrusion through a double screw to obtain styrene polymer-based conductive master batch based on a carbon nano tube and graphene compound system; the processing temperature of the twin-screw extruder during melt extrusion is 190-230 ℃, the rotating speed is shown in table 2, and the length-diameter ratio of the twin-screw extruder is 55.
TABLE 1 formulation of conductive masterbatch, mass ratio
TABLE 2 treatment parameters
Technical effects
The master batch samples manufactured in the above examples and comparative examples were mixed with ABS to prepare a conductive material, the content of the conductive carbon material in the final product was guaranteed to be 1%, then the final product was pressed into a sheet using a flat vulcanizing machine, the pressing temperature was 220 ℃, 30 seconds, and then the surface resistance test was performed, the results are shown in table 3, and the stability of the granulation was observed according to the extrusion process, which was classified into good, normal, and poor, and the stability of the properties was observed according to the conductivity of the sheet tested at multiple points.
TABLE 3 comparison of Properties
As can be seen from the results in table 3, the conductive masterbatch of styrene polymer with excellent conductivity and stable processing can be obtained by combining the carbon material and the compatibilizer according to the present invention. The electrical property is reduced due to the excessively high or excessively low content of the compatilizer, the electrical property is reduced due to the excessively high content of the carbon material, the processing stability is poor although the electrical conductivity is good, and the electrical conductivity effect is poor due to the excessively low content of the carbon material; meanwhile, a sheet prepared from the master batch in the embodiment 6 is taken, a sample is taken from each of four corners and the middle of the sheet, and tests show that the resistance and the fluctuation are in the same order of magnitude; and (3) taking the sheet prepared from the master batch in the comparative example 2, and taking a sample at each of four corners and the middle of the sheet, wherein the test shows that the resistance and the fluctuation reach 3-4 orders of magnitude.
In conclusion, the simple and effective conductive master batch based on the styrene polymer base material of the compounding system of the carbon nano tube and the graphene and the preparation method thereof can obtain the conductive master batch with excellent conductive performance, and are stable to process and simple to use.
The invention has many applications, and the above description is only a preferred embodiment of the invention. It should be noted that the above examples are only for illustrating the present invention, and are not intended to limit the scope of the present invention. It will be apparent to those skilled in the art that various modifications can be made without departing from the principles of the invention and these modifications are to be considered within the scope of the invention.
Claims (5)
1. The styrene polymer-based conductive master batch based on the carbon nanotube and graphene compound system is prepared from the following raw materials in percentage by weight through twin-screw melt extrusion:
styrene Polymer 90%
0.4 percent of carbon nano tube
2 percent of graphene
1.8 percent of compatilizer
5.8 percent of dispersant
The styrene polymer is ABS and/or ASA;
the compatilizer is styrene-acrylonitrile-glycidyl methacrylate terpolymer; the number average molecular weight of the terpolymer is 50000-90000; in the terpolymer, the mass percent of the glycidyl methacrylate is 5-20 wt%;
the dispersing agent is styrene-acrylonitrile copolymer; the number average molecular weight of the random copolymer is 10000-30000;
the average diameter of the carbon nano tube is less than 20nm, the average length is 1-20 mu m, and the average wall layer number is less than 15;
the average number of wall layers of the graphene is less than 15;
the preparation method of the styrene polymer-based conductive master batch based on the carbon nano tube and graphene compound system comprises the following steps:
(1) respectively dispersing carbon nanotubes and graphene in an inert volatile solvent, and stirring at normal temperature for 10-30 min to obtain a carbon nanotube suspension and a graphene suspension;
(2) respectively treating the carbon nanotube suspension and the graphene suspension for 1h by using a 400W ultrasonic treatment device to obtain a carbon nanotube dispersion liquid and a graphene dispersion liquid;
(3) mixing and stirring the carbon nanotube dispersion liquid, the graphene dispersion liquid and a dispersing agent to obtain a dispersing material; the rotating speed of the stirring is 1500 rpm;
(4) mixing the dispersing material with a compatilizer, and then carrying out melt extrusion through a double screw to obtain styrene polymer-based conductive master batch based on a carbon nano tube and graphene compound system; the processing temperature of the twin-screw melt extrusion is 190-230 ℃, and the rotating speed is 300 rpm.
2. The styrene polymer-based conductive masterbatch based on the carbon nanotube and graphene compound system according to claim 1, wherein the melt index of the terpolymer at 235 ℃/2.16kg is 5-15 g/10 min; the melt index of the random copolymer at 190 ℃/5kg is 40-100 g/10 min.
3. The styrene polymer-based conductive masterbatch based on the carbon nanotube and graphene compound system according to claim 1, wherein the styrene-acrylonitrile-glycidyl methacrylate terpolymer comprises 75% by mass, 25% by mass and 5% by mass of styrene, acrylonitrile and glycidyl methacrylate; the number average molecular weight of the styrene-acrylonitrile-glycidyl methacrylate terpolymer is 75000-82000.
4. The styrene polymer-based conductive masterbatch based on the carbon nanotube and graphene compound system according to claim 1, wherein the styrene-acrylonitrile copolymer comprises 75% and 25% of styrene and acrylonitrile by mass respectively; the number average molecular weight of the styrene-acrylonitrile copolymer is 18000-21000.
5. The application of the styrene polymer-based conductive masterbatch based on the carbon nanotube and graphene compound system as defined in claim 1 in preparing conductive materials.
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| CN102947372A (en) * | 2010-04-22 | 2013-02-27 | 阿克马法国公司 | Thermoplastic and/or elastomeric composite material containing carbon nanotubes and graphenes |
| CN106189167A (en) * | 2016-07-22 | 2016-12-07 | 佳易容相容剂江苏有限公司 | Efficient anti-static PC/ABS composite and preparation method thereof |
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| CN102947372A (en) * | 2010-04-22 | 2013-02-27 | 阿克马法国公司 | Thermoplastic and/or elastomeric composite material containing carbon nanotubes and graphenes |
| CN102850735A (en) * | 2012-08-23 | 2013-01-02 | 上海梵和聚合材料有限公司 | PBT / ASA composition with high conductivity, and preparation equipment, preparation method and application thereof |
| CN106189167A (en) * | 2016-07-22 | 2016-12-07 | 佳易容相容剂江苏有限公司 | Efficient anti-static PC/ABS composite and preparation method thereof |
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| 石墨烯/碳纳米管/硅橡胶导电复合材料的研究;刘寅;《中国优秀硕士学位论文全文数据库 工程科技I辑》;中国学术期刊电子杂志社;20120715;B020-289 * |
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