CN112552581A - Conductive thermoplastic elastomer composite material and preparation method thereof - Google Patents
Conductive thermoplastic elastomer composite material and preparation method thereof Download PDFInfo
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- CN112552581A CN112552581A CN201910918905.XA CN201910918905A CN112552581A CN 112552581 A CN112552581 A CN 112552581A CN 201910918905 A CN201910918905 A CN 201910918905A CN 112552581 A CN112552581 A CN 112552581A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/16—Ethene-propene or ethene-propene-diene copolymers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/041—Carbon nanotubes
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Abstract
The invention discloses a conductive thermoplastic elastomer composite material which comprises the following components in parts by weight: 45-70 parts of thermoplastic elastomer material, 25-50 parts of conductive master batch, 0.2-0.5 part of antioxidant and 0.5-1 part of high-efficiency dispersant, wherein the conductive master batch is prepared by compounding multi-wall carbon nano tube, conductive carbon black and coupling agent. The conductive master batch adopts the multi-walled carbon nanotube and the conductive carbon black to be matched for use, wherein the multi-walled carbon nanotube can be embedded into the composite material to play a role in bridging connection, so that the whole system is communicated, the electrical property is excellent, and meanwhile, the carbon nanotube has good toughness, so that the good toughness of the composite material is ensured. The coupling agent is added into the conductive master batch, so that the compatibility among material components can be improved, the bonding strength between the multi-walled carbon nanotube and the conductive carbon black and the composite material can be improved, and the prepared conductive thermoplastic elastomer composite material is low in surface resistivity, excellent in conductive performance and good in toughness and hardness.
Description
Technical Field
The invention belongs to the technical field of polymer processing, and particularly relates to a conductive thermoplastic elastomer composite material and a preparation method thereof.
Background
The traditional plastic composite material is used for automobiles, electronic appliances, articles for daily use and the like, the requirement on the electrical property of the material is relatively low, and various battery industries are developed rapidly in succession along with the development of the electronic appliances and new energy electric vehicles. The injection molding product needs to have the performances of electric conduction, static elimination and the like.
Carbon nanotubes are one-dimensional materials with good flexibility, and researchers have put the carbon nanotubes under 1011MPa of water pressure (equivalent to 10000 meters of pressure under water), and the carbon nanotubes are flattened due to the huge pressure. After the pressure is removed, the carbon nanotubes immediately recover their shape like a spring, showing good toughness. This suggests that carbon nanotubes can be used to make light and thin springs for use in automobiles and trains as shock absorbing devices. The invention uses the characteristic of the carbon nano tube and the conductive carbon black to cooperate to modify the thermoplastic elastomer, thereby ensuring the toughness of the elastomer material and achieving the purpose of conductivity.
Disclosure of Invention
In view of the above limitations of the prior art, it is an object of the present invention to provide an electrically conductive thermoplastic elastomer composite and a method for preparing the same.
The purpose of the invention is realized by the following technical scheme:
the conductive thermoplastic elastomer composite material comprises the following components in parts by weight:
the conductive master batch is prepared by compounding a multi-wall carbon nano tube, conductive carbon black and a coupling agent.
In a further aspect, the thermoplastic elastomer material is a blend of PP as a hard segment and EPDM as a soft segment, and has a gel content of 20% or more.
In a further scheme, the mass ratio of the multi-wall carbon nano tube, the conductive carbon black and the coupling agent in the conductive master batch is 1: 2: 0.5-1: 4: 2.
in a further scheme, the multi-wall carbon nano tube is an industrial carboxylated multi-wall carbon nano tube, the purity of the multi-wall carbon nano tube is more than or equal to 95 percent, and the diameter of the multi-wall carbon nano tube is 10-40 nm; the conductive carbon black is superconductive carbon black with the particle size less than 35 nm; the coupling agent is at least one of silane coupling agent and titanate coupling agent.
In a further scheme, the antioxidant is at least one of antioxidant 1010, antioxidant DSTDP and antioxidant 168.
In a further scheme, the high-efficiency dispersant is a dispersant with a multifunctional group structure and high-activity anchoring groups.
Another object of the present invention is to provide a method for preparing the above conductive thermoplastic elastomer composite, comprising the steps of:
(1) putting the multi-walled carbon nanotube, the conductive carbon black and the coupling agent into a high-speed mixer according to the proportion, and mixing to obtain a compound conductive master batch;
(2) adding the thermoplastic elastomer material, the antioxidant and the high-efficiency dispersant into a high-speed mixer, and continuously mixing to obtain a mixture;
(3) and adding the mixture into a double-screw extruder for granulation to obtain the conductive thermoplastic elastomer composite material.
In the step (3), the temperature of the twin-screw extruder from the feed opening to the die opening is 170-; the rotating speed of the extruder is 150-350 rpm; the vacuum degree is-0.07 to-0.03 MPa
Compared with the prior art, the invention has the following beneficial effects:
(1) the conductive master batch adopts the multi-walled carbon nanotube and the conductive carbon black to be matched for use, wherein the multi-walled carbon nanotube can be embedded into the composite material to play a role in bridging connection, so that the whole system is communicated, the electrical property is excellent, and meanwhile, the carbon nanotube has good toughness, so that the good toughness of the composite material is ensured.
(2) The coupling agent is added into the conductive master batch to premix the multi-walled carbon nanotube and the conductive carbon black, and the coupling agent can improve the compatibility among material components, so that the material components are uniformly dispersed in the later extrusion process, and the bonding strength among the multi-walled carbon nanotube, the conductive carbon black and the composite material is improved.
(3) The conductive thermoplastic elastomer composite material prepared by the invention has low surface resistivity, excellent conductive performance and good toughness and hardness; and the preparation method is simple, is suitable for industrial production and has great application prospect.
Detailed Description
The present invention will be further described with reference to the following examples. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The types and suppliers of reagents used in this example were as follows: the thermoplastic elastomer material is TPV 10-65A, TPV10-73A, TPV10-85A of Shandong Doran high polymer materials GmbH; the conductive carbon black is BP2000, Cambot chemical Co., Ltd; multi-walled carbon nanotubes, Nanjing Xiancheng nanomaterial science and technology Co., Ltd; the coupling agent is commercial KH 550; the high-efficiency dispersant is P121 of degussa; the antioxidants 1010, 168 and DSTDP are commercially available.
The reagents are provided only for illustrating the sources and components of the reagents used in the experiments of the present invention, so as to be fully disclosed, and do not indicate that the present invention cannot be realized by using other reagents of the same type or other reagents supplied by other suppliers.
Example 1
(1) Firstly, multi-wall carbon nano-tubes: conductive carbon black: the coupling agent is mixed according to the mass ratio of 1: 2: adding into a high-speed mixer at a ratio of 0.5, mixing for 1min, and preparing conductive masterbatch;
(2) and then mixing 45 parts of TPV 10-65A, 50 parts of conductive master batch, 0.2 part of antioxidant 1010, 0.3 part of antioxidant 168 and 1 part of high-efficiency dispersant P121 in a high-speed mixer for 2min, adding the uniformly mixed mixture into an extruder, performing melt extrusion, water cooling and then granulating to obtain the conductive thermoplastic elastomer composite material. Wherein the processing temperature of the extruder is 175 ℃, 185 ℃, 190 ℃, 200 ℃, 205 ℃, the rotation speed of a main engine is 150r/min and the vacuum degree is-0.07 MPa from the feed opening to the die orifice in sequence.
Example 2
(1) Firstly, multi-wall carbon nano-tubes: conductive carbon black: the coupling agent is mixed according to the mass ratio of 1: 4: 2, putting the mixture into a high-speed mixer in proportion, and mixing for 2min to prepare conductive master batches;
(2) and then mixing 70 parts of TPV10-73A, 25 parts of conductive master batch, 0.1 part of antioxidant 1010, 0.1 part of antioxidant 168 and 0.5 part of efficient dispersant P121 in a high-speed mixer for 2min, adding the uniformly mixed materials into an extruder, performing melt extrusion, water cooling and granulating to obtain the conductive thermoplastic elastomer composite material. Wherein the processing temperature of the extruder is 175 ℃, 185 ℃, 190 ℃, 200 ℃, 205 ℃, the rotation speed of the main machine is 350r/min, and the vacuum degree is-0.03 MPa from the feed opening to the die orifice in sequence.
Example 3
(1) Firstly, multi-wall carbon nano-tubes: conductive carbon black: the coupling agent is mixed according to the mass ratio of 1: 3: 1, putting the mixture into a high-speed mixer in proportion, and mixing for 2min to prepare conductive master batches;
(2) and then mixing 57 parts of TPV10-85A, 38 parts of conductive master batch, 0.1 part of antioxidant 1010, 0.1 part of antioxidant 168 and 0.5 part of efficient dispersant P121 in a high-speed mixer for 2min, adding the uniformly mixed materials into an extruder, performing melt extrusion, water cooling and granulating to obtain the conductive thermoplastic elastomer composite material. Wherein the processing temperature of the extruder is 175 ℃, 185 ℃, 190 ℃, 200 ℃, 205 ℃, the rotating speed of a main engine is 250r/min, and the vacuum degree is-0.04 MPa from the feed opening to the die orifice in sequence.
Comparative example 1
Mixing 57 parts of TPV10-85A, 38 parts of multi-walled carbon nanotubes, 0.1 part of antioxidant 1010, 0.1 part of antioxidant 168 and 0.5 part of efficient dispersant P121 in a high-speed mixer for 2min, adding the uniformly mixed mixture into an extruder, performing melt extrusion, water cooling and granulating to obtain the conductive thermoplastic elastomer composite material. Wherein the processing temperature of the extruder is 175 ℃, 185 ℃, 190 ℃, 200 ℃, 205 ℃, the rotating speed of a main engine is 250r/min, and the vacuum degree is-0.04 MPa from the feed opening to the die orifice in sequence.
Comparative example 2
Mixing 57 parts of TPV10-85A, 38 parts of conductive carbon black, 0.1 part of antioxidant 1010, 0.1 part of antioxidant 168 and 0.5 part of efficient dispersant P121 in a high-speed mixer for 2min, adding the uniformly mixed mixture into an extruder, performing melt extrusion, water cooling and granulating to obtain the conductive thermoplastic elastomer composite material. Wherein the processing temperature of the extruder is 175 ℃, 185 ℃, 190 ℃, 200 ℃, 205 ℃, the rotating speed of a main engine is 250r/min, and the vacuum degree is-0.04 MPa from the feed opening to the die orifice in sequence.
The conductive thermoplastic elastomer composite materials prepared in the above examples 1 to 3 and comparative examples 1 to 2 were tested according to the ISO standard, that is, extruded pellets were molded by an injection molding machine to obtain test specimens and pieces, and after stabilization for 24 hours at 23 ℃ and 50% relative humidity, performance test and surface resistivity test were carried out. The surface resistivity is shown in table 1 below:
TABLE 1
Remarking: the sample size and test conditions for the above test were:
(1) in the cantilever beam notch impact strength test, the cantilever beam notch impact spline is 80 x 10 x 4mm, wherein the notch depth is 2mm, and the impact pendulum energy is 5.5J;
(2) the thickness of the Shore hardness test sample piece is 4mm, and the weight of the weight is 5 KG;
(3) the surface resistivity is tested by adopting a high-resistance meter to test the size of a sample wafer
The thickness is 2 mm.
It can be seen from the examples 1-3 and the comparative examples 1 and 2 that the conductive masterbatch is prepared by premixing the multi-walled carbon nanotube, the conductive carbon black and the coupling agent, and then mixing with other components and extruding and granulating by a double screw, so that the conductive masterbatch is more uniformly distributed, and the prepared conductive thermoplastic elastomer composite material has excellent conductive effect and lower surface resistivity. Meanwhile, the conductive thermoplastic elastomer composite material keeps good toughness and hardness while conducting. In a single conductive material, such as conductive carbon black or multi-walled carbon nanotubes, a conductive network formed in the material has defects of different degrees, which means that the conductivity of the material cannot achieve the optimal effect.
The embodiments described above are intended to facilitate one of ordinary skill in the art in understanding and using the present invention. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the embodiments described herein, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (8)
1. An electrically conductive thermoplastic elastomer composite characterized by: the composition comprises the following components in parts by weight:
the conductive master batch is prepared by compounding a multi-wall carbon nano tube, conductive carbon black and a coupling agent.
2. The electrically conductive thermoplastic elastomer composite of claim 1, wherein: the thermoplastic elastomer material is a blend of PP as a hard segment and EPDM as a soft segment.
3. The electrically conductive thermoplastic elastomer composite of claim 1, wherein: the mass ratio of the multi-walled carbon nanotube, the conductive carbon black and the coupling agent in the conductive master batch is 1: 2: 0.5-1: 4: 2.
4. the electrically conductive thermoplastic elastomer composite of claim 1, wherein: the multi-walled carbon nanotube is an industrial-grade carboxylated multi-walled carbon nanotube with the diameter of 10-40 nm; the conductive carbon black is superconductive carbon black with the particle size less than 35 nm; the coupling agent is at least one of silane coupling agent and titanate coupling agent.
5. The electrically conductive thermoplastic elastomer composite of claim 1, wherein: the antioxidant is at least one of antioxidant 1010, antioxidant DSTDP and antioxidant 168.
6. The electrically conductive thermoplastic elastomer composite of claim 1, wherein: the high-efficiency dispersant is a dispersant with a multi-functional group structure and high-activity anchoring groups.
7. The method for preparing an electrically conductive thermoplastic elastomer composite as claimed in any one of claims 1 to 6, wherein: the method comprises the following steps:
(1) putting the multi-walled carbon nanotube, the conductive carbon black and the coupling agent into a high-speed mixer according to the proportion, and mixing to obtain a compound conductive master batch;
(2) adding the thermoplastic elastomer material, the antioxidant and the high-efficiency dispersant into a high-speed mixer, and continuously mixing to obtain a mixture;
(3) and adding the mixture into a double-screw extruder for granulation to obtain the conductive thermoplastic elastomer composite material.
8. The method of claim 7, wherein: in the step (3), the temperature of the double-screw extruder from the feed opening to the die opening is 170-205 ℃; the rotating speed of the extruder is 150-350 rpm; the vacuum degree is-0.07 to-0.03 MPa.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114133665A (en) * | 2021-12-15 | 2022-03-04 | 广州润锋科技股份有限公司 | High-conductivity composite master batch containing carbon black and carbon nano tubes and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114133665A (en) * | 2021-12-15 | 2022-03-04 | 广州润锋科技股份有限公司 | High-conductivity composite master batch containing carbon black and carbon nano tubes and preparation method thereof |
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