CN111499973B - Conductive carbon fiber resin composition and preparation method thereof - Google Patents
Conductive carbon fiber resin composition and preparation method thereof Download PDFInfo
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- CN111499973B CN111499973B CN202010367710.3A CN202010367710A CN111499973B CN 111499973 B CN111499973 B CN 111499973B CN 202010367710 A CN202010367710 A CN 202010367710A CN 111499973 B CN111499973 B CN 111499973B
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
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- 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
- C08K2201/004—Additives being defined by their length
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The invention relates to a conductive carbon fiber resin composition and a preparation method thereof, wherein the conductive carbon fiber resin composition comprises the following raw materials in parts by weight: 68-85 parts of thermoplastic resin; 5-12 parts of chopped carbon fibers; grinding 10-15 parts of carbon fibers; 0.5-0.8 part of conductive additive. Compared with the prior art, the resin composition prepared by the invention has excellent conductivity, and the surface resistivity is stably up to 10 1 ‑10 4 Ohm shows stable conduction uniformity under different injection molding processes, has excellent cleanness, and is very suitable for occasions with high cleanness requirements.
Description
Technical Field
The invention relates to a thermoplastic compound, in particular to a conductive carbon fiber resin composition and a preparation method thereof.
Background
Compared with metal materials, the conductive thermoplastic resin has excellent processability and chemical resistance, and can realize light weight and low cost. Therefore, the conductive thermoplastic resin is more and more widely used in the industries of electronics, electrical appliances and automobiles for replacing metal materials. We generally set the surface resistivity to 10 or less 5 Ohmic materials are classified as conducting grade materials, and achieving this level of conductivity generally requires the addition of conductive fillers, including conductive carbon black, carbon fibers, carbon nanotubes, graphite, graphene, metal powders, metal fibers, and the like, to the resin.
Conductive carbon black is the most commonly used conductive filler, and has excellent conductivity, no anisotropy and good conductivity uniformity. What achieves high conductivity of conductive carbon black is the high structure of carbon black, which describes that primary particles of carbon black (typically having a particle size of 40nm) are interconnected in three-dimensional space to form a developed three-dimensional "grape bunch" structure, which has a very high specific surface area. Characterization of the high carbon Black Structure is generally characterized by the parameter DBP oil absorptionGenerally, the DBP oil absorption of the conductive carbon black is 150 to 600ml/100g, and the higher the DBP oil absorption, the less the amount added in the resin matrix, the same conductivity is achieved. The surface resistivity is generally less than or equal to 10 5 Ohm, the adding amount of the conductive carbon black in different matrixes is 3-25%. However, in some occasions with high cleanliness requirements, the carbon black conductive resin cannot meet the requirements. Because the particle size of the conductive carbon black is small and the addition amount is high, black slag can appear when parts are cleaned or worn, which is a common industrial problem of carbon black conductive resin.
Carbon nanotubes and graphene have a high aspect ratio, and therefore the required addition amount is small, usually 1-5%, and this addition amount also has a problem that the cleanliness cannot meet the requirement. The realization of lower addition amount is generally in the development stage, the dispersed phase state needs to be strictly controlled, and the challenge is brought to the scale-up and stable production.
The diameter of the carbon fiber is 5-15 microns, the carbon fiber has excellent conductivity, rigidity and wear resistance, and the carbon fiber conductive resin has the characteristic of very high cleanness, and is suitable for occasions with high cleanness requirements. However, due to the characteristic of anisotropy of the fiber, the electrical conductivity of the carbon fiber resin composite is generally very uneven, the electrical resistivity of different positions of an injection-molded part fluctuates by more than 10 orders of magnitude, and meanwhile, the electrical resistivity is greatly influenced by the injection molding process, and the electrical conductivity is unstable and uneven. This disadvantage limits the wide use of carbon fiber conductive resins. The uniformity of conductivity can be improved by adding carbon black to the carbon fiber resin composition, but since the amount of carbon black added is at least 2%, the conductive resin composition also has the problem of "black residue removal".
CN104845361 discloses a highly conductive thermoplastic obtained by mixing chopped carbon fiber, conductive carbon black/graphene and resin, which cannot be used in occasions requiring high cleanness because of the high content of carbon black or graphene because of the addition of 2-10 parts of carbon black/graphene.
CN106317750 discloses a carbon fiber reinforced conductive ABS, which is added with 10-40 parts of conductive carbon black, and is not suitable for occasions with high cleanness requirements.
Therefore, it is a difficult problem to solve the surface conduction nonuniformity while maintaining the high cleanliness characteristics of the carbon fiber resin composition, and there is a recent report on solving this problem.
Disclosure of Invention
The present invention is directed to overcoming the above-mentioned drawbacks of the prior art and providing a conductive carbon fiber resin composition and a method for preparing the same.
The purpose of the invention can be realized by the following technical scheme:
the conductive carbon fiber resin composition is characterized by comprising the following raw materials in parts by weight:
the thermoplastic resin is selected from one or more of polypropylene, polybutylene terephthalate, polycarbonate, polyamide, polyphenylene sulfide, polyetherimide or polyformaldehyde.
The length of the chopped carbon fiber is 3-12 mm.
The chopped carbon fibers are used for easy processing operability, and too long carbon fibers cause difficult feeding.
The milled carbon fibers have a length of 20 to 500 microns.
The conductive auxiliary agent is conductive carbon black.
The conductive carbon black is high-structure conductive carbon black, and the DBP oil absorption of the conductive carbon black is at least 300ml/100 g.
The DBP oil absorption is the amount of dibutyl phthalate absorbed by every 100g of carbon black, the DBP oil absorption of the general conductive carbon black is 150-600 ml/100g, and the higher the DBP oil absorption, the higher the content of the conductive carbon black, the lower the content of the conductive carbon black in the resin matrix, the same conductivity can be achieved. More advanced high structure carbon blacks are selected in the present invention to reduce the amount of conductive carbon black added while maintaining the formation of a conductive network.
The surface resistivity of the carbon fiber resin composition is 10 1 ～10 4 Ohm.
The prepared conductive carbon fiber resin composition is subjected to injection molding to obtain a molded part, and the fluctuation range of the resistivity of each point on the surface of the molded part prepared from the carbon fiber resin composition is within two orders of magnitude.
The conductive carbon fiber resin composition of the present invention further comprises one or more of a resin filler, a stabilizer, a flame retardant, an impact modifier, a colorant or a mold release agent.
The carbon fiber resin composition prepared by the invention has excellent conductivity and surface resistivity of 10 1 -10 4 In the ohm range, the surface resistivity of the molded part is uniformly distributed, and the resistivity at different positions fluctuates within two orders of magnitude; meanwhile, the carbon fiber resin composition keeps the characteristic of high cleanness of the original carbon fiber resin composition and is very suitable for occasions with high cleanness requirements.
The invention also provides a preparation method of the conductive carbon fiber resin composition, which is characterized by comprising the following steps:
(1) preparing the following components in percentage by weight: 68-85 parts of thermoplastic resin, 5-12 parts of chopped carbon fibers, 10-15 parts of ground carbon fibers and 0.5-0.8 part of conductive additive;
(2) and melting and extruding all the raw material components through a double-screw extruder, and cooling and granulating to obtain the carbon fiber resin composition.
Compared with the prior art, the invention has the following advantages:
(1) the invention adopts three conductive fillers to obtain an efficient conductive network: the chopped carbon fibers, the ground carbon fibers and the conductive carbon black are cooperated to obtain a high-efficiency conductive network through proper proportion. The chopped and ground carbon fibers are used as a main conductive path, and the conductive carbon black with a high structure further perfects the conductive path among the carbon fibers, so that the material realizes high conductivity, and the surface resistivity is 10 1 -10 4 In the ohmic range.
(2) The invention adopts the ground carbon fiber to improve the unstable and uneven conductivity caused by the anisotropy of the carbon fiber, and the ground carbon fiber is compounded with the conductive carbon black to promote the formation of more conductive paths, and the conductive network formed by the fillers with different sizes is not easily influenced by injection molding shearing, thereby showing excellent conductive uniformity and shearing stability.
(3) The invention adopts 0.5 to 0.8 weight part of compounded conductive carbon black, and the addition amount is obviously less than the conventional addition amount (more than 2 percent), thereby keeping the characteristic of high cleanness of the carbon fiber resin composition. No black material appeared during cleaning and rubbing.
(4) The carbon fiber resin composition prepared by the invention realizes the characteristic of high conductivity, the minimum total mass fraction of the conductive filler is only 15.5%, and the low addition amount is beneficial to realizing the characteristics of low cost, high toughness and high fluidity.
(5) The preparation method has the advantages of simple process, stable product performance and low cost, and is very suitable for industrial production.
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 conductive carbon fiber resin composition comprises the following raw materials in parts by weight:
wherein the thermoplastic resin is selected from one or more of polypropylene (PP), polybutylene terephthalate (PBT), Polycarbonate (PC), Polyamide (PA) and polyphenylene sulfide (PPS). The thermoplastic resin phase or matrix may be composed of any desired thermoplastic resin conventionally satisfactory for use in the manufacture of electrically conductive resin compositions. For example, according to the following examples, the thermoplastic resin phase may also include Polyetherimide (PEI) and Polyoxymethylene (POM).
The length of the chopped carbon fiber is 3-12 mm, the chopped carbon fiber is adopted for easy processing operability, and the overlong carbon fiber causes difficult feeding.
The milled carbon fibers have a length of 20 to 500 microns.
The conductive auxiliary agent is conductive carbon black.
The conductive carbon black is high-structure conductive carbon black, the DBP oil absorption of the conductive carbon black is at least 300ml/100g, namely, every 100g of carbon black absorbs more than 300ml of dibutyl phthalate, the DBP oil absorption of the general conductive carbon black is 150-600 ml/100g, the higher the DBP oil absorption, the same conductivity is achieved, and the less the additive amount in the resin matrix is. More advanced high structure carbon blacks are selected in the present invention to reduce the amount of conductive carbon black added while maintaining the formation of a conductive network.
The surface resistivity of the carbon fiber resin composition was 10 1 ～10 4 Ohm.
The composition of this embodiment may also further comprise additives, and the disclosed compositions may further optionally include one or more additives conventionally used in the manufacture of resin-containing compositions, provided that the additives do not adversely affect the desired properties of the resulting carbon fiber resin composition. For example, the disclosed resin compositions may include one or more of fillers, stabilizers, flame retardants, impact modifiers, colorants, mold release agents.
The resulting carbon fiber resin composition can be further processed into shaped, formed, molded articles by various methods. For example, the compositions can be molded into useful shaped articles by a variety of means such as injection molding, extrusion, rotational molding, blow molding, and thermoforming.
The preparation method of the conductive carbon fiber resin composition comprises the following steps:
(1) preparing the following components in percentage by weight: 68-85 parts of thermoplastic resin, 5-12 parts of chopped carbon fibers, 10-15 parts of ground carbon fibers and 0.5-0.8 part of conductive additive;
(2) and melting and extruding all the raw material components through a double-screw extruder, and cooling and granulating to obtain the carbon fiber resin composition.
Performance evaluation mode and implementation standard thereof
Preparing a sample plate: the plastic pellets of the conductive carbon fiber resin composition obtained were injection molded to obtain a sample plate having a size of 350mm x 150mm x 3mm, and 5 pieces were injection molded by three injection molding processes (low speed, medium speed, high speed).
Conductivity evaluation: the surface resistivity of the sample was measured using ASTM D257, 5 plates were tested per condition, 8 points were taken for each plate, and the fluctuation range of the surface resistivity was recorded.
And (3) evaluating cleanliness: 2g of the particles were placed on a white paper, the particles were pressed with a load of 10N, and the particles were slid at a speed of 10cm/s, and a length of a scribe line was 20cm, after which it was examined whether a black mark was left on the white paper.
The following is a specific implementation process of the invention:
information on the raw materials used in the following examples and comparative examples:
thermoplastic resins are commercially available
Chopped carbon fiber CF 6mm in length is commercially available
Milled carbon fiber Gr-CF1 commercially available at 20 micron length
Milled carbon fiber Gr-CF2 commercially available at 100 micron length
Milled carbon fiber Gr-CF3 commercially available at 500 micron length
Milled carbon fiber Gr-CF4 is commercially available at 800-
Conductive carbon black CB1 DBP oil absorption of 360ml/100g is commercially available
Conductive carbon black CB2 DBP oil absorption of 495ml/100g on the market
Conductive carbon black CB3 DBP oil absorption of 150ml/100g is commercially available
Examples 1 to 11
The formula of the conductive carbon fiber resin composition is shown in Table 1, and the preparation method comprises the steps of preparing raw material components according to the formula, then carrying out melt extrusion on the raw material components through a double-screw extruder, and cooling and granulating to obtain the carbon fiber resin composition.
TABLE 1 raw Material compositions of conductive carbon fiber resin compositions of examples 1 to 11
Note: the unit of the content of each component in table 1 is part by weight.
Comparative examples 1 to 11
The formula of the conductive carbon fiber resin composition is shown in Table 2, and the preparation method comprises the steps of preparing raw material components according to the formula, then carrying out melt extrusion on the raw material components through a double-screw extruder, and cooling and granulating to obtain the carbon fiber resin composition.
TABLE 2 raw material composition of conductive carbon fiber resin compositions of comparative examples 1 to 11
Note: the unit of the content of each component in table 2 is part by weight.
The compositions obtained in examples 1 to 11 and comparative examples 1 to 11 were subjected to performance evaluation, and the evaluation results are shown in tables 3 and 4.
TABLE 3 results of conductivity test of conductive carbon fiber resin compositions of examples 1 to 11
TABLE 4 results of conductivity test of the conductive carbon fiber resin compositions of comparative examples 1 to 11
Analysis is carried out by combining tables 1-4, and the carbon fiber resin material prepared by reasonably compounding the three conductive fillers in the embodiments 1-11 has four characteristics: (ii) excellent conductivity, having 10 1 ～10 4 Ohmic surface resistivity, resistivity is small; secondly, the electrical resistivity of different positions of the injection molding plate is distributed uniformly, and the electrical resistivity of different positions fluctuates within two orders of magnitude; thirdly, different injection molding processes, namely under different shearing rates, the influence of conductivity is small, the resistivity fluctuates within two orders of magnitude, and the injection molding process has better processing performance; and fourthly, no black mark is found, and the cleanliness is excellent.
Comparative examples 1-11 show that the reduction of the carbon fiber content directly leads to the reduction of the conductivity, the chopped carbon fibers are the main conductive path of the whole system, the surface conductivity uniformity is improved by grinding the carbon fibers, the conductive network is enhanced by the carbon black, the conductivity and the uniformity are improved, and the cleanliness of the material is reduced by excessive carbon black. The amounts of chopped carbon fibers, milled carbon fibers, and conductive aids all affect the final conductivity and uniformity of conductivity.
Example 12
A conductive carbon fiber resin composition comprises the following components in percentage by weight: 68 parts of thermoplastic resin; 5 parts of short carbon fiber; grinding 10 parts of carbon fiber; 0.5 part of conductive additive, wherein the thermoplastic resin is polypropylene, the length of the chopped carbon fiber is 3mm, the length of the ground carbon fiber is 20mm, and the conductive additive is conductive carbon black. The preparation method comprises the steps of preparing raw material components according to a formula, then carrying out melt extrusion on the raw material components through a double-screw extruder, and carrying out cooling granulation to obtain the carbon fiber resin composition.
Example 13
A conductive carbon fiber resin composition comprises the following components in percentage by weight: 85 parts of thermoplastic resin; 12 parts of chopped carbon fibers; grinding 15 parts of carbon fibers; 0.8 part of conductive additive, wherein the thermoplastic resin is polypropylene, the length of the chopped carbon fiber is 12mm, the length of the ground carbon fiber is 500mm, and the conductive additive is conductive carbon black. The preparation method comprises the steps of preparing raw material components according to a formula, then carrying out melt extrusion on the raw material components through a double-screw extruder, and carrying out cooling granulation to obtain the carbon fiber resin composition.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes or modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (6)
1. The conductive carbon fiber resin composition is characterized by comprising the following raw materials in parts by weight:
68-85 parts of thermoplastic resin;
5-12 parts of chopped carbon fibers;
grinding 10-15 parts of carbon fibers;
0.5-0.8 part of conductive additive;
the length of the chopped carbon fiber is 3-12 mm;
the length of the milled carbon fibers is 20-500 microns;
the conductive auxiliary agent is high-structure conductive carbon black, and the DBP oil absorption of the conductive auxiliary agent is at least 300ml/100 g.
2. The conductive carbon fiber resin composition as claimed in claim 1, wherein the thermoplastic resin is selected from one or more of polypropylene, polybutylene terephthalate, polycarbonate, polyamide, polyphenylene sulfide, polyetherimide, and polyoxymethylene.
3. The conductive carbon fiber resin composition of claim 1, wherein the carbon fiber resin composition has a surface resistivity of 10 1 ~10 4 Ohm.
4. The conductive carbon fiber resin composition according to claim 1, wherein the range of variation in resistivity at each point on the surface of a molded part prepared from the carbon fiber resin composition is within two orders of magnitude.
5. The conductive carbon fiber resin composition of claim 1, further comprising one or more of a resin filler, a stabilizer, a flame retardant, an impact modifier, a colorant, or a mold release agent.
6. A method for preparing the conductive carbon fiber resin composition according to claim 1, comprising the steps of:
(1) preparing the following components in percentage by weight: 68-85 parts of thermoplastic resin, 5-12 parts of chopped carbon fibers, 10-15 parts of ground carbon fibers and 0.5-0.8 part of conductive additive;
(2) and melting and extruding all the raw material components through a double-screw extruder, and cooling and granulating to obtain the carbon fiber resin composition.
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| CN114773847B (en) * | 2022-04-12 | 2023-12-29 | 江苏苏中药业集团医疗器械有限公司 | Multi-morphology conductive carbon material synergistically modified PPS composite material for medical instrument and preparation method and application thereof |
| CN115850971B (en) * | 2022-11-30 | 2024-02-13 | 金发科技股份有限公司 | High-modulus high-conductivity carbon fiber reinforced material and preparation method and application thereof |
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| JP2000336265A (en) * | 1999-06-01 | 2000-12-05 | Tosoh Corp | Conductive polyphenylene sulfide resin composition |
| US20040113129A1 (en) * | 2002-07-25 | 2004-06-17 | Waggoner Marion G. | Static dissipative thermoplastic polymer composition |
| JP2004269810A (en) * | 2003-03-12 | 2004-09-30 | Mitsubishi Engineering Plastics Corp | Conductive thermoplastic resin composition |
| JP2007098255A (en) * | 2005-10-04 | 2007-04-19 | Sumitomo Bakelite Co Ltd | Method for preparing ground fiber, ground fiber, resin molding material, and molded article |
| CN103205109A (en) * | 2013-04-16 | 2013-07-17 | 常熟市凯力达蜂窝包装材料有限公司 | Preparation method of black flame resistant polyamide composite material reinforced by glass fibers |
| CN104845361B (en) * | 2015-05-13 | 2017-12-29 | 扬州利贞复合材料有限公司 | Chopped carbon fiber, conductive nano carbon black/graphene collaboration strengthen highly conductive thermoplastic and preparation method thereof |
| CN110204891A (en) * | 2018-02-28 | 2019-09-06 | 杜邦公司 | Antistatic polymer composite |
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