CN112852157A - Conductive PPS composite material with good epoxy adhesive force and preparation method thereof - Google Patents
Conductive PPS composite material with good epoxy adhesive force and preparation method thereof Download PDFInfo
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- CN112852157A CN112852157A CN202011609730.3A CN202011609730A CN112852157A CN 112852157 A CN112852157 A CN 112852157A CN 202011609730 A CN202011609730 A CN 202011609730A CN 112852157 A CN112852157 A CN 112852157A
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- 239000002131 composite material Substances 0.000 title claims abstract description 74
- 229920006332 epoxy adhesive Polymers 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title abstract description 20
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 72
- 239000000463 material Substances 0.000 claims abstract description 63
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 48
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 47
- 239000004593 Epoxy Substances 0.000 claims abstract description 41
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 40
- 239000004917 carbon fiber Substances 0.000 claims abstract description 40
- 239000003822 epoxy resin Substances 0.000 claims abstract description 39
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 39
- 239000003365 glass fiber Substances 0.000 claims abstract description 38
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 35
- 239000007822 coupling agent Substances 0.000 claims abstract description 34
- 239000012745 toughening agent Substances 0.000 claims abstract description 17
- 239000000203 mixture Substances 0.000 claims description 53
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 42
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 33
- 238000002156 mixing Methods 0.000 claims description 27
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical group O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 21
- 229920002725 thermoplastic elastomer Polymers 0.000 claims description 20
- 238000005303 weighing Methods 0.000 claims description 10
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 4
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 3
- 229910052731 fluorine Inorganic materials 0.000 claims description 3
- 239000011737 fluorine Substances 0.000 claims description 3
- 239000004519 grease Substances 0.000 claims description 3
- RKISUIUJZGSLEV-UHFFFAOYSA-N n-[2-(octadecanoylamino)ethyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCCNC(=O)CCCCCCCCCCCCCCCCC RKISUIUJZGSLEV-UHFFFAOYSA-N 0.000 claims description 3
- 229920001296 polysiloxane Polymers 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 2
- 229920003986 novolac Polymers 0.000 claims 1
- 238000001125 extrusion Methods 0.000 abstract description 22
- 239000011231 conductive filler Substances 0.000 abstract description 5
- 238000012986 modification Methods 0.000 abstract description 4
- 230000004048 modification Effects 0.000 abstract description 4
- 239000002861 polymer material Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 27
- 238000005469 granulation Methods 0.000 description 16
- 230000003179 granulation Effects 0.000 description 16
- 229920005989 resin Polymers 0.000 description 10
- 239000011347 resin Substances 0.000 description 10
- 230000009286 beneficial effect Effects 0.000 description 9
- 239000002994 raw material Substances 0.000 description 9
- 238000011056 performance test Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 6
- 239000006229 carbon black Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 230000001070 adhesive effect Effects 0.000 description 4
- 239000000945 filler Substances 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 3
- 229920006335 epoxy glue Polymers 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229920006465 Styrenic thermoplastic elastomer Polymers 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000002048 multi walled nanotube Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 238000004382 potting Methods 0.000 description 2
- 239000002109 single walled nanotube Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005292 diamagnetic effect Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 238000005290 field theory Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- -1 phenolic aldehyde Chemical class 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000011208 reinforced composite material Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L81/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen or carbon only; Compositions of polysulfones; Compositions of derivatives of such polymers
- C08L81/02—Polythioethers; Polythioether-ethers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/022—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the choice of material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/04—Particle-shaped
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention discloses a conductive PPS composite material with good epoxy adhesive force and a preparation method thereof, belonging to the technical field of modification of high polymer materials. The conductive PPS composite material with good epoxy adhesive force comprises the following components in parts by weight: PPS: 30-80 parts of glass fiber: 10-20 parts of conductive carbon black: 10-20 parts, Carbon Nanotube (CNT): 1-5 parts of carbon fiber: 1-10 parts of a toughening agent: 1-10 parts of epoxy resin: 1-10 parts of coupling agent: 0.1-1 part of release agent and 0.1-1 part of mould release agent. The PPS material adopts the glass fiber, the conductive carbon black, the carbon nano tube and the carbon fiber to be compositely filled to improve the strength and the conductivity of the PPS material, adopts a secondary extrusion mode to improve the dispersibility of the conductive filler, ensures the stability of the conductivity of the material, simultaneously improves the bonding force of the PPS to the epoxy resin through the addition of the toughening agent and the epoxy resin, and is suitable for the field which simultaneously puts higher requirements on the conductivity and the epoxy bonding property of the PPS material.
Description
Technical Field
The invention relates to the technical field of modification of high polymer materials, in particular to a conductive PPS composite material with good epoxy binding power and a preparation method thereof.
Background
The PPS resin structure is formed by alternately connecting rigid benzene rings and flexible thioether bonds, and molecular chains have high rigidity and regularity, so that the PPS is a crystalline polymer and has a plurality of excellent properties, namely heat resistance, flame retardance, corrosion resistance and the like. Meanwhile, the lone pair electrons on the sulfur atom ensure that the PPS resin has good affinity with glass fiber, inorganic filler and the like, so that the PPS resin can be easily prepared into various reinforced composite materials and alloys and is widely applied to various electrical equipment.
Epoxy resin is excellent in performance, and is often used as sealing and potting adhesive of electrical equipment to achieve the purpose of sealing, so that the PPS material is required to have good epoxy adhesive force to ensure the tight combination of the electrical equipment and the sealing and potting adhesive. However, the unmodified PPS resin has poor adhesion with epoxy glue and cannot achieve good effectAnd (4) sealing effect. Meanwhile, due to the rapid development of the 5G technology, the requirements of mobile terminals and base stations on electromagnetic shielding of electrical equipment are increasing day by day, and due to the short millimeter wave wavelength and the large transmission loss, higher requirements are provided for the shielding effect of the electrical equipment. According to the electromagnetic field theory, the smaller the resistance value of the shielding material, the larger the eddy current and the larger the diamagnetic field generated, the better the shielding effect, and generally speaking, the material with the resistivity not more than 10 is required for shielding4。
Therefore, it is an urgent technical problem to be solved by those skilled in the art to provide a conductive PPS composite material having excellent conductive performance and good epoxy adhesion, so that the PPS composite material can be used as an electromagnetic shielding material.
Disclosure of Invention
In view of the above, the invention provides a conductive PPS composite material with good epoxy adhesive force and a preparation method thereof, wherein the conductive carbon black is introduced to endow the material with excellent conductivity; the conductivity of the material is further improved by introducing Carbon Nanotubes (CNTs) and carbon fibers, and the strength of the material is increased to a certain degree; the epoxy bonding performance of the material is improved by introducing epoxy resin; by introducing the epoxy group toughening agent, the dispersibility of the epoxy resin is improved so as to further improve the epoxy cohesiveness of the material and improve the toughness of the material; by introducing a coupling agent, the mechanical property of the material is improved; by introducing the release agent, the material processing window is widened, and the processing performance is improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
firstly, the invention provides a conductive PPS composite material with good epoxy adhesive force, which comprises the following components in parts by weight:
30-80 parts of PPS, 10-20 parts of glass fiber, 10-20 parts of conductive carbon black, 1-5 parts of carbon nano tube, 1-10 parts of carbon fiber, 1-10 parts of toughening agent, 1-10 parts of epoxy resin, 0.1-1 part of coupling agent and 0.1-1 part of release agent.
Further, the conductive PPS composite material with good epoxy bonding force comprises the following components in parts by weight:
40-70 parts of PPS, 12-18 parts of glass fiber, 12-18 parts of conductive carbon black, 1-4 parts of carbon nano tube, 2-8 parts of carbon fiber, 2-8 parts of toughening agent, 2-8 parts of epoxy resin, 0.1-0.8 part of coupling agent and 0.1-0.8 part of release agent.
Further, the conductive PPS composite material with good epoxy bonding force comprises the following components in parts by weight:
47 parts of PPS, 16 parts of glass fiber, 16 parts of conductive carbon black, 3 parts of carbon nanotube, 5 parts of carbon fiber, 6 parts of toughening agent, 6 parts of epoxy resin, 0.5 part of coupling agent and 0.5 part of release agent.
By adopting the technical scheme, the conductive PPS composite material with good epoxy adhesive force has high mechanical strength and resistivity lower than 105Omega cm conductivity and good epoxy adhesive property.
Preferably, the PPS melt index is between 300-500g/10 min.
The beneficial effects of the preferred technical scheme are as follows: if the PPS melt index is less than 300g/10min, the conductive carbon black, carbon fiber and other fillers are not uniformly dispersed, the material flowability is poor, and the molding is not facilitated; if the PPS melt index is more than 500g/10min, the toughness of the material is reduced; the PPS melt index is between 300-500g/10min, so that the filler can be fully dispersed, and the obtained conductive PPS composite material with good epoxy bonding force has certain toughness.
Preferably, the glass fiber is a PPS special chopped glass fiber.
The beneficial effects of the preferred technical scheme are as follows: the chopped fibers are easy to process, and the unique impregnating compound of the chopped fibers special for PPS ensures the good compatibility of the glass fibers and the PPS resin of the matrix, and improves the mechanical strength of the composite material.
Preferably, the conductive carbon black has a resistivity of < 103Ω·cm。
The beneficial effects of the preferred technical scheme are as follows: if the electrical resistivity of the conductive carbon black is more than 103Omega cm, the target conductivity can be achieved by adding more parts, which leads to the increase of cost and the reduction of mechanical strength of materials, and the resistivity is adoptedLess than 103The omega cm carbon black not only ensures the premise of material performance, but also saves the material cost.
Preferably, the carbon nanotubes are single-walled carbon nanotubes or multi-walled carbon nanotubes or a mixture of the two.
The beneficial effects of the preferred technical scheme are as follows: the Carbon Nano Tube (CNT) and the carbon black play a synergistic conductive role, so that a conductive network is conveniently formed, and the conductive performance of the composite material is improved.
Preferably, the carbon fiber is a highly conductive high strength carbon fiber.
The beneficial effects of the preferred technical scheme are as follows: the high-conductivity and high-strength carbon fiber further improves the conductivity of the composite material and improves the mechanical property of the material to a certain extent.
Preferably, the toughening agent is a maleic anhydride grafted styrenic thermoplastic elastomer.
The beneficial effects of the preferred technical scheme are as follows: the maleic anhydride grafted styrene thermoplastic elastomer is adopted to improve the polarity of the PPS material and the wettability to epoxy, and improve the epoxy adhesive force of the PPS material.
Preferably, the epoxy resin is one or a mixture of bisphenol A epoxy, brominated bisphenol A epoxy and phenolic aldehyde epoxy.
The beneficial effects of the preferred technical scheme are as follows: the epoxy resin can be uniformly dispersed in the PPS resin of the matrix, and is fully combined with the epoxy colloid after being heated and melted, so that the whole epoxy adhesive force of the composite material is improved.
Preferably, the coupling agent is one or a mixture of two of gamma-aminopropyltriethoxysilane and gamma-glycidoxypropyltrimethoxysilane.
The beneficial effects of the preferred technical scheme are as follows: the coupling agent can improve the interaction force between the surface of the filler and the matrix resin to form a chemical bond or a hydrogen bond, thereby improving the mechanical property of the material.
Preferably, the release agent is one or a mixture of two of N, N' -ethylene bis stearamide, silicone powder and fluorine-containing grease.
The beneficial effects of the preferred technical scheme are as follows: the release agent can improve the surface lubricity of the material, thereby shortening the molding period and widening the molding process window.
The invention also provides a preparation method of the conductive PPS composite material with good epoxy adhesive force, which comprises the following steps:
s1, weighing PPS, glass fiber, conductive carbon black, carbon nano tubes, carbon fibers, a toughening agent, epoxy resin, a coupling agent and a release agent according to parts by weight for later use;
s2, uniformly mixing the PPS and the conductive carbon black to obtain a conductive master batch mixture;
s3, adding the conductive master batch mixture obtained in the step S1 into a main material port of an extruder, and extruding and granulating at the rotating speed of 240-300rpm and the temperature of each section of 290-310 ℃ to obtain the PPS conductive master batch;
s4, uniformly mixing the PPS conductive master batch prepared in the step S3 with the carbon nano tube, the carbon fiber, the toughening agent, the epoxy resin, the coupling agent and the release agent to obtain a mixture;
s5, adding the mixture obtained in the step S4 into the main material port of the extruder, adding glass fiber into the side feed, and extruding and granulating at the rotating speed of 240-300rpm and the temperature of 290-310 ℃ in each section to obtain the conductive PPS composite material with good epoxy adhesive force
Further, the mixing temperature in the step S2 is 70-90 ℃, preferably 80 ℃, and the mixing speed is 300-800 rpm.
Further, the extrusion speed in step S3 was 280rpm, and the main feed speed was 30-50 rpm.
Further, the temperatures of the sections of the extruder in the step S3 include a first zone temperature of 290-.
Further, the mixing temperature of step S4 is 70-90 deg.C, preferably 80 deg.C, and the mixing speed is 300-800 rpm.
Further, the extrusion speed of step S5 is 280rpm, the main feeding speed is 30-50rpm, and the side feeding speed is 10-30 rpm.
Further, the temperatures of the sections of the extruder in the step S5 include a first zone temperature of 290-.
According to the technical scheme, compared with the prior art, the invention discloses a conductive PPS composite material with good epoxy bonding force and a preparation method thereof, and the conductive PPS composite material has the following technical effects:
1) according to the conductive PPS composite material with good epoxy adhesive force, the polarity of the PPS material and the wettability to epoxy are improved by introducing the special styrene elastomer and the epoxy resin, so that the toughness of the material is improved while the good epoxy adhesive force is given to the material;
2) the conductive PPS composite material with good epoxy binding power provided by the invention avoids the processing difficulty and low mechanical property caused by single carbon black conductive modification through the optimized proportioning and composite filling of the conductive carbon black, the Carbon Nano Tube (CNT) and the carbon fiber, and improves the mechanical strength of the material to a certain extent;
3) the preparation method of the conductive PPS composite material with good epoxy bonding force provided by the invention ensures the sufficient dispersion of the conductive filler through a secondary extrusion process, is used for obtaining the conductive PPS composite material with stable electrical property, and is particularly suitable for the application fields with high conductivity and epoxy bonding requirements.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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 raw materials used in the following examples: the PPS melt index is 300-500g/10min, the glass fiber is the special PPS chopped glass fiber, and the used conductive carbon black has the resistivity of less than 103The carbon black is characterized in that Carbon Nanotubes (CNT) are one or a mixture of single-walled carbon nanotubes or multi-walled carbon nanotubes, the carbon fibers are high-conductivity and high-strength carbon fibers, the toughening agent is maleic anhydride grafted styrene thermoplastic elastomer, the epoxy resin is one or a mixture of bisphenol A epoxy, brominated bisphenol A epoxy and phenolic epoxy, the coupling agent is one or a mixture of gamma-aminopropyltriethoxysilane and gamma-glycidylethoxypropyltrimethoxysilane, and the release agent is one or a mixture of N, N' -ethylene bis-stearamide, silicone powder and fluorine-containing lubricating grease.
Example 1
A conductive PPS composite material with good epoxy adhesive force comprises the following components in parts by weight: 300-500g/10min melt index PPS 48 parts, glass fiber 15 parts, conductive carbon black 18 parts, Carbon Nano Tube (CNT)3 parts, carbon fiber 5 parts, maleic anhydride grafted styrene thermoplastic elastomer 5 parts, epoxy resin 5 parts, coupling agent 0.5 part and release agent 0.5 part.
The preparation method of the conductive PPS composite material with good epoxy adhesive force comprises the following steps:
s1, weighing the raw materials in parts by weight for later use;
s2, adding the PPS and the conductive carbon black into a high-speed mixer at 500rpm, and uniformly mixing at 80 ℃ to obtain a conductive master batch mixture;
s3, setting the temperature of each section of the extruder as follows: setting the screw rotation speed at 260rpm at 290 ℃, 300 ℃, 310 ℃, 300 ℃ and 310 ℃, adding the conductive master batch mixture obtained in the step S1 into the main material port, and performing extrusion granulation at 40rpm to obtain PPS conductive master batches;
s4, adding the PPS conductive master batch prepared in the step S3, the carbon nano tube, the carbon fiber, the maleic anhydride grafted styrene thermoplastic elastomer, the epoxy resin, the coupling agent and the release agent into a high-speed mixer at 500rpm, and uniformly mixing at 80 ℃ to obtain a mixture;
s5, setting the temperature of each section of the extruder as follows: 290 ℃, 300 ℃, 310 ℃, 300 ℃ and 310 ℃, the screw rotating speed is set to 260rpm, the main material port feeding rotating speed is 40rpm, the mixture obtained in the step S4 is added, the side feeding rotating speed is 20rpm, the glass fiber is added, and the conductive PPS composite material with good epoxy adhesive force is obtained after extrusion granulation.
Example 2
A conductive PPS composite material with good epoxy adhesive force comprises the following components in parts by weight: 300-500g/10min melt index PPS 32 parts, glass fiber 20 parts, conductive carbon black 20 parts, Carbon Nano Tube (CNT)5 parts, carbon fiber 8 parts, maleic anhydride grafted styrene thermoplastic elastomer 6 parts, epoxy resin 8 parts, coupling agent 0.5 part and release agent 0.5 part.
The preparation method of the conductive PPS composite material with good epoxy adhesive force comprises the following steps:
s1, weighing the raw materials in parts by weight for later use;
s2, adding the PPS and the conductive carbon black into a high-speed mixer at 500rpm, and uniformly mixing at 80 ℃ to obtain a conductive master batch mixture;
s3, setting the temperature of each section of the extruder as follows: setting the screw rotation speed at 260rpm at 290 ℃, 300 ℃, 310 ℃, 300 ℃ and 310 ℃, adding the conductive master batch mixture obtained in the step S1 into the main material port, and performing extrusion granulation at 40rpm to obtain PPS conductive master batches;
s4, adding the PPS conductive master batch prepared in the step S3, the carbon nano tube, the carbon fiber, the maleic anhydride grafted styrene thermoplastic elastomer, the epoxy resin, the coupling agent and the release agent into a high-speed mixer at 500rpm, and uniformly mixing at 80 ℃ to obtain a mixture;
s5, setting the temperature of each section of the extruder as follows: 290 ℃, 300 ℃, 310 ℃, 300 ℃ and 310 ℃, the screw rotating speed is set to 260rpm, the main material port feeding rotating speed is 40rpm, the mixture obtained in the step S4 is added, the side feeding rotating speed is 20rpm, the glass fiber is added, and the conductive PPS composite material with good epoxy adhesive force is obtained after extrusion granulation.
Example 3
A conductive PPS composite material with good epoxy adhesive force comprises the following components in parts by weight: 300-500g/10min melt index PPS 48 parts, glass fiber 15 parts, conductive carbon black 18 parts, Carbon Nano Tube (CNT)3 parts, carbon fiber 5 parts, maleic anhydride grafted styrene thermoplastic elastomer 5 parts, epoxy resin 5 parts, coupling agent 0.5 part and release agent 0.5 part.
The preparation method of the conductive PPS composite material with good epoxy adhesive force comprises the following steps:
s1, weighing the raw materials in parts by weight for later use;
s2, adding the PPS and the conductive carbon black into a high-speed mixer at 500rpm, and uniformly mixing at 80 ℃ to obtain a conductive master batch mixture;
s3, setting the temperature of each section of the extruder as follows: setting the screw rotation speed at 260rpm at 290 ℃, 300 ℃, 310 ℃, 300 ℃ and 310 ℃, adding the conductive master batch mixture obtained in the step S1 into the main material port, and performing extrusion granulation at 40rpm to obtain PPS conductive master batches;
s4, adding the PPS conductive master batch prepared in the step S3, the carbon nano tube, the carbon fiber, the maleic anhydride grafted styrene thermoplastic elastomer, the epoxy resin, the coupling agent and the release agent into a high-speed mixer at 500rpm, and uniformly mixing at 80 ℃ to obtain a mixture;
s5, setting the temperature of each section of the extruder as follows: 290 ℃, 300 ℃, 310 ℃, 300 ℃ and 310 ℃, the screw rotating speed is set to 260rpm, the main material port feeding rotating speed is 40rpm, the mixture obtained in the step S4 is added, the side feeding rotating speed is 20rpm, the glass fiber is added, and the conductive PPS composite material with good epoxy adhesive force is obtained after extrusion granulation.
Comparative example 1
A conductive PPS composite material with good epoxy adhesive force comprises the following components in parts by weight: 300-500g/10min of PPS 63 parts, 18 parts of conductive carbon black, 3 parts of Carbon Nano Tubes (CNT), 5 parts of carbon fibers, 5 parts of maleic anhydride grafted styrene thermoplastic elastomer, 5 parts of epoxy resin, 0.5 part of coupling agent and 0.5 part of release agent.
The preparation method of the conductive PPS composite material with good epoxy adhesive force comprises the following steps:
s1, weighing the raw materials in parts by weight for later use;
s2, adding the PPS and the conductive carbon black into a high-speed mixer at 500rpm, and uniformly mixing at 80 ℃ to obtain a conductive master batch mixture;
s3, setting the temperature of each section of the extruder as follows: setting the screw rotation speed at 260rpm at 290 ℃, 300 ℃, 310 ℃, 300 ℃ and 310 ℃, adding the conductive master batch mixture obtained in the step S1 into the main material port, and performing extrusion granulation at 40rpm to obtain PPS conductive master batches;
s4, adding the PPS conductive master batch prepared in the step S3, the carbon nano tube, the carbon fiber, the maleic anhydride grafted styrene thermoplastic elastomer, the epoxy resin, the coupling agent and the release agent into a high-speed mixer at 500rpm, and uniformly mixing at 80 ℃ to obtain a mixture;
s5, setting the temperature of each section of the extruder as follows: and (3) adding the mixture obtained in the step (S4) into the mixture at a screw rotating speed of 260rpm and a main material port feeding rotating speed of 40rpm at 290 ℃, 300 ℃, 310 ℃, 300 ℃, 310 ℃ and 310 ℃ for extrusion granulation to obtain the conductive PPS composite material with good epoxy adhesive force.
Comparative example 2
A conductive PPS composite material with good epoxy adhesive force comprises the following components in parts by weight: 300-500g/10min of PPS, 15 parts of glass fiber, 26 parts of conductive carbon black, 5 parts of maleic anhydride grafted styrene thermoplastic elastomer, 5 parts of epoxy resin, 0.5 part of coupling agent and 0.5 part of release agent.
The preparation method of the conductive PPS composite material with good epoxy adhesive force comprises the following steps:
s1, weighing the raw materials in parts by weight for later use;
s2, adding the PPS and the conductive carbon black into a high-speed mixer at 500rpm, and uniformly mixing at 80 ℃ to obtain a conductive master batch mixture;
s3, setting the temperature of each section of the extruder as follows: setting the screw rotation speed at 260rpm at 290 ℃, 300 ℃, 310 ℃, 300 ℃ and 310 ℃, adding the conductive master batch mixture obtained in the step S1 into the main material port, and performing extrusion granulation at 40rpm to obtain PPS conductive master batches;
s4, adding the PPS conductive master batch prepared in the step S3, the carbon nano tube, the maleic anhydride grafted styrene thermoplastic elastomer, the epoxy resin, the coupling agent and the release agent into a high-speed mixer at 500rpm, and uniformly mixing at 80 ℃ to obtain a mixture;
s5, setting the temperature of each section of the extruder as follows: 290 ℃, 300 ℃, 310 ℃, 300 ℃ and 310 ℃, the screw rotating speed is set to 260rpm, the main material port feeding rotating speed is 40rpm, the mixture obtained in the step S4 is added, the side feeding rotating speed is 20rpm, the glass fiber is added, and the conductive PPS composite material with good epoxy adhesive force is obtained after extrusion granulation.
Comparative example 3
A conductive PPS composite material with good epoxy adhesive force comprises the following components in parts by weight: 300-500g/10min melt index PPS 53 parts, glass fiber 15 parts, conductive carbon black 18 parts, Carbon Nano Tube (CNT)3 parts, carbon fiber 5 parts, epoxy resin 5 parts, coupling agent 0.5 part and release agent 0.5 part.
The preparation method of the conductive PPS composite material with good epoxy adhesive force comprises the following steps:
s1, weighing the raw materials in parts by weight for later use;
s2, adding the PPS and the conductive carbon black into a high-speed mixer at 500rpm, and uniformly mixing at 80 ℃ to obtain a conductive master batch mixture;
s3, setting the temperature of each section of the extruder as follows: setting the screw rotation speed at 260rpm at 290 ℃, 300 ℃, 310 ℃, 300 ℃ and 310 ℃, adding the conductive master batch mixture obtained in the step S1 into the main material port, and performing extrusion granulation at 40rpm to obtain PPS conductive master batches;
s4, adding the PPS conductive master batch prepared in the step S3, the carbon nano tube, the carbon fiber, the epoxy resin, the coupling agent and the release agent into a high-speed mixer with 500rpm, and uniformly mixing at 80 ℃ to obtain a mixture;
s5, setting the temperature of each section of the extruder as follows: 290 ℃, 300 ℃, 310 ℃, 300 ℃ and 310 ℃, the screw rotating speed is set to 260rpm, the main material port feeding rotating speed is 40rpm, the mixture obtained in the step S4 is added, the side feeding rotating speed is 20rpm, the glass fiber is added, and the conductive PPS composite material with good epoxy adhesive force is obtained after extrusion granulation.
Comparative example 4
A conductive PPS composite material with good epoxy adhesive force comprises the following components in parts by weight: 50 parts of 300-DEG 500g/10min melt index PPS, 15 parts of glass fiber, 18 parts of conductive carbon black, 3 parts of Carbon Nano Tube (CNT), 5 parts of carbon fiber, 5 parts of maleic anhydride grafted styrene thermoplastic elastomer, 0.5 part of coupling agent and 0.5 part of release agent.
The preparation method of the conductive PPS composite material with good epoxy adhesive force comprises the following steps:
s1, weighing the raw materials in parts by weight for later use;
s2, adding the PPS and the conductive carbon black into a high-speed mixer at 500rpm, and uniformly mixing at 80 ℃ to obtain a conductive master batch mixture;
s3, setting the temperature of each section of the extruder as follows: setting the screw rotation speed at 260rpm at 290 ℃, 300 ℃, 310 ℃, 300 ℃ and 310 ℃, adding the conductive master batch mixture obtained in the step S1 into the main material port, and performing extrusion granulation at 40rpm to obtain PPS conductive master batches;
s4, adding the PPS conductive master batch prepared in the step S3, the carbon nano tube, the carbon fiber, the maleic anhydride grafted styrene thermoplastic elastomer, the coupling agent and the release agent into a high-speed mixer at 500rpm, and uniformly mixing at 80 ℃ to obtain a mixture;
s5, setting the temperature of each section of the extruder as follows: 290 ℃, 300 ℃, 310 ℃, 300 ℃ and 310 ℃, the screw rotating speed is set to 260rpm, the main material port feeding rotating speed is 40rpm, the mixture obtained in the step S4 is added, the side feeding rotating speed is 20rpm, the glass fiber is added, and the conductive PPS composite material with good epoxy adhesive force is obtained after extrusion granulation.
Comparative example 5
A conductive PPS composite material with good epoxy adhesive force comprises the following components in parts by weight: 49 parts of 300-one 500g/10min melt index PPS, 15 parts of glass fiber, 18 parts of conductive carbon black, 3 parts of Carbon Nano Tube (CNT), 5 parts of carbon fiber, 5 parts of maleic anhydride grafted styrene thermoplastic elastomer and 5 parts of epoxy resin.
The preparation method of the conductive PPS composite material with good epoxy adhesive force comprises the following steps:
s1, weighing the raw materials in parts by weight for later use;
s2, adding the PPS and the conductive carbon black into a high-speed mixer at 500rpm, and uniformly mixing at 80 ℃ to obtain a conductive master batch mixture;
s3, setting the temperature of each section of the extruder as follows: setting the screw rotation speed at 260rpm at 290 ℃, 300 ℃, 310 ℃, 300 ℃ and 310 ℃, adding the conductive master batch mixture obtained in the step S1 into the main material port, and performing extrusion granulation at 40rpm to obtain PPS conductive master batches;
s4, adding the PPS conductive master batch prepared in the step S3, the carbon nano tube, the carbon fiber, the maleic anhydride grafted styrene thermoplastic elastomer and the epoxy resin into a high-speed mixer at 500rpm, and uniformly mixing at 80 ℃ to obtain a mixture;
s5, setting the temperature of each section of the extruder as follows: 290 ℃, 300 ℃, 310 ℃, 300 ℃ and 310 ℃, the screw rotating speed is set to 260rpm, the main material port feeding rotating speed is 40rpm, the mixture obtained in the step S4 is added, the side feeding rotating speed is 20rpm, the glass fiber is added, and the conductive PPS composite material with good epoxy adhesive force is obtained after extrusion granulation.
Comparative example 6
A conductive PPS composite material with good epoxy adhesive force comprises the following components in parts by weight: 300-500g/10min melt index PPS 48 parts, glass fiber 15 parts, conductive carbon black 18 parts, Carbon Nano Tube (CNT)3 parts, carbon fiber 5 parts, maleic anhydride grafted styrene thermoplastic elastomer 5 parts, epoxy resin 5 parts, coupling agent 0.5 part, and release agent 0.5 part
The preparation method of the conductive PPS composite material with good epoxy adhesive force comprises the following steps:
the preparation method of the conductive PPS composite material with good epoxy adhesive force comprises the following steps: uniformly mixing the obtained PPS with conductive carbon black, Carbon Nano Tubes (CNT), carbon fibers, maleic anhydride grafted styrene thermoplastic elastomer, epoxy resin, a coupling agent and a release agent to obtain a mixture, extruding and granulating the mixture through a double-screw extruder, adding glass fibers from a side feed, and setting the temperature of each section of the extruder at the temperature as follows: 290 ℃, 300 ℃, 310 ℃, 300 ℃, 310 ℃ and the screw speed is set to 260 rpm.
In order to further illustrate the technical effects of the present invention, the PPS composite materials of examples 1 to 3 and comparative examples 1 to 6 were subjected to performance tests, and the test results are shown in tables 1.1 and 1.2.
Wherein, the tensile strength test is carried out by adopting a plastic tensile property test method (ISO 527-2); testing the balance water absorption rate by adopting 'determination of impact strength of plastic simply supported beam' (ISO 179); test method for measuring insulation resistance of solid insulation material (IEC 60167) surface resistance test was carried out; and (3) bonding the PPS sample strip by using epoxy glue, and then performing a tensile test to evaluate the epoxy bonding force of the material.
Table 1.1 results of performance testing of conductive PPS composites with good epoxy adhesion for examples 1-3
Item | Example 1 | Example 2 | Example 3 |
Tensile Strength (MPa) | 93 | 102 | 91 |
Notched impact strength (kJ/m)2) | 6.9 | 7.5 | 6.7 |
Surface resistance (Ohm/sq) | 3*104 | 2*103 | 2*104 |
Adhesive force (MPa) | 41.1 | 43.9 | 41.3 |
TABLE 1.2 PA6 composite Performance test results for comparative examples 1-8
As can be seen from the data in tables 1.1 and 1.2, it can be seen from the results of the performance tests of comparative examples 1-3 and comparative example 1 that the tensile strength and the electrical conductivity of examples 1-6 are superior to those of comparative example 1 because the glass fiber reinforcement of examples 1-3 increases the fraction of the conductive filler in the matrix resin, thus the mechanical strength is higher and the electrical conductivity is better.
As can be seen from the data in tables 1.1 and 1.2, it can be seen from the results of the performance tests of comparative examples 1-3 and comparative example 2 that the tensile strength and impact strength of examples 1-3 are significantly higher than those of comparative example 2 because the single conductive carbon black filling used in comparative example 2 requires more carbon black fraction to achieve the same conductive performance as the examples than the conductive carbon black of examples 1-3 and Carbon Nanotube (CNT) and carbon fiber composite filling, resulting in significant decrease in mechanical properties.
As can be seen from the data in tables 1.1 and 1.2, it can be seen from the results of the performance tests of comparative examples 1-3 and comparative example 3 that the epoxy adhesion of examples 1-3 is significantly higher than that of comparative example 3, because examples 1-3 adopt the preferred toughening agent maleic anhydride grafted styrenic thermoplastic elastomer, improving the polarity of the PPS material and thus increasing the epoxy adhesion of the material.
As can be seen from the data in tables 1.1 and 1.2, it can be seen from the results of the performance tests of comparative examples 1-3 and comparative example 4 that the epoxy adhesion of examples 1-3 is significantly higher than that of comparative example 4 because the epoxy resin is selected for examples 1-3 to improve the wettability of the composite material to the epoxy glue, thereby improving the epoxy adhesion of the material.
As can be seen from the data in tables 1.1 and 1.2, it can be seen from the results of the performance tests of comparative examples 1-3 and comparative example 5 that the tensile strength and impact strength of examples 1-3 are significantly better than those of comparative example 5 because the suitable coupling agent and release agent are selected in examples 1-3, which effectively improves the compatibility of the filler and resin and improves the processability of the material.
As can be seen from the data in tables 1.1 and 1.2, it can be seen from the results of the performance tests of comparative examples 1 to 3 and comparative example 6 that the conductive properties of examples 1 to 3 are significantly higher than those of comparative example 6 because the conductive filler is sufficiently dispersed in the resin by the secondary extrusion to improve the conductive properties of the material.
According to the test results, the conductive PPS composite material with good epoxy adhesive force provided by the embodiment of the invention can be prepared by adding glass fiber, conductive carbon black, Carbon Nano Tube (CNT), carbon fiber, toughening agent, epoxy resin, coupling agent and release agent, and the PPS composite material with good epoxy adhesive force and conductive property can be obtained, and the mechanical property is kept good.
On the other hand, the preparation method of the conductive PPS composite material with good epoxy adhesive force provided by the embodiment of the invention effectively ensures the full dispersion of all components, especially conductive filler, through the optimization of a secondary extrusion mode and a processing technology, thereby ensuring that the material has excellent conductive performance, mechanical performance and epoxy adhesive performance.
According to the conductive PPS composite material with good epoxy adhesive force, the polarity of the material is improved and the epoxy adhesive force of the material is improved by introducing the styrene thermoplastic elastomer and the epoxy resin; by introducing low-resistivity conductive carbon black, Carbon Nano Tubes (CNT) and conductive carbon fibers, the electrical property of the material is improved and the conductive level is achieved; by introducing glass fibers, the material is endowed with higher mechanical strength; the mechanical property of the material is improved by introducing a coupling agent; by introducing the release agent, the fluidity of the material is improved, and the processing window of the material is widened. On the other hand, the preparation method of the conductive PPS composite material with good epoxy adhesive force provided by the embodiment of the invention comprises the steps of mixing and extruding the PPS and the conductive carbon black to prepare conductive master batches; then adding the Carbon Nano Tube (CNT), the conductive master batch, the toughening agent, the epoxy resin, the carbon fiber, the coupling agent and the release agent into a high-speed mixer in proportion, uniformly mixing, and adding the glass fiber from a side feed, so that the conductive PPS composite material with good epoxy bonding force is particularly suitable for the application fields with high conductivity and epoxy bonding requirements.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. The conductive PPS composite material with good epoxy adhesive force is characterized by comprising the following components in parts by weight:
30-80 parts of PPS, 10-20 parts of glass fiber, 10-20 parts of conductive carbon black, 1-5 parts of carbon nano tube, 1-10 parts of carbon fiber, 1-10 parts of toughening agent, 1-10 parts of epoxy resin, 0.1-1 part of coupling agent and 0.1-1 part of release agent.
2. A conductive PPS composite material having good epoxy adhesion as claimed in claim 1 wherein the PPS melt index is between 300-500g/10 min.
3. The conductive PPS composite material with good epoxy bonding of claim 1 wherein the glass fiber is PPS specific chopped glass fiber.
4. The conductive PPS composite with good epoxy adhesion as claimed in claim 1 wherein said conductive carbon black has a resistivity < 103Ω·cm。
5. The conductive PPS composite material with good epoxy adhesion as claimed in claim 1 wherein said carbon fiber is a high conductivity and high strength carbon fiber.
6. The conductive PPS composite with good epoxy adhesion as claimed in claim 1, wherein said toughening agent is maleic anhydride grafted styrene type thermoplastic elastomer.
7. The conductive PPS composite material with good epoxy adhesion as claimed in claim 1, wherein the epoxy resin is one or more of bisphenol A epoxy, brominated bisphenol A epoxy, and novolac epoxy.
8. The conductive PPS composite material with good epoxy bonding force as claimed in claim 1, wherein the coupling agent is one or a mixture of two of gamma-aminopropyltriethoxysilane and gamma-glycidoxypropyltrimethoxysilane.
9. The conductive PPS composite material with good epoxy bonding force as claimed in claim 1, wherein the release agent is one or a mixture of two of N, N' -ethylene bis stearamide, silicone powder and fluorine-containing grease.
10. A method for preparing a conductive PPS composite material with good epoxy adhesion as claimed in claims 1-9, comprising the steps of:
s1, weighing PPS, glass fiber, conductive carbon black, carbon nano tubes, carbon fibers, a toughening agent, epoxy resin, a coupling agent and a release agent according to parts by weight for later use;
s2, uniformly mixing the PPS and the conductive carbon black to obtain a conductive master batch mixture;
s3, extruding and granulating the conductive master batch mixture obtained in the step S1 at the rotating speed of 240-300rpm and the temperature of each section of 290-310 ℃ to obtain the PPS conductive master batch;
s4, uniformly mixing the PPS conductive master batch prepared in the step S2 with the carbon nano tube, the carbon fiber, the toughening agent, the epoxy resin, the coupling agent and the release agent to obtain a mixture;
s5, adding the mixture obtained in the step S4 into a main material port of an extruder, adding glass fiber into a side feed, and extruding and granulating at the rotation speed of 240-300rpm and the temperature of 290-310 ℃ in each section to obtain the conductive PPS composite material with good epoxy adhesive force.
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