CN116855078A - Slurry for carbon fiber prepreg, preparation method and preparation method of prepreg - Google Patents
Slurry for carbon fiber prepreg, preparation method and preparation method of prepreg Download PDFInfo
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 46
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 45
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 239000002002 slurry Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 57
- 239000000843 powder Substances 0.000 claims abstract description 24
- 239000004094 surface-active agent Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- 229920005992 thermoplastic resin Polymers 0.000 claims abstract description 10
- 239000002612 dispersion medium Substances 0.000 claims abstract description 5
- 239000000725 suspension Substances 0.000 claims abstract description 4
- 229920005989 resin Polymers 0.000 claims description 27
- 239000011347 resin Substances 0.000 claims description 27
- 239000000835 fiber Substances 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000013530 defoamer Substances 0.000 claims description 13
- -1 polyoxyethylene stearate Polymers 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 229920008285 Poly(ether ketone) PEK Polymers 0.000 claims description 7
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 238000007598 dipping method Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000004513 sizing Methods 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 238000012360 testing method Methods 0.000 claims description 6
- 229920012266 Poly(ether sulfone) PES Polymers 0.000 claims description 5
- 238000010907 mechanical stirring Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 239000004034 viscosity adjusting agent Substances 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 239000002041 carbon nanotube Substances 0.000 claims description 4
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 4
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 4
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 4
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 3
- 239000004593 Epoxy Substances 0.000 claims description 3
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 3
- HPTYUNKZVDYXLP-UHFFFAOYSA-N aluminum;trihydroxy(trihydroxysilyloxy)silane;hydrate Chemical compound O.[Al].[Al].O[Si](O)(O)O[Si](O)(O)O HPTYUNKZVDYXLP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000806 elastomer Substances 0.000 claims description 3
- 229920001971 elastomer Polymers 0.000 claims description 3
- 239000000839 emulsion Substances 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 3
- 229910052621 halloysite Inorganic materials 0.000 claims description 3
- 238000007603 infrared drying Methods 0.000 claims description 3
- 239000005543 nano-size silicon particle Substances 0.000 claims description 3
- 239000002071 nanotube Substances 0.000 claims description 3
- 229920000570 polyether Polymers 0.000 claims description 3
- 229920001296 polysiloxane Polymers 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 2
- 150000002170 ethers Chemical class 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000005070 sampling Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000002131 composite material Substances 0.000 abstract description 17
- 229920001169 thermoplastic Polymers 0.000 abstract description 14
- 239000004416 thermosoftening plastic Substances 0.000 abstract description 13
- 239000012752 auxiliary agent Substances 0.000 abstract description 4
- 239000002518 antifoaming agent Substances 0.000 abstract 1
- 239000011159 matrix material Substances 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 13
- 239000004734 Polyphenylene sulfide Substances 0.000 description 7
- 229920000069 polyphenylene sulfide Polymers 0.000 description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 239000004696 Poly ether ether ketone Substances 0.000 description 4
- 239000004697 Polyetherimide Substances 0.000 description 4
- 229920002401 polyacrylamide Polymers 0.000 description 4
- 239000004417 polycarbonate Substances 0.000 description 4
- 229920002530 polyetherether ketone Polymers 0.000 description 4
- 229920001601 polyetherimide Polymers 0.000 description 4
- 230000002787 reinforcement Effects 0.000 description 4
- 238000010008 shearing Methods 0.000 description 4
- 239000001768 carboxy methyl cellulose Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000011229 interlayer Substances 0.000 description 3
- 239000004677 Nylon Substances 0.000 description 2
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 2
- JUPQTSLXMOCDHR-UHFFFAOYSA-N benzene-1,4-diol;bis(4-fluorophenyl)methanone Chemical compound OC1=CC=C(O)C=C1.C1=CC(F)=CC=C1C(=O)C1=CC=C(F)C=C1 JUPQTSLXMOCDHR-UHFFFAOYSA-N 0.000 description 2
- 239000000805 composite resin Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 229920001778 nylon Polymers 0.000 description 2
- 239000012994 photoredox catalyst Substances 0.000 description 2
- 229920000515 polycarbonate Polymers 0.000 description 2
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 2
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 241000218378 Magnolia Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004918 carbon fiber reinforced polymer Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000003733 fiber-reinforced composite Substances 0.000 description 1
- 238000012613 in situ experiment Methods 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000012783 reinforcing fiber Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000008832 zhongfu Substances 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
-
- C—CHEMISTRY; METALLURGY
- 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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
- C08J5/241—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs using inorganic fibres
- C08J5/243—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs using inorganic fibres using carbon fibres
-
- C—CHEMISTRY; METALLURGY
- 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
- C08J2381/00—Characterised by the use 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; Polysulfones; Derivatives of such polymers
- C08J2381/02—Polythioethers; Polythioether-ethers
-
- C—CHEMISTRY; METALLURGY
- 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
- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2471/08—Polyethers derived from hydroxy compounds or from their metallic derivatives
- C08J2471/10—Polyethers derived from hydroxy compounds or from their metallic derivatives from phenols
-
- C—CHEMISTRY; METALLURGY
- 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
- C08J2481/00—Characterised by the use 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; Polysulfones; Derivatives of such polymers
- C08J2481/06—Polysulfones; Polyethersulfones
-
- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Reinforced Plastic Materials (AREA)
Abstract
The application discloses a slurry for carbon fiber prepreg, a preparation method and a preparation method of the prepreg, wherein the slurry is prepared by 1-50% of thermoplastic resin powder, 50-99% of slurry dispersion medium, 0.01-5% of surfactant, 0.01-5% of defoaming agent, 0.01-20% of viscosity regulator, 0.01-5% of modified material A and 5-50% of modified material B by weight, and the carbon fiber prepreg is prepared by a powder suspension method, so that the interfacial compatibility between carbon fiber and thermoplastic resin and the interfacial bonding capability between carbon fiber thermoplastic composite material layers are effectively improved. In addition, the application can improve the toughness of the thermoplastic prepreg and enhance the interface bonding strength of the thermoplastic prepreg by adding less auxiliary agents, thereby improving the comprehensive performance of the prepreg.
Description
Technical Field
The application relates to an auxiliary agent of carbon fiber prepreg and the preparation field thereof, in particular to a slurry for carbon fiber prepreg, a preparation method and a preparation method of prepreg.
Background
The carbon fiber reinforced thermoplastic composite material has excellent performance of replacing metal, is light in weight and high in toughness, is easy to process, and has an application range almost related to various fields of national economy.
The improvement in the properties of carbon fiber reinforced composites depends on the improvement in interfacial bonding strength. Common resin-based composite materials can be structurally divided into three phases: a matrix phase, a reinforcement phase and an interfacial phase. The interface is an extremely important microstructure of the composite material, and is used as a bridge for connecting the reinforcement body and the matrix, and is also used for transmitting stress, so that the physical and mechanical properties of the composite material are greatly influenced. The interface property directly affects various mechanical properties of the composite material, especially the interlayer shearing, fracture, impact resistance and other properties, so that with the development of composite material science and application, the composite material interface and the mechanical behavior thereof are increasingly emphasized.
For reinforced thermoplastic composites, the problem of interfacial bonding is even more important because the matrix itself lacks reactive functionalities, which are difficult to create good chemical bond bonds with the fibers.
Disclosure of Invention
The application aims to: in order to solve the problems in the prior art, the application provides the slurry for the carbon fiber prepreg, the preparation method and the preparation method of the prepreg, and the bonding strength of the thermoplastic carbon fiber prepreg interface is effectively enhanced, so that the comprehensive performance of the thermoplastic carbon fiber prepreg is submitted.
The technical scheme is as follows: in order to achieve the above purpose, the present application adopts the following technical scheme:
the sizing agent for the carbon fiber prepreg is characterized by comprising the following preparation raw materials in parts by weight: 1 to 50 percent of thermoplastic resin powder, 50 to 99 percent of slurry dispersion medium, 0.01 to 5 percent of surfactant, 0.01 to 5 percent of defoamer, 0.01 to 20 percent of viscosity modifier, 0.01 to 5 percent of modified material A and 5 to 50 percent of modified material B.
Further, the thermoplastic resin powder has a density of more than 1g/cm 3 The average powder particle diameter D50 is less than 50 μm.
Further, the thermoplastic resin powder is selected from one or more of nylon PA, polycarbonate PC, polyphenylene sulfide PPS, polyetheretherketone PEEK, polyetherimide PEI.
Further, the slurry dispersion medium is deionized water.
Further, in order to improve the compatibility of the thermoplastic powder with water, the surfactant is one or more of sodium dodecyl sulfonate, sodium dodecyl benzene sulfonate, polyoxyethylene stearate, polyoxyethylene octanol ether, and cetyl trimethyl ammonium bromide.
Further, in order to eliminate bubbles in the slurry, the defoamer is one or more of DOW Corning 1520, QX930T polysiloxane defoamers.
Further, in order to improve the direct compatibility of the fibers with the resin, the modifying material A is specifically selected fromPrime 4983R、/>Emulsion 48625M1、/>One or more of Emulsion91735, hydrosizeTM U6-01, hydrosizeTM U2022, hydrosizeTM PP2-01, hydrosizeTM HP3-02, hydrosizeTM HP-1632, hydroubTM 723, FGLASSM X90, FGLASSM X48.
Further, the modified material A is specificallyPrime 4983R、HydrosizeTM PP2-01、HydrosizeTM U6-01。
More preferably, the modified material a specifically includes: hydrosizeTM U6-01.
In order to improve the toughness of the thermoplastic prepreg and improve the interlaminar shear strength, the modified material B is specifically selected from one or more of carbon nanotubes, halloysite nanotubes, polyether ester elastomers, polyvinyl alcohol, polyether sulfone PES, polyether ketone PEK and nano silicon dioxide particles.
Further, the modified material B is specifically a carbon nanotube, polyethersulfone PES, and polyetherketone PEK, and more preferably, the modified material B is specifically: polyetherketone PEK.
The principle of the synergistic effect of the modified material A and the modified material B is as follows:
common resin-based composite materials can be structurally divided into three phases: a matrix phase, a reinforcement phase and an interfacial phase. The interfacial phase is the tie and stress transfer bridge between the reinforcement and the resin matrix. In general, the contact and infiltration process between the thermoplastic resin matrix and the reinforcing fibers is poor in compatibility with the fibers due to the relatively weak polarity of the thermoplastic resin.
The application improves the interfacial compatibility between the carbon fiber and the resin by selecting the modified material A for addition. The modified material B is mainly made of nano materials, and the other is made of high-toughness materials similar to resin, so that the modified material B can be mixed with a resin matrix in a nano scale when the prepreg is subjected to melt extrusion, and the modified material B serving as a reinforcing effect is fully mixed with the resin matrix. When the prepreg is subjected to stress (the fiber reinforced composite material is subjected to stress mainly by fibers), the stress on the fibers can be transmitted to the resin through the interface layer (the modified material a). The resin matrix can generate corresponding deformation after being stressed, if the deformation of the resin is asynchronous with the deformation of the fiber after being stressed, the reinforced fiber and the resin matrix are separated, namely the fiber and the resin are layered, cracks generated by the layering become stress concentration points, and under the continuous stress loading, the cracks are diffused from the concentration points, so that the finishing performance of the composite material is greatly reduced. The matrix resin can be promoted to be transformed from the brittle material to the ductile material by adding the modified material B, and after the matrix resin is subjected to stress, the deformation (elongation at break) of the resin is greater than or equal to the deformation of the fiber, so that the delamination of the fiber and the matrix resin is avoided.
The application also discloses a preparation method of the sizing agent for the carbon fiber prepreg, which comprises the following steps:
(1) Weighing deionized water, surfactant, defoamer and viscosity regulator according to the proportion, and starting mechanical stirring at 400-1000r/min; after dissolution is completed, sampling is carried out to carry out viscosity test, and whether the viscosity of the slurry is in the range of 0.1-50cps is judged;
(2) Respectively weighing resin powder, a modified material A and a modified material B according to a proportion; slowly adding the materials into the step (1) in batches to fully mix the materials with water; the stirring time is at least 6 hours, and the stirring rotating speed is 400-1000r/min to obtain the needed slurry.
The application also discloses a method for preparing the carbon fiber prepreg by using the slurry, which is prepared by a powder suspension method, wherein the carbon fiber is one or more of domestic conventional carbon fibers, namely SYT-49S, HF-10m, SYT-45S and HF-30 m.
Further, the preparation method comprises the following steps:
(1) Transferring the prepared slurry into a gum dipping tank for standby;
(2) Selecting carbon fibers, installing yarn bundles according to the requirement of producing wide widths, and installing 6-72 carbon fibers;
(3) Carrying out heat treatment on the carbon fiber by a high-temperature infrared oven to remove the epoxy sizing agent on the surface of the fiber;
(4) And adsorbing the slurry in the carbon fiber through a gum dipping tank, removing volatile substances in the slurry through an infrared drying box, and finally heating and extruding the resin powder through a die to infiltrate the fiber to obtain the prepreg.
The beneficial effects are that: the application has the following advantages: 1) The interfacial compatibility between the carbon fiber and the thermoplastic resin and the interfacial bonding capability between the carbon fiber thermoplastic composite material layers are effectively improved. 2) Less auxiliary agent is added, so that the toughness of the thermoplastic prepreg is improved, the interfacial bonding strength of the thermoplastic prepreg is enhanced, and the comprehensive performance of the prepreg is improved. 3) The preparation method of the powder suspension method disperses the auxiliary agent in water in a dissolving or suspending mode, so that the fiber uniformly takes away the corresponding material when absorbing the slurry, and the comprehensive performance of the prepreg is further improved.
Detailed Description
The application is described in further detail below in connection with specific examples:
the sources of the raw materials used in the examples and comparative examples are as follows:
thermoplastic plastics such as nylon PA, polycarbonate PC, polyphenylene sulfide PPS, polyetheretherketone PEEK, polyetherimide PEI, etc. are derived from Shanghai Ubbelo chemical industry limited company such as sodium dodecyl sulfonate, sodium dodecyl benzene sulfonate, polyoxyethylene stearate, polyoxyethylene octanol ethers, cetyl trimethyl ammonium bromide, etc.;
DOW Corning 1520, QX930T polysiloxane defoamer, sodium carboxymethylcellulose (CMC), polyvinyl alcohol (PVA), polyacrylamide (PAM) from Ledong commercial Co., guangzhou;
Prime 4983R、/>Emuls ion 48625M1、/>emuls ion91735, hydrosizeU 6-01, hydrosizeU 2022, hydrosizePP 2-01, hydrosizeHP 3-02, hydrosizeHP-1632, hydroube723, FGLASSM X90, FGLASSM X48 from Michelia New material Co., ltd;
the carbon nanotube halloysite nanotube, polyether ester elastomer, polyvinyl alcohol, polyether sulfone PES, polyether ketone PEK and nano silicon dioxide particles are from Shanghai Guangyun real company;
SYT-49S, SYT-45S was from Zhongfu Shenying eagle carbon fiber Co., ltd;
HF-10m, HF-30m was from Jiangsu Hengshen Co., ltd.
The slurries of examples 1-3 and comparative examples 1-2 were prepared as follows:
example 1:
(1) 75kg of deionized water, 1.0kg of surfactant, 0.5kg of defoamer and 2.0kg of viscosity regulator are weighed into a dispersing barrel, and the mechanical stirring is started, wherein the stirring speed is 700r/min.
Wherein the surfactant is sodium dodecyl sulfonate; the defoamer is DOW Corning 1520; the viscosity modifier is sodium carboxymethyl cellulose.
(2) 25kg of the resin powder, 0.5kg of the modified material A and 10kg of the modified material B were slowly added to (1) in portions, and thoroughly mixed with water, followed by stirring for 12 hours. Wherein the resin powder is polyphenylene sulfide; modified material A selectionPrime 4983R, the modified material B is polyether sulfone PES.
Example 2:
(1) 80kg of deionized water, 0.9kg of surfactant, 0.45kg of defoamer and 1.8kg of viscosity regulator are weighed into a dispersing barrel, and the mechanical stirring is started, wherein the stirring speed is 700r/min.
Wherein the surfactant is sodium dodecyl benzene sulfonate; the defoamer is QX930T; the viscosity modifier is Polyacrylamide (PAM).
(2) 20kg of the resin powder, 0.4kg of the modified material A and 9kg of the modified material B were slowly added to (1) in portions, and thoroughly mixed with water, followed by stirring for 12 hours. Wherein the resin powder is polyphenylene sulfide; the modified material A is HydrosizeTM U6-01, and the modified material B is polyether ketone PEK.
Example 3:
(1) 70kg of deionized water, 1.2kg of surfactant, 0.6kg of defoamer and 2.2kg of viscosity regulator are weighed into a dispersing barrel, and the mechanical stirring is started, wherein the stirring speed is 700r/min.
Wherein the surfactant is polyoxyethylene octanol ether; the defoamer is QX930T; the viscosity modifier is polyvinyl alcohol (PVA).
(2) 30kg of the resin powder, 0.6kg of the modified material A and 11kg of the modified material B were slowly added to (1) in portions, and thoroughly mixed with water, followed by stirring for 12 hours. Wherein the resin powder is polyphenylene sulfide; the modified material A is HydrosizeTM U6-01, and the modified material B is polyether ketone PEK.
Comparative example 1:
other embodiments are substantially the same as in example 1, except that the modifying material B is not added in step (2).
Comparative example 2:
other embodiments are substantially the same as in example 1, except that the modified material a and the modified material B are not added in step (2).
Comparative example 3:
other embodiments are substantially the same as in example 1, except that the modifying material a is not added in step (2).
The preparation method of the thermoplastic prepreg using the slurries prepared in the above example 1 and comparative examples 1 to 3 comprises the following specific steps:
(1) The above-prepared slurries (example 1, comparative examples 1 to 3) were transferred to a dipping tank, respectively, for standby.
(2) SYT49S was selected to produce a wide (150 mm) prepreg, requiring 33 carbon fibers to be installed.
(3) And (3) carrying out heat treatment on the carbon fiber by a high-temperature infrared oven to remove the epoxy sizing agent on the surface of the fiber.
(4) And adsorbing the slurry in the carbon fiber through a gum dipping tank, removing volatile substances in the slurry through an infrared drying box, and finally heating and extruding the resin powder through a die to infiltrate the fiber to obtain the prepreg.
(5) The prepared prepreg is pressed into a plate through a mould pressing process, so that the interlayer shearing performance test is facilitated, and the thickness of the laminated plate is 4mm.
Test method and data:
current methods for characterizing composite interfacial strength fall broadly into three categories: macroscopic experiments of composite materials, micro-composite material experimental methods, in-situ experiments of composite materials and the like. The macroscopic experiment method is to evaluate the interface bonding state of the fiber and the matrix through the macroscopic property of the composite material, and interlayer shearing (short beam shearing) is most commonly used.
The carbon fiber prepregs prepared by the above preparation method using the slurries prepared in example 1 and comparative examples 1-2 were first unidirectional laid-up, and then the prepregs were transferred into a molding press for compression molding, test bars of corresponding specification and size were prepared according to the ISO 14130-1997 standard and tested for interlaminar shear strength. Tensile strength test standard: ISO 527-5.
The specific test result data are shown in table 1:
table 1 comparison of the test results of prepregs prepared in examples and comparative examples
As can be seen from the data of Table 1, compared with comparative example 2, the interlaminar shear strength of both the example 1 and the comparative examples 1 and 3 is significantly improved, and the interlaminar shear strength of the example 1 is 12.6% higher than that of the comparative example 1, and the tensile strength of the prepreg laminated plate is improved by more than 10% in the examples 1 to 3 compared with the comparative examples 1 to 3, wherein the various properties of the example 3 are optimal (explanation: two different substances of fiber and resin, poor interfacial compatibility per se, and the interfacial bonding strength is improved by interfacial modification), thereby improving the tensile properties); the data show that the interface bonding strength of the carbon fiber thermoplastic composite material can be improved to a certain extent by adding the modified material A and the modified material B, and the superposition and use effects of the modified material A and the modified material B are better.
It should be noted that the above-mentioned embodiments illustrate rather than limit the scope of the application, and that those skilled in the art, after reading this disclosure, will be able to modify the application in various equivalent forms within the scope of the application as defined by the appended claims.
Claims (10)
1. The sizing agent for the carbon fiber prepreg is characterized by comprising the following preparation raw materials in parts by weight: 1 to 50 percent of thermoplastic resin powder, 50 to 99 percent of slurry dispersion medium, 0.01 to 5 percent of surfactant, 0.01 to 5 percent of defoamer, 0.01 to 20 percent of viscosity modifier, 0.01 to 5 percent of modified material A and 5 to 50 percent of modified material B.
2. The slurry for carbon fiber prepregs according to claim 1, characterized in that: the thermoplastic resin powder has a high densityAt 1g/cm 3 The average powder particle diameter D50 is less than 50 μm.
3. The slurry for carbon fiber prepregs according to claim 1, characterized in that: the slurry dispersion medium is deionized water.
4. The slurry for carbon fiber prepregs according to claim 1, characterized in that: the surfactant is one or more of sodium dodecyl sulfonate, sodium dodecyl benzene sulfonate, polyoxyethylene stearate, polyoxyethylene octanol ethers and cetyl trimethyl ammonium bromide.
5. The slurry for carbon fiber prepregs according to claim 1, characterized in that: the defoamer is one or more of DOW Corning 1520 and QX930T polysiloxane defoamers.
6. The slurry for carbon fiber prepregs according to claim 1, characterized in that: the modifying material A is specifically selected fromPrime 4983R、/>Emulsion 48625M1、/>One or more of Emulsion91735, hydrosizeTM U6-01, hydrosizeTM U2022, hydrosizeTM PP2-01, hydrosizeTM HP3-02, hydrosizeTM HP-1632, hydroubTM 723, FGLASSM X90, FGLASSM X48.
7. The slurry for carbon fiber prepregs according to claim 1, characterized in that: the modified material B is specifically selected from one or more of carbon nanotube halloysite nanotubes, polyether ester elastomer, polyvinyl alcohol, polyether sulfone PES, polyether ketone PEK and nano silicon dioxide particles.
8. A method for preparing the slurry for carbon fiber prepreg according to claim 1, comprising the steps of:
(1) Weighing deionized water, surfactant, defoamer and viscosity regulator according to the proportion, and starting mechanical stirring at 400-1000r/min; after dissolution is completed, sampling is carried out to carry out viscosity test, and whether the viscosity of the slurry is in the range of 0.1-50cps is judged;
(2) Respectively weighing resin powder, a modified material A and a modified material B according to a proportion; slowly adding the materials into the step (1) in batches to fully mix the materials with water; the stirring time is at least 6 hours, and the stirring rotating speed is 400-1000r/min to obtain the needed slurry.
9. A method for preparing a carbon fiber prepreg by using the slurry according to claim 1, which is characterized in that the preparation is carried out by adopting a powder suspension method, and the carbon fiber is one or more of domestic conventional carbon fibers, in particular SYT-49S, HF-10m, SYT-45S and HF-30 m.
10. The method for producing a carbon fiber prepreg according to claim 9, wherein:
(1) Transferring the prepared slurry into a gum dipping tank for standby;
(2) Selecting carbon fibers, installing yarn bundles according to the requirement of producing wide widths, and installing 6-72 carbon fibers;
(3) Carrying out heat treatment on the carbon fiber by a high-temperature infrared oven to remove the epoxy sizing agent on the surface of the fiber;
(4) And adsorbing the slurry in the carbon fiber through a gum dipping tank, removing volatile substances in the slurry through an infrared drying box, and finally heating and extruding the resin powder through a die to infiltrate the fiber to obtain the prepreg.
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