CN114729185B - Flame-retardant carbon fiber reinforced polyamide composite material and preparation method thereof, and preparation method of surface grafted carbon fiber - Google Patents
Flame-retardant carbon fiber reinforced polyamide composite material and preparation method thereof, and preparation method of surface grafted carbon fiber Download PDFInfo
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- CN114729185B CN114729185B CN202280000287.0A CN202280000287A CN114729185B CN 114729185 B CN114729185 B CN 114729185B CN 202280000287 A CN202280000287 A CN 202280000287A CN 114729185 B CN114729185 B CN 114729185B
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- 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
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/59—Polyamides; Polyimides
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- 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
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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- 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
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/06—Polyamides derived from polyamines and polycarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/53—Phosphorus bound to oxygen bound to oxygen and to carbon only
- C08K5/5313—Phosphinic compounds, e.g. R2=P(:O)OR'
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- 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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- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
Abstract
The application provides a flame-retardant carbon fiber reinforced polyamide composite material, a preparation method thereof and a preparation method of surface grafted carbon fiber, wherein the flame-retardant carbon fiber reinforced polyamide composite material comprises the following components in percentage by weight: polyamide matrix, 65% -85%; 10% -20% of surface grafted carbon fiber, wherein the surface grafted carbon fiber comprises carbon fiber, and semi-aromatic polyamide is grafted on the surface of the carbon fiber, and the semi-aromatic polyamide is polyamide with a molecular main chain comprising aromatic rings and aliphatic chains; 5 to 15 percent of flame retardant. According to the technical scheme, the flame retardant property, the mechanical property and the heat release property of the carbon fiber reinforced polyamide composite material can be improved.
Description
Technical Field
The application relates to the field of composite materials, in particular to a flame-retardant carbon fiber reinforced polyamide composite material, a preparation method thereof and a preparation method of surface grafted carbon fiber.
Background
At present, research on polymer flame-retardant composite materials for aerospace mainly focuses on thermosetting composite materials, and flame retardant performance can be improved but flame retardant efficiency is not high through adding flame retardant into resin or introducing high-carbon forming units.
Compared with carbon fiber reinforced thermosetting composite materials, carbon fiber reinforced thermoplastic composite materials (CFRTP) become a mainstream trend of aviation composite material development due to the advantages of light weight, high strength, impact resistance, short molding cycle, recycling and the like. In addition, CFRTP has the characteristics of flow processability, low cost, easy recovery and the like, and is particularly suitable for manufacturing aviation complex structure parts.
Disclosure of Invention
The application solves the technical problem of providing a flame-retardant carbon fiber reinforced polyamide composite material, a preparation method thereof and a preparation method of surface grafted carbon fiber, and improves the flame retardance, mechanical property and heat release property of the carbon fiber reinforced polyamide composite material.
The technical problem is not solved, and the technical scheme of the application provides a flame-retardant carbon fiber reinforced polyamide composite material, which comprises the following components in percentage by weight: polyamide matrix, 65% -85%; 10% -20% of surface grafted carbon fiber, wherein the surface grafted carbon fiber comprises carbon fiber, and semi-aromatic polyamide is grafted on the surface of the carbon fiber, and the semi-aromatic polyamide is polyamide with a molecular main chain comprising aromatic rings and aliphatic chains; 5 to 15 percent of flame retardant.
In some embodiments of the application, the semiaromatic polyamide is grafted onto the surface of the carbon fiber by melt blending.
In some embodiments of the application, the semiaromatic polyamide is prepared from an aromatic diacid and a diamine.
In some embodiments of the present application, the polyamide matrix comprises PA6 and/or PA66, the semi-aromatic polyamide comprises at least one of PA6T, PA9T, PA T, and the carbon fibers are inorganic carbon fibers with a mass percentage of carbon elements higher than 90%.
In some embodiments of the application, the flame retardant comprises aluminum diethylphosphinate.
The technical scheme of the application also provides a preparation method of the flame-retardant carbon fiber reinforced polyamide composite material, which comprises the following steps: and carrying out melt blending on the polyamide matrix, the surface grafted carbon fiber and the flame retardant to obtain the flame-retardant carbon fiber reinforced polyamide composite material.
In some embodiments of the application, melt blending is performed in a torque rheometer and the temperature at which the melt blending occurs is 220 ℃ to 240 ℃ and the torque is 50rpm to 80rpm for 5 minutes to 8 minutes.
The technical scheme of the application also provides a preparation method of the surface grafted carbon fiber, which comprises the following steps: melt blending carbon fiber and semi-aromatic polyamide to obtain a carbon fiber reinforced semi-aromatic polyamide composite material; adding the carbon fiber reinforced semi-aromatic polyamide composite material into a solvent for heating and dispersing, and taking out insoluble matters; and cleaning and drying the insoluble matters to obtain the surface grafted semi-aromatic polyamide carbon fiber.
In some embodiments of the application, the weight ratio of the carbon fiber to the semiaromatic polyamide when melt blended is (10-20) to (80-90); in the obtained carbon fiber reinforced semi-aromatic polyamide composite material, the weight percentage of the carbon fiber is 10-20%.
In some embodiments of the application, melt blending is performed in a torque rheometer and the temperature at which the melt blending occurs is 240 ℃ to 260 ℃, the torque is 50rpm to 80rpm, and the time is 5 minutes to 8 minutes; the temperature during heating and dispersing is 70-80 ℃ and the time is 24-48 h; the temperature is 80-110 ℃ and the time is 24-48 h during drying.
In some embodiments of the application, the solvent comprises m-cresol.
Compared with the prior art, the technical scheme of the application has the following beneficial effects:
the large pi conjugated structure of carbon-carbon six-membered rings orderly arranged in carbon fiber molecules and pi-pi conjugated effect between benzene rings in semi-aromatic polyamide are utilized, and the semi-aromatic polyamide molecular chains can be grafted to the carbon fiber surfaces only through simple melt blending, so that the carbon fiber surfaces are not required to be subjected to chemical treatment, the carbon fiber molecular structures are not damaged, and the excellent mechanical properties and thermal properties of the carbon fibers are maintained to the greatest extent.
The semi-aromatic polyamide molecular chain is arranged in the surface grafted carbon fiber molecular structure, and has good compatibility with polyamide matrix material, so that the semi-aromatic polyamide molecular chain can be well dispersed in the matrix material and forms a strong interface with the matrix, thereby the composite material has outstanding impact resistance.
The semi-aromatic polyamide with low heat release and high mechanical strength is introduced, so that the thermal stability and mechanical strength of the carbon fiber reinforced polyamide composite material can be effectively improved.
Drawings
Fig. 1 is a schematic flow chart of a preparation method of a surface grafted carbon fiber according to an embodiment of the application.
Detailed Description
The following description provides specific applications and requirements of the application to enable any person skilled in the art to make and use the application. Various modifications to the disclosed embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments and applications without departing from the spirit and scope of the application. Thus, the present application is not limited to the embodiments shown, but is to be accorded the widest scope consistent with the claims.
Based on the problems that the existing thermosetting composite material has high flame retardant performance by adding a flame retardant into resin or introducing a high carbon forming unit, but has low flame retardant efficiency, the embodiment of the application provides a flame retardant carbon fiber reinforced polyamide composite material, a preparation method thereof and a preparation method of surface grafted carbon fiber, so as to comprehensively improve the flame retardant performance, mechanical performance and heat release performance of the carbon fiber reinforced polyamide composite material.
Specifically, the flame-retardant carbon fiber reinforced polyamide composite material of the embodiment of the application comprises the following components in percentage by weight: 65-85% of polyamide matrix, 10-20% of surface grafted carbon fiber and 5-15% of flame retardant. When the weight ratio of the polyamide matrix to the surface grafted carbon fiber to the flame retardant is in the range, the flame retardant carbon fiber reinforced polyamide composite material has better flame retardant property, mechanical property and heat release property and optimal comprehensive performance.
Wherein the material of the polyamide matrix comprises polyamide, and the polyamide is a polymer containing repeated amide groups (- [ NHCO ] -) on the molecular main chain, called PA for short, and for example, the polyamide matrix can comprise at least one of PA6 (nylon 6) and PA66 (nylon 66).
The surface grafted carbon fiber comprises carbon fiber, and semi-aromatic polyamide is grafted on the surface of the carbon fiber, wherein the semi-aromatic polyamide is polyamide with a molecular main chain comprising an aromatic ring and an aliphatic chain. The semiaromatic polyamide comprises at least one of PA6T, PA9T, PA T. The method of grafting the semiaromatic polyamide on the surface of the carbon fiber may be melt blending. In some embodiments, the semiaromatic polyamide is prepared from an aromatic diacid and a diamine. In the embodiment of the application, the carbon fibers are inorganic carbon fibers with the mass percentage of carbon elements higher than 90%. The inorganic carbon fibers include acrylonitrile-based carbon fibers. The flame retardant comprises aluminum diethylphosphinate.
In the flame-retardant carbon fiber reinforced polyamide composite material provided by the embodiment of the application, the carbon fiber with the semi-aromatic polyamide grafted on the surface is introduced, and the semi-aromatic polyamide molecular chain has good compatibility in the matrix material, so that the surface grafted carbon fiber can be well dispersed in the polyamide matrix, and meanwhile, the surface grafted carbon fiber and the polyamide matrix form a strong-adhesion interface, so that the flame-retardant carbon fiber reinforced polyamide composite material provided by the embodiment of the application has good impact resistance. In addition, the semi-aromatic polyamide molecular chain grafted on the surface can provide low heat release and high mechanical strength, so that the flame-retardant carbon fiber reinforced polyamide composite material provided by the embodiment of the application has both thermal stability and mechanical strength.
Referring to fig. 1, the preparation method of the surface grafted carbon fiber according to the embodiment of the application includes:
step S1: melt blending carbon fiber and semi-aromatic polyamide to obtain a carbon fiber reinforced semi-aromatic polyamide composite material;
step S2: adding the carbon fiber reinforced semi-aromatic polyamide composite material into a solvent for heating and dispersing, and taking out insoluble matters;
step S3: and cleaning and drying the insoluble matters to obtain the surface grafted semi-aromatic polyamide carbon fiber.
In step S1, since the carbon fiber and the semiaromatic polyamide are grafted by pi-pi conjugation, but the pi-pi conjugation is weak, the surface grafting rate of the carbon fiber is low. Therefore, the weight ratio of carbon fiber to semi-aromatic polyamide is extremely important. When the weight ratio of the carbon fiber to the semi-aromatic polyamide is (10-20) to (80-90) in the melt blending process, the surface grafting rate of the carbon fiber can reach a proper value. The surface grafting rate of the carbon fiber obtained by the embodiment of the application is about 5%, for example, the surface grafting rate of the carbon fiber is 4% -6%. The surface grafting ratio = total mass of semi-aromatic polyamide grafted onto carbon fiber/total mass of carbon fiber x 100%.
In the obtained carbon fiber reinforced semi-aromatic polyamide composite material, the weight percentage of the carbon fiber is 1-20%. By controlling the weight ratio of the carbon fiber and the semiaromatic polyamide at the time of melt blending, it is possible to ensure that the weight percentage of the carbon fiber in the carbon fiber having the semiaromatic polyamide grafted on the surface is within the above-described range.
In some embodiments, the melt blending is performed in a torque rheometer, and the temperature during the melt blending is controlled to be 240-260 ℃, the torque is 50-80 rpm, and the time is 5-8 min, so that the guarantee is provided for the carbon fiber with higher surface grafting rate. In particular, the temperature during melt blending is not too high, which can lead to thermal degradation of the material, while too low a temperature can result in excessive viscosity of the melt system. When the torque during melt blending is within the above range, the carbon fibers can be uniformly blended with the semiaromatic polyamide while the carbon fibers are not broken by the shearing force. If the time is too long, the material can be heated for a long time and the shearing force acts, so that the grafted product is thermally degraded or sheared and degraded, and if the time is too short, insufficient grafting can be caused, and the surface grafting rate is lower. Therefore, the temperature, torque and time during melt blending need to be matched with each other, and the surface grafting rate can be influenced by adjusting any one of the parameters.
In the step S2, m-cresol is used as a solvent for dispersion, the insoluble matters are carbon fibers of which the surfaces are grafted with semi-aromatic polyamide, and the dissolved parts are the semi-aromatic polyamide which is not grafted successfully. The temperature during heating and dispersing is 70-80 ℃ and the time is 24-48 h. By controlling the parameters, the semi-aromatic polyamide which is not grafted successfully is ensured to be fully dissolved, and the purity of the product is improved. The semi-aromatic polyamide which is not grafted successfully can be recycled and used as the raw material for the next grafting.
And step S3, cleaning the insoluble matters until the cleaning liquid is in a clear state and has no turbid matters, and stopping cleaning. When the cleaned insoluble matters are dried, the temperature is controlled to be 80-110 ℃ and the time is controlled to be 24-48 hours, so that the structure of the surface grafted semi-aromatic polyamide carbon fiber is not damaged.
The preparation method of the flame-retardant carbon fiber reinforced polyamide composite material provided by the embodiment of the application comprises the following steps: and carrying out melt blending on the polyamide matrix, the surface grafted semi-aromatic polyamide carbon fiber and the flame retardant to obtain the flame-retardant carbon fiber reinforced polyamide composite material. The preparation method is simple and is easy for industrial production. In the embodiment of the application, the melt blending is performed in a torque rheometer, and the temperature during the melt blending is controlled to be 220-240 ℃, the torque is 50-80 rpm, and the time is 5-8 min. When the temperature is in the range, the problem of thermal degradation of the material caused by overhigh temperature is avoided, and the problem that the surface grafted carbon fiber is not easy to disperse due to overlarge melt viscosity is avoided. When the torque is within the above range, the problem that the grafting structure of the surface grafted carbon fiber is damaged due to the overlarge shearing force caused by overlarge torque can be well avoided, and finally the surface grafted carbon fiber cannot play a role. When the torque is smaller, the shearing force is smaller, so that the surface grafted carbon fiber, the polyamide matrix and the flame retardant are unevenly mixed, and the comprehensive performance of the final flame-retardant carbon fiber reinforced polyamide composite material is also affected. When the time for melt blending is too long, it results in a material that is subject to long-term heating and shearing, and is susceptible to thermal or shear degradation. When the time for melt blending is too short, the mixing and dispersing effects are also affected.
Example 1
(1) Preparation of surface grafted carbon fiber
10g of carbon fiber and 40g of semi-aromatic polyamide (PA 6T) are mixed and added into a Hash torque rheometer, and melt blending is carried out for 8 minutes under the conditions of 220 ℃ and 50rpm, so as to obtain a carbon fiber reinforced semi-aromatic polyamide composite material;
grinding the carbon fiber reinforced semi-aromatic polyamide composite material into powder in a grinder, adding the powder into m-cresol, heating to 70 ℃, performing ultrasonic dispersion for 48 hours, and taking out insoluble matters, wherein the insoluble matters are the semi-aromatic polyamide which does not participate in grafting, and the insoluble matters are the carbon fibers of which the surfaces are grafted with the semi-aromatic polyamide;
and (3) cleaning insoluble matters by deionized water for more than 10 times, and placing the insoluble matters in a vacuum oven, and drying the insoluble matters at 80 ℃ for 48 hours to obtain the surface grafted semi-aromatic polyamide carbon fiber with the grafting rate of 5%.
(2) Preparation of flame-retardant carbon fiber reinforced polyamide composite material
Adding 65% by weight of PA6 and 20% by weight of the prepared surface grafted carbon fiber and 15% by weight of diethyl phosphinic acid aluminum into a Hark torque rheometer, and carrying out melt blending for 5min at 220 ℃ and 50rpm to obtain the flame-retardant carbon fiber reinforced polyamide composite material.
Examples 2 to 6
The formulations of examples 2-6 are shown in Table 1, the melt blending process parameters are shown in Table 2, and the process steps are described in example 1.
Comparative examples 1 to 6
The formulations of comparative examples 1 to 6 are shown in Table 1, the melt blending process parameters are shown in Table 2, and the process steps are described in example 1.
Table 1 formulations of examples and comparative examples
Table 2 melt blending process parameters for examples and comparative examples
The flame retardant properties, mechanical properties and thermal properties of the composites prepared in examples 1 to 6 and comparative examples 1 to 6 were tested as follows:
flame retardant test: referring to FAR 25.853 international aviation standards, the vertical burn time, vertical char length, horizontal burn average rate of the composite samples were measured, 10 bars were measured for each group of samples, and the average was taken and the results are shown in table 3.
Mechanical testing: with reference to FAR 25.853 international aviation standards, the tensile strength, flexural strength, interlaminar shear strength, compressive strength after impact of the composite material samples were measured, 10 bars were measured for each group of samples, and the average was taken and the results are shown in table 3.
Heat release test: referring to the FAR 25.853 international aviation standard, the total heat release during the initial 2 minutes and the maximum average heat release rate during 5 minutes of the composite samples were measured, 10 bars were measured for each group of samples, and the average was taken, and the results are shown in table 3.
As can be seen from table 3, after the surface grafting of the semi-aromatic polyamide on the carbon fiber by adopting the blending melting process, the semi-aromatic polyamide and the polyamide matrix have good compatibility, so that the carbon fiber is well dispersed in the polyamide matrix, the interfacial adhesion between the carbon fiber and the polyamide matrix is improved, and the semi-aromatic polyamide with high heat resistance, high impact resistance and low heat release is introduced, so that the flame retardant property, mechanical property and heat release property of the composite material are remarkably improved, and all the FAR 25.853 international aviation standard can be met, so that the flame retardant carbon fiber reinforced polyamide composite material of the embodiment of the application can be used as the preparation material of structural parts in a passenger plane.
Finally, it is to be understood that the embodiments of the application disclosed herein are illustrative of the principles of embodiments of the present application. Other modified embodiments are also within the scope of the application. Accordingly, the disclosed embodiments are illustrative only and not limiting. Those skilled in the art can adopt alternative configurations to implement the application of the present application according to embodiments of the present application. Accordingly, embodiments of the application are not limited to those precisely described in the application.
Claims (11)
1. A flame retardant carbon fiber reinforced polyamide composite material comprising, in weight percent:
a polyamide matrix, 65% -85%, wherein the polyamide matrix comprises PA6 and/or PA66;
1-20% of surface grafted carbon fiber, wherein the surface grafted carbon fiber comprises carbon fiber, the surface of the carbon fiber is grafted with semi-aromatic polyamide, the semi-aromatic polyamide is polyamide with a molecular main chain comprising aromatic rings and aliphatic chains, and the surface grafting rate of the carbon fiber is 4-6%;
5% -15% of flame retardant;
and carrying out melt blending on the polyamide matrix, the surface grafted carbon fiber and the flame retardant to obtain the flame-retardant carbon fiber reinforced polyamide composite material, wherein the temperature is 220-240 ℃ and the torque is 50-80 rpm during melt blending, and the time is 5-8 min.
2. The flame retardant carbon fiber reinforced polyamide composite material according to claim 1, wherein said semi-aromatic polyamide is grafted on the surface of said carbon fiber by a melt blending method.
3. The flame retardant carbon fiber reinforced polyamide composite material according to claim 2, wherein said semi-aromatic polyamide is prepared from an aromatic diacid and a diamine.
4. The flame retardant carbon fiber reinforced polyamide composite material according to claim 1, wherein the semi-aromatic polyamide comprises at least one of PA6T, PA9T, PA T, and the carbon fiber is an inorganic carbon fiber with a mass percentage of carbon element higher than 90%.
5. The flame retardant carbon fiber reinforced polyamide composite material according to claim 1, wherein said flame retardant comprises aluminum diethylphosphinate.
6. A method of preparing a flame retardant carbon fiber reinforced polyamide composite material according to any one of claims 1 to 5, comprising: and carrying out melt blending on the polyamide matrix, the surface grafted carbon fiber and the flame retardant to obtain the flame-retardant carbon fiber reinforced polyamide composite material, wherein the temperature is 220-240 ℃ and the torque is 50-80 rpm during melt blending, and the time is 5-8 min.
7. The method of preparing a flame retardant carbon fiber reinforced polyamide composite material according to claim 6 wherein the melt blending is performed in a torque rheometer.
8. The preparation method of the surface grafted carbon fiber is characterized by comprising the following steps:
melt blending carbon fiber and semi-aromatic polyamide to obtain a carbon fiber reinforced semi-aromatic polyamide composite material, wherein the weight ratio of the carbon fiber to the semi-aromatic polyamide when melt blended is (10-20): (80-90), the temperature during melt blending is 240-260 ℃, the torque is 50-80 rpm, and the time is 5-8 min;
adding the carbon fiber reinforced semi-aromatic polyamide composite material into a solvent for heating and dispersing, and taking out insoluble matters;
and cleaning and drying the insoluble matters to obtain the surface grafted semi-aromatic polyamide carbon fiber.
9. The method for preparing surface grafted carbon fiber according to claim 8, wherein the weight percentage of carbon fiber in the obtained carbon fiber reinforced semi-aromatic polyamide composite material is 10% -20%.
10. The method for preparing surface grafted carbon fiber according to claim 8, wherein the temperature during heating and dispersing is 70-80 ℃ for 24-48 hours; the temperature is 80-110 ℃ and the time is 24-48 h during drying.
11. The method for preparing surface-grafted carbon fiber according to claim 8, wherein the solvent comprises meta-cresol.
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| PCT/CN2022/077429 WO2023159378A1 (en) | 2022-02-23 | 2022-02-23 | Flame-retardant carbon fiber reinforced polyamide composite material and preparation method therefor, and preparation method for surface grafted carbon fiber |
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| JP2018053089A (en) * | 2016-09-28 | 2018-04-05 | 富士ゼロックス株式会社 | Resin composition and resin molded material |
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| JP5606650B2 (en) * | 2012-03-09 | 2014-10-15 | 帝人株式会社 | Carbon fiber bundle and manufacturing method thereof |
| US20130309491A1 (en) * | 2012-05-15 | 2013-11-21 | Satoshi Seike | Milled carbon fiber |
| CN106978728A (en) * | 2013-03-06 | 2017-07-25 | 住友精化株式会社 | Fibre finish, the carbon fiber handled with fibre finish and the carbon fibre composite containing the carbon fiber |
| US20160090685A1 (en) * | 2014-09-25 | 2016-03-31 | E I Du Pont De Nemours And Company | Carbon fibers |
| US10072141B2 (en) * | 2015-08-04 | 2018-09-11 | Fuji Xerox Co., Ltd. | Resin composition, resin molded article, and method of preparing resin composition |
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2022
- 2022-02-23 CN CN202280000287.0A patent/CN114729185B/en active Active
- 2022-02-23 WO PCT/CN2022/077429 patent/WO2023159378A1/en unknown
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS53106752A (en) * | 1977-03-02 | 1978-09-18 | Toho Rayon Co Ltd | Reinforcing material and its composition for molding product |
| JPH03113075A (en) * | 1989-09-27 | 1991-05-14 | Takemoto Oil & Fat Co Ltd | Surface coating method for carbon fiber and surface-coated carbon fiber |
| JPH07310286A (en) * | 1994-05-13 | 1995-11-28 | Mitsui Toatsu Chem Inc | Carbon fiber for reinforcing highly heat-resistant resin and its resin composition |
| CN103993484A (en) * | 2013-02-18 | 2014-08-20 | 金发科技股份有限公司 | Carbon-fiber-surface modifying emulsion, preparation method thereof, and modified carbon fiber and polyamide complex prepared from same |
| JP2018053089A (en) * | 2016-09-28 | 2018-04-05 | 富士ゼロックス株式会社 | Resin composition and resin molded material |
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| CN114729185A (en) | 2022-07-08 |
| WO2023159378A1 (en) | 2023-08-31 |
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