CN114729185A - Flame-retardant carbon fiber reinforced polyamide composite material, preparation method thereof and preparation method of surface grafted carbon fiber - Google Patents
Flame-retardant carbon fiber reinforced polyamide composite material, preparation method thereof and preparation method of surface grafted carbon fiber Download PDFInfo
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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 fibers, wherein the flame-retardant carbon fiber reinforced polyamide composite material comprises the following components in percentage by weight: 65% -85% of polyamide matrix; 10% -20% of surface grafted carbon fibers, wherein the surface grafted carbon fibers comprise carbon fibers, semi-aromatic polyamide is grafted on the surfaces of the carbon fibers, and the semi-aromatic polyamide is polyamide with a molecular main chain comprising an aromatic ring and an aliphatic chain; 5 to 15 percent of flame retardant. The technical scheme of the application can improve the flame retardant property, the mechanical property and the heat release property of the carbon fiber reinforced polyamide composite material.
Description
Technical Field
The application relates to the field of composite materials, in particular to a flame-retardant carbon fiber reinforced polyamide composite material and a preparation method thereof, and a preparation method of surface grafted carbon fibers.
Background
At present, the research on polymer flame-retardant composite materials for aerospace mainly focuses on thermosetting composite materials, and flame retardant performance can be improved by adding a flame retardant into resin or introducing a high char formation unit, but flame retardant efficiency is not high.
Compared with carbon fiber reinforced thermosetting composite materials, carbon fiber reinforced thermoplastic composite materials (CFRTP) are the mainstream trend of aviation composite material development due to the advantages of light weight, high strength, impact resistance, short molding period, cyclic utilization and the like. Moreover, the CFRTP also has the characteristics of flow processability, low cost, easiness in recycling and the like, and is particularly suitable for manufacturing aviation complex-structure parts.
Disclosure of Invention
The technical problem to be solved by the application is to provide a flame-retardant carbon fiber reinforced polyamide composite material, a preparation method thereof and a preparation method of surface grafted carbon fibers, so that the flame retardant property, the mechanical property and the heat release property of the carbon fiber reinforced polyamide composite material are improved.
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: 65% -85% of polyamide matrix; 10% -20% of surface grafted carbon fibers, wherein the surface grafted carbon fibers comprise carbon fibers, semi-aromatic polyamide is grafted on the surfaces of the carbon fibers, and the semi-aromatic polyamide is polyamide with a molecular main chain comprising an aromatic ring and an aliphatic chain; 5 to 15 percent of flame retardant.
In some embodiments herein, the semi-aromatic polyamide is grafted to the surface of the carbon fiber by a melt blending process.
In some embodiments herein, the semi-aromatic 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, PA12T, and the carbon fibers are inorganic carbon fibers having a carbon content higher than 90% by mass.
In some embodiments of the present 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 fibers and the flame retardant to obtain the flame-retardant carbon fiber reinforced polyamide composite material.
In some embodiments of the present application, the melt blending is performed in a torque rheometer, and the temperature at the time of melt blending is 220 ℃ to 240 ℃, the torque is 50rpm to 80rpm, and the time is 5min to 8 min.
The technical scheme of the application also provides a preparation method of the surface grafted carbon fiber, which comprises the following steps: melting and blending the carbon fiber and the 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 substances; and washing and drying the insoluble substance to obtain the surface grafted semi-aromatic polyamide carbon fiber.
In some embodiments of the present disclosure, the weight ratio of the carbon fibers to the semi-aromatic polyamide when melt blended is (10-20): (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, the melt blending is performed in a torque rheometer, and the temperature of the melt blending is 240-260 ℃, the torque is 50-80 rpm, and the time is 5-8 min; the temperature is 70-80 ℃ during heating and dispersing, and the time is 24-48 h; the temperature during drying is 80-110 ℃, and the time is 24-48 h.
In some embodiments of the present application, the solvent comprises m-cresol.
Compared with the prior art, the technical scheme of the application has the following beneficial effects:
by utilizing a large pi conjugated structure of carbon-carbon six-membered rings regularly arranged in carbon fiber molecules and a pi-pi conjugated effect between benzene rings in the semi-aromatic polyamide, molecular chains of the semi-aromatic polyamide can be grafted to the surface of the carbon fiber only through simple melt blending without carrying out chemical treatment on the surface of the carbon fiber, the molecular structure of the carbon fiber is not damaged, and the excellent mechanical property and thermal property of the carbon fiber are maintained to the greatest extent.
The semi-aromatic polyamide molecular chain in the surface grafting carbon fiber molecular structure has good compatibility with a polyamide matrix material, so that the semi-aromatic polyamide molecular chain can be well dispersed in the matrix material and form a strong-adhesion interface with the matrix, and 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 the mechanical strength of the carbon fiber reinforced polyamide composite material can be effectively improved.
Drawings
Fig. 1 is a schematic flow chart of a method for preparing a surface-grafted carbon fiber according to an embodiment of the present application.
Detailed Description
The following description is presented to enable any person skilled in the art to make and use the present disclosure, and is provided in the context of a particular application and its requirements. Various modifications to the disclosed embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be applied to other embodiments and applications without departing from the spirit and scope of the present 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 problem that the flame retardant performance is improved but the flame retardant efficiency is not high by adding a flame retardant into resin or introducing a high carbon forming unit in the existing thermosetting composite material, 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 fibers, so that the flame retardant performance, the mechanical property and the heat release performance of the carbon fiber reinforced polyamide composite material are comprehensively improved.
Specifically, the flame-retardant carbon fiber reinforced polyamide composite material of the embodiment of the present application includes, by weight: 65 to 85 percent of polyamide matrix, 10 to 20 percent of surface graft carbon fiber and 5 to 15 percent of flame retardant. When the weight ratio of the polyamide matrix, the surface grafted carbon fibers and the flame retardant is in the range, the flame retardant carbon fiber reinforced polyamide composite material has good flame retardant property, mechanical property and heat release property, and the comprehensive performance is optimal.
Wherein the material of the polyamide matrix comprises polyamide, and the polyamide is a polymer containing a repeating amide group (- [ NHCO ] -) in a molecular main chain, abbreviated as PA, for example, the polyamide matrix may comprise at least one of PA6 (nylon 6) and PA66 (nylon 66).
The surface grafted carbon fiber comprises carbon fiber, 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 an aromatic ring and an aliphatic chain. The semi-aromatic polyamide comprises at least one of PA6T, PA9T and PA 12T. The method of grafting the semi-aromatic polyamide on the surface of the carbon fiber may be melt blending. In some embodiments, the semi-aromatic polyamide is prepared from an aromatic diacid and a diamine. In the embodiment of the present application, the carbon fiber is an inorganic carbon fiber in which the mass percentage of carbon element is 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 an interface with strong adhesion, 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 disclosed by the embodiment of the application has both thermal stability and mechanical strength.
Referring to fig. 1, a method for preparing a surface-grafted carbon fiber according to an embodiment of the present application includes:
step S1: melting and blending the carbon fiber and the 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 substances;
step S3: and washing and drying the insoluble substance to obtain the surface grafted semi-aromatic polyamide carbon fiber.
In step S1, since the carbon fiber and the semi-aromatic polyamide are grafted by means of π - π conjugation, but the π - π conjugation is weak, the surface grafting yield of the carbon fiber is low. Therefore, the weight ratio of the carbon fiber and the semi-aromatic polyamide is very important. When the weight ratio of the carbon fiber and the semi-aromatic polyamide in the embodiment of the application is (10-20) to (80-90), the surface grafting ratio of the carbon fiber can reach a proper value. The surface grafting rate of the carbon fiber obtained in 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 is equal to the total mass of the semi-aromatic polyamide grafted onto the carbon fiber/total mass of the carbon fiber × 100%.
In the obtained carbon fiber reinforced semi-aromatic polyamide composite material, the weight percentage of the carbon fiber is 1O% -20%. By controlling the weight ratio of the carbon fiber and the semi-aromatic polyamide at the time of melt blending, it can be ensured that the weight percentage of the carbon fiber is within the above range in the carbon fiber having the semi-aromatic polyamide grafted on the surface thereof.
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 controlled to be 50-80 rpm, and the time is controlled to be 5-8 min, so that the guarantee is provided for the carbon fiber to have higher surface grafting rate. Specifically, the temperature for melt blending should not be too high, which would result in thermal degradation of the material, and too low which would result in excessive viscosity of the molten system. When the torque at the time of melt blending is within the above range, the carbon fiber and the semi-aromatic polyamide can be uniformly blended without being damaged by a shearing force. Too long a time for melt blending results in long-term exposure to heat and shear forces, resulting in thermal or shear degradation of the grafted product, while too short a time results in insufficient grafting, resulting in a lower surface grafting yield. Therefore, the temperature, torque and time during melt blending need to be matched, and any parameter can be adjusted to affect the surface grafting rate.
In step S2, m-cresol is used as a solvent for dispersion, and the insoluble material taken out is carbon fibers having semi-aromatic polyamide grafted to the surface thereof, and the dissolved portion is semi-aromatic polyamide which has not been successfully grafted. The temperature is 70-80 ℃ during heating and dispersing, and the time is 24-48 h. By controlling the parameters, the semi-aromatic polyamide which is not successfully grafted is 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 a raw material for the next grafting.
And step S3, the insoluble substances are cleaned until the cleaning solution is in a clear state and has no turbid substances, and the cleaning can be stopped. And when the cleaned insoluble substance is dried, controlling the temperature to be 80-110 ℃ and the time to be 24-48 h so as to ensure that the structure of the semi-aromatic polyamide carbon fiber grafted on the surface is not damaged.
The preparation method of the flame-retardant carbon fiber reinforced polyamide composite material 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 easy for industrial production. In the embodiment of the application, the melt blending is carried out in a torque rheometer, and the temperature during the melt blending is controlled to be 220-240 ℃, the torque is controlled to be 50-80 rpm, and the time is controlled to be 5-8 min. When the temperature is in the range, the problem of material thermal degradation caused by overhigh temperature is avoided, and the problem that the surface grafted carbon fibers are not easy to disperse due to overhigh melt viscosity is avoided. When the torque is within the range, the problem that the grafting structure is damaged due to excessive shearing force on the surface grafting carbon fiber caused by excessive torque can be better avoided, and finally the surface grafting carbon fiber cannot play a due role. When the torque is small, the shearing force is small, so that the surface grafted carbon fibers, the polyamide matrix and the flame retardant are mixed unevenly, 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, the material is subjected to heat and shear for a long time, and thermal degradation or shear degradation is likely to occur. When the time for melt blending is too short, the effect of mixing and dispersing is also affected.
Example 1
(1) Preparation of surface-grafted carbon fibers
Mixing 10g of carbon fiber and 40g of semi-aromatic polyamide (PA6T) and adding into a Haake torque rheometer, and melting and blending for 8min at 220 ℃ and 50rpm 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 ℃, dispersing for 48 hours by adopting ultrasonic, and taking out insoluble substances, wherein the dissolved semi-aromatic polyamide which does not participate in grafting is dissolved, and the insoluble substances are carbon fibers of which the surfaces are grafted with the semi-aromatic polyamide;
and (3) washing the insoluble substances for more than 10 times by using deionized water, and drying the insoluble substances in a vacuum oven for 48 hours at the temperature of 80 ℃ 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 weight percent of PA6, 20 weight percent of the prepared surface grafted carbon fiber and 15 weight percent of diethyl aluminum phosphinate into a Haake 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 to 6 are shown in Table 1, the melt blending process parameters are shown in Table 2, and the description of the process steps is given 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 description of the process steps is given in example 1.
TABLE 1 formulation 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 composite materials prepared in examples 1-6 and comparative examples 1-6 were tested as follows:
and (3) flame retardant test: the vertical burning time, the vertical burning length and the horizontal burning average rate of the composite material sample are measured according to FAR 25.853 international aviation standard, 10 sample bars are measured for each group of samples, and the average value is taken, and the result is shown in Table 3.
And (3) mechanical testing: the tensile strength, flexural strength, interlaminar shear strength, and post-impact compressive strength of the composite samples were measured with reference to FAR 25.853 International aeronautical Standard, 10 specimens were measured for each set of samples, and the results are shown in Table 3.
Heat release test: the total heat release in the initial 2 minutes and the maximum average heat release rate in the 5 minutes of the composite samples were measured with reference to FAR 25.853 International aeronautical Standard, 10 bars were measured for each set of samples, and the results are given in Table 3.
As can be seen from table 3, after the surface grafting of the semi-aromatic polyamide is performed on the carbon fiber by the blending and 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, the mechanical property and the heat release property of the composite material are remarkably improved, and all the requirements of the FAR 25.853 international aviation standard can be met, so that the flame retardant reinforced carbon fiber polyamide composite material in the embodiment of the present application can be used as a preparation material for structural parts in airliners.
Finally, it should be understood that the embodiments of the application disclosed herein are illustrative of the principles of the embodiments of the present application. Other modified embodiments are also within the scope of the present application. Accordingly, the disclosed embodiments are presented by way of example only, and not limitation. Those skilled in the art may implement the present application in alternative configurations according to the embodiments of the present application. Thus, embodiments of the present application are not limited to those embodiments described with precision in the application.
Claims (11)
1. A flame-retardant carbon fiber reinforced polyamide composite material comprises the following components in percentage by weight:
65% -85% of polyamide matrix;
10% -20% of surface grafted carbon fibers, wherein the surface grafted carbon fibers comprise carbon fibers, semi-aromatic polyamide is grafted on the surfaces of the carbon fibers, and the semi-aromatic polyamide is polyamide with a molecular main chain comprising an aromatic ring and an aliphatic chain;
5 to 15 percent of flame retardant.
2. The flame retardant carbon fiber reinforced polyamide composite material according to claim 1, wherein the semi-aromatic polyamide is grafted on the surface of the carbon fiber by a melt blending method.
3. The flame retardant carbon fiber reinforced polyamide composite material according to claim 2, wherein the 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 polyamide matrix comprises PA6 and/or PA66, the semi-aromatic polyamide comprises at least one of PA6T, PA9T, PA12T, and the carbon fiber is an inorganic carbon fiber with a carbon element mass percentage higher than 90%.
5. The flame retardant carbon fiber reinforced polyamide composite material of claim 1, wherein the flame retardant comprises aluminum diethylphosphinate.
6. A method for producing 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 fibers and the flame retardant to obtain the flame-retardant carbon fiber reinforced polyamide composite material.
7. The preparation method of the flame-retardant carbon fiber reinforced polyamide composite material according to claim 6, characterized in that the melt blending is carried out in a torque rheometer, and the temperature during the melt blending is 220-240 ℃, the torque is 50-80 rpm, and the time is 5-8 min.
8. A preparation method of surface-grafted carbon fibers is characterized by comprising the following steps:
melting and blending the carbon fiber and the 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 substances;
and washing and drying the insoluble substance 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 ratio of the carbon fiber to the semi-aromatic polyamide 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%.
10. The method for preparing the surface-grafted carbon fiber according to claim 8, wherein the melt blending is performed in a torque rheometer, and the temperature during the melt blending is 240 ℃ to 260 ℃, the torque is 50rpm to 80rpm, and the time is 5min to 8 min; the temperature is 70-80 ℃ during heating and dispersing, and the time is 24-48 h; the temperature during drying is 80-110 ℃, and the time is 24-48 h.
11. The method for producing surface-grafted carbon fiber according to claim 8, wherein the solvent comprises m-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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| 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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| WO2023159378A1 (en) | 2023-08-31 |
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