A flame-resistant high-performance fiber composite material and its preparation method
By combining modified basalt fiber with phenolic fiber and polyimide fiber, a three-dimensional network structure is constructed, which solves the problem of insufficient flame retardancy of polyamide materials and achieves efficient flame retardant effect and improved safety.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-21
- Publication Date
- 2026-04-03
AI Technical Summary
Existing polyamide materials have insufficient flame retardancy, making them flammable and prone to continuous combustion in flames, producing a large amount of black smoke, which threatens safety. Existing flame retardants are ineffective and pose environmental hazards.
A composite of modified basalt fiber, phenolic fiber, and polyimide fiber is used. By coating the surface of the basalt fiber with aluminum phosphate to form a flame-retardant layer, a three-dimensional network structure is constructed during combustion. Combined with interface compatibilizers and flame retardants, a physical barrier is formed to hinder the diffusion of heat and oxygen.
It significantly improves the flame retardancy of the material, slows down heat transfer and oxygen diffusion, forms a dense char layer to isolate combustion, enhances low-temperature resistance and chemical corrosion resistance, reduces the release of combustible gases, and strengthens char formation and thermal shock resistance.
Abstract
Description
Technical Field
[0001] This invention relates to the field of fiber composite materials technology, and in particular to a flame-resistant high-performance fiber composite material and its preparation method. Background Technology
[0002] Polyamide (PA), also known as nylon, is a class of polymeric compounds formed through the condensation reaction of diacids and diamines. Its molecular backbone is rich in amide bonds (-CONH-). As one of the core materials in the field of engineering plastics, polyamide has been widely used in many key areas such as electronics, automotive manufacturing, aerospace, rail transportation, and consumer goods due to its excellent comprehensive properties. For example, in the electronics field, polyamide is often used to manufacture precision components such as connectors, switches, and relay housings; in the automotive industry, it can be used for engine peripheral parts, gears, bearings, and other components requiring high heat resistance and wear resistance; in the industrial transmission field, polyamide gears, pulleys, and other products can significantly reduce equipment energy consumption due to their low coefficient of friction and high self-lubricating properties.
[0003] However, with the continuous expansion of polyamide applications, the requirements for its flame retardancy are becoming increasingly stringent. The insufficient flame retardancy of polyamide is mainly due to its inherently poor flame retardancy caused by its molecular structure. On the one hand, although the amide bond (-CONH-) is highly polar, it does not contain typical flame-retardant elements such as halogens, phosphorus, and silicon, and therefore cannot inhibit combustion reactions through intramolecular interactions. On the other hand, polyamide decomposes and releases small molecule flammable substances (such as ammonia and low-carbon hydrocarbons) under high temperatures or flame conditions. Simultaneously, its significant melting and dripping phenomenon easily ignites surrounding materials, leading to the spread of fire. Experimental data shows that the limiting oxygen index (LOI) of unmodified polyamide is typically only 20%-24% (the oxygen concentration in air is approximately 21%), classifying it as a typical flammable material. It is prone to continuous combustion in a flame, producing large amounts of black smoke, seriously threatening safety.
[0004] In existing technologies, flame retardants are often added to improve the flame retardant properties of polyamides. However, existing flame retardants for polyamides often have problems such as poor flame retardant effect, large dosage, and environmental hazards. Summary of the Invention
[0005] In view of the shortcomings of the prior art described above, the purpose of this invention is to provide a flame-retardant high-performance fiber composite material and its preparation method, so as to solve the problem of insufficient flame retardancy of fiber composite materials in the prior art.
[0006] To achieve the above and other related objectives, the present invention is obtained through the following technical solution.
[0007] The first aspect of this invention is to provide a flame-retardant high-performance fiber composite material, comprising the following raw materials in parts by weight: 100 parts polyamide resin, 30-60 parts composite fiber, 0.4-0.5 parts antioxidant, 10-18 parts flame retardant, 1-2 parts interface compatibilizer, 0.5-1 part lubricant, and 0.5-1 part zinc borate; wherein the flame retardant comprises diatomaceous earth, aluminum diethylphosphinate, and polyphosphoramide; wherein the composite fiber comprises modified basalt fiber, phenolic fiber, and polyimide fiber; and wherein the method for preparing the modified basalt fiber comprises the following steps:
[0008] S1. Mix basalt fiber acidic solution, aluminum hydroxide, phosphoric acid and water, adjust the pH to 4-5 and react to obtain the first basalt fiber;
[0009] S2. Add 4,4'-(3-triethoxysilylpropoxy)azobenzene to ethanol to prepare a treatment solution, add the first basalt fiber, and stir under ultrasonic conditions for 1-2 hours to obtain the second basalt fiber.
[0010] S3. At 0-5℃, the second basalt fiber is immersed in a polyamic acid solution, dried, and then heated in stages to obtain modified basalt fiber.
[0011] A second aspect of the present invention is to provide a method for preparing a flame-resistant high-performance fiber composite material as described above, comprising the following steps:
[0012] (1) Mix composite fibers, flame retardant, and part of the interface compatibilizer, and then add polyamide resin, antioxidant, lubricant, zinc borate, and the remaining interface compatibilizer to obtain a mixture;
[0013] (2) The mixture is extruded and granulated to obtain a fiber composite material.
[0014] As described above, the flame-retardant high-performance fiber composite material and its preparation method of the present invention have the following beneficial effects:
[0015] (1) The present invention modifies basalt and coats aluminum phosphate on the surface of basalt fiber, thereby forming a flame retardant layer on the surface of basalt fiber. At the same time, it increases the roughness of the surface of basalt fiber and then forms polyamide on the outside of aluminum phosphate, which facilitates further improvement of the compatibility between basalt fiber and polyamide resin, thereby improving the dispersibility of basalt fiber in polyamide resin, facilitating better formation of network structure, and providing flame retardancy of composite material.
[0016] (2) By introducing an interface compatibilizer, a flame retardant, and composite fibers, the composite fibers are uniformly dispersed in the polyamide matrix to form a three-dimensional network structure. The flame retardant is distributed within the formed fiber network structure, which is equivalent to building a "physical barrier" during combustion. When the material is heated and burned, the fiber layer can delay the transfer of heat to the interior (reduce the heat conduction rate) and at the same time hinder the diffusion of oxygen to the unburned area (reduce the oxygen concentration). The addition of the interface compatibilizer facilitates further improvement of the dispersion of composite fibers and flame retardants in polyamide resin, thereby improving the flame retardancy of the composite material. Detailed Implementation
[0017] To make the inventive objectives, technical solutions, and beneficial effects of this invention clearer, the invention will be further described in detail below with reference to embodiments. Those skilled in the art can easily understand other advantages and effects of this invention from the content disclosed in this specification.
[0018] The first aspect of this invention is to provide a flame-retardant high-performance fiber composite material, comprising the following raw materials in parts by weight: 100 parts polyamide resin, 30-60 parts composite fiber, 0.4-0.5 parts antioxidant, 10-18 parts flame retardant, 1-2 parts interface compatibilizer, 0.5-1 part lubricant, and 0.5-1 part zinc borate; wherein the flame retardant comprises diatomaceous earth, aluminum diethylphosphinate, and polyphosphoramide; wherein the composite fiber comprises modified basalt fiber, phenolic fiber, and polyimide fiber; and wherein the method for preparing the modified basalt fiber comprises the following steps:
[0019] S1. Mix basalt fiber acidic solution, aluminum hydroxide, phosphoric acid and water, adjust the pH to 4-5 and react to obtain the first basalt fiber;
[0020] S2. Add 4,4'-(3-triethoxysilylpropoxy)azobenzene to ethanol to prepare a treatment solution, add the first basalt fiber, and stir under ultrasonic conditions for 1-2 hours to obtain the second basalt fiber.
[0021] S3. At 0-5℃, the second basalt fiber is immersed in a polyamic acid solution, dried, and then heated in stages to obtain modified basalt fiber.
[0022] Composite fibers include modified basalt fibers, phenolic fibers, and polyimide fibers. Polyimide (PI) fibers, in particular, contain numerous imide rings (-CO-N-CO-) and benzene rings in their molecular chains, exhibiting high polarity (the density of polar groups is approximately 1.5 times that of polyamide (PA). Although PI's polarity is slightly lower than that of polyamide (PA), the polar groups of both (such as -C=O in PI and -NH- in PA) can still interact through weak hydrogen bonds (-NH…O=C-) and van der Waals forces, reducing interfacial energy. Furthermore, the benzene rings on the PI fiber surface and the benzene rings in the PA molecular chain (if PA is aromatic, such as PA6T) can further enhance interfacial bonding and improve compatibility through π-π stacking interactions. Phenolic fibers are made from phenolic resin through carbonization or cross-linking, and their surface contains numerous phenolic hydroxyl groups (-OH), carbonyl groups (C=O), and ether bonds (-O-), exhibiting strong polarity. The -C=O group in the amide group (-CONH-) of PA can form bidirectional hydrogen bonds (-NH…O=C- and -C=O…HO-) with the -OH group of phenolic fibers, while simultaneously forming an "interpenetrating network" structure at the interface, enhancing the bonding strength between the two phases. This strong interaction allows phenolic fibers to be stably dispersed in the PA matrix, rather than existing as "foreign particles".
[0023] Uniformly dispersed fibers form a three-dimensional network structure within the polyamide matrix, with flame retardants distributed within this fibrous network, effectively creating a "physical barrier" during combustion. When the material is heated and burns, the fiber layer slows down heat transfer inward (reducing the heat conduction rate) and simultaneously hinders oxygen diffusion to unburned areas (reducing oxygen concentration). Phenolic fibers are typical "char-forming" flame-retardant fibers, forming a dense char layer through dehydration and cross-linking reactions during combustion. Basalt fibers, while not combustible, have surface silica components (SiO2) that catalyze the dehydration and cross-linking of polyamide molecular chains at high temperatures, promoting char layer formation. Polyimide fibers exhibit extremely high thermal stability, maintaining structural integrity before polyamide decomposes and delaying the release of combustible gases. When these three types of fibers are uniformly dispersed, their char-forming or char-promoting effects synergistically work within the polyamide matrix, forming a thicker, denser char layer that effectively isolates oxygen and heat. Modified basalt fiber, phenolic fiber, and polyimide fiber are all non-combustible or flame-retardant materials. Their addition dilutes the proportion of flammable components in the polyamide. Uniformly dispersed fibers ensure that this "dilution effect" is evenly distributed throughout the material, avoiding the formation of localized highly flammable areas.
[0024] The composite of basalt fiber and polyimide fiber significantly improves the material's low-temperature resistance and chemical corrosion resistance. The high bond energy of the imide ring makes it less prone to breakage at high temperatures, and the fiber can still retain some strength at 800℃. Polyimide fiber sublimates and decomposes at high temperatures, releasing inert gases and diluting the oxygen concentration in the combustion zone. When polyimide fiber burns, it generates nitrogen-containing char residue, which covers the material surface and hinders heat transfer and the volatilization of combustibles. The composite of basalt fiber and phenolic fiber significantly enhances the material's char-forming properties and thermal shock resistance. The phenolic fiber molecular chains form a three-dimensional network structure through methylene bridging, which is not easily decomposed at high temperatures. During combustion, it releases phosphorus / nitrogen-containing small molecules to quench free radicals, while the benzene ring and ether bond dehydrate to form char.
[0025] In some embodiments of the present invention, the flame-retardant high-performance fiber composite material comprises the following raw materials in parts by weight: 100 parts polyamide resin, 40-50 parts composite fiber, 0.4-0.5 parts antioxidant, 16-17 parts flame retardant, 1-2 parts interface compatibilizer, 0.5-1 part lubricant, and 0.5-1 part zinc borate.
[0026] In some embodiments of the present invention, the mass ratio of basalt fiber, aluminum hydroxide, and phosphoric acid is 10-15:1-2:8-10.
[0027] In some embodiments of the present invention, the solvent of the polyamic acid solution in step S3 is NMP solvent, and the concentration of the polyamic acid solution is 14-15%.
[0028] In some embodiments of the present invention, the stepwise heating in step S3 involves first holding the temperature at 70-85°C for 25-35 minutes; then holding the temperature at 110-130°C for 25-35 minutes; and then holding the temperature at 200-230°C for 55-75 minutes.
[0029] In some embodiments of the present invention, the composite fiber is composed of modified basalt fiber, phenolic fiber and polyimide fiber in a mass ratio of 5-7:1-2:1-2.
[0030] In some embodiments of the present invention, the antioxidant is selected from one or more of 1010, 168 or 1076.
[0031] In some embodiments of the present invention, the flame retardant is composed of diatomaceous earth, aluminum diethylphosphonate, and polyphosphoramide in a mass ratio of 2-4:3-5:1-3.
[0032] In some embodiments of the present invention, the interface compatibilizer is selected from one or more of maleic anhydride-grafted PP, maleic anhydride-grafted POE, maleic anhydride-grafted EVA, maleic anhydride-grafted EPDM, maleic anhydride-grafted ABS, maleic anhydride-grafted PS, or silane coupling agents.
[0033] In some embodiments of the present invention, the lubricant is selected from one or more of oleamide, stearamide, and ethylene bis-stearamide.
[0034] In some embodiments of the present invention, 4-10 parts of a reinforcing agent are further included, wherein the reinforcing agent is selected from two or more of p-aminobenzenesulfonic acid, nano-silica, or kaolin. Preferably, the reinforcing agent is composed of p-aminobenzenesulfonic acid, nano-silica, and kaolin in a mass ratio of 1-2:4-5:2-3. The nano-silica is silane coupling agent modified nano-silica.
[0035] In some embodiments of the present invention, the use of silane coupling agents to modify silica is a conventional technique in the art, and the operation is carried out using conventional methods in the art. By modifying nano-silica with silane coupling agents, the nanoparticles, after being modified with silane coupling agents, can be dispersed in the resin and migrate to the fiber-resin interface. The interface slippage is restricted through the "physical pinning" effect, while the high specific surface area of the nanoparticles increases the interfacial bonding area.
[0036] In some embodiments of the present invention, the kaolin is modified kaolin, and the preparation method of the modified kaolin includes the following steps:
[0037] (1) Add kaolin to 1 / 2 of the isopropanol aqueous solution, heat and stir rapidly to form kaolin pretreatment solution;
[0038] (2) Add hexadecyltrimethylammonium bromide and sulfuric acid to the remaining isopropanol aqueous solution, heat and stir evenly to obtain the functional solution;
[0039] (3) Add the kaolin pretreatment solution from step (1) to the functional solution from step (2), heat and stir rapidly, filter, wash the filter residue with isopropanol aqueous solution until neutral, dry and grind, and sieve to obtain the final product.
[0040] By modifying kaolin with hexadecyltrimethylammonium bromide as a modifier, some hexadecyltrimethylammonium bromide molecules can fill the spaces between kaolin layers, increasing the interlayer spacing and thus enabling better bonding between the resin matrix and the kaolin layers. The kaolin layers dispersed in the resin matrix can block the entry of gas molecules, increasing the diffusion path of gas molecules and decreasing the permeability coefficient, giving the composite material excellent gas barrier properties. Due to the barrier effect formed by the layered structure of kaolin, flammable gases released during combustion are less likely to disperse within the polymer. The diffusion process slows down the combustion process of the composite material. Simultaneously, introducing hexadecyltrimethylammonium bromide into the interlayer of kaolin makes the kaolin surface hydrophobic, giving it good expansion properties. This allows the kaolin sheet surface to be covered by hexadecyltrimethylammonium bromide molecular chains. The hexadecyltrimethylammonium bromide molecules covering the kaolin sheet surface can form NH…N type hydrogen bonds between the nitrogen-containing flame retardant molecules, allowing the nitrogen-containing flame retardant to be evenly distributed within the composite material, further inhibiting combustion, improving the flame retardant properties of the composite material, and preventing the generation of large amounts of smoke and toxic gases during combustion.
[0041] A second aspect of the present invention is to provide a method for preparing a flame-resistant high-performance fiber composite material as described above, comprising the following steps:
[0042] (1) Mix composite fibers, flame retardant, and part of the interface compatibilizer, and then add polyamide resin, antioxidant, lubricant, zinc borate, and the remaining interface compatibilizer to obtain a mixture;
[0043] (2) The mixture is extruded and granulated to obtain a fiber composite material.
[0044] In some embodiments of the present invention, the extrusion temperature in step (2) is 150-200°C.
[0045] In some embodiments of the present invention, a reinforcing agent is also included, which is added in step (1).
[0046] The present invention will be further illustrated by the following examples, but these examples do not limit the scope of the invention.
[0047] When numerical ranges are given in the embodiments, it should be understood that, unless otherwise stated in the present invention, both endpoints of each numerical range and any value between the two endpoints may be selected. Unless otherwise defined, all technical and scientific terms used in this invention have the same meaning as commonly understood by one of ordinary skill in the art. Where specific conditions are not specified in the embodiments, conventional conditions or conditions recommended by the manufacturer shall apply. All reagents or instruments whose manufacturers are not specified are conventional products that can be purchased commercially. In addition to the specific methods, equipment, and materials used in the embodiments, based on the knowledge of the prior art possessed by one of ordinary skill in the art and the description of this invention, any prior art methods, equipment, and materials similar to or equivalent to those described, used, and materials in the embodiments of this invention may be used to implement this invention.
[0048] Example
[0049] Table 1. Raw material composition ratios of flame-retardant high-performance fiber composite materials in Examples 1-4
[0050] Ingredients / serving Example 1 Example 2 Example 3 Example 4 polyamide resin 100 100 100 100 Composite Fiber 30 50 60 50 antioxidants 0.4 0.4 0.5 0.4 Flame retardant 10 16 18 16 Interface compatibilizer 1 1 2 1 lubricant 0.5 0.7 1 0.7 Zinc borate 0.5 0.7 1 0.7 enhancer / / / 6
[0051] Example 1
[0052] This embodiment provides a flame-retardant high-performance fiber composite material, the raw material components and formulations of which are shown in Table 1. Specifically, the polyamide resin is PA6, the flame retardant is composed of diatomaceous earth, aluminum diethylphosphinate, and polyphosphoramide in a mass ratio of 2:3:1; the antioxidant is antioxidant 1010; the interface compatibilizer is composed of maleic anhydride-grafted PP and silane coupling agent KH550 in a mass ratio of 1:1; and the lubricant is oleamide. The composite fiber is composed of modified basalt fiber, phenolic fiber, and polyimide fiber in a mass ratio of 5:1:1; wherein the phenolic fiber has a length of 1-1.5 mm and an aspect ratio of 20-30; and the polyimide fiber has a length of 0.2-3 mm and an aspect ratio of 30-50.
[0053] The method for preparing the modified basalt fiber includes the following steps:
[0054] S1. 100g of basalt fiber (5-10mm in length, 5-10μm in diameter) was dispersed in 1000ml of water, and then mixed with a 40% sulfuric acid solution to adjust the pH to 2, resulting in an acidic basalt fiber solution. 11.7g of aluminum hydroxide (particle size ≤100 mesh), 86.7g of 2mol / L phosphoric acid, and 100ml of water were then added and mixed thoroughly. The mixture was heated to 70℃ in a water bath, and then ammonia solution was added dropwise by magnetic stirring to adjust the pH to 4.8, resulting in phosphate precipitation. The precipitate was filtered and washed with deionized water. After the reaction, the fiber was washed three times with deionized water and then vacuum dried at 80℃ (-0.08MPa) for 6h to obtain the first basalt fiber.
[0055] S2. 4,4'-(3-triethoxysilylpropoxy)azobenzene was added to 95% ethanol to prepare a treatment solution. Sodium dodecyl sulfate was then added, followed by the first basalt fiber. The mixture was stirred under ultrasonic conditions for 1 hour to obtain the second basalt fiber. The mass-to-volume ratio of the first basalt fiber to the treatment solution was 1:15. The concentration of the treatment solution was 1%. The amount of sodium dodecyl sulfate added was 0.1% of the first basalt fiber.
[0056] S3. At 0-5℃, the second basalt fiber is immersed in a polyamic acid solution with a solid-liquid ratio of 1:8, and the temperature is controlled at 26℃. The fiber is mechanically stirred and impregnated for 2 hours. After impregnation, the fiber is removed and placed in a vacuum drying oven at -0.08MPa and 75℃ for 5 hours. After drying, the temperature is gradually increased to obtain the modified basalt fiber. The gradual temperature increase is as follows: 80℃ (1℃ / min) for 30 minutes; then 130℃ (2℃ / min) for 30 minutes; and finally 220℃ (5℃ / min) for 60 minutes. The concentration of the polyamic acid solution is 15%, and the solvent is N-methylpyrrolidone.
[0057] This embodiment provides a method for preparing a flame-resistant, high-performance fiber composite material, comprising the following steps:
[0058] (1) Mix composite fiber, flame retardant, and 1 / 2 of interface compatibilizer, then add polyamide resin, antioxidant, lubricant, zinc borate, and the remaining interface compatibilizer to obtain a mixture;
[0059] (2) The mixture is extruded and granulated to obtain a fiber composite material. The extrusion temperature is 190℃.
[0060] Example 2
[0061] This embodiment provides a flame-retardant high-performance fiber composite material, the raw material components and proportions of which are shown in Table 1. The difference from Embodiment 1 is that the raw material component proportions are different.
[0062] Example 3
[0063] This embodiment provides a flame-retardant high-performance fiber composite material, the raw material components and proportions of which are shown in Table 1. The difference from Embodiment 1 lies in the different raw material component proportions. Specifically, the flame retardant is composed of diatomaceous earth, aluminum diethylphosphinate, and polyphosphoramide in a mass ratio of 4:5:3; the composite fiber is composed of modified basalt fiber, phenolic fiber, and polyimide fiber in a mass ratio of 7:2:2.
[0064] Example 4
[0065] This embodiment provides a flame-retardant high-performance fiber composite material, the raw material components and proportions of which are shown in Table 1. The difference from Embodiment 2 lies in the different raw material component proportions. A reinforcing agent is also added; specifically, the reinforcing agent consists of p-aminobenzenesulfonic acid, silane-modified nano-silica, and kaolin in a mass ratio of 1:4:2. The preparation method of the silane-modified nano-silica is as follows: 0.8 parts of nano-SiO2 are added to 20 parts of toluene, and ultrasonically dispersed for 30 minutes at room temperature using an ultrasonic cleaner (300W) to obtain a uniform suspension. Then, 0.364 parts of KH-560 are added to the suspension, and ultrasonically mixed for 5 minutes. The mixture is reacted in a 90℃ constant temperature bath for 6 hours. The reaction solution is centrifuged at 12000 r / min at room temperature to obtain modified nano-SiO2, and then ultrasonically centrifuged 6 times. The mixture is then vacuum dried for 8 hours to obtain the final product.
[0066] This embodiment provides a method for preparing a flame-resistant, high-performance fiber composite material, comprising the following steps:
[0067] (1) Mix composite fiber, flame retardant, reinforcing agent, and 1 / 2 of interface compatibilizer, then add polyamide resin, antioxidant, lubricant, zinc borate, and the remaining interface compatibilizer to obtain a mixture;
[0068] (2) The mixture is extruded and granulated to obtain a fiber composite material. The extrusion temperature is 190℃.
[0069] Example 5
[0070] This embodiment provides a flame-retardant high-performance fiber composite material, which differs from Embodiment 4 in that the kaolin is modified kaolin, and the preparation method of the modified kaolin includes the following steps:
[0071] (1) Add kaolin to a portion of the isopropanol aqueous solution, heat to 70°C and stir rapidly to form a kaolin pretreatment solution; wherein the concentration of the isopropanol aqueous solution is 50%; the mass ratio of the kaolin to the isopropanol aqueous solution is 1:10.
[0072] (2) Mix hexadecyltrimethylammonium bromide and the remaining isopropanol aqueous solution and stir until completely dissolved. Then, slowly add 0.3M sulfuric acid to adjust the pH to 4.5, heat to 70℃ and stir evenly to obtain the functional solution; the hexadecyltrimethylammonium bromide is 5% of the mass of kaolin.
[0073] (3) Add the kaolin pretreatment solution from step (1) to the functional solution from step (2), heat to 75°C and stir rapidly for 4 hours, filter, wash the filter residue with 50% isopropanol aqueous solution until neutral, dry and grind, and sieve to obtain the final product.
[0074] Comparative Example
[0075] Comparative Example 1
[0076] The difference between this comparative example and Example 1 is that basalt fiber is used instead of modified basalt fiber.
[0077] Comparative Example 2
[0078] The difference between this comparative example and Example 1 is that the composite fiber is basalt fiber.
[0079] Comparative Example 3
[0080] The difference between this comparative example and Example 1 is that the composite fiber is modified basalt fiber.
[0081] Performance testing
[0082] Flame retardant performance test:
[0083] The flame-retardant properties of the flame-retardant high-performance fiber composite materials prepared in Examples 1-5 and Comparative Examples 1-3 were tested. The flame-retardant properties were measured using a horizontal / vertical burning tester in accordance with the UL94 standard, and the heat distortion temperature was determined in accordance with GB / T1634.2-2004. The results are shown in Table 2.
[0084] Table 2. Performance test results of flame-retardant high-performance fiber composite materials in Examples 1-5 and Comparative Examples 1-3
[0085] Serial Number Vertical burning 3.2mm / 1.6mm Heat distortion temperature (°C) Example 1 V-0 / V-0 187 Example 2 V-0 / V-0 193 Example 3 V-0 / V-0 190 Example 4 V-0 / V-0 196 Example 5 V-0 / V-0 198 Comparative Example 1 V-0 / V-0 182 Comparative Example 2 V-0 / V-1 181 Comparative Example 3 V-0 / V-0 183
[0086] The flame-resistant high-performance fiber composite material prepared by this invention has excellent flame-retardant properties.
[0087] The above embodiments are merely illustrative of the principles and effects of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or alter the above embodiments without departing from the spirit and scope of the present invention. Therefore, all equivalent modifications or alterations made by those skilled in the art without departing from the spirit and technical concept disclosed in the present invention should still be covered by the claims of the present invention.
Claims
1. A flame-retardant high-performance fiber composite material, characterized in that, The raw materials include the following parts by weight: 100 parts polyamide resin, 30-60 parts composite fiber, 0.4-0.5 parts antioxidant, 10-18 parts flame retardant, 1-2 parts interface compatibilizer, 0.5-1 part lubricant, and 0.5-1 part zinc borate; the flame retardant includes diatomaceous earth, aluminum diethylphosphinate, and polyphosphoramide; the flame retardant is composed of diatomaceous earth, aluminum diethylphosphinate, and polyphosphoramide in a mass ratio of 2-4:3-5:1-3; the composite fiber includes modified basalt fiber, phenolic fiber, and polyimide fiber; the composite fiber is composed of modified basalt fiber, phenolic fiber, and polyimide fiber in a mass ratio of 5-7:1-2:1-2; the preparation method of the modified basalt fiber includes the following steps: S1. Mix basalt fiber acidic solution, aluminum hydroxide, phosphoric acid and water, adjust the pH to 4-5 and react to obtain the first basalt fiber; S2. Add 4,4'-(3-triethoxysilylpropoxy)azobenzene to ethanol to prepare a treatment solution, add the first basalt fiber, and stir under ultrasonic conditions for 1-2 hours to obtain the second basalt fiber. S3. At 0-5℃, the second basalt fiber is immersed in a polyamic acid solution, dried, and then heated in stages to obtain modified basalt fiber.
2. The flame-retardant high-performance fiber composite material according to claim 1, characterized in that: It also includes 4-10 parts of a reinforcing agent, which is selected from two or more of p-aminobenzenesulfonic acid, nano-silica, or kaolin.
3. The flame-retardant high-performance fiber composite material according to claim 2, characterized in that: The reinforcing agent is composed of p-aminobenzenesulfonic acid, nano-silica, and kaolin in a mass ratio of 1-2:4-5:2-3.
4. The flame-retardant high-performance fiber composite material according to claim 1, characterized in that: The antioxidant is selected from one or more of 1010, 168, or 1076.
5. The flame-retardant high-performance fiber composite material according to claim 1, characterized in that: The lubricant is selected from one or more of oleamide, stearamide, and ethylene bis-stearamide.
6. The flame-retardant high-performance fiber composite material according to claim 1, characterized in that: The interface compatibilizer is selected from one or more of maleic anhydride-grafted PP, maleic anhydride-grafted POE, maleic anhydride-grafted EVA, maleic anhydride-grafted EPDM, maleic anhydride-grafted ABS, maleic anhydride-grafted PS, or silane coupling agents.
7. A method for preparing a flame-retardant high-performance fiber composite material as described in any one of claims 1-6, characterized in that: Includes the following steps: (1) Mix composite fibers, flame retardant, and part of the interface compatibilizer, and then add polyamide resin, antioxidant, lubricant, zinc borate, and the remaining interface compatibilizer to obtain a mixture; (2) The mixture is extruded and granulated to obtain a fiber composite material.
8. The preparation method according to claim 7, characterized in that: It also includes a reinforcing agent, which is added in step (1).
Citation Information
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