Fireproof fiber composite board and preparation method thereof

Abstract

The invention relates to the technical field of fireproof fiber composite boards, in particular to a fireproof fiber composite board and a preparation method thereof.The fireproof fiber composite board is prepared from, by weight, 200-500 parts of fiber material, 300-600 parts of resin material, 100-300 parts of composite flame retardant, 50-150 parts of silicon dioxide aerogel, 5-30 parts of release agent, 10-50 parts of curing agent and 2-20 parts of accelerant. According to the fireproof fiber composite board and the preparation method thereof, the fireproof fiber composite board has excellent fireproof, mechanical, heat-insulation and sound-insulation performance, and the environment-friendly performance is improved by introducing the bio-based resin, so that the requirements of modern buildings on high-performance and environment-friendly building materials are met.

Description

Technical Field

[0001] This invention relates to the field of fire-resistant fiber composite board technology, and in particular to a fire-resistant fiber composite board and its preparation method. Background Technology

[0002] With the accelerating pace of global urbanization, the construction industry is experiencing rapid growth. Simultaneously, people's emphasis on building safety and environmental protection is continuously increasing, leading to the widespread application of fire-resistant fiber composite panels in the construction field. From interior decoration of high-rise buildings to structural construction of large commercial complexes, from wall materials in industrial plants to fire-resistant partitions in public facilities, fire-resistant fiber composite panels, with their unique fire-resistant properties, have become one of the key materials for ensuring building safety.

[0003] However, traditional fire-resistant fiber composite panels have gradually revealed numerous problems in practical applications. Regarding fire resistance, when exposed to high temperatures or prolonged combustion, some traditional panels struggle to maintain their integrity, increasing the risk of fire spread. In terms of mechanical properties, their impact resistance and compressive strength are limited, making them unable to withstand significant external forces and prone to structural damage under extreme conditions such as earthquakes and strong winds. Regarding thermal insulation, traditional panels have a relatively high thermal conductivity, making it difficult to effectively block heat transfer and affecting the building's energy-saving performance. These limitations make traditional fire-resistant fiber composite panels unsuitable for the demands of high-rise buildings, data centers, hospitals, and other locations with extremely high requirements for building material performance.

[0004] Furthermore, the traditional manufacturing process of wood-based panels also presents serious environmental problems. It utilizes large amounts of petroleum-based resins as binders, materials that are not only non-renewable but also release significant amounts of greenhouse gases and toxic substances during production, use, and disposal, placing considerable pressure on the ecological environment. Therefore, developing a new type of fire-resistant fiber composite panel with superior performance and environmental friendliness is of significant practical importance. Summary of the Invention

[0005] The purpose of this invention is to provide a fire-resistant fiber composite board and its preparation method, which not only has excellent fire resistance, mechanical properties, and thermal and sound insulation properties, but also improves environmental performance by introducing bio-based resin, so as to meet the needs of modern buildings for high-performance and environmentally friendly building materials.

[0006] To achieve the above objectives, the present invention provides a fire-resistant fiber composite board, comprising the following raw materials by weight: 200-500 parts fiber material, 300-600 parts resin material, 100-300 parts composite flame retardant, 50-150 parts silica aerogel, 5-30 parts release agent, 10-50 parts curing agent, and 2-20 parts accelerator; the fiber material includes basalt fiber, carbon fiber, ceramic fiber, aramid fiber, and glass fiber cloth; the resin material is a mixture of petroleum-based resin and bio-based resin in a mass ratio of 7:3; the composite flame retardant includes aluminum hydroxide, dimethyl methylphosphonate, and nitrogen-phosphorus intumescent flame retardant.

[0007] Preferably, the amount of basalt fiber is 30-40% of the total fiber mass, the amount of carbon fiber is 20-30% of the total fiber mass, the amount of ceramic fiber is 20-30% of the total fiber mass, and the amount of aramid fiber is 10-20% of the total fiber mass.

[0008] Preferably, the basalt fiber has a diameter of 10-15μm and a length of 5-8mm, the carbon fiber has a diameter of 7-10μm and a length of 3-5mm, the ceramic fiber has a diameter of 5-8μm and a length of 2-4mm, and the aramid fiber has a linear density of 1.5-2.0dtex.

[0009] Preferably, the bio-based resin is cashew phenol epoxy resin with an epoxy value of 0.3-0.5 ep / kg and a hydroxyl value of 0.1-0.3 ep / kg, and the petroleum-based resin is bisphenol A type epoxy resin with an epoxy equivalent of 180-200 g / eq and a chlorine content of less than 0.5%.

[0010] Preferably, the amount of aluminum hydroxide is 50-60% of the total mass of the composite flame retardant, the amount of dimethyl methylphosphonate is 10-20% of the total mass of the composite flame retardant, and the amount of nitrogen-phosphorus intumescent flame retardant is 20-30% of the total mass of the composite flame retardant.

[0011] Preferably, the silica aerogel has particles with a diameter of 50-100 μm, a density of 0.05-0.2 g / cm3, and a specific surface area of ​​≥800 m2 / g.

[0012] Preferably, the release agent includes one or more combinations of zinc stearate, calcium stearate, and polyvinyl alcohol.

[0013] Preferably, the curing agent includes one or more of methyl ethyl ketone peroxide, cyclohexanone peroxide, and tert-butyl peroxide.

[0014] Preferably, the accelerator includes one or more of cobalt isooctanoate, cobalt naphthenate, and N,N-dimethylaniline.

[0015] The preparation method of the above-mentioned fire-resistant fiber composite board includes the following steps:

[0016] S1. Mix aluminum hydroxide, dimethyl methylphosphonate and nitrogen-phosphorus intumescent flame retardant, and stir at 1000-1500 r / min for 30-40 min to obtain a composite flame retardant;

[0017] S2. Soak basalt fiber, carbon fiber, ceramic fiber and aramid fiber in a 2-3% silane coupling agent ethanol solution for 1-2 hours, and then dry them in an oven at 80-100℃ for 2-3 hours.

[0018] S3. First, add petroleum-based resin and bio-based resin to the reactor, then add composite flame retardant, release agent, curing agent and accelerator and stir evenly. Finally, add silica aerogel and continue stirring for 20-30 minutes to obtain resin solution.

[0019] S4. Mix the basalt fiber and carbon fiber treated by S2 evenly, and make a three-dimensional mesh structure using three-dimensional weaving technology. Then, immerse it in the resin liquid of S3 for pre-forming and cure it at 100-120℃ for 2-3 hours to obtain the inner fiber reinforced skeleton.

[0020] S5. The ceramic fibers and aramid fibers treated in S2 are alternately laid in layers with a thickness of 0.5-1.0 mm. After spraying the resin solution of S3, they are laminated with the inner fiber-reinforced skeleton and hot-pressed at 120-140℃ and 1-2MPa pressure for 30-40 minutes to obtain the intermediate layer.

[0021] S6. Immerse the glass fiber cloth in silicone resin, and after full impregnation, attach it to the surface of the intermediate layer of S5. Cure it at 150-180℃ for 1-2 hours to form an outer protective layer and obtain a fireproof fiber composite board.

[0022] S7. After cutting, grinding, and trimming the fireproof fiber composite board, inspect and package it.

[0023] The beneficial effects of this invention are:

[0024] (1) The multi-component composite flame retardant system of the present invention has the synergistic effect of each flame retardant to improve the flame retardant efficiency of fireproof fiber composite board.

[0025] (2) This invention introduces silica aerogel to construct a high-efficiency heat insulation network, thereby improving the heat insulation performance. It also adds bio-based resins such as cashew phenol epoxy resin to replace part of the petroleum-based resin. The bio-based resin is derived from renewable resources, which can reduce the dependence on petrochemical raw materials, reduce carbon emissions in the production process, and improve the environmental performance of the board. At the same time, the bio-based resin has good adhesion and mechanical properties and will not affect the overall quality of the board.

[0026] (3) The present invention improves the high compressive strength, flexural strength and impact toughness of fireproof fiber composite board by forming a biomimetic multi-layered interlaced reinforcement structure through an inner fiber reinforced skeleton, a middle layer and an outer protective layer, so that it can withstand greater external forces and is suitable for various building structures and usage scenarios.

[0027] The technical solution of the present invention will be further described in detail below through embodiments. Detailed Implementation

[0028] The present invention will be further described below with reference to embodiments. Unless otherwise defined, the technical or scientific terms used in this invention should have the ordinary meaning understood by one of ordinary skill in the art. The features mentioned above or in the specific examples mentioned in this invention can be combined arbitrarily, and these specific embodiments are only used to illustrate the invention and are not intended to limit the scope of the invention.

[0029] This invention provides a fire-resistant fiber composite board, comprising the following raw materials by weight: 200-500 parts fiber material, 300-600 parts resin material, 100-300 parts composite flame retardant, 50-150 parts silica aerogel, 5-30 parts release agent, 10-50 parts curing agent, and 2-20 parts accelerator; the fiber material includes basalt fiber, carbon fiber, ceramic fiber, aramid fiber, and glass fiber cloth; the resin material is a mixture of petroleum-based resin and bio-based resin in a mass ratio of 7:3; the composite flame retardant includes aluminum hydroxide, dimethyl methylphosphonate, and nitrogen-phosphorus intumescent flame retardant.

[0030] Preferably, the amount of basalt fiber is 30-40% of the total fiber mass, the amount of carbon fiber is 20-30% of the total fiber mass, the amount of ceramic fiber is 20-30% of the total fiber mass, and the amount of aramid fiber is 10-20% of the total fiber mass.

[0031] Preferably, the basalt fiber has a diameter of 10-15μm and a length of 5-8mm, the carbon fiber has a diameter of 7-10μm and a length of 3-5mm, the ceramic fiber has a diameter of 5-8μm and a length of 2-4mm, and the aramid fiber has a linear density of 1.5-2.0dtex.

[0032] A further preferred option is to use fiberglass cloth with a specification of 200-300g / m2 for outer layer protection.

[0033] Preferably, the bio-based resin is cashew phenol epoxy resin with an epoxy value of 0.3-0.5 ep / kg and a hydroxyl value of 0.1-0.3 ep / kg, and the petroleum-based resin is bisphenol A type epoxy resin with an epoxy equivalent of 180-200 g / eq and a chlorine content of less than 0.5%.

[0034] This invention replaces part of the petroleum-based resin with bio-based resin. Bio-based resin is a renewable resource, which can reduce dependence on petrochemical raw materials, reduce carbon emissions in the production process, and improve the environmental performance of the board. At the same time, bio-based resin has good adhesion and mechanical properties and will not affect the overall quality of the board.

[0035] Preferably, the amount of aluminum hydroxide is 50-60% of the total mass of the composite flame retardant, the amount of dimethyl methylphosphonate is 10-20% of the total mass of the composite flame retardant, and the amount of nitrogen-phosphorus intumescent flame retardant is 20-30% of the total mass of the composite flame retardant.

[0036] In the composite flame retardant system of this invention, each flame retardant plays a different role at different stages of a fire. Aluminum hydroxide decomposes and absorbs heat, releases water of crystallization to cool down, and forms an alumina heat insulation layer. Dimethyl methylphosphonate participates in gas-phase flame retardancy and inhibits free radicals. Nitrogen-phosphorus intumescent flame retardant expands at high temperature to form a carbonaceous foam layer to isolate oxygen and heat, thus jointly improving flame retardant efficiency.

[0037] A further preferred method is to prepare a nitrogen-phosphorus intumescent flame retardant by reacting melamine, pentaerythritol, and phosphoric acid at 180-200℃ for 3-4 hours under the action of a catalyst, followed by cooling and pulverization.

[0038] In some specific embodiments of the present invention, the nitrogen-phosphorus intumescent flame retardant is prepared by the following method: melamine, pentaerythritol, and phosphoric acid in a molar ratio of 1:1:1.2 are added to a reaction vessel, along with 0.5% by mass of p-toluenesulfonic acid as a catalyst. Stirring is started at a speed of 200-250 r / min. After the raw materials are uniformly mixed, the reaction system is heated to 180-200°C using an oil bath, and the reaction is continued within this temperature range for 3-4 hours. After the reaction is complete, the heating device is turned off, and the material is cooled to room temperature using air cooling. The cooled product is then transferred to a pulverizer, and the particle size is set to 80-100 mesh for pulverization.

[0039] Preferably, the silica aerogel has particles with a diameter of 50-100 μm, a density of 0.05-0.2 g / cm3, and a specific surface area of ​​≥800 m2 / g.

[0040] This invention introduces silica aerogel, which has extremely low thermal conductivity and high porosity, to construct a highly efficient thermal insulation network inside the board, thereby reducing the heat transfer rate and significantly improving thermal insulation performance.

[0041] Preferably, the release agent includes one or more combinations of zinc stearate, calcium stearate, and polyvinyl alcohol.

[0042] A further preferred option is zinc stearate as the release agent.

[0043] Preferably, the curing agent includes one or more of methyl ethyl ketone peroxide, cyclohexanone peroxide, and tert-butyl peroxide.

[0044] A further preferred curing agent is methyl ethyl ketone peroxide.

[0045] Preferably, the accelerator includes one or more of cobalt isooctanoate, cobalt naphthenate, and N,N-dimethylaniline.

[0046] A further preferred accelerator is cobalt isooctanoate.

[0047] The preparation method of the above-mentioned fire-resistant fiber composite board includes the following steps:

[0048] S1. Mix aluminum hydroxide, dimethyl methylphosphonate and nitrogen-phosphorus intumescent flame retardant, and stir at 1000-1500 r / min for 30-40 min to obtain a composite flame retardant;

[0049] S2. Soak basalt fiber, carbon fiber, ceramic fiber and aramid fiber in a 2-3% silane coupling agent ethanol solution for 1-2 hours, and then dry them in an oven at 80-100℃ for 2-3 hours.

[0050] S3. First, add petroleum-based resin and bio-based resin to the reactor, then add composite flame retardant, release agent, curing agent and accelerator and stir evenly. Finally, add silica aerogel and continue stirring for 20-30 minutes to obtain resin solution.

[0051] S4. Mix the basalt fiber and carbon fiber treated by S2 evenly, and make a three-dimensional mesh structure using three-dimensional weaving technology. Then, immerse it in the resin liquid of S3 for pre-forming and cure it at 100-120℃ for 2-3 hours to obtain the inner fiber reinforced skeleton.

[0052] S5. The ceramic fibers and aramid fibers treated in S2 are alternately laid in layers with a thickness of 0.5-1.0 mm. After spraying the resin solution of S3, they are laminated with the inner fiber-reinforced skeleton and hot-pressed at 120-140℃ and 1-2MPa pressure for 30-40 minutes to obtain the intermediate layer.

[0053] S6. Immerse the glass fiber cloth in silicone resin, and after full impregnation, attach it to the surface of the intermediate layer of S5. Cure it at 150-180℃ for 1-2 hours to form an outer protective layer and obtain a fireproof fiber composite board.

[0054] S7. After cutting, grinding, and trimming the fireproof fiber composite board, inspect and package it.

[0055] The fire-resistant fiber composite board of this invention has a biomimetic multi-layered interlaced reinforcement structure consisting of an inner fiber-reinforced skeleton, a middle layer, and an outer protective layer. The inner layer is a three-dimensional mesh skeleton woven from high-strength basalt fibers and carbon fibers to provide mechanical support; the middle layer is an alternating arrangement of high-temperature resistant ceramic fibers and flexible aramid fibers to enhance flexibility and impact resistance; the outer layer is a protective layer formed by impregnating glass fiber cloth with silicone resin to improve surface hardness and wear resistance. The close bonding of each layer gives the fire-resistant fiber composite board both high strength and good toughness.

[0056] Example 1

[0057] This invention provides a fireproof fiber composite board, which comprises the following raw materials by weight: 200g fiber material, 300g resin material, 100g composite flame retardant, 50g silica aerogel, 5g zinc stearate as a release agent, 10g methyl ethyl ketone peroxide as a curing agent, and 2g cobalt isooctanoate as an accelerator.

[0058] The fiber material comprises 30% basalt fiber, 25% carbon fiber, 25% ceramic fiber, 20% aramid fiber, and 200 g / m² glass fiber cloth. The resin material is a mixture of bisphenol A epoxy resin and cashew nut shell epoxy resin in a mass ratio of 7:3. The composite flame retardant comprises 50% aluminum hydroxide, 20% dimethyl methylphosphonate, and 30% nitrogen-phosphorus intumescent flame retardant.

[0059] The preparation method of the above-mentioned fire-resistant fiber composite board includes the following steps:

[0060] S1. Mix aluminum hydroxide, dimethyl methylphosphonate and nitrogen-phosphorus intumescent flame retardant, and stir at 1000 r / min for 30 min to obtain a composite flame retardant.

[0061] S2. Soak basalt fiber, carbon fiber, ceramic fiber and aramid fiber in a 2% silane coupling agent ethanol solution for 1 hour, and then dry them in an oven at 80°C for 2 hours.

[0062] S3. First, add petroleum-based resin and bio-based resin to the reactor, then add composite flame retardant, release agent, curing agent and accelerator and stir evenly. Finally, add silica aerogel and continue stirring for 20 minutes to obtain resin solution.

[0063] S4. The basalt fiber and carbon fiber treated in S2 are mixed evenly and made into a three-dimensional mesh structure using three-dimensional weaving technology. Then, the mesh structure is pre-formed by immersing it in the resin solution of S3 and cured at 100°C for 2 hours to obtain the inner fiber reinforced skeleton.

[0064] S5. The ceramic fibers and aramid fibers treated in S2 are alternately laid in layers with a thickness of 0.5 mm per layer. After being sprayed with resin adhesive of S3, they are laminated with the inner fiber-reinforced skeleton and hot-pressed at 120℃ and 1MPa pressure for 30 min to obtain the intermediate layer.

[0065] S6. Immerse the glass fiber cloth in silicone resin, and after full impregnation, attach it to the surface of the intermediate layer of S5. Cure at 150°C for 1 hour to form an outer protective layer, thus obtaining a fireproof fiber composite board.

[0066] S7. After cutting, grinding, and trimming the fireproof fiber composite board, inspect and package it.

[0067] Example 2

[0068] This invention provides a fireproof fiber composite board, which comprises the following raw materials by weight: 300g fiber material, 400g resin material, 150g composite flame retardant, 75g silica aerogel, 10g zinc stearate as a release agent, 18g methyl ethyl ketone peroxide as a curing agent, and 7g cobalt isooctanoate as an accelerator.

[0069] The fiber material comprises 35% basalt fiber, 20% carbon fiber, 30% ceramic fiber, 15% aramid fiber, and 250 g / m² glass fiber cloth. The resin material is a mixture of bisphenol A epoxy resin and cashew nut shell epoxy resin in a mass ratio of 7:3. The composite flame retardant comprises 55% aluminum hydroxide, 20% dimethyl methylphosphonate, and 25% nitrogen-phosphorus intumescent flame retardant.

[0070] The preparation method of the above-mentioned fire-resistant fiber composite board includes the following steps:

[0071] S1. Mix aluminum hydroxide, dimethyl methylphosphonate and nitrogen-phosphorus intumescent flame retardant, and stir at 1200 r / min for 35 min to obtain a composite flame retardant.

[0072] S2. Soak basalt fiber, carbon fiber, ceramic fiber and aramid fiber in a 3% silane coupling agent ethanol solution for 1.5 hours, and then dry them in a 90℃ oven for 2.5 hours.

[0073] S3. First, add petroleum-based resin and bio-based resin to the reactor, then add composite flame retardant, release agent, curing agent and accelerator and stir evenly. Finally, add silica aerogel and continue stirring for 25 minutes to obtain resin solution.

[0074] S4. The basalt fiber and carbon fiber treated in S2 are mixed evenly and made into a three-dimensional mesh structure using three-dimensional weaving technology. Then, the mesh structure is pre-formed by immersing it in the resin solution of S3 and cured at 110℃ for 2.5h to obtain the inner fiber reinforced skeleton.

[0075] S5. The ceramic fibers and aramid fibers treated in S2 are alternately laid in layers with a thickness of 0.8 mm per layer. After being sprayed with the resin solution of S3, they are laminated with the inner fiber-reinforced skeleton and hot-pressed at 130℃ and 1.5 MPa for 35 min to obtain the intermediate layer.

[0076] S6. Immerse the glass fiber cloth in silicone resin, and after full impregnation, attach it to the surface of the intermediate layer of S5. Cure at 160℃ for 1.5h to form an outer protective layer and obtain a fireproof fiber composite board.

[0077] S7. After cutting, grinding, and trimming the fireproof fiber composite board, inspect and package it.

[0078] Example 3

[0079] This invention provides a fireproof fiber composite board, which comprises the following raw materials by weight: 350g fiber material, 450g resin material, 200g composite flame retardant, 100g silica aerogel, 15g zinc stearate, 25g methyl ethyl ketone peroxide, and 12g cobalt isooctanoate.

[0080] The fiber material comprises 35% basalt fiber, 30% carbon fiber, 20% ceramic fiber, 15% aramid fiber, and 250 g / m² glass fiber cloth. The resin material is a mixture of bisphenol A epoxy resin and cashew nut shell epoxy resin in a mass ratio of 7:3. The composite flame retardant comprises 60% aluminum hydroxide, 10% dimethyl methylphosphonate, and 30% nitrogen-phosphorus intumescent flame retardant.

[0081] The preparation method of the above-mentioned fire-resistant fiber composite board includes the following steps:

[0082] S1. Mix aluminum hydroxide, dimethyl methylphosphonate and nitrogen-phosphorus intumescent flame retardant, and stir at 1200 r / min for 35 min to obtain a composite flame retardant.

[0083] S2. Soak basalt fiber, carbon fiber, ceramic fiber and aramid fiber in a 3% silane coupling agent ethanol solution for 2 hours, and then dry them in an oven at 100°C for 3 hours.

[0084] S3. First, add petroleum-based resin and bio-based resin to the reactor, then add composite flame retardant, release agent, curing agent and accelerator and stir evenly. Finally, add silica aerogel and continue stirring for 30 minutes to obtain resin solution.

[0085] S4. The basalt fiber and carbon fiber treated in S2 are mixed evenly and made into a three-dimensional mesh structure using three-dimensional weaving technology. Then, the mesh structure is pre-formed by immersing it in the resin solution of S3 and cured at 120°C for 3 hours to obtain the inner fiber reinforced skeleton.

[0086] S5. The ceramic fibers and aramid fibers treated in S2 are alternately laid in layers with a thickness of 1.0 mm. After being sprayed with the resin solution of S3, they are laminated with the inner fiber-reinforced skeleton and hot-pressed at 140℃ and 2MPa pressure for 40 min to obtain the intermediate layer.

[0087] S6. Immerse the fiberglass cloth in silicone resin, and after full impregnation, attach it to the surface of the intermediate layer of S5. Cure at 180°C for 2 hours to form an outer protective layer, thus obtaining a fireproof fiber composite board.

[0088] S7. After cutting, grinding, and trimming the fireproof fiber composite board, inspect and package it.

[0089] Example 4

[0090] This invention provides a fireproof fiber composite board, which comprises the following raw materials by weight: 400g fiber material, 500g resin material, 250g composite flame retardant, 120g silica aerogel, 20g zinc stearate as a release agent, 30g methyl ethyl ketone peroxide as a curing agent, and 16g cobalt isooctanoate as an accelerator.

[0091] The fiber material comprises 30% basalt fiber, 30% carbon fiber, 30% ceramic fiber, 10% aramid fiber, and 300g / m² fiber. 2 Fiberglass cloth. The resin material is a mixture of bisphenol A epoxy resin and cashew phenol epoxy resin in a mass ratio of 7:3. The composite flame retardant includes 60% aluminum hydroxide, 10% dimethyl methylphosphonate, and 30% nitrogen-phosphorus intumescent flame retardant.

[0092] The preparation method of the above-mentioned fire-resistant fiber composite board includes the following steps:

[0093] S1. Mix aluminum hydroxide, dimethyl methylphosphonate and nitrogen-phosphorus intumescent flame retardant, and stir at 1500 r / min for 40 min to obtain a composite flame retardant.

[0094] S2. Soak basalt fiber, carbon fiber, ceramic fiber and aramid fiber in a 3% silane coupling agent ethanol solution for 2 hours, and then dry them in an oven at 100°C for 3 hours.

[0095] S3. First, add petroleum-based resin and bio-based resin to the reactor, then add composite flame retardant, release agent, curing agent and accelerator and stir evenly. Finally, add silica aerogel and continue stirring for 30 minutes to obtain resin solution.

[0096] S4. The basalt fiber and carbon fiber treated in S2 are mixed evenly and made into a three-dimensional mesh structure using three-dimensional weaving technology. Then, the mesh structure is pre-formed by immersing it in the resin solution of S3 and cured at 120°C for 3 hours to obtain the inner fiber reinforced skeleton.

[0097] S5. The ceramic fibers and aramid fibers treated in S2 are alternately laid in layers with a thickness of 1.0 mm. After being sprayed with the resin solution of S3, they are laminated with the inner fiber-reinforced skeleton and hot-pressed at 140℃ and 2MPa pressure for 40 min to obtain the intermediate layer.

[0098] S6. Immerse the fiberglass cloth in silicone resin, and after full impregnation, attach it to the surface of the intermediate layer of S5. Cure at 180°C for 2 hours to form an outer protective layer, thus obtaining a fireproof fiber composite board.

[0099] S7. After cutting, grinding, and trimming the fireproof fiber composite board, inspect and package it.

[0100] Example 5

[0101] This invention provides a fireproof fiber composite board, comprising the following raw materials by weight: 500g fiber material, 600g resin material, 300g composite flame retardant, 150g silica aerogel, 30g zinc stearate as a release agent, 50g methyl ethyl ketone peroxide as a curing agent, and 20g cobalt isooctanoate as an accelerator.

[0102] The fiber material comprises 40% basalt fiber, 20% carbon fiber, 20% ceramic fiber, 20% aramid fiber, and 300 g / m² glass fiber cloth. The resin material is a mixture of bisphenol A epoxy resin and cashew nut shell epoxy resin in a mass ratio of 7:3. The composite flame retardant comprises 60% aluminum hydroxide, 20% dimethyl methylphosphonate, and 20% nitrogen-phosphorus intumescent flame retardant.

[0103] The preparation method of the above-mentioned fire-resistant fiber composite board includes the following steps:

[0104] S1. Mix aluminum hydroxide, dimethyl methylphosphonate and nitrogen-phosphorus intumescent flame retardant, and stir at 1500 r / min for 40 min to obtain a composite flame retardant.

[0105] S2. Soak basalt fiber, carbon fiber, ceramic fiber and aramid fiber in a 3% silane coupling agent ethanol solution for 2 hours, and then dry them in an oven at 100°C for 3 hours.

[0106] S3. First, add petroleum-based resin and bio-based resin to the reactor, then add composite flame retardant, release agent, curing agent and accelerator and stir evenly. Finally, add silica aerogel and continue stirring for 30 minutes to obtain resin solution.

[0107] S4. The basalt fiber and carbon fiber treated in S2 are mixed evenly and made into a three-dimensional mesh structure using three-dimensional weaving technology. Then, the mesh structure is pre-formed by immersing it in the resin solution of S3 and cured at 120°C for 3 hours to obtain the inner fiber reinforced skeleton.

[0108] S5. The ceramic fibers and aramid fibers treated in S2 are alternately laid in layers with a thickness of 1.0 mm. After being sprayed with the resin solution of S3, they are laminated with the inner fiber-reinforced skeleton and hot-pressed at 140℃ and 2MPa pressure for 40 min to obtain the intermediate layer.

[0109] S6. Immerse the fiberglass cloth in silicone resin, and after full impregnation, attach it to the surface of the intermediate layer of S5. Cure at 180°C for 2 hours to form an outer protective layer, thus obtaining a fireproof fiber composite board.

[0110] S7. After cutting, grinding, and trimming the fireproof fiber composite board, inspect and package it.

[0111] Comparative Example 1

[0112] Based on Example 3, the difference is that the resin material is only bisphenol A type epoxy resin, without cashew phenol epoxy resin. Everything else is the same as in Example 3.

[0113] Comparative Example 2

[0114] Based on Example 3, the difference from Example 3 is that the fiber material is only carbon fiber.

[0115] Comparative Example 3

[0116] Based on Example 3, the difference from Example 3 is that the flame retardant is a mixture of aluminum hydroxide and dimethyl methylphosphonate, without nitrogen-phosphorus intumescent flame retardant.

[0117] Fire resistance performance test: The fire resistance performance of the boards in Examples 1-5 and Comparative Examples 1-3 was tested using an oxygen index tester and a vertical burning tester. The results are shown in Table 1.

[0118] Table 1 Fire resistance test data of different composite panels

[0119]

[0120]

[0121] As shown in Table 1, the flammability ratings of Examples 1-5 are all A2, with limiting oxygen indices between 32% and 36%, and vertical burning ratings reaching V-0. They exhibit low peak heat release rates and low total heat release, demonstrating excellent fire resistance. Comparative Example 1, lacking bio-based resin, has slightly lower limiting oxygen indices and heat release rates than the Examples. Comparative Example 2, using only carbon fiber, has a flammability rating reduced to B1, showing a significant decrease in fire resistance. Comparative Example 3, lacking nitrogen-phosphorus intumescent flame retardants, has a higher heat release than the Examples. The fire-resistant fiber composite boards prepared in these embodiments exhibit excellent flame-retardant properties and low heat release characteristics in fires, effectively delaying the spread of fire.

[0122] Mechanical property testing: The compressive strength, flexural strength and impact toughness of the sheet were tested using a universal testing machine. The results are shown in Table 2.

[0123] Table 2 Mechanical property test data of different composite boards

[0124]

[0125]

[0126] As shown in Table 2, the compressive strength of Examples 1-5 is 120-150 MPa, the flexural strength is 45-58 MPa, and the impact toughness is 25-32 kJ / m. 2 The mechanical properties of the samples are superior to those of the comparative examples. Comparative Example 1, which uses only petroleum-based resin, has mechanical properties similar to but slightly lower than those of the examples. Comparative Example 2, using a single fiber, suffers from a significant decrease in various mechanical properties. Comparative Example 3, lacking an intumescent flame retardant, has slightly inferior mechanical properties compared to the examples. The fire-resistant fiber composite panels prepared according to the embodiments of this invention can better withstand external forces and are suitable for various building structures and usage scenarios.

[0127] Thermal insulation performance test: The thermal insulation of the board was tested in a high-temperature furnace. The temperature rise of the back of the board at 1000℃ was recorded within 1 hour. The results are shown in Table 3.

[0128] Table 3. Test data on the thermal insulation performance of different composite panels

[0129]

[0130] As shown in Table 3, the thermal conductivity of Examples 1-5 ranges from 0.030 to 0.035 W / (m·K), the temperature rise on the back side is 10-15℃ after 1 hour at 1000℃, and the temperature resistance range is -40℃ to 180℃, demonstrating outstanding thermal insulation performance. Comparative Example 1 has slightly higher thermal conductivity and temperature rise, Comparative Example 2 has significantly poorer thermal insulation performance, and Comparative Example 3 lacks an intumescent flame retardant, resulting in a slightly weaker thermal insulation effect than the Examples. The fireproof fiber composite board prepared by the embodiments of this invention can effectively block heat transfer and improve the thermal insulation and energy-saving effect of buildings.

[0131] Sound insulation performance test: The sound insulation performance of the board was tested using a sound insulation testing device. The results are shown in Table 4.

[0132] Table 4. Test data on the sound insulation performance of different composite panels

[0133]

[0134] As shown in Table 4, the sound insulation of Examples 1-5 is 32-36 dB, which is good. The sound insulation of Comparative Examples 1-3 is lower than that of Examples 1-5, with Comparative Example 2 having the worst sound insulation performance. This shows that multi-fiber composite and reasonable formula can improve the sound insulation effect.

[0135] Environmental performance test: The content of volatile organic compounds (VOCs) in the board was detected by gas chromatography-mass spectrometry, and the results are shown in Table 5.

[0136] Table 5. Environmental performance test data for different composite panels

[0137]

[0138] As shown in Table 5, Examples 1-5 have low volatile organic compound (VOC) content, no formaldehyde detected, and a carbon footprint of 7-8 kg CO2, demonstrating excellent environmental performance. Comparative Examples 1-3, due to the lack of bio-based resin or formulation defects, have higher VOC and formaldehyde release levels, resulting in a larger carbon footprint and inferior environmental performance compared to the Examples. This indicates that the fire-resistant fiber composite board prepared according to the embodiments of the present invention meets the requirements of modern buildings for environmentally friendly materials.

[0139] In summary, the fireproof fiber composite board of the present invention has excellent fire resistance, superior mechanical strength, good thermal insulation effect and outstanding environmental protection characteristics, which can meet the needs of places with extremely high requirements for building material performance, such as super high-rise buildings, data centers, and hospitals.

[0140] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and not to limit them. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can still be made to the technical solutions of the present invention, and these modifications or equivalent substitutions cannot cause the modified technical solutions to deviate from the spirit and scope of the technical solutions of the present invention.

Claims

1. A fire-resistant fiber composite board, characterized in that: The raw materials, by weight, include the following: 200-500 parts fiber material, 300-600 parts resin material, 100-300 parts composite flame retardant, 50-150 parts silica aerogel, 5-30 parts release agent, 10-50 parts curing agent, and 2-20 parts accelerator; the fiber material includes basalt fiber, carbon fiber, ceramic fiber, aramid fiber, and glass fiber cloth; the resin material is a mixture of petroleum-based resin and bio-based resin in a mass ratio of 7:3; the composite flame retardant includes aluminum hydroxide, dimethyl methylphosphonate, and nitrogen-phosphorus intumescent flame retardant.

2. The fire-resistant fiber composite board according to claim 1, characterized in that: The amount of basalt fiber used is 30-40% of the total fiber mass, the amount of carbon fiber used is 20-30% of the total fiber mass, the amount of ceramic fiber used is 20-30% of the total fiber mass, and the amount of aramid fiber used is 10-20% of the total fiber mass.

3. The fire-resistant fiber composite board according to claim 1, characterized in that: Basalt fibers have a diameter of 10-15μm and a length of 5-8mm, carbon fibers have a diameter of 7-10μm and a length of 3-5mm, ceramic fibers have a diameter of 5-8μm and a length of 2-4mm, and aramid fibers have a linear density of 1.5-2.0dtex.

4. The fire-resistant fiber composite board according to claim 1, characterized in that: The bio-based resin is cashew phenol epoxy resin with an epoxy value of 0.3-0.5 ep / kg and a hydroxyl value of 0.1-0.3 ep / kg. The petroleum-based resin is bisphenol A type epoxy resin with an epoxy equivalent of 180-200 g / eq and a chlorine content of less than 0.5%.

5. The fire-resistant fiber composite board according to claim 1, characterized in that: The amount of aluminum hydroxide is 50-60% of the total mass of the composite flame retardant, the amount of dimethyl methylphosphonate is 10-20% of the total mass of the composite flame retardant, and the amount of nitrogen-phosphorus intumescent flame retardant is 20-30% of the total mass of the composite flame retardant.

6. The fire-resistant fiber composite board according to claim 1, characterized in that: Silica aerogel consists of particles with a diameter of 50-100 μm and a density of 0.05-0.2 g / cm³. 3 Specific surface area ≥800m² 2 / g.

7. The fire-resistant fiber composite board according to claim 1, characterized in that: Release agents include one or more combinations of zinc stearate, calcium stearate, and polyvinyl alcohol.

8. The fire-resistant fiber composite board according to claim 1, characterized in that: The curing agent includes one or more of methyl ethyl ketone peroxide, cyclohexanone peroxide, and tert-butyl peroxide.

9. A fire-resistant fiber composite board according to claim 1, characterized in that: Accelerators include one or more of cobalt isooctanoate, cobalt naphthenate, and N,N-dimethylaniline.

10. A method for preparing a fire-resistant fiber composite board as described in any one of claims 1-9, characterized in that, The following steps are involved: S1. Mix aluminum hydroxide, dimethyl methylphosphonate and nitrogen-phosphorus intumescent flame retardant, and stir at 1000-1500 r / min for 30-40 min to obtain a composite flame retardant; S2. Soak basalt fiber, carbon fiber, ceramic fiber and aramid fiber in a 2-3% silane coupling agent ethanol solution for 1-2 hours, and then dry them in an oven at 80-100℃ for 2-3 hours. S3. First, add petroleum-based resin and bio-based resin to the reactor, then add composite flame retardant, release agent, curing agent and accelerator and stir evenly. Finally, add silica aerogel and continue stirring for 20-30 minutes to obtain resin solution. S4. Mix the basalt fiber and carbon fiber treated by S2 evenly, and make a three-dimensional mesh structure using three-dimensional weaving technology. Then, immerse it in the resin liquid of S3 for pre-forming and cure it at 100-120℃ for 2-3 hours to obtain the inner fiber reinforced skeleton. S5. The ceramic fibers and aramid fibers treated in S2 are alternately laid in layers with a thickness of 0.5-1.0 mm. After spraying the resin solution of S3, they are laminated with the inner fiber-reinforced skeleton and hot-pressed at 120-140℃ and 1-2MPa pressure for 30-40 minutes to obtain the intermediate layer. S6. Immerse the glass fiber cloth in silicone resin, and after full impregnation, attach it to the surface of the intermediate layer of S5. Cure it at 150-180℃ for 1-2 hours to form an outer protective layer and obtain a fireproof fiber composite board. S7. After cutting, grinding, and trimming the fireproof fiber composite board, inspect and package it.

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