Fireproof cloak with aerogel composite multilayer structure

Abstract

The invention discloses a fireproof cloak with an aerogel composite multi-layer structure, and belongs to the technical field of fireproof cloaks. Comprising an outer layer, a middle layer and an inner layer, wherein the outer layer is made of carbon fiber cloth; the middle layer is made of modified aerogel; and the inner layer is made of breathable flame-retardant cloth. According to the prepared cloak, the outer layer is the carbon fiber cloth, the carbon fiber structure is stable, middle-layer aerogel can be protected, external mechanical damage can be borne, the mass is light, and the wearing burden is reduced; the middle layer of the prepared cloak is the modified aerogel, so that the cloak is endowed with excellent heat insulation property and fire resistance; the inner layer of the prepared cloak is the aramid staple fiber needle-punched cloth, so that the cloak has the fireproof performance and also has certain wearing comfort; in conclusion, through the three-layer composite design of the carbon fiber outer layer, the modified aerogel middle layer and the aramid fiber inner layer, the composite material has the advantages of being ultra-light, high in fireproof performance and high in comfort and has important application value in the technical field of fireproof cloaks.

Description

Technical Field

[0001] The present invention belongs to the technical field of fireproof cloaks, and in particular relates to a fireproof cloak with an aerogel composite multi-layer structure. Background Art

[0002] With the rapid development of modern industrialization and urbanization, the frequency and severity of fire accidents have increased year by year, posing a serious threat to people's lives and property. In the field of fire escape and emergency protection, fireproof capes are an important personal protective equipment, and their performance is directly related to the life safety of the user.

[0003] Traditional fireproof cloaks, mostly made of fiberglass, have long dominated the market for emergency escape and industrial protection, thanks to their relatively low production costs and generally acceptable insulation performance. However, with technological advancements and rising user demands for safety and user experience, the drawbacks of traditional fiberglass cloaks have gradually become apparent. First, fiberglass itself carries significant health risks. Its fibers are easily shed and inhaled, and long-term exposure can cause respiratory illnesses and even skin irritation and damage. Second, traditional fiberglass cloaks offer limited thermal insulation. In high-temperature environments, they often struggle to effectively block heat transfer for long periods, effectively preventing the wearer from escaping. Furthermore, these cloaks are dense, creating a noticeable weight when worn, hindering mobility and potentially delaying escape in critical situations. Furthermore, their brittle material and poor tear resistance make them susceptible to damage during folding, carrying, or use, significantly compromising their protective effectiveness and creating a poor user experience.

[0004] In recent years, the rapid development of nanomaterial technology has opened up new possibilities for the innovation of fireproofing materials. Aerogel, an emerging nanoporous material, has attracted considerable attention due to its ultra-lightness, ultra-thinness, and excellent thermal insulation properties. Aerogel's unique structure enables it to effectively block the transfer of high-temperature heat while maintaining an extremely low density and excellent flexibility. These properties make it an ideal choice for fireproof cloaks. However, pure aerogel materials still face challenges in practical applications, such as insufficient mechanical strength and flame retardancy. Therefore, addressing these issues is urgent to meet the increasing demands of fireproof cloak technology. Summary of the Invention

[0005] The purpose of the present invention is to overcome the defects of the prior art and provide a fireproof cloak with an aerogel composite multi-layer structure.

[0006] The purpose of the present invention can be achieved through the following technical solutions: A fireproof cloak with an aerogel composite multilayer structure comprises an outer layer, a middle layer and an inner layer; wherein the outer layer is made of carbon fiber cloth; the middle layer is made of modified aerogel; and the inner layer is made of breathable flame-retardant cloth.

[0007] As a further technical solution, the carbon fiber cloth is T700 grade carbon fiber woven cloth, with a single fiber diameter of 7-8 μm and a surface density of 200-250 g / m 2 .

[0008] As a further technical solution, the modified aerogel is prepared by the following steps: A1. Under a nitrogen atmosphere, add the reaction raw material 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and the reaction solvent N,N-dimethylformamide to a dry three-necked flask. Mechanically stir for 10-20 minutes to accelerate the dissolution of DOPO. Then add phosphorus pentasulfide and heat the apparatus until the temperature reaches 70-80°C. Keep stirring for 5-6 hours. After the reaction is complete, post-process and obtain the primary product. A2. Under a nitrogen atmosphere, add the reaction raw material, vinyltrimethoxysilane, and the reaction solvent toluene to a dry three-necked flask, stir evenly, and then add azobisisobutyronitrile (initiator). Heat the apparatus until the temperature reaches 80-85°C. Under magnetic stirring, keep the temperature for 6-8 hours. After the reaction is complete, post-process and obtain the modifier. A3. Mix ethyl orthosilicate, ethanol and water, add hydrochloric acid solution (mass fraction 12%) to adjust the pH to 3-4, and magnetically stir for 30-60 minutes to form a uniform sol; then add the modifier and continue stirring for 1-1.5 hours. After stirring, add ammonia water (mass fraction 28%) dropwise to adjust the pH to 5-6, and let it stand at room temperature for 12-24 hours to form a wet gel. Soak it in ethanol for 24-48 hours to remove unreacted monomers, and then replace ethanol with liquid CO2. Finally, dry it in a supercritical CO2 drying equipment for 8-12 hours to obtain a modified aerogel.

[0009] As a further technical solution, in step A1, the ratio of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, N,N-dimethylformamide, and phosphorus pentasulfide is 21.6 g:100 mL:6.9-7.3 g.

[0010] As a further technical solution, the ratio of the initial product, vinyltrimethoxysilane, toluene, and azobisisobutyronitrile used in step A2 is 25.9 g:14.8 g:120 mL:0.31 g.

[0011] As a further technical solution, in step A3, the ratio of the amount of ethyl orthosilicate, ethanol, water, and modifier is 9.9-11.3 g:50 mL:5 mL:3.1-3.7 g.

[0012] The reaction formula of step A1 of the present invention is as follows: The present invention first uses phosphorus pentasulfide to react with DOPO to introduce the S element, and then reacts it with vinyltrimethoxysilane under the catalysis of azobisisobutyronitrile to undergo a nucleophilic addition reaction to obtain a modifier. During the process, the modifier is hydrolyzed to -Si(OH)3, which reacts with the SiO2 network derived from ethyl orthosilicate through a condensation reaction to form Si-O-Si bonds, ultimately obtaining a modified aerogel.

[0013] Compared with ordinary aerogels, the modified aerogel prepared by the present invention introduces DOPO. The decomposition products of DOPO (PO·, HPO· free radicals) can capture H· and OH· free radicals in the combustion chain reaction, inhibiting flame propagation; and can also generate phosphoric acid substances to promote carbonization. Finally, the introduced sulfur element can act synergistically with DOPO to further improve the flame retardant properties of the aerogel.

[0014] As a further technical solution, the breathable flame retardant fabric is aramid 1313 staple fiber needle punched fabric with a surface density of 100-120g / m 2 .

[0015] Beneficial effects of the present invention: Advantages 1. The outer layer of the cloak prepared by the present invention is carbon fiber cloth. The carbon fiber structure is stable, can protect the middle layer aerogel, and can withstand external mechanical damage. It is light in weight and reduces the burden of wearing. Advantage 2: The middle layer of the cloak prepared by the present invention is modified aerogel, which gives the cloak excellent thermal insulation and fire resistance; Advantage 3: The inner layer of the cloak made by the present invention is aramid staple fiber needle-punched cloth, which has fire resistance and is comfortable to wear; In summary, the present invention solves the core pain points of traditional fireproof cloaks, such as bulkiness, brittleness, and insufficient thermal insulation, through a three-layer composite design of a carbon fiber outer layer, a modified aerogel middle layer, and an aramid inner layer. It is ultra-light, highly fireproof, and highly comfortable, and has important application value in the field of fireproof cloak technology. DETAILED DESCRIPTION

[0016] The following is a clear and complete description of the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts are within the scope of protection of the present invention.

[0017] Example 1 Preparation of modified aerogel: A1. Under a nitrogen atmosphere, add 21.6 g of the reaction raw material 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and 100 mL of the reaction solvent N,N-dimethylformamide to a dry three-necked flask. Stir mechanically for 10 minutes to accelerate the dissolution of DOPO. Then add 6.9 g of phosphorus pentasulfide and heat the apparatus until the temperature reaches 70°C. Keep stirring for 5 hours. After the reaction is complete, cool to room temperature in an ice bath. Filter to remove unreacted azobisisobutyronitrile residue, rotary evaporate, wash with n-hexane, and dry to obtain a primary product. A2. Under a nitrogen atmosphere, 25.9 g of the initial product, 14.8 g of vinyltrimethoxysilane, and the reaction solvent toluene were added to a dry three-necked flask. After stirring, azobisisobutyronitrile was added and the apparatus was heated until the temperature reached 80 ° C. Under magnetic stirring, the reaction was kept warm for 6 h. After the reaction was completed, the mixture was filtered, rotary evaporated, and purified by group chromatography to obtain a modifier. A3. Mix 9.9 g of tetraethyl orthosilicate, 50 mL of ethanol, and 5 mL of water, add hydrochloric acid solution (mass fraction 12%) to adjust the pH to 3, and stir magnetically for 30 minutes to form a uniform sol; then add 3.1 g of modifier and continue stirring for 1 hour. After stirring, add ammonia water (mass fraction 28%) dropwise and adjust the pH to 5. Let it stand at room temperature for 12 hours to form a wet gel, which is then soaked in ethanol for 24 hours to remove unreacted monomers, and then replace the ethanol with liquid CO2. Finally, dry it in a supercritical CO2 drying equipment for 8-12 hours to obtain a modified aerogel; A fireproof cloak with an aerogel composite multilayer structure is prepared by the following steps: The diameter of the monofilament is 7 μm and the surface density is 200 g / m 2 The T700 grade carbon fiber woven cloth was spread flat on the workbench, and a layer of silicone resin was evenly applied on the surface with a thickness of 0.05mm. The modified aerogel was then laminated on the carbon fiber woven cloth, rolled three times with a roller press, and placed in a 120℃ oven for 2h to form an "outer layer-middle layer" composite structure. The surface density of the aerogel was 100g / m 2 The aramid 1313 staple fiber needle-punched cloth is laid flat, and the surface is also coated with a thin silicone resin with a thickness of 0.05mm. It is then bonded to the "outer layer-middle layer" composite structure and placed in a 120℃ oven for 2 hours to complete the composite curing of the three-layer structure. The composite fabric is then cut according to the design size of the cloak, and Velcro is sewn at the collar for wearing and fixing, thus obtaining a fire-resistant cloak with an aerogel composite multi-layer structure.

[0018] Example 2 Preparation of modified aerogel: A1. Under a nitrogen atmosphere, add 21.6 g of the reaction raw material 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and 100 mL of the reaction solvent N,N-dimethylformamide to a dry three-necked flask. Stir mechanically for 20 min to accelerate the dissolution of DOPO. Then add 7.3 g of phosphorus pentasulfide and heat the apparatus until the temperature reaches 80°C. Keep stirring for 6 h. After the reaction is complete, cool to room temperature in an ice bath. Filter to remove unreacted azobisisobutyronitrile residue, rotary evaporate, wash with n-hexane, and dry to obtain a primary product. A2. Under a nitrogen atmosphere, 25.9 g of the initial product, 14.8 g of vinyltrimethoxysilane, and toluene as the reaction solvent were added to a dry three-necked flask. After stirring, azobisisobutyronitrile was added and the apparatus was heated until the temperature reached 85 ° C. Under magnetic stirring, the reaction was kept warm for 8 h. After the reaction was completed, the mixture was filtered, rotary evaporated, and purified by group chromatography to obtain a modifier. A3. Mix 11.3 g of ethyl orthosilicate, 50 mL of ethanol, and 5 mL of water, add hydrochloric acid solution (mass fraction 12%) to adjust the pH to 4, and magnetically stir for 60 min to form a uniform sol; then add 3.7 g of modifier and continue stirring for 1.5 h. After stirring, add ammonia water (mass fraction 28%) dropwise to adjust the pH to 6, and let it stand at room temperature for 24 h to form a wet gel, which is then soaked in ethanol for 48 h to remove unreacted monomers, and then the ethanol is replaced with liquid CO2. Finally, it is dried in a supercritical CO2 drying equipment for 12 h to obtain a modified aerogel; A fireproof cloak with an aerogel composite multilayer structure is prepared by the following steps: The diameter of the monofilament is 8 μm and the surface density is 250 g / m 2 The T700 grade carbon fiber woven cloth was spread flat on the workbench, and a layer of silicone resin was evenly applied on the surface with a thickness of 0.05mm. The modified aerogel was then laminated on the carbon fiber woven cloth, rolled three times with a roller press, and placed in a 120℃ oven for 2h to form an "outer layer-middle layer" composite structure. The surface density of the aerogel was 120g / m 2 The aramid 1313 staple fiber needle-punched cloth is laid flat, and the surface is also coated with a thin silicone resin with a thickness of 0.05mm. It is then bonded to the "outer layer-middle layer" composite structure and placed in a 120℃ oven for 2 hours to complete the composite curing of the three-layer structure. The composite fabric is then cut according to the design size of the cloak, and Velcro is sewn at the collar for wearing and fixing, thus obtaining a fire-resistant cloak with an aerogel composite multi-layer structure.

[0019] Comparative Example 1 The only difference between this comparative example and Example 2 is that in this comparative example, unmodified ordinary aerogel is used.

[0020] Comparative Example 2 Use a fiberglass cape.

[0021] The following performance tests were performed on Examples 1 and 2 and Comparative Examples 1 and 2: Adopting GB / T 5455-2014 standard, the time for the back temperature to rise to 60°C under a 1200°C flame is tested (≥30 minutes is qualified); Use GB / T 5455-2014 standard to determine vertical burning grade; GB / T 3917.3-2009 standard was used to determine the tear strength; Adopt GB / T 5453-1997 standard to measure air permeability; The measured results are shown in the following table: Test items Example 1 Example 2 Comparative Example 1 Comparative Example 2 Insulation time (1200℃) / min 32 35 26 19 Flame retardant grade (UL94) V0 V0 V1 V1 Tear strength / N 45 48 47 36 Air permeability mm / s 550 550 550 320 It can be seen from the above table that the cloak prepared in the embodiment of the present invention has good thermal insulation, flame retardancy, mechanical properties, and therefore, the present invention has important application value in the field of fireproof cloak technology.

[0022] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the invention can be embodied in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as illustrative and non-restrictive, and the scope of the invention is defined by the appended claims rather than the foregoing description, and it is intended that all variations that come within the meaning and range of equivalents of the claims be embraced therein.

Claims

1. A fireproof cloak with an aerogel composite multilayer structure, characterized in that: It comprises an outer layer, a middle layer and an inner layer. The outer layer is made of carbon fiber cloth; the middle layer is made of modified aerogel; and the inner layer is made of breathable flame-retardant cloth.

2. The fireproof cloak of aerogel composite multilayer structure according to claim 1, characterized in that: The modified aerogel is prepared by the following steps: A1. Under a nitrogen atmosphere, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and N,N-dimethylformamide were mechanically stirred for 10-20 minutes, and then phosphorus pentasulfide was added. The reaction was stirred at 70-80°C for 5-6 hours. The reaction was completed to obtain a primary product. A2. Under a nitrogen atmosphere, the primary product, vinyltrimethoxysilane, and toluene were stirred evenly, and then azobisisobutyronitrile was added. The mixture was stirred at 80-85°C for 6-8 hours. The reaction was completed to obtain a modifier. A3. Mix ethyl orthosilicate, ethanol and water, adjust the pH to 3-4, stir for 30-60 minutes, then add the modifier and continue stirring for 1-1.5 hours. After stirring, adjust the pH to 5-6, let it stand at room temperature for 12-24 hours, soak it in ethanol for 24-48 hours, replace the ethanol with liquid CO2, and finally dry it in a supercritical CO2 drying equipment for 8-12 hours to obtain a modified aerogel.

3. The fireproof cloak of aerogel composite multilayer structure according to claim 2, characterized in that: In step A1, the ratio of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, N,N-dimethylformamide, and phosphorus pentasulfide is 21.6 g:100 mL:6.9-7.3 g.

4. The fireproof cloak of aerogel composite multilayer structure according to claim 2, characterized in that: In step A2, the ratio of the initial product, vinyltrimethoxysilane, toluene, and azobisisobutyronitrile is 25.9 g:14.8 g:120 mL:0.31 g.

5. The fireproof cloak of aerogel composite multilayer structure according to claim 2, characterized in that: In step A3, the ratio of ethyl orthosilicate, ethanol, water, and modifier is 9.9-11.3 g:50 mL:5 mL:3.1-3.7 g.

6. The fireproof cloak of aerogel composite multilayer structure according to claim 1, characterized in that: The carbon fiber cloth is T700 grade carbon fiber woven cloth, with a single filament diameter of 7-8 μm and a surface density of 200-250 g / m 2 .

7. The fireproof cloak of aerogel composite multilayer structure according to claim 1, characterized in that: The breathable flame retardant fabric is aramid 1313 staple fiber needle punched fabric with a surface density of 100-120g / m 2 .

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