High-temperature-resistant textile fabric and preparation method thereof
By improving the three-layer structure of the thermal insulation layer of the thermal protective clothing, and by using a double cross-linked silica aerogel-montmorillonite composite layer and plasma-etched aramid fibers, the problem of insufficient stability of silica aerogel was solved, and the stability and thermal insulation performance of the material at high temperatures were improved.
Patent Information
- Application Number
- CN202511087882.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-08-05
- Publication Date
- 2025-11-21
AI Technical Summary
The compressibility limit of silica aerogel in the insulation layer of existing thermal protective clothing is low, resulting in large plastic deformation and insufficient stability after repeated use.
The insulation layer employs a three-layer structure, including a double cross-linked silica aerogel-montmorillonite composite layer, modified montmorillonite, and plasma-etched aramid fibers. Stability is improved by forming an interpenetrating network and mechanical interlocking, combining the high-temperature stability of the polytetrafluoroethylene layer with the heat resistance of the aramid fibers.
It improves the high-temperature resistance and stability of thermal protective clothing, reduces the gas thermal conductivity, enhances the compressive strength of the fabric and the bonding strength of the material at high temperatures, and provides good thermal insulation and comfort.
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Figure CN120986004A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the technical field of textile fabrics, specifically a high-temperature resistant textile fabric and its preparation method. Background Technology
[0002] Thermal protective clothing is a type of protective garment used to protect personnel working in high or ultra-high temperature conditions, preventing heat sources from causing harm to the human body. Its performance directly affects the life safety and health of personnel. In extreme heat environments or during emergency rescue operations, fully utilizing the thermal protection function of protective clothing is crucial for ensuring the safety of workers and efficiently performing tasks.
[0003] Thermal protective clothing protects the body by reducing the rate at which heat is transferred to the skin, thus delaying the onset of burns. Current thermal protective clothing typically consists of a flame-retardant layer, a waterproof layer, a heat insulation layer, and a comfort layer, from the outside in. The flame-retardant layer is usually a woven fabric composed of one or more flame-retardant fibers or high-performance fibers. It is located on the outermost layer of the fabric system and is directly exposed to flames and other forms of heat hazards. The waterproof layer is the second layer, immediately following the flame-retardant layer, and prevents external moisture from penetrating into the inner fabric layers. The heat insulation layer material must have excellent heat insulation capabilities and a certain degree of moisture permeability to facilitate sweat evaporation. Finally, the comfort layer is the innermost layer of the fabric system, in close contact with the skin, providing both comfort and flame-retardant properties. It is generally made of flame-retardant fiber woven or knitted fabric.
[0004] Currently, improvements are being made to the insulation layer using silica aerogel materials. Due to the porous network structure of silica aerogel with its nano- and micro-pore composites, it imparts excellent thermal insulation properties to the insulation layer, thereby improving the high-temperature insulation performance of fabrics in thermal protective clothing. However, despite the abundant silanyl methyl groups on the surface of the silica aerogel skeleton, its compressive strength limit is low, and after repeated use, plastic deformation increases significantly, requiring further improvement in its stability as a fabric in thermal protective clothing. Summary of the Invention
[0005] This application provides a high-temperature resistant textile fabric and its preparation method. By improving the silica aerogel in the heat insulation layer, the compressive strength of the high-temperature resistant textile fabric is further increased, and the stability of the thermal protective clothing after multiple uses is further improved.
[0006] This application provides a high-temperature resistant textile fabric, which, when worn, comprises a waterproof and breathable layer, a heat insulation layer, and a comfort layer from the outside to the inside. The heat insulation layer has a three-layer structure, comprising a sub-outer layer, a core layer, and a sub-inner layer. The core layer is mainly composed of double-crosslinked silica aerogel, modified montmorillonite, and cellulose nanocrystals. One side of the sub-outer layer is laminated to the waterproof and breathable layer, and the other side of the sub-outer layer is laminated to the core layer. The main components of the sub-outer layer include waterborne polyurethane and montmorillonite. One side of the sub-inner layer is laminated to the comfort layer, and the other side of the sub-inner layer is laminated to the core layer. The main component of the sub-inner layer is aramid fiber based on plasma etching.
[0007] By adopting the above technical solution, the thermal insulation layer in this application has a three-layer structure, with the most important core layer being a double-crosslinked aerogel-montmorillonite composite layer. The aerogel nanopores confine the mean free path of air molecules within a certain range, thereby reducing the gas thermal conductivity. The double bonds of vinyltriethoxysilane, after curing, form an interpenetrating network with the Si-CH3 of methyltrimethoxysilane, significantly reducing the elastic modulus. Simultaneously, the Si-CH3 bond energy is higher than that of Si-OH, thus greatly improving thermal stability. Furthermore, the organic segments on vinyltriethoxysilane form an elastic network through photocrosslinking, synergistically dissipating stress with the inorganic SiO2 framework.
[0008] In addition, the montmorillonite in this application is modified by silane coupling agent and surfactant, so that the surface amino groups (-NH2) on the montmorillonite and the fluorine groups (-CF2) on the polytetrafluoroethylene on the waterproof and breathable layer form a dipole-dipole interaction, which improves the bonding energy between the two; in addition, the montmorillonite sheets are embedded in the polyurethane matrix, thereby improving the peel strength through mechanical interlocking, and thus improving the stability of high-temperature textile fabrics.
[0009] In addition, the main component of the innermost layer is aramid fiber, which forms nanogrooves through plasma etching and is then processed with Ar... + When the surface of aramid is bombarded, O2 plasma oxidizes it to generate -COOH / -OH groups, thereby increasing the surface energy of the aramid base fabric. At high temperature, it promotes the dehydration of aramid to generate a conjugated fused ring carbon layer, thereby improving the heat resistance of high temperature resistant textile fabrics.
[0010] Preferably, the main components of the double crosslinked silica aerogel include ethyl silicate, methyltrimethoxysilane, and vinyltriethoxysilane; the mass ratio of ethyl silicate, methyltrimethoxysilane, and vinyltriethoxysilane is (6-3):(4-2):(2-1).
[0011] Preferably, the raw materials for the modified intercalated montmorillonite mainly include montmorillonite, silane coupling agents, and long-chain alkylammonium salt ionic surfactants; the silane coupling agents include γ-aminopropyltriethoxysilane, 3-aminopropyltrimethoxysilane, and N-(2-aminoethyl)-3-aminopropyltrimethoxysilane; the long-chain alkylammonium salt ionic surfactants include hexadecyltrimethylammonium bromide, hexadecyltrimethylammonium chloride, octadecyltrimethylammonium chloride, and dioctadecyldimethylammonium chloride.
[0012] Preferably, the waterproof and breathable layer mainly comprises a polytetrafluoroethylene layer and a photocured fluorinated acrylate nano-coating; the comfort layer mainly comprises an aramid base fabric layer.
[0013] By adopting the above technical solution, the waterproof and breathable layer in this application is a polytetrafluoroethylene (PTFE) layer, and a fluorinated acrylate nano-coating is photocured and laminated onto the PTFE layer. The PTFE membrane achieves the function of "liquid water barrier - gaseous water permeability" through micropores of 0.1-0.5 μm. Simultaneously, the CF bond energy on PTFE is as high as 400 kJ / mol or more, enabling it to withstand a flame at 800℃ for a short period, and the decomposition products (such as CF4) at high temperatures can dilute oxygen and delay combustion.
[0014] In addition, the comfort layer is an aramid base fabric layer, in which aramid fibers can remain stable at high temperatures. The thermal decomposition temperature of aramid reaches over 500℃. At the same time, aramid fibers have a soft and comfortable touch, and have the advantages of wrinkle resistance and high elongation. Furthermore, aramid fibers have a low density and good softness, providing a good experience for the wearer when worn close to the skin.
[0015] On the other hand, this application discloses a method for preparing a high-temperature resistant textile fabric, including the preparation of a core layer, the coating of a secondary outer layer, the modification of a secondary inner layer, the preparation of a waterproof and breathable layer, the preparation of a comfort layer, and the composite of multiple layers of fabric; the preparation step of the core layer includes the following steps: S1, dispersing a certain mass of montmorillonite material in deionized water, adding a long-chain alkylammonium salt ionic surfactant, and magnetically stirring at a certain temperature for a certain time, then removing the supernatant by centrifugation, then continuing to add a long-chain alkylammonium salt ionic surfactant, while adding ethanol and a silane coupling agent, stirring at a certain temperature and centrifuging and drying to obtain modified intercalated montmorillonite; S2, mixing ethyl silicate, methyltrimethoxysilane and vinyltriethoxysilane according to... Weigh out the appropriate amount of ethanol and deionized water, stir for a certain time at a certain temperature and adjust the pH value until the solution becomes transparent to achieve pre-hydrolysis; then add cellulose nanocrystals and sonicate, then add the modified intercalated montmorillonite and continue sonication to obtain a uniformly dispersed system; S3, pour the uniformly dispersed system into a polytetrafluoroethylene mold and form a wet gel under a constant temperature water bath; S4, immerse the wet gel in anhydrous ethanol for a certain time and replace the aqueous phase at intervals, then transfer the gel to n-hexane and immerse for a certain time, then transfer the gel to TMCS / n-hexane solution for a certain time to complete surface hydrophobicity, and finally place the aerogel in a UV curing oven to obtain a double crosslinked silica aerogel.
[0016] Preferably, the coating step of the secondary outer layer includes the following steps: mixing montmorillonite material and waterborne polyurethane in deionized water at a certain ratio, then stirring magnetically for a certain time, and then degassing under vacuum for a certain time to obtain the secondary outer layer modified liquid, which is then sprayed onto the surface of the core layer and thermo-cured on the sprayed surface of the core layer.
[0017] Preferably, the modification of the sub-inner layer includes the following steps: cleaning and drying the aramid base fabric with ethanol, then placing it in a plasma chamber, introducing an argon / oxygen mixture, starting the pulsed plasma, controlling the vacuum level and processing time, to obtain the sub-inner layer.
[0018] Preferably, the preparation of the waterproof and breathable layer includes the following steps: spraying a photocurable coating containing fluorinated acrylate and nano-silica onto a polytetrafluoroethylene layer to initiate cross-linking and obtain the waterproof and breathable layer.
[0019] Preferably, the preparation of the comfort layer includes the following steps: washing and drying the aramid base fabric layer with ethanol to obtain the comfort layer.
[0020] Preferably, the composite of the multi-layered fabric includes the following steps: placing a core layer coated with the secondary outer layer in a hot press; superimposing the waterproof and breathable layer on the side of the core layer coated with the secondary outer layer; superimposing the secondary inner layer and the comfort layer on the other side of the core layer in sequence; and then controlling the temperature and pressure of the hot press to obtain a high-temperature resistant textile fabric.
[0021] One or more technical solutions provided in this application have at least the following technical effects or advantages:
[0022] 1. The core layer in this application is a double cross-linked aerogel-montmorillonite composite layer. The mean free path of air molecules is confined within a certain range through the nanopores of the aerogel, thereby reducing the thermal conductivity of the gas. The double bond of vinyltriethoxysilane is cured and forms an interpenetrating network with Si-CH3 of methyltrimethoxysilane, which greatly reduces the elastic modulus. At the same time, the Si-CH3 bond energy is higher than that of Si-OH, which greatly improves the thermal stability.
[0023] 2. The silane coupling agent in the outermost layer of this application forms a dipole-dipole interaction between the surface amino groups (-NH2) on montmorillonite and the fluorine groups (-CF2) on polytetrafluoroethylene in the waterproof and breathable layer, thereby improving the bonding energy between the two; in addition, the montmorillonite sheets are embedded in the polyurethane matrix, thereby improving the peel strength through mechanical interlocking, and thus improving the stability of the high-temperature resistant textile fabric.
[0024] 3. The main component of the innermost layer in this application is aramid fiber, and nanogrooves are formed by plasma etching, followed by Ar... + When the surface of aramid is bombarded, O2 plasma oxidizes it to generate -COOH / -OH groups, thereby increasing the surface energy of the aramid base fabric. At high temperature, it promotes the dehydration of aramid to generate a conjugated fused ring carbon layer, thereby improving the heat resistance of high temperature resistant textile fabrics.
[0025] 4. The waterproof and breathable layer of this application uses a polytetrafluoroethylene (PTFE) layer, which can achieve the function of "liquid water barrier - gaseous water permeability"; the PTFE layer can withstand flames up to 800℃ for a short period of time, and the decomposition products (such as CF4) at high temperatures can dilute oxygen and delay combustion. The comfort layer is an aramid-based fabric layer, in which aramid fibers can remain stable at high temperatures. At the same time, aramid fibers have a soft and comfortable touch, and have the advantages of wrinkle resistance and high elongation; in addition, aramid fibers have a low density and good softness, providing a good experience for the wearer against the skin. Attached Figure Description
[0026] To more clearly illustrate the technical solutions in the embodiments of the present invention, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the accompanying drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0027] Figure 1 This is a cross-sectional view of the fabric in an embodiment of this application.
[0028] Explanation of reference numerals in the attached diagram: 1. Waterproof and breathable layer; 2. Thermal insulation layer; 3. Comfort layer; 21. Secondary outer layer; 22. Core layer; 23. Secondary inner layer. Detailed Implementation
[0029] This application provides a high-temperature resistant textile fabric and its preparation method. By improving the silica aerogel in the heat insulation layer, the compressive strength of the high-temperature resistant textile fabric is further increased, and the stability of the thermal protective clothing after multiple uses is further improved.
[0030] The technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only a part of the embodiments of this application, and not all of them. All other embodiments obtained by those skilled in the art based on the embodiments of this application without creative effort are within the scope of protection of this application.
[0031] It should be noted that the terms "first," "second," etc., in the specification, claims, and accompanying drawings of this application are used to distinguish similar objects and are not necessarily used to describe a specific order or sequence. It should be understood that such data can be interchanged where appropriate so that the embodiments of this application described herein can be implemented in orders other than those illustrated or described herein. Furthermore, the terms "comprising" and "having," and any variations thereof, are intended to cover non-exclusive inclusion; for example, a process, method, system, product, or server that comprises a series of steps or units is not necessarily limited to those steps or units explicitly listed, but may include other steps or modules not explicitly listed or inherent to such processes, methods, products, or devices.
[0032] raw material
[0033] Ethyl silicate CAS No.: 1109-96-2 Molecular weight: 520.661 Purity: 95.0%;
[0034] Methyltrimethoxysilane CAS No.: 1185-55-3 Molecular weight: 136.222 Purity: 98.0%;
[0035] Vinyltriethoxysilane CAS No.: 78-08-0 Molecular weight: 190.312 Purity: 98.0%;
[0036] Montmorillonite: This application uses commercially available organic montmorillonite with a particle size of 800 mesh, montmorillonite content ≥98%, density of 30 g / cm³, and apparent viscosity of 20 mPa·s.
[0037] Aramid base fabric: This application uses commercially available aramid base fabric; the main component is Kevlar fiber; the basis weight is 60-70 (g / ㎡);
[0038] Example
[0039] Example 1
[0040] The preparation of the high-temperature resistant textile fabric in this application includes six steps, namely the preparation of the core layer, the coating of the outermost layer, the modification of the innermost layer, the preparation of the waterproof and breathable layer, the preparation of the comfort layer, and the composite of multiple layers of fabric.
[0041] The preparation of the core layer includes the following steps:
[0042] 100g of montmorillonite material was dispersed in 2.0L of deionized water, and 20g of hexadecyltrimethylammonium bromide was added. The mixture was magnetically stirred at 70℃ for 4h, and then the supernatant was removed by centrifugation. The mixture was washed three times with ethanol until no bromide ions were detected (no precipitate was detected by AgNO3). Then, 20g of hexadecyltrimethylammonium bromide, 500ml of ethanol, and 10g of γ-aminopropyltriethoxysilane were added. The mixture was stirred and centrifuged at 60℃, and finally dried at 60℃ for 12 hours to obtain modified intercalated montmorillonite.
[0043] S2. Weigh the ethyl silicate, methyltrimethoxysilane, and vinyltriethoxysilane according to the following proportions: 6 mol (1.25 L) of ethyl silicate, 3 mol (0.45 L) of methyltrimethoxysilane, and 1 mol (0.21 L) of vinyltriethoxysilane.
[0044] Add 18.4 L of ethanol and 2.16 L of deionized water, and adjust the pH to 4.5 with 0.1 M HCl; stir at 25 °C for 5 h until the solution becomes clear to achieve pre-hydrolysis;
[0045] Then, 5g of cellulose nanocrystals were added and ultrasonically treated, followed by the addition of 100g of modified intercalated montmorillonite and continued ultrasonic treatment to ensure that the modified intercalated montmorillonite sheets did not agglomerate, resulting in a uniformly dispersed system. The cellulose nanocrystals formed hydrogen bonds with the modified intercalated montmorillonite sheets through surface hydroxyl groups, inhibiting MMT agglomeration. The amino groups (-NH2) of the intercalated montmorillonite condensed with silanols to form Si-O-Si bonds, enhancing interfacial bonding.
[0046] S3. Pour the uniformly dispersed system into a polytetrafluoroethylene mold and form a wet gel in a constant temperature water bath at 60°C.
[0047] S4. Soak the wet gel in anhydrous ethanol for 12 hours and replace the aqueous phase every 4 hours. Then, transfer the gel to n-hexane and soak for 12 hours. Then, transfer the gel to TMCS / n-hexane (volume ratio 1:5) solution for 24 hours to complete the surface hydrophobicization. Finally, place the aerogel in a UV curing oven to obtain double crosslinked silica aerogel.
[0048] The application of the outermost layer includes the following steps:
[0049] 200g of commercially available organic montmorillonite and 450g of waterborne polyurethane were mixed in 1.5L of deionized water, then magnetically stirred for 6 hours, and then vacuum degassed for 6 hours to obtain the secondary outer layer modified liquid, which was sprayed onto the surface of the core layer and then thermo-cured on the sprayed surface of the core layer.
[0050] The modification of the innermost layer includes the following steps:
[0051] Commercially available aramid base fabric was cleaned three times with ethanol and dried. Then it was placed in a plasma chamber and an argon / oxygen mixture (4:1, flow rate 50 sccm, vacuum degree 5 Pa) was introduced. Pulsed plasma (power 200W, duty cycle 50%) was started for 5 minutes and then quickly superimposed on one side of the core layer for the next step of processing.
[0052] The preparation of the waterproof and breathable layer and the comfort layer is consistent with the existing technology; the waterproof and breathable layer is obtained by spraying a light-curing coating containing fluorinated acrylate and nano silica onto a polytetrafluoroethylene layer to initiate cross-linking; the comfort layer is prepared by washing and drying an aramid base fabric layer with ethanol.
[0053] The lamination of multi-layered fabrics includes the following steps:
[0054] The core layer coated with the outermost layer is placed in a hot press; a waterproof and breathable layer is superimposed on the side of the core layer coated with the outermost layer; the innermost layer and the comfort layer are superimposed on the other side of the core layer in sequence, and then the temperature of the hot press is controlled at 150℃, the pressure at 1MPa, and the time at 5 minutes; the pressure is maintained and cooled to below 50℃, and the composite fabric is taken out to obtain a high-temperature resistant textile fabric.
[0055] Reference Figure 1 The high-temperature resistant textile fabric prepared in this application has a three-layer main structure, which, from the outside to the inside, includes a waterproof and breathable layer 1, a heat insulation layer 2, and a comfort layer 3. The comfort layer 3 is a layer of fabric close to the human body surface, while the waterproof and breathable layer 1 is a layer of fabric away from the human body surface.
[0056] Specifically, the insulation layer 2 has a three-layer structure, which includes a secondary outer layer 21, a core layer 22, and a secondary inner layer 23 in sequence. One side of the secondary outer layer 21 is bonded to the waterproof and breathable layer 1, and the other side of the secondary outer layer 21 is bonded to the core layer 22; one side of the secondary inner layer 23 is bonded to the comfort layer 3, and the other side of the secondary inner layer 23 is bonded to the core layer 22.
[0057] Examples 2-4
[0058] The difference between Examples 2-4 and Example 1 is that the proportions of ethyl silicate, methyltrimethoxysilane, and vinyltriethoxysilane added to the double crosslinked silica aerogel are different during the preparation of the core layer, as summarized in Table 1 below.
[0059] Table 1. Component Proportions of Double Crosslinked Silica Aerogels in Examples 1-4
[0060] Ethyl silicate Methyltrimethoxysilane Vinyltriethoxysilane Example 1 6mol 3mol 1mol Example 2 5mol 4mol 2mol Example 3 4mol 2mol 1mol Example 4 3mol 3mol 2mol
[0061] Examples 5-9
[0062] The difference between Examples 5-9 and Example 1 lies in the selection of raw materials for the modified intercalated montmorillonite, as summarized in Table 2 below.
[0063] Table 2, Raw material ratio table for modified intercalated montmorillonite in Examples 1 and 5-9
[0064]
[0065] Comparative Example
[0066] Comparative Example 1
[0067] The difference between Comparative Example 1 and Example 1 is that, in the preparation of the core layer 22, a traditional silica aerogel framework was used instead of a double cross-linked aerogel and montmorillonite composite to form the core layer 22.
[0068] The difference between Comparative Example 2 and Example 1 is that, in the preparation of the heat insulation layer 2, the outermost layer 21 was not used to coat one side of the core layer 22.
[0069] The difference between Comparative Example 3 and Example 1 is that, in the preparation of the insulation layer 2, the innermost layer 23 was not laminated onto the other side of the core layer 22. Performance testing experiment.
[0070] To further investigate the effects of each component and preparation parameters on high-temperature resistant textile fabrics, this application further conducts the following verification examples.
[0071] The high-temperature resistant textile fabrics prepared in each example and each comparative example were subjected to performance testing in accordance with Examples 1-9 and Comparative Examples 1-3.
[0072] 1. Flame retardant performance test
[0073] According to GB / T5455-2014 "Determination of Vertical Damage Length, Afterflame and Afterburning Time of Textiles", the afterburning time, afterflame time and damage length of the test sample are tested.
[0074] 2. Thermal insulation performance test
[0075] According to GB / T 39074-2020 "Test and Evaluation of Thermal Insulation Performance of Textiles", thermal insulation textile fabrics must be thermally insulated. Under certain pressure, when the sample is in contact with the heat source for 30 seconds, the temperature of the surface in contact with human skin must be <70℃. After 3 minutes of contact, there must be no scorching or melting marks on the surface in contact with the heat source. Based on the standard, this application classifies thermal insulation products into grades from high to low as "*", "+", and "-".
[0076] 3. Thermal stability test
[0077] The high-temperature resistant textile fabric prepared in this application was tested according to the standard of GB / T 39074-2020 "Test and Evaluation of Thermal Insulation Performance of Textiles". It was placed in environments of 150℃, 200℃, 250℃ and 300℃ for 3 minutes respectively, and then removed and cooled to room temperature. The thermal insulation test was then repeated 10 times. The modulus retention rate and tensile strength retention rate of the high-temperature resistant textile fabric were then tested using an Instron universal testing machine. The modulus retention rate and tensile strength retention rate of the high-temperature resistant textile fabric that did not undergo thermal insulation testing were taken as 100%.
[0078] Table 3, Performance Test Tables of Examples 1-9 and Comparative Examples 1-3
[0079]
[0080] Conclusion Analysis
[0081] Based on the test data, Examples 1-4 were first analyzed. During the preparation of the core layer 22, the addition ratios of ethyl silicate, methyltrimethoxysilane, and vinyltriethoxysilane in the double-crosslinked silica aerogel were different. By adjusting the different ratios of these three components, the ratio of Si-CH3 in the double-crosslinked silica aerogel was increased, thereby optimizing the physical structure of the core layer 22 and improving the heat resistance and thermal stability of the high-temperature resistant textile fabric. Based on the data analysis, Example 1 is the most preferred embodiment.
[0082] Based on the data analysis of Examples 1 and 5-9, the difference between Examples 1 and 5-9 lies in the choice of raw materials for the modified intercalated montmorillonite. Because the silane coupling agent on the modified intercalated montmorillonite forms a dipole-dipole interaction between the surface amino groups (-NH2) on the montmorillonite and the fluorine groups (-CF2) on the polytetrafluoroethylene in the waterproof and breathable layer 1, the stability of the high-temperature resistant textile fabric can be improved. According to the data comparison between Examples 1 and 5-9, when the silane coupling agent is γ-aminopropyltriethoxysilane and the surfactant is bis(octadecyl)dimethylammonium chloride, better thermal stability is achieved; therefore, Example 7 is the optimal example.
[0083] In addition, an analysis was conducted between Example 1 and Comparative Example 1. The difference between Comparative Example 1 and Example 1 is that, in the preparation process of the core layer 22, a traditional silica aerogel framework was used, and the core layer 22 was not formed by combining double cross-linked aerogel with montmorillonite.
[0084] Compared to traditional silica aerogel frameworks, the hydrolysis and condensation reactions of silicon sources generate Si-OH bonds, intermediate products containing hydroxyl groups. Furthermore, the surface chemistry of silica aerogels also contributes to the formation of Si-OH bonds in subsequent reactions. The Si-CH3 network formed by the technology used in this application, due to the higher bond energy of Si-CH3 compared to Si-OH, can improve the elastic modulus of high-temperature resistant textile fabrics. Therefore, the thermal stability of the high-temperature resistant textile fabric in Comparative Example 1 is lower than that in Example 1.
[0085] Furthermore, comparing Example 1 with Comparative Example 2, the difference between Comparative Example 2 and Example 1 is that, in the preparation of the heat insulation layer 2, the outermost layer 21 was not used to coat one side of the core layer 22. In Comparative Example 2, montmorillonite sheets were not embedded in the polyurethane matrix, so mechanical interlocking was not used to improve peel strength, resulting in a lower thermal stability of the high-temperature textile fabric compared to Example 1.
[0086] Finally, comparing Example 1 and Comparative Example 3, the difference between Comparative Example 3 and Example 1 lies in the fact that, in the preparation of the heat insulation layer 2, the innermost layer 23 was not laminated onto the other side of the core layer 22. In Example 1, the core layer 22 was not directly laminated to the fabric of the comfort layer 3. Instead, plasma etching was performed on the aramid base in contact with the core layer 22, forming nanogrooves on the surface of the aramid base fabric. This increased the surface energy of the aramid base fabric, promoting dehydration of the aramid at high temperatures to generate a conjugated fused ring carbon layer, thereby improving the heat resistance of the high-temperature resistant textile fabric. Therefore, the high-temperature resistance of Example 1 is slightly better than that of Comparative Example 1.
[0087] It should be noted that the order of the embodiments described above is merely for descriptive purposes and does not represent the superiority or inferiority of the embodiments. Furthermore, specific embodiments have been described above. Other embodiments are within the scope of the appended claims. In some cases, the actions or steps described in the claims can be performed in a different order than that shown in the embodiments and still achieve the desired result. Additionally, the processes depicted in the drawings do not necessarily require a specific or sequential order to achieve the desired result. In some embodiments, multitasking and parallel processing are also possible or may be advantageous.
[0088] The above description is only a preferred embodiment of this application and is not intended to limit this application. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this application should be included within the protection scope of this application.
[0089] This specification and accompanying drawings are merely illustrative examples of this application and are intended to cover any and all modifications, variations, combinations, or equivalents within the scope of this application. Clearly, those skilled in the art can make various alterations and modifications to this application without departing from its scope. Therefore, if such modifications and modifications fall within the scope of this application and its equivalents, this application intends to include such modifications and modifications.
Claims
1. A high-temperature resistant textile fabric, characterized in that, The fabric, when worn, includes a waterproof and breathable layer, a heat insulation layer, and a comfort layer from the outside to the inside. The heat insulation layer has a three-layer structure, which includes a secondary outer layer, a core layer and a secondary inner layer in sequence; the raw materials of the core layer mainly include double cross-linked silica aerogel, modified montmorillonite and cellulose nanocrystals. One side of the sub-outer layer is bonded to the waterproof and breathable layer, and the other side of the sub-outer layer is bonded to the core layer. The main components of the sub-outer layer include waterborne polyurethane and montmorillonite. One side of the sub-inner layer is laminated to the comfort layer, and the other side of the sub-inner layer is laminated to the core layer. The main component of the sub-inner layer is aramid fiber based on plasma etching.
2. The high-temperature resistant textile fabric as described in claim 1, characterized in that, The main components of the double crosslinked silica aerogel include ethyl silicate, methyltrimethoxysilane and vinyltriethoxysilane; the mass ratio of ethyl silicate, methyltrimethoxysilane and vinyltriethoxysilane is (6-3):(4-2):(2-1).
3. The high-temperature resistant textile fabric as described in claim 2, characterized in that, The raw materials for the modified intercalated montmorillonite mainly include montmorillonite, silane coupling agents, and long-chain alkylammonium salt ionic surfactants. The silane coupling agent includes γ-aminopropyltriethoxysilane, 3-aminopropyltrimethoxysilane, and N-(2-aminoethyl)-3-aminopropyltrimethoxysilane; The long-chain alkylammonium salt ionic surfactants include hexadecyltrimethylammonium bromide, hexadecyltrimethylammonium chloride, octadecyltrimethylammonium chloride, and dioctadecyldimethylammonium chloride.
4. The high-temperature resistant textile fabric as described in claim 1, characterized in that, The waterproof and breathable layer mainly comprises a polytetrafluoroethylene layer and a photocured fluorinated acrylate nano-coating; the comfort layer mainly comprises an aramid base fabric layer.
5. A method for preparing a high-temperature resistant textile fabric as described in any one of claims 1-4, characterized in that, This includes the preparation of the core layer, the coating of the outermost layer, the modification of the innermost layer, the preparation of the waterproof and breathable layer, the preparation of the comfort layer, and the composite of multiple layers of fabric; The preparation steps of the core layer include the following steps: S1. A certain mass of montmorillonite material is dispersed in deionized water, and long-chain alkylammonium salt ionic surfactants are added. The mixture is magnetically stirred at a certain temperature for a certain time. Then, the supernatant is removed by centrifugation. Long-chain alkylammonium salt ionic surfactants are added, along with ethanol and silane coupling agent. The mixture is stirred at a certain temperature and then centrifuged and dried to obtain modified intercalated montmorillonite. S2. Weigh ethyl silicate, methyltrimethoxysilane and vinyltriethoxysilane in proportion, add a certain proportion of ethanol and deionized water, stir at a certain temperature for a certain time and adjust the pH value until the solution is transparent to achieve pre-hydrolysis; then add cellulose nanocrystals and sonicate, then add the modified intercalated montmorillonite and continue sonication to obtain a uniformly dispersed system. S3. Pour the uniformly dispersed system into a polytetrafluoroethylene mold and form a wet gel under a constant temperature water bath. S4. The wet gel is soaked in anhydrous ethanol for a certain period of time, and the aqueous phase is replaced at intervals. Then the gel is transferred to n-hexane and soaked for a certain period of time. Then the gel is transferred to TMCS / n-hexane solution for a certain period of time to complete the surface hydrophobicity. Finally, the aerogel is placed in a UV curing oven to obtain double crosslinked silica aerogel.
6. The method for preparing high-temperature resistant textile fabric as described in claim 5, characterized in that, The coating process for the outermost layer includes the following steps: Montmorillonite material and waterborne polyurethane are mixed in deionized water in a certain proportion, then magnetically stirred for a certain time, and then vacuum degassed for a certain time to obtain the outermost modified liquid, which is then sprayed onto the surface of the core layer and thermo-cured on the sprayed surface of the core layer.
7. The method for preparing high-temperature resistant textile fabric as described in claim 6, characterized in that, The modification of the sub-inner layer includes the following steps: The aramid base fabric is cleaned and dried with ethanol, then placed in a plasma chamber, and an argon / oxygen mixture is introduced. The pulsed plasma is started, and the vacuum level and processing time are controlled to obtain the inner layer.
8. The method for preparing high-temperature resistant textile fabric as described in claim 7, characterized in that, The preparation of the waterproof and breathable layer includes the following steps: A light-cured coating containing fluorinated acrylate and nano-silica is sprayed onto a polytetrafluoroethylene layer to induce cross-linking and obtain a waterproof and breathable layer.
9. The method for preparing high-temperature resistant textile fabric as described in claim 8, characterized in that, The preparation of the comfort layer includes the following steps: the aramid base fabric layer is washed and dried with ethanol to obtain the comfort layer.
10. The method for preparing high-temperature resistant textile fabric as described in claim 9, characterized in that, The composite of the multi-layered fabric includes the following steps: placing a core layer coated with the outermost layer in a hot press; stacking the waterproof and breathable layer on the side of the core layer coated with the outermost layer; stacking the innermost layer and the comfort layer on the other side of the core layer in sequence; and then controlling the temperature and pressure of the hot press to obtain a high-temperature resistant textile fabric.