Self-response temperature-adjusting flame-retardant micro-nano heat-insulating fabric and preparation method thereof

Abstract

The invention discloses a self-response temperature-regulating flame-retardant micro-nano heat-insulating fabric and a preparation method thereof. The fabric comprises base cloth and a micro-nano structure coating, the base cloth comprises a double-layer fabric woven by using core-sheath yarns as independent warp yarns and weft yarns; wherein the core-sheath yarn is formed by spinning self-response flame-retardant filaments serving as core filaments wrapped with flame-retardant and temperature-adjusting fibers; the self-response flame-retardant filament is a sheath-core composite fiber; the micro-nano structure coating is a pattern constructed on the surface of the fabric after a metal coating is subjected to acid treatment. When the self-response temperature-regulating flame-retardant micro-nano heat-insulating fabric encounters a heat source, the self-response flame-retardant filaments uniformly distributed in the fabric are heated and expanded to form air cavities, so that the thickness and the density of the fabric are increased, and the self-response flame-retardant filaments and heat reflection dissipation of the micro-nano structure patterns of the fabric synergistically exert thermal protection performance; the fabric integrates multiple functions of self-response, intelligent temperature regulation, flame retardance, heat insulation and static prevention, is simple in process, is green and environment-friendly, and can be used for developing thermal protection clothing in the fields of electric power, metallurgy, petrifaction, fire fighting and the like.

Description

Technical Field

[0001] The present application relates to a self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric and a preparation method thereof, and belongs to the technical field of preparation of multifunctional textiles. Background Art

[0002] With the acceleration of social development and urbanization, the risk of thermal disasters such as fire is increasing, which puts higher demands on disaster prevention and relief work. In the process of hot environment operations and thermal disaster rescue, operators and rescuers not only need to face extreme environments such as high temperature and flames, but also need to ensure their own safety in order to effectively perform operations and rescue tasks. Therefore, the development of high-performance, lightweight and comfortable thermal protective clothing is crucial to ensure the safety of hot environment operations and rescue personnel.

[0003] Thermal protective clothing must be able to reduce the speed of heat transfer, reduce the accumulation of heat on human skin, have good flame retardancy, high thermal insulation performance, be able to prevent itself from being ignited, burning with flames and igniting after contact with flames and hot objects, and protect the human body from various thermal injuries. The key to the development of thermal protective clothing lies in the development of thermal insulation fabrics. The thermal insulation fabrics used must be able to remain stable at high temperatures, not easy to burn, and be able to isolate the transfer of heat. At the same time, thermal insulation fabrics should have a certain degree of comfort and breathability to ensure that the wearer can remain comfortable during long-term high-temperature operations, reduce physical exertion, and improve work efficiency.

[0004] The main technical measures for the preparation of thermal insulation fabrics in the prior art include constructing microstructures, designing multi-layer fabrics and coating finishing. In terms of constructing microstructures, the most typical technical means is to prepare various types of microstructures or aerogel fibers. For example, patent CN114481357A discloses a microstructure fiber, which consists of a cladding layer and a core layer. After the fiber is formed, the thermal expansion microspheres expand when the fiber is heated, so that the fiber has a microstructure; in addition, when preparing aerogel fibers, a more mature technical solution is to use supercritical or freeze-drying technology to replace the solvent inside the fiber to obtain aerogel fibers with a nano-scale porous network structure, and then the prepared aerogel fibers are processed into various types of aerogel fabrics using weaving, non-woven or knitting technology. Summary of the invention

[0005] According to one aspect of the present application, a self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric is provided, comprising: a base fabric and a micro-nano structure coating;

[0006] The base fabric comprises core-sheath yarns, wherein the core-sheath yarns are woven as independent warp yarns and weft yarns into a double-layer structure having a surface layer and an inner layer, and the surface layer of the base fabric is woven with conductive yarns;

[0007] The core-sheath yarn is made of a self-responsive flame-retardant filament as the core yarn and a flame-retardant and temperature-regulating fiber mixture as the outer layer;

[0008] The self-responsive flame-retardant filament is a sheath-core composite fiber filament;

[0009] The micro-nano structure coating is a metal coating that is treated with acid to construct a micro-nano structure pattern on the fabric surface of the base fabric.

[0010] Preferably, the mass per unit area of ​​the base fabric is 220 g / m 2 ~260g / m 2 The warp density of the base fabric is 435 to 505 yarns / 10cm, the weft density of the base fabric is 395 to 440 yarns / 10cm, the surface fabric structure of the base fabric is plain or variable twill, and the inner fabric structure is plain or twill. The core-sheath yarn arrangement ratio of the surface fabric of the base fabric and the core-sheath yarn of the inner fabric is 1:1 to 3:2, and the linear density of the core-sheath yarn of the surface fabric of the base fabric and the core-sheath yarn of the inner fabric are 11.36 tex×2 to 14.76 tex×2 respectively;

[0011] The core-sheath yarn of the surface fabric is a high-performance flame-retardant core-sheath yarn, wherein the limiting oxygen index (LOI) of the high-performance flame-retardant core-sheath yarn is greater than 30%;

[0012] The core-sheath yarn of the inner fabric is a temperature-regulating flame-retardant core-sheath yarn.

[0013] Preferably, the linear density of the self-responsive flame-retardant filament is 2.22 tex to 7.78 tex, the self-responsive flame-retardant filament is a concentric core-skin composite fiber, and the self-responsive flame-retardant filament includes a core material and a skin material;

[0014] The concentric cross-sectional area ratio of the core material and the skin layer is 2-3:3-2;

[0015] The core material is a low boiling point flame retardant;

[0016] The skin layer is a thermoplastic flame retardant elastomer.

[0017] Preferably, the low boiling point flame retardant comprises a low boiling point high molecular polymer and a low boiling point flame retardant liquid;

[0018] The mass ratio of the low boiling point high molecular polymer to the low boiling point flame retardant liquid is 3:2;

[0019] The low boiling point high molecular polymer is any one of ethyl acetate, isobutyl acetate and tert-amyl alcohol or a mixture of equal weight of several of them;

[0020] The low boiling point flame retardant liquid is any one of tributyl phosphate and ammonium pentaborate or a mixture of equal mass of the two;

[0021] Preferably, the flame retardant thermoplastic elastomer is any one of styrene divinyl benzene (SBC), triphenylphosphine oxide (TPO), and thermoplastic polyurethane (TPU), or a mixture of several of them.

[0022] According to another aspect of the present application, a method for preparing a self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric is provided, and the preparation method comprises the following steps:

[0023] Step 1: preparing a self-responsive flame retardant filament using a low boiling point flame retardant as a core material and a thermoplastic flame retardant elastomer as a skin material;

[0024] Step 2: using the self-responsive flame-retardant filament as the core yarn, and wrapping the flame-retardant fiber and the temperature-regulating fiber respectively to prepare a high-performance flame-retardant core-sheath yarn and a temperature-regulating flame-retardant core-sheath yarn;

[0025] Step 3: Using high-performance flame-retardant core-sheath yarn and temperature-regulating flame-retardant core-sheath yarn as independent warp yarn and weft yarn to form the surface layer and inner layer of the fabric respectively, weaving a double-layer structure fabric, and introducing conductive yarn into the surface layer of the fabric to finally prepare the base fabric;

[0026] Step 4: finishing the base fabric coating prepared in step 3 with a flame-retardant polymer metal finishing solution, followed by acid treatment, alkali neutralization and water washing, and constructing a micro-nano structure pattern on the fabric surface after high-temperature drying, wherein the drying temperature is 100° C. to 120° C.;

[0027] In step 2, the high-performance flame-retardant fiber is formed by mixing flame-retardant fibers; and the temperature-regulating flame-retardant fiber is formed by mixing temperature-regulating fibers and flame-retardant fibers.

[0028] Preferably, in step 1, the specific preparation process of the self-responsive flame-retardant filament is:

[0029] Firstly, a primary fiber with a low-boiling-point flame retardant as a core material and a flame retardant elastomer as a skin material is prepared by melt spinning;

[0030] Then, the as-spun fiber is prepared into a self-responsive flame-retardant filament through heat drawing, oiling and winding;

[0031] Wherein, the melt spinning extrusion temperature in the melt filament extrusion process is 110°C to 140°C;

[0032] In the heat stretching process, the heat stretching temperature is 100° C. to 110° C., and the stretching multiple is 1.0 to 3.0 times.

[0033] Preferably, the high-performance flame-retardant fiber is a mixture of one or more of aramid 1313, aramid 1414, aramid sulfone, polyimide fiber and flame-retardant viscose fiber;

[0034] The temperature-regulating flame-retardant fiber is a mixture of temperature-regulating fiber and aramid 1313, aramid 1414, flame-retardant viscose and flame-retardant nitrile fiber.

[0035] The phase change temperature range of the temperature regulating fiber is 28°C to 50°C.

[0036] Preferably, the flame retardant polymer metal finishing solution comprises metal powder, adhesive and dispersant;

[0037] The metal powder comprises 45-60wt%, a binder comprises 35-45wt%, and a dispersant comprises 5-10wt%. The metal powder comprises one or more of aluminum powder, zinc powder and iron powder.

[0038] Preferably, in step 4, the coating treatment process includes:

[0039] S1, coating finishing;

[0040] S2, low temperature drying;

[0041] S3, acid bath, alkali bath and water bath are performed in sequence;

[0042] S4, performing high temperature drying treatment.

[0043] Among them, in S1, the coating thickness is 0.10 mm to 0.30 mm, and the coating speed is 8 m / min to 12 m / min;

[0044] In S2, the drying temperature is 100°C to 110°C;

[0045] In S3, in the acid bath, the acid solution used includes any one of a hydrochloric acid solution with a concentration of 5% to 10% and a sulfuric acid solution with a concentration of 10% to 25% or a mixture of the two, the treatment temperature of the acid bath is 15° C. to 25° C., and the treatment time is 25 seconds to 50 seconds;

[0046] In the alkaline bath, the alkaline solution used includes a 5% to 10% sodium bicarbonate solution, the treatment temperature of the alkaline solution is 15° C. to 25° C., and the treatment time is 25 seconds to 50 seconds;

[0047] In the water bath, the treatment temperature is 85°C to 95°C, and the treatment time is 120 seconds to 360 seconds;

[0048] In S4, the drying temperature is 100°C to 120°C.

[0049] Compared with the prior art, the present invention has the following advantages:

[0050] In the present application, self-responsive flame-retardant filaments are used as the core material, and the flame-retardant and temperature-regulating skin layers are wrapped to respectively spin high-performance flame-retardant core-sheath yarns and temperature-regulating flame-retardant core-sheath yarns to weave a double-layer structural fabric. Through the weaving process, conductive wires are introduced into the surface layer of the double-layer structural fabric to obtain a base fabric with a double-layer structure. The base fabric is subjected to metal coating and acid treatment to construct a micro-nano structure pattern on the surface of the fabric. When the fabric is worn and encounters a heat source, the self-responsive flame-retardant filaments as the core yarn expand due to heat to form air cavities, thereby increasing the thickness and density of the fabric, and synergizing with the heat reflection and dissipation of the micro-nano structure pattern of the fabric to exert thermal protection performance, and the self-insulating fabric returns to its original state after being away from the heat source.

[0051] In the preparation method of the self-responsive temperature-adjusting flame-retardant micro-nano thermal insulation fabric provided in the present application, in the present application, the self-responsive temperature-adjusting flame-retardant micro-nano thermal insulation fabric introduces nano-metal powder on the surface of the fabric by means of coating finishing, and creatively dissolves the nano-metal powder embedded in the surface of the fabric through acid treatment to construct a metal micro-nano structure pattern, which can dissipate heat by multiple reflections, thereby significantly improving the thermal protection performance of the fabric;

[0052] By introducing self-responsive flame-retardant filaments as deformation air cavities, the long process from spinning to weaving to directly use microstructured or aerogel fibers is avoided, and the fiber structure is destroyed during combing, drawing, and twisting, thus ensuring thermal protection performance;

[0053] At the same time, by adopting the preparation method of the present application, the self-responsive flame-retardant fiber is used as the macro structure, and the micro-nano structure constructed on the surface of the fabric is used as the micro-nano structure, combining the "macro-meso-micro" to jointly exert the thermal protection performance. BRIEF DESCRIPTION OF THE DRAWINGS

[0054] Figure 1 This is a schematic diagram of the cross section of the self-responsive flame-retardant filament of the present application;

[0055] Figure 2 This is a SEM image of the micro-nano structure of the self-responsive temperature-regulating flame-retardant thermal insulation fabric prepared in this application;

[0056] In the accompanying drawings, 1 is the core material; 2 is the skin layer. DETAILED DESCRIPTION

[0057] The present application provides a self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric, comprising: a base fabric and a micro-nano structure coating;

[0058] The base fabric is woven with core and sheath yarns as independent warp yarns and weft yarns to form a double-layer structure with a surface layer and an inner layer, and the surface layer of the base fabric is woven with conductive yarns;

[0059] The core-sheath yarn is made of a self-responsive flame-retardant filament as the core yarn and a flame-retardant and temperature-regulating fiber mixture as the outer layer;

[0060] The self-responsive flame-retardant filament is a sheath-core composite fiber filament;

[0061] The micro-nano structure coating is a metal coating that is treated with acid to construct a micro-nano structure pattern on the surface of the fabric.

[0062] It should be noted that when the self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric described in the present application is worn and used by workers, when it encounters a heat source, the core material in the sheath-core composite fiber filament expands due to the heat, "deforms" and forms an "air cavity", while the flame-retardant thermoplastic elastomer of the skin material wrapped around the core material is easy to soften and elastic, and deforms accordingly, which significantly increases the thickness and density of the fabric, hinders the flow of heat, and improves the thermal protection performance of the fabric; and the micro-nano structure coating introduces nano-metal powder on the surface of the fabric with the help of coating finishing, and creatively dissolves the nano-metal powder embedded in the surface of the fabric through acid treatment to construct a micro-nano structure pattern, which can reflect and dissipate heat multiple times, further significantly improving the thermal protection performance of the fabric.

[0063] At the same time, the self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric uses self-responsive flame-retardant filaments as the macro structure and the micro-nano structure constructed on the fabric surface as the micro-nano structure, combining "macro-meso-micro" to jointly exert thermal protection performance.

[0064] At the same time, the cracked micro-nano pattern solves the technical problem of coating rupture in the existing coating film when the fabric expands in self-response; and the self-responsive flame-retardant filament reduces the processing difficulty caused by poor mechanical properties of microstructure or aerogel fiber, and at the same time, avoids the direct use of microstructure or aerogel fiber, and the long process from spinning to weaving. The fiber damages the microstructure during combing, drawing, and twisting, ensuring the thermal protection performance. Before encountering the heat source, the self-responsive flame-retardant filament is almost the same as the commonly used textile fiber in performance, and the processing is simple and easy, and pure spinning high-temperature resistant fabrics can be developed. At the same time, after the fabric is away from the heat source, the self-responsive flame-retardant filament can return to its original shape, which is a reversible deformation of multiple bidirectional cycles, solving the "edema" defect of the fabric caused by unidirectional expansion and deformation of the fabric, and can be used to develop high-performance lightweight protective clothing, which can effectively reduce the skeleton burden of the operator and improve work efficiency.

[0065] In the present application, the self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric has an intelligent temperature-regulating function through phase change temperature fibers. On the one hand, it can reduce the thermal stress generated by wearing clothes in a hot environment and enhance the thermal protection performance of the fabric; on the other hand, it can prevent sudden changes in temperature inside the clothes and improve the wet and hot comfort performance of the thermal protection fabric.

[0066] Furthermore, the mass per unit area of ​​the base fabric is 220 g / m 2 ~260g / m 2The warp density of the base fabric is 435 to 505 yarns / 10cm, the weft density of the base fabric is 395 to 440 yarns / 10cm, the surface fabric structure of the base fabric is plain or variable twill, and the inner fabric structure is plain or twill. The core-sheath yarn arrangement ratio of the surface fabric of the base fabric and the core-sheath yarn of the inner fabric is 1:1 to 3:2, and the linear density of the core-sheath yarn of the surface fabric of the base fabric and the core-sheath yarn of the inner fabric are 11.36 tex×2 to 14.76 tex×2 respectively;

[0067] The core-sheath yarn of the surface fabric is a high-performance flame-retardant core-sheath yarn;

[0068] The core-sheath yarn of the inner fabric is a temperature-regulating flame-retardant core-sheath yarn.

[0069] It should be noted that in the present application, the core-sheath yarn of the surface fabric is a high-performance flame-retardant core-sheath yarn; the core-sheath yarn of the inner fabric is a temperature-regulating flame-retardant core-sheath yarn, thereby improving the flame-retardant performance and the moist and hot comfort of wearing.

[0070] Further, the linear density of the self-responsive flame-retardant filament is 2.22tex to 7.78tex, and the self-responsive flame-retardant filament is as shown in the attached Figure 1 The figure shows a concentric core-skin composite fiber, wherein the self-responsive flame-retardant filament comprises a core material and a skin material;

[0071] The concentric cross-sectional area ratio of the core material and the skin layer is 2-3:3-2;

[0072] The core material is a low boiling point flame retardant;

[0073] The skin layer is a thermoplastic flame retardant elastomer.

[0074] It should be noted that in the present application, the core material is set to be a low-boiling point flame retardant, which improves its sensitivity to temperature and allows it to deform quickly at the first time; the skin layer is set to be a thermoplastic flame retardant elastomer, so that it can cooperate with the core material to deform when encountering temperature changes, and also provide support for the core material.

[0075] Furthermore, the low boiling point flame retardant includes a low boiling point high molecular polymer and a low boiling point flame retardant liquid;

[0076] The mass ratio of the low boiling point high molecular polymer to the low boiling point flame retardant liquid is 3:2;

[0077] The low boiling point high molecular polymer is any one of ethyl acetate, isobutyl acetate and tert-amyl alcohol or a mixture of equal weight of several of them;

[0078] The low boiling point flame retardant liquid is any one of tributyl phosphate and ammonium pentaborate or a mixture of equal mass of the two;

[0079] Furthermore, the flame retardant thermoplastic elastomer is any one of styrene divinyl benzene (SBC), triphenylphosphine oxide (TPO), and thermoplastic polyurethane (TPU), or a mixture of several of them.

[0080] A method for preparing a self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric, the preparation method comprising the following steps:

[0081] Step 1: using a low-boiling point flame retardant as a core material and a thermoplastic flame retardant elastomer as a skin material to prepare a self-responsive flame retardant filament;

[0082] Among them, in the concentric circle cross section of the prepared self-responsive flame-retardant filament, the area ratio of the skin layer to the core layer is 2-3:3-2, and the linear density of the self-responsive flame-retardant skin-core filament is 2.22tex-7.78tex;

[0083] The specific preparation process of self-responsive flame-retardant filament is as follows:

[0084] Firstly, a primary fiber with a low-boiling-point flame retardant as a core material and a flame retardant elastomer as a skin material is prepared by melt spinning;

[0085] Then, the as-spun fiber is prepared into a self-responsive flame-retardant filament through heat drawing, oiling and winding;

[0086] Wherein, the melt spinning extrusion temperature in the melt filament extrusion process is 110°C to 140°C;

[0087] In the heat stretching process, the heat stretching temperature is 100° C. to 110° C., and the stretching multiple is 1.0 to 3.0 times.

[0088] Step 2: using the self-responsive flame-retardant filament as the core yarn, and respectively wrapping the high-performance flame-retardant fiber and the temperature-regulating flame-retardant fiber to prepare the high-performance flame-retardant core-sheath yarn and the temperature-regulating flame-retardant core-sheath yarn;

[0089] The number of the core yarn self-responsive flame-retardant filaments is 1 to 3, and the linear density of the core sheath yarn is 11.36 tex×2 to 14.76 tex×2.

[0090] Step 3: Using high-performance flame-retardant core-sheath yarn and temperature-regulating flame-retardant core-sheath yarn as independent warp yarn and weft yarn to form the surface layer and inner layer of the fabric respectively, weaving a double-layer structure fabric, and introducing conductive yarn into the surface layer of the fabric to finally prepare the base fabric;

[0091] Among them, the high-performance flame-retardant core-sheath yarn outer covering fiber is a mixture of one or more of aramid 1313, aramid 1414, aramid sulfone, polyimide fiber and flame-retardant viscose fiber;

[0092] The outer fiber of the temperature-regulating flame-retardant core-sheath yarn is a mixture of temperature-regulating fiber and aramid 1313, aramid 1414, flame-retardant viscose and flame-retardant nitrile chlorofiber.

[0093] The phase change temperature range of the phase change temperature regulating fiber is 28°C to 50°C.

[0094] The surface fabric structure of the base fabric is plain or variable twill, and the inner fabric structure of the base fabric is plain or twill;

[0095] The base fabric has a mass per unit area of ​​220 g / m 2 ~260g / m 2 .

[0096] The arrangement ratio of the surface fabric yarn and the inner fabric yarn of the base fabric is 1:1 to 3:2;

[0097] The base fabric has a warp density of 435 to 505 strands / 10cm, and a weft density of 395 to 440 strands / 10cm;

[0098] Step 4: finishing the base fabric coating prepared in step 3 with a flame-retardant polymer metal finishing solution, followed by acid treatment, alkali neutralization and water washing, and constructing a micro-nano structure pattern on the fabric surface after high-temperature drying, wherein the drying temperature is 100° C. to 120° C.;

[0099] Wherein, the flame retardant polymer metal finishing solution comprises metal powder, adhesive and dispersant;

[0100] The metal powder is 45-60wt%, the binder is 35-45wt%, and the dispersant is 5-10wt%, and the total mass fraction of the above components is 100%;

[0101] The metal powder includes any one or more of aluminum powder, zinc powder and iron powder.

[0102] The metal powder comprises 45-55wt% aluminum, 25-35wt% zinc, and 10-20wt% iron, and the total mass fraction of the above components is 100%.

[0103] The coating process includes:

[0104] S1, coating finishing;

[0105] S2, low temperature drying;

[0106] S3, acid bath, alkali bath and water bath are performed in sequence;

[0107] S4, performing high temperature drying treatment.

[0108] Among them, in S1, the coating thickness is 0.10 mm to 0.30 mm, and the coating speed is 8 m / min to 12 m / min;

[0109] In S2, the drying temperature is 100°C to 110°C;

[0110] In S3, in the acid bath, the acid solution used includes any one of a hydrochloric acid solution with a concentration of 5% to 10% and a sulfuric acid solution with a concentration of 10% to 25%, or a mixture of the two. In the present application, the mixed liquid is preferably a hydrochloric acid solution with a concentration of 5% to 10% and a sulfuric acid solution with a concentration of 10% to 25%;

[0111] The treatment temperature of the acid bath is 15°C to 25°C, and the treatment time is 25 seconds to 50 seconds;

[0112] In the alkaline bath, the alkaline solution used includes a 5% to 10% sodium bicarbonate solution, the treatment temperature of the alkaline solution is 15° C. to 25° C., and the treatment time is 25 seconds to 50 seconds;

[0113] In the water bath, the treatment temperature is 85°C to 95°C, and the treatment time is 120 seconds to 360 seconds;

[0114] In S4, the drying temperature is 100°C to 120°C.

[0115] It should be noted that:

[0116] The fabric developed by the present invention integrates self-response, intelligent temperature regulation, flame retardancy, heat insulation and anti-static functions. The process is simple and easy, and it is green, environmentally friendly and pollution-free, including but not limited to being used to develop thermal protective clothing for use in the fields of electricity, metallurgy, petroleum, chemical industry, fire protection, etc.

[0117] The present application is described in detail below with reference to embodiments, but the present application is not limited to these embodiments.

[0118] In the following examples, styrene divinylbenzene (SBC) was purchased from Hubei Xinyuhong Biomedical Technology Co., Ltd., triphenylphosphine oxide (TPO) was purchased from Shanghai Weifang Fine Chemical Co., Ltd., thermoplastic polyurethane (TPU) was purchased from Tianjin Daqiuzhuang Foam Plastic Co., Ltd.; tributyl phosphate was purchased from Jinan Yingyu Chemical Co., Ltd., ammonium pentaborate was purchased from Jiangsu Keluoji Health Technology Co., Ltd.; ethyl acetate, isobutyl acetate and tert-amyl alcohol were all purchased from Tianjin Damao Chemical Reagent Factory.

[0119] Example 1

[0120] A method for preparing a self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric comprises the following steps:

[0121] Step 1, preparation of self-responsive flame retardant filament:

[0122] The flame retardant thermoplastic elastomer masterbatch is melted into a melt by a screw extruder and enters the skin channel of the concentric skin-core structure spinneret as the skin material; the low boiling point high molecular polymer enters the core channel of the concentric skin-core structure spinneret, is extruded through the spinneret hole, and then cooled by side blowing to form primary fibers;

[0123] The spun fibers are subjected to heat drawing, oiling and winding to prepare concentric core-skin composite fibers (ie, self-responsive flame-retardant filaments) having self-responsive and flame-retardant properties.

[0124] Step 2, Spinning of core-sheath yarn:

[0125] Firstly, the high-performance intrinsic flame-retardant fiber mixture and the temperature-regulating / flame-retardant fiber mixture are sequentially spun through the process of oiling and moistening → premixing → cleaning and combing → drawing → roving → spinning to obtain high-performance flame-retardant core-sheath yarn and temperature-regulating flame-retardant core-sheath yarn.

[0126] Step 3, preparation of base fabric:

[0127] Through the design of fabric structure, high-performance flame-retardant core-sheath yarn is used as the surface warp and weft, and temperature-regulating flame-retardant core-sheath yarn is used as the inner warp and weft. Warping, sizing, reeding, weaving, and cloth repairing are carried out in sequence to obtain a double-layer structure fabric. Conductive threads are woven into the surface intervals of the double-layer structure fabric to prepare the base fabric.

[0128] Step 4, preparation of self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric:

[0129] Firstly, a flame-retardant polymer metal finishing solution was prepared using metal powder with a particle size of 20 nm;

[0130] Then, the base fabric obtained in step 3 is subjected to coating finishing;

[0131] Next, the base fabric after coating is dried at low temperature;

[0132] After the coating is dried, it is sequentially passed through an acid bath I for an acid bath, an alkaline bath II for an alkali bath, and a water bath III for a water bath, and finally subjected to a high-temperature drying treatment to realize the preparation of a self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric.

[0133] In step 1 of this embodiment:

[0134] The flame retardant thermoplastic elastomer is thermoplastic polyurethane (TPU);

[0135] The low boiling point flame retardant as the core layer is a mixture of a low boiling point high molecular polymer and a low boiling point flame retardant liquid, and the mass ratio of the low boiling point high molecular polymer to the low boiling point flame retardant liquid is 3:2;

[0136] The low boiling point high molecular polymer is a mixture of equal weights of ethyl isoacetate, isobutyl acetate and tert-amyl alcohol;

[0137] The low boiling point flame retardant is a mixture of tributyl phosphate and ammonium pentaborate in equal weight;

[0138] The melt spinning extrusion temperature was 140°C;

[0139] In the hot drawing process, the hot drawing temperature is 110°C and the drawing ratio is 3.0 times;

[0140] The area ratio of the skin layer to the core layer of the prepared adaptive flame-retardant yarn is 2:3.

[0141] In step 2 of this embodiment:

[0142] The outer fiber of the high-performance flame-retardant core-sheath yarn is composed of 70% aramid 1313, 25% polyimide, and 5% aramid 1414;

[0143] The outer fiber of the temperature-regulating flame-retardant core-sheath yarn includes 45% temperature-regulating fiber, 35% aramid 1313, 15% flame-retardant nitrile chlorofiber, and 5% aramid 1414. The phase change temperature of the phase-change temperature-regulating fiber is 38°C.

[0144] In the core-sheath yarn, the number of core yarn self-responsive flame-retardant filaments is 3, and the linear density is 2.22tex; the linear density of high-performance flame-retardant core-sheath yarn and temperature-regulating flame-retardant core-sheath yarn is 13.12tex×2;

[0145] In step 3 of this embodiment:

[0146] The surface fabric structure of the base fabric is a variable twill weave, and the inner fabric structure of the base fabric is a twill weave;

[0147] The arrangement ratio of the surface fabric yarn and the inner fabric yarn of the base fabric is 3:2;

[0148] The base fabric has a warp density of 490 strands / 10 cm and a weft density of 440 strands / 10 cm;

[0149] The mass per unit area of ​​the base fabric is 260 g / m 2 .

[0150] In step 4 of this embodiment:

[0151] The prepared flame-retardant polymer metal finishing solution is a mixture of metal powder, adhesive and dispersant;

[0152] Among them, metal powder accounts for 60%, binder accounts for 35%, dispersant accounts for 5%, and the total mass fraction of the above components is 100%;

[0153] In the metal powder, aluminum accounts for 55%, zinc accounts for 35%, and iron accounts for 10%;

[0154] The binder in the flame-retardant high molecular polymer metal finishing solution is a mixture of flame-retardant SEBS resin, high temperature resistant epoxy resin and flame-retardant polyurethane in equal proportions;

[0155] In the coating finishing process, the coating thickness is 0.30 mm, the coating speed is 8 m / min, and the drying temperature is 110 °C;

[0156] The acid bath process is carried out in an acid bath I, wherein the acid solution used in the acid bath I is a mixture of equal masses of a hydrochloric acid solution having a concentration of 10% and a sulfuric acid solution having a concentration of 15%; the treatment temperature is 25° C., and the treatment time is 50 seconds;

[0157] The alkaline bath process is carried out in an alkaline bath II, wherein the alkaline solution used in the alkaline bath II is composed of a sodium bicarbonate solution with a concentration of 10%; the treatment temperature is 15°C, and the treatment time is 50 seconds;

[0158] In the water bath, the treatment temperature is 95°C and the treatment time is 360 seconds;

[0159] In S4, the drying temperature is 110°C.

[0160] Example 2

[0161] A method for preparing a self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric comprises the following steps:

[0162] Step 1, preparation of self-responsive flame retardant filament:

[0163] The flame retardant thermoplastic elastomer masterbatch is melted into a melt by a screw extruder and enters the skin channel of the concentric skin-core structure spinneret as the skin material; the low boiling point high molecular polymer enters the core channel of the concentric skin-core structure spinneret, is extruded through the spinneret hole, and then cooled by side blowing to form primary fibers;

[0164] The spun fibers are subjected to heat drawing, oiling and winding to prepare concentric core-skin composite fibers (ie, self-responsive flame-retardant filaments) having self-responsive and flame-retardant properties.

[0165] Step 2, Spinning of core-sheath yarn:

[0166] Firstly, the high-performance intrinsic flame-retardant fiber mixture and the temperature-regulating / flame-retardant fiber mixture are sequentially spun through the process of oiling and moistening → premixing → cleaning and combing → drawing → roving → spinning to obtain high-performance flame-retardant core-sheath yarn and temperature-regulating flame-retardant core-sheath yarn.

[0167] Step 3, preparation of base fabric:

[0168] Through the design of fabric structure, high-performance flame-retardant core-sheath yarn is used as the surface warp and weft, and temperature-regulating flame-retardant core-sheath yarn is used as the inner warp and weft. Warping, sizing, reeding, weaving, and cloth repairing are carried out in sequence to obtain a double-layer structure fabric. Conductive threads are woven into the surface intervals of the double-layer structure fabric to prepare the base fabric.

[0169] Step 4, preparation of self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric:

[0170] Firstly, a flame-retardant polymer metal finishing solution was prepared using metal powder with a particle size of 20 nm;

[0171] Then, the base fabric obtained in step 3 is subjected to coating finishing;

[0172] Next, the base fabric after coating is dried at low temperature;

[0173] After the coating is dried, it is sequentially passed through an acid bath I for an acid bath, an alkaline bath II for an alkali bath, and a water bath III for a water bath, and finally subjected to a high-temperature drying treatment to realize the preparation of a self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric.

[0174] In step 1 of this embodiment:

[0175] The flame retardant thermoplastic elastomer is triphenylphosphine oxide (TPO);

[0176] The low boiling point flame retardant as the core layer is a mixture of a low boiling point high molecular polymer and a low boiling point flame retardant liquid, and the mass ratio of the low boiling point high molecular polymer to the low boiling point flame retardant liquid is 3:2;

[0177] The low boiling point high molecular polymer is a mixture of equal weights of ethyl isoacetate, isobutyl acetate and tert-amyl alcohol;

[0178] The low boiling point flame retardant is a mixture of tributyl phosphate and ammonium pentaborate in equal weight;

[0179] The melt spinning extrusion temperature was 130°C;

[0180] In the hot drawing process, the hot drawing temperature is 100°C and the drawing ratio is 2.0 times;

[0181] The area ratio of the skin layer to the core layer of the prepared adaptive flame-retardant yarn is 3:3.

[0182] In step 2 of this embodiment:

[0183] The outer covering fiber of high-performance flame-retardant core-sheath yarn is composed of 70% aramid 1313, 15% polyimide, 10% flame-retardant viscose, and 5% aramid 1414.

[0184] The outer fiber of the temperature-regulating flame-retardant core-sheath yarn includes 45% of the temperature-regulating fiber, 30% of the aramid 1313, 20% of the flame-retardant nitrile chlorofiber, and 5% of the aramid 1414. The phase change temperature of the phase-change temperature-regulating fiber is 50°C.

[0185] In the core-sheath yarn, the number of core yarn self-responsive flame-retardant filaments is 1, and the linear density is 5.55 tex; the linear density of high-performance flame-retardant core-sheath yarn and temperature-regulating flame-retardant core-sheath yarn is 11.81 tex×2;

[0186] In step 3 of this embodiment:

[0187] The surface fabric structure of the base fabric is a plain weave, and the inner fabric structure of the base fabric is a twill weave;

[0188] The arrangement ratio of the surface fabric yarn and the inner fabric yarn of the base fabric is 4:3;

[0189] The base fabric has a warp density of 505 strands / 10 cm and a weft density of 440 strands / 10 cm;

[0190] The mass per unit area of ​​the base fabric is 240 g / m 2 .

[0191] In step 4 of this embodiment:

[0192] The prepared flame-retardant polymer metal finishing solution is a mixture of metal powder, adhesive and dispersant;

[0193] Among them, metal powder accounts for 50%, binder accounts for 45%, dispersant accounts for 5%, and the total mass fraction of the above components is 100%;

[0194] In the metal powder, aluminum accounts for 45%, zinc accounts for 35%, and iron accounts for 20%;

[0195] The binder in the flame-retardant high molecular polymer metal finishing solution is a mixture of flame-retardant SEBS resin, high temperature resistant epoxy resin and flame-retardant polyurethane in equal proportions;

[0196] In the coating finishing process, the coating thickness is 0.20 mm, the coating speed is 10 m / min, and the drying temperature is 110 °C;

[0197] The acid bath process is carried out in an acid bath I, wherein the acid solution used in the acid bath I is a mixture of an 8% hydrochloric acid solution and a 12% sulfuric acid solution in equal amounts; the treatment temperature is 20° C., and the treatment time is 30 seconds;

[0198] The alkaline bath process is carried out in an alkaline bath II, wherein the alkaline solution used in the alkaline bath II is composed of a sodium bicarbonate solution with a concentration of 8%; the treatment temperature is 20°C and the treatment time is 30 seconds;

[0199] In the water bath, the treatment temperature is 90°C and the treatment time is 240 seconds;

[0200] In S4, the drying temperature is 110°C.

[0201] Example 3

[0202] A method for preparing a self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric comprises the following steps:

[0203] Step 1, preparation of self-responsive flame retardant filament:

[0204] The flame retardant thermoplastic elastomer masterbatch is melted into a melt by a screw extruder and enters the skin channel of the concentric skin-core structure spinneret as the skin material; the low boiling point high molecular polymer enters the core channel of the concentric skin-core structure spinneret, is extruded through the spinneret hole, and then cooled by side blowing to form primary fibers;

[0205] The spun fibers are subjected to heat drawing, oiling and winding to prepare concentric core-skin composite fibers (ie, self-responsive flame-retardant filaments) having self-responsive and flame-retardant properties.

[0206] Step 2, Spinning of core-sheath yarn:

[0207] Firstly, the high-performance intrinsic flame-retardant fiber mixture and the temperature-regulating / flame-retardant fiber mixture are sequentially spun through the process of oiling and moistening → premixing → cleaning and combing → drawing → roving → spinning to obtain high-performance flame-retardant core-sheath yarn and temperature-regulating flame-retardant core-sheath yarn.

[0208] Step 3, preparation of base fabric:

[0209] Through the design of fabric structure, high-performance flame-retardant core-sheath yarn is used as the surface warp and weft, and temperature-regulating flame-retardant core-sheath yarn is used as the inner warp and weft. Warping, sizing, reeding, weaving, and cloth repairing are carried out in sequence to obtain a double-layer structure fabric. Conductive threads are woven into the surface intervals of the double-layer structure fabric to prepare the base fabric.

[0210] Step 4, preparation of self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric:

[0211] Firstly, a flame-retardant polymer metal finishing solution was prepared using metal powder with a particle size of 20 nm;

[0212] Then, the base fabric obtained in step 3 is subjected to coating finishing;

[0213] Next, the substrate after coating is dried at low temperature;

[0214] After the coating is dried, it is sequentially passed through an acid bath I for an acid bath, an alkaline bath II for an alkali bath, and a water bath III for a water bath, and finally subjected to a high-temperature drying treatment to realize the preparation of a self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric.

[0215] In step 1 of this embodiment:

[0216] The flame retardant thermoplastic elastomer is styrene divinyl benzene (SBC);

[0217] The low boiling point flame retardant as the core layer is a mixture of a low boiling point high molecular polymer and a low boiling point flame retardant liquid, and the mass ratio of the low boiling point high molecular polymer to the low boiling point flame retardant liquid is 3:2;

[0218] The low boiling point high molecular polymer is a mixture of equal weights of ethyl isoacetate, isobutyl acetate and tert-amyl alcohol;

[0219] The low boiling point flame retardant is a mixture of tributyl phosphate and ammonium pentaborate in equal weight;

[0220] The melt spinning extrusion temperature was 110°C;

[0221] In the hot drawing process, the hot drawing temperature is 100°C and the drawing ratio is 2.0 times;

[0222] The area ratio of the skin layer to the core layer of the prepared adaptive flame-retardant yarn is 3:2.

[0223] In step 2 of this embodiment:

[0224] The outer fiber of the high-performance flame-retardant core-sheath yarn is 95% aramid 1313 and 5% aramid 1414;

[0225] The outer fiber of the temperature-regulating flame-retardant core-sheath yarn includes 30% temperature-regulating fiber, 40% aramid 1313, 15% flame-retardant viscose, and 15% flame-retardant nitrile chlorofiber; the phase change temperature of the phase-change temperature-regulating fiber is 28°C;

[0226] In the core-sheath yarn, the number of core yarn self-responsive flame-retardant filaments is 2, and the linear density is 2.22tex; the linear density of high-performance flame-retardant core-sheath yarn is 12.30tex×2, and the linear density of temperature-adjustable flame-retardant core-sheath yarn is 11.36tex×2;

[0227] In step 3 of this embodiment:

[0228] The surface fabric structure of the base fabric is a plain weave, and the inner fabric structure of the base fabric is a plain weave;

[0229] The arrangement ratio of the surface fabric yarn and the inner fabric yarn of the base fabric is 1:1;

[0230] The base fabric has a warp density of 440 strands / 10 cm and a weft density of 435 strands / 10 cm;

[0231] The mass per unit area of ​​the base fabric is 220 g / m 2 .

[0232] In step 4 of this embodiment:

[0233] The prepared flame-retardant polymer metal finishing solution is a mixture of metal powder, adhesive and dispersant;

[0234] Among them, metal powder accounts for 45%, binder accounts for 45%, dispersant accounts for 10%, and the total mass fraction of the above components is 100%;

[0235] In the metal powder, aluminum accounts for 50%, zinc accounts for 35%, and iron accounts for 15%;

[0236] The binder in the flame-retardant high molecular polymer metal finishing solution is a mixture of flame-retardant SEBS resin, high temperature resistant epoxy resin and flame-retardant polyurethane in equal proportions;

[0237] In the coating finishing process, the coating thickness is 0.10 mm, the coating speed is 12 m / min, and the drying temperature is 100 °C;

[0238] The acid bath process is carried out in an acid bath I, wherein the acid solution used in the acid bath I is a mixture of 5% hydrochloric acid solution and 10% sulfuric acid solution in equal amounts; the treatment temperature is 15° C., and the treatment time is 25 seconds;

[0239] The alkaline bath process is carried out in an alkaline bath II, wherein the alkaline solution used in the alkaline bath II is composed of a sodium bicarbonate solution with a concentration of 5%; the treatment temperature is 15°C and the treatment time is 25 seconds;

[0240] In the water bath, the treatment temperature is 85°C and the treatment time is 120 seconds;

[0241] In S4, the drying temperature is 100°C.

[0242] Example 4

[0243] A method for preparing a self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric comprises the following steps:

[0244] Step 1, preparation of self-responsive flame retardant filament:

[0245] The flame retardant thermoplastic elastomer masterbatch is melted into a melt by a screw extruder and enters the skin channel of the concentric skin-core structure spinneret as the skin material; the low boiling point high molecular polymer enters the core channel of the concentric skin-core structure spinneret, is extruded through the spinneret hole, and then cooled by side blowing to form primary fibers;

[0246] The spun fibers are subjected to heat drawing, oiling and winding to prepare concentric core-skin composite fibers (ie, self-responsive flame-retardant filaments) having self-responsive and flame-retardant properties.

[0247] Step 2, Spinning of core-sheath yarn:

[0248] Firstly, the high-performance intrinsic flame-retardant fiber mixture and the temperature-regulating / flame-retardant fiber mixture are sequentially spun through the process of oiling and moistening → premixing → cleaning and combing → drawing → roving → spinning to obtain high-performance flame-retardant core-sheath yarn and temperature-regulating flame-retardant core-sheath yarn.

[0249] Step 3, preparation of base fabric:

[0250] Through the design of fabric structure, high-performance flame-retardant core-sheath yarn is used as the surface warp and weft, and temperature-regulating flame-retardant core-sheath yarn is used as the inner warp and weft. Warping, sizing, reeding, weaving, and cloth repairing are carried out in sequence to obtain a double-layer structure fabric. Conductive threads are woven into the surface intervals of the double-layer structure fabric to prepare the base fabric.

[0251] Step 4, preparation of self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric:

[0252] Firstly, a flame-retardant polymer metal finishing solution was prepared using metal powder with a particle size of 20 nm;

[0253] Then, the base fabric obtained in step 3 is subjected to coating finishing;

[0254] Next, the base fabric after coating is dried at low temperature;

[0255] After the coating is dried, it is sequentially passed through an acid bath I for an acid bath, an alkaline bath II for an alkali bath, and a water bath III for a water bath, and finally subjected to a high-temperature drying treatment to realize the preparation of a self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric.

[0256] In step 1 of this embodiment:

[0257] The flame retardant thermoplastic elastomer is triphenylphosphine oxide (TPO);

[0258] The low boiling point flame retardant as the core layer is a mixture of a low boiling point high molecular polymer and a low boiling point flame retardant liquid, and the mass ratio of the low boiling point high molecular polymer to the low boiling point flame retardant liquid is 3:2;

[0259] The low boiling point high molecular polymer is a mixture of equal weights of ethyl isoacetate, isobutyl acetate and tert-amyl alcohol;

[0260] The low boiling point flame retardant is a mixture of tributyl phosphate and ammonium pentaborate in equal weight;

[0261] The melt spinning extrusion temperature was 120°C;

[0262] In the hot drawing process, the hot drawing temperature is 110°C and the drawing ratio is 1.0 times;

[0263] The area ratio of the skin layer to the core layer of the prepared adaptive flame-retardant yarn is 2:3.

[0264] In step 2 of this embodiment:

[0265] The outer covering fiber of high-performance flame-retardant core-sheath yarn is composed of 75% aramid 1313, 10% aramid sulfone, and 15% aramid 1414.

[0266] The outer fiber of the temperature-regulating flame-retardant core-sheath yarn includes 40% temperature-regulating fiber, 30% aramid 1313, 10% flame-retardant viscose, 15% flame-retardant nitrile chlorofiber, and 5% aramid 1414. The phase change temperature of the phase-change temperature-regulating fiber is 32°C.

[0267] In the core-sheath yarn, the number of core yarn self-responsive flame-retardant filaments is 1, and the linear density is 7.78ex; the linear density of high-performance flame-retardant core-sheath yarn and temperature-regulating flame-retardant core-sheath yarn is 14.76tex×2;

[0268] In step 3 of this embodiment:

[0269] The surface fabric structure of the base fabric is a variable twill weave, and the inner fabric structure of the base fabric is a twill weave;

[0270] The arrangement ratio of the surface fabric yarn and the inner fabric yarn of the base fabric is 1:1;

[0271] The base fabric has a warp density of 435 strands / 10 cm and a weft density of 395 strands / 10 cm;

[0272] The mass per unit area of ​​the base fabric is 260 g / m 2 .

[0273] In step 4 of this embodiment:

[0274] The prepared flame-retardant polymer metal finishing solution is a mixture of metal powder, adhesive and dispersant;

[0275] Among them, metal powder accounts for 55%, binder accounts for 35%, dispersant accounts for 10%, and the total mass fraction of the above components is 100%;

[0276] In the metal powder, aluminum accounts for 55%, zinc accounts for 25%, and iron accounts for 20%;

[0277] The binder in the flame-retardant high molecular polymer metal finishing solution is a mixture of flame-retardant SEBS resin, high temperature resistant epoxy resin and flame-retardant polyurethane in equal proportions;

[0278] In the coating finishing process, the coating thickness is 0.25 mm, the coating speed is 9 m / min, and the drying temperature is 110 °C;

[0279] The acid bath process is carried out in an acid bath I, wherein the acid solution used in the acid bath I is a mixture of 5% hydrochloric acid solution and 15% sulfuric acid solution in equal amounts; the treatment temperature is 20° C., and the treatment time is 50 seconds;

[0280] The alkaline bath process is carried out in an alkaline bath II, wherein the alkaline solution used in the alkaline bath II is composed of a sodium bicarbonate solution with a concentration of 8%; the treatment temperature is 20°C and the treatment time is 50 seconds;

[0281] In the water bath, the treatment temperature is 90°C and the treatment time is 3000 seconds;

[0282] In S4, the drying temperature is 100°C.

[0283] Comparative Example 1

[0284] A method for preparing a self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric. In step 1, when preparing a self-responsive flame-retardant filament, a flame-retardant thermoplastic elastomer masterbatch is melted into a melt by a screw extruder, and then extruded through a spinneret hole and then cooled by side blowing to form a primary fiber without a skin-core structure. The rest is the same as in Example 1.

[0285] Comparative Example 2

[0286] A method for preparing a self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric. In step 4, when preparing the self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric, the base fabric after coating is dried at low temperature and then no treatment is performed. The rest is the same as Example 1.

[0287] Comparative Example 3

[0288] A method for preparing a self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric. In step 2, when spinning the core-sheath yarn, the temperature-regulating fiber of the outer fiber of the temperature-regulating flame-retardant core-sheath yarn is replaced with ordinary viscose fiber of the same specification, and the rest is the same as Example 1.

[0289] The preparation methods of the self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabrics prepared in Examples 1-4 and Comparative Examples 1-3 were tested for flame retardancy and thermal insulation properties according to the standards GB 8965.1-2020 "Flame-retardant clothing for protective clothing" and GB 38453-2019 "Thermal insulation clothing for protective clothing". According to the phase change temperature-regulating fabric performance detection method in Appendix A of the T / CTES1005-2017 "Evaluation of phase change temperature-regulating microcapsules for textiles and their application functions", the dynamic temperature rise and fall maximum temperature control value of the test sample was tested. The measured data of various technical indicators are shown in Table 1.

[0290] Table 1 Test results of various indicators of lightweight micro-nano porous three-dimensional high-heat protection materials

[0291]

[0292] By comparing the test data of the self-responsive temperature-adjusting flame-retardant micro-nano thermal insulation fabrics prepared in Example 1 of the present application and Comparative Example 1, it can be seen that:

[0293] Comparing the thermal protection performance of the fabrics prepared by the two methods, the thermal protection coefficient of the fabric containing the self-flame retardant filaments with a skin-core structure prepared in Example 1 is 1852 kW·s / m 2 The thermal protection coefficient of the fabric containing the ordinary flame retardant filament prepared in Comparative Example 1 is only 1172kW·s / m 2 It can be concluded that when the prepared flame-retardant filament does not have a skin-core structure, the thermal protection coefficient of the protective material drops sharply. When the self-responsive flame-retardant filament is made by the technical solution of the present invention, the thermal protection coefficient of the fabric can be increased by 58.0%, and its technical advantages are obvious.

[0294] By comparing the thermal insulation properties of the fabrics prepared by the two, it was found that the fabric containing ordinary flame-retardant filaments prepared in Comparative Example 1 had a convective heat conductivity grade of B2, a radiant heat conductivity grade of C2, and a contact heat conductivity grade of F1; while the fabric containing the self-responsive flame-retardant filaments prepared in Example 1 had a convective heat conductivity grade of B3, a radiant heat conductivity grade of C3, and a contact heat conductivity grade of F3. It can be seen that after the self-responsive flame-retardant filaments prepared by the technical solution of the present application are made, adding them to the fabric can significantly improve the thermal protection and thermal insulation properties of the fabric.

[0295] Comparative analysis of the test data of the self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabrics prepared in Example 1 and Comparative Example 2 shows that when the coated fabric is not acid-treated, that is, the fabric surface does not have a micro-nano structure pattern, the thermal protection coefficient of the fabric in Comparative Example 2 is only 1495 kW·s / m 2 When the micro-nano pattern is formed on the surface of the fabric by acid treatment in Example 1, the thermal protection coefficient can be increased by 42.2%, and the technical advantage is obvious. At the same time, by comparing and analyzing the thermal insulation performance, it is found that the thermal insulation performance of the fabric prepared by the process of Example 1 is improved. It can be seen that constructing a micro-nano pattern on the surface of the fabric can significantly improve the thermal protection and thermal insulation performance of the fabric.

[0296] By comparing and analyzing the test data of the self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabrics prepared in Example 1 and Comparative Example 3, it can be seen that when the core sheath yarn contains temperature-regulating fibers, the dynamic heating and cooling maximum temperature control value of the fabric is 4.3°C, and the introduction of temperature-regulating fibers improves the comfort performance of the fabric; when the core sheath yarn does not contain temperature-regulating fibers, the thermal protection coefficient of the fabric of Comparative Example 3 is reduced by 23.8%. It can be seen that the introduction of temperature-regulating fibers can not only improve the comfort performance of the fabric, but also enhance the flame retardant and thermal insulation properties of the fabric.

[0297] At the same time, if Figure 2 From the SEM image of the self-responsive temperature-regulating flame-retardant heat-insulating fabric micro-nano structure shown in the present application, it can be seen that an uneven micro-nano structure pattern is formed on the surface of the fabric, which can dissipate heat by multiple reflections.

[0298] The above are only a few embodiments of the present application and do not constitute any form of limitation to the present application. Although the present application is disclosed as above with preferred embodiments, it is not intended to limit the present application. Any technician familiar with the profession, without departing from the scope of the technical solution of the present application, using the technical content disclosed above to make slight changes or modifications are equivalent to equivalent implementation cases and fall within the scope of the technical solution.

Claims

1. A self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric, characterized in that: The self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric comprises: a base fabric and a micro-nano structure coating; The base fabric comprises core-sheath yarns, wherein the core-sheath yarns are woven as independent warp yarns and weft yarns into a double-layer structure having a surface layer and an inner layer, and the surface layer of the base fabric is woven with conductive yarns; The core-sheath yarn is made of a self-responsive flame-retardant filament as the core yarn and a flame-retardant and temperature-regulating fiber mixture as the outer layer; The self-responsive flame-retardant filament is a sheath-core composite fiber; The micro-nano structure coating is a micro-nano structure pattern constructed on the fabric surface of the base fabric after the metal coating is treated with acid.

2. The self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric according to claim 1, characterized in that: The mass per unit area of ​​the base fabric is 220 g / m 2 ~260g / m 2 The warp density of the base fabric is 435 to 505 yarns / 10cm, the weft density of the base fabric is 395 to 440 yarns / 10cm, the surface fabric structure of the base fabric is plain or variable twill, and the inner fabric structure is plain or twill. The core-sheath yarn arrangement ratio of the surface fabric of the base fabric and the core-sheath yarn of the inner fabric is 1:1 to 3:2, and the linear density of the core-sheath yarn of the surface fabric of the base fabric and the core-sheath yarn of the inner fabric are 11.36 tex×2 to 14.76 tex×2 respectively; The core-sheath yarn of the surface fabric is a high-performance flame-retardant core-sheath yarn, wherein the limiting oxygen index of the high-performance flame-retardant core-sheath yarn is greater than 30%; The core-sheath yarn of the inner fabric is a temperature-regulating flame-retardant core-sheath yarn.

3. The self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric according to claim 1, characterized in that: The linear density of the self-responsive flame-retardant filament is 2.22 tex to 7.78 tex, the self-responsive flame-retardant filament is a concentric core-skin composite fiber, and the self-responsive flame-retardant filament includes a core material and a skin layer; The concentric cross-sectional area ratio of the core material and the skin layer is 2-3:3-2; The core material is a low boiling point flame retardant; The skin layer is a thermoplastic flame retardant elastomer.

4. The self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric according to claim 3, characterized in that: The low boiling point flame retardant comprises a low boiling point high molecular polymer and a low boiling point flame retardant liquid; The mass ratio of the low boiling point high molecular polymer to the low boiling point flame retardant liquid is 3:2; The low boiling point high molecular polymer is any one of ethyl acetate, isobutyl acetate and tert-amyl alcohol or a mixture of equal weight of several of them; The low boiling point flame retardant liquid is any one of tributyl phosphate and ammonium pentaborate or a mixture of the two of equal mass.

5. The self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric according to claim 3, characterized in that: The flame retardant thermoplastic elastomer is any one of styrene divinyl benzene, triphenylphosphine oxide and thermoplastic polyurethane or a mixture of several of them.

6. A method for preparing a self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric, characterized in that: The preparation method comprises the following steps: Step 1: preparing a self-responsive flame retardant filament using a low boiling point flame retardant as a core material and a thermoplastic flame retardant elastomer as a skin material; Step 2: using the self-responsive flame-retardant filament as the core yarn, and respectively wrapping the high-performance flame-retardant fiber and the temperature-regulating flame-retardant fiber to prepare the high-performance flame-retardant core-sheath yarn and the temperature-regulating flame-retardant core-sheath yarn; Step 3: Using high-performance flame-retardant core-sheath yarn and temperature-regulating flame-retardant core-sheath yarn as independent warp yarn and weft yarn to form the surface layer and inner layer of the fabric respectively, weaving a double-layer structure fabric, and introducing conductive yarn into the surface layer of the fabric to finally prepare the base fabric; Step 4: finishing the base fabric coating prepared in step 3 with a flame-retardant polymer metal finishing solution, followed by acid treatment, alkali neutralization and water washing, and constructing a micro-nano structure pattern on the fabric surface after high-temperature drying, wherein the drying temperature is 100° C. to 120° C.; In step 2, the high-performance flame-retardant fiber is formed by mixing flame-retardant fibers; and the temperature-regulating flame-retardant fiber is formed by mixing temperature-regulating fibers and flame-retardant fibers.

7. The method for preparing a self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric according to claim 6, characterized in that: In step 1, the specific preparation process of the self-responsive flame-retardant filament is as follows: Firstly, a primary fiber with a low-boiling-point flame retardant as a core material and a flame retardant elastomer as a skin material is prepared by melt spinning; Then, the as-spun fiber is prepared into a self-responsive flame-retardant filament through heat drawing, oiling and winding; The melt spinning extrusion temperature in the melt filament extrusion process is 110°C to 140°C; In the heat stretching process, the heat stretching temperature is 100° C. to 110° C., and the stretching multiple is 1.0 to 3.0 times.

8. The method for preparing a self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric according to claim 6, characterized in that: The high-performance flame-retardant fiber is a mixture of one or more of aramid 1313, aramid 1414, aramid sulfone, polyimide fiber and flame-retardant viscose fiber; The temperature-regulating flame-retardant fiber is a mixture of the temperature-regulating fiber and aramid 1313, aramid 1414, flame-retardant viscose fiber and flame-retardant nitrile fiber. The phase change temperature range of the temperature regulating fiber is 28°C to 50°C.

9. The method for preparing a self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric according to claim 6, characterized in that: The flame retardant polymer metal finishing solution comprises metal powder, adhesive and dispersant; The metal powder is 45-60wt%, the binder is 35-45wt%, and the dispersant is 5-10wt%; The metal powder includes any one or more of aluminum powder, zinc powder and iron powder.

10. The method for preparing a self-responsive temperature-regulating flame-retardant micro-nano thermal insulation fabric according to claim 6, characterized in that: In step 4, the coating treatment process includes: S1, coating finishing; S2, low temperature drying; S3, acid bath, alkali bath and water bath are performed in sequence; S4, performing high temperature drying treatment; Among them, in S1, the coating thickness is 0.10 mm to 0.30 mm, and the coating speed is 8 m / min to 12 m / min; In S2, the drying temperature is 100°C to 110°C; In S3, in the acid bath, the acid solution used includes any one of a hydrochloric acid solution with a concentration of 5% to 10% and a sulfuric acid solution with a concentration of 10% to 25% or a mixture of the two, the treatment temperature of the acid bath is 15° C. to 25° C., and the treatment time is 25 seconds to 50 seconds; In the alkaline bath, the alkaline solution used includes a 5% to 10% sodium bicarbonate solution, the treatment temperature of the alkaline solution is 15° C. to 25° C., and the treatment time is 25 seconds to 50 seconds; In the water bath, the treatment temperature is 85°C to 95°C, and the treatment time is 120 seconds to 360 seconds; In S4, the drying temperature is 100°C to 120°C.

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