Lightweight flexible temperature-regulating thermal protective composite fabric and method of making same

Abstract

The present application provides a kind of lightweight flexible temperature regulating thermal protective composite fabric and its preparation method.The present application first carries out flame-retardant finishing to temperature regulating filament, constructs temperature regulating flame-retardant coaxial yarn structure;Then the coaxial yarn is used as warp and weft yarn, and hot melt filament is woven into the inner layer of fabric to obtain base cloth;Finally, hot melt filament is melted by hot pressing, so that the base cloth and the waterproof and breathable film mesh format are bonded to form a coated fabric.The temperature regulating thermal protective composite fabric prepared by the present application uses hot melt wire as adhesive, realizes the precise control of the quantity and position of adhesive;The mesh format bonding used ensures the bonding strength while realizing the flexible design of the fabric, and can form a three-dimensional array of air cavities on the surface of the fabric, significantly improving the thermal protective performance of the fabric;The introduction of intelligent temperature regulating filament further improves the moisture comfort and thermal protective performance of the fabric.The fabric is lightweight, soft, waterproof and breathable, and has excellent comfort and thermal protective performance.

Description

TECHNICAL FIELD

[0001] The present application belongs to the field of preparation of flame-retardant and heat-insulating multifunctional textiles, and relates to a light and flexible temperature-regulating heat protective composite fabric and a preparation method thereof. BACKGROUND

[0002] People in life, industrial production, rescue and war and other activities will encounter various forms of heat sources, such as fire, explosion, molten metal spray, electric arc and various places that may produce high-temperature steam all exist heat damage or potential heat hazards. The temperature range of such heat sources is 60-2000℃, among which flame, high-temperature gas and hot steam are in the form of heat convection to transfer heat, contact heat, spark and molten metal are in the form of heat conduction, and radiant heat is in the form of heat radiation. It can be seen that heat energy mainly causes harm to the human body through contact, radiation or heat convection.

[0003] In order to avoid the harm caused by various heat sources in high-temperature environments in the fields of fire protection, electricity, metallurgy and military to individuals, people began to widely use heat protective clothing. Heat protective clothing refers to the individual protective equipment that can promote the dissipation of human body heat, prevent heat stroke, burns and other hazards in high-temperature environments. Wearing heat protective clothing can protect the human body from various heat injuries, and its protection principle is mainly to reduce the heat transfer speed and reduce the accumulation of heat on the skin, so as to ensure that the skin is not burned or scalded. Therefore, heat protective clothing such as high-temperature resistant and fireproof clothing must be flame-retardant (non-continuous combustion, not shrinkage, not melting, not emitting harmful gases or forming charred carbon to become a dangerous factor), have perfect and reliable quality (tear-resistant, solid and durable, etc.), have heat insulation, windproof and waterproof functions.

[0004] There are mainly two ways to develop heat protection composite fabric at present. One is to coat a reflective heat insulation coating on the surface of the fabric base cloth or to spray a metal aluminum film on the surface of the fabric base cloth to obtain a coated or metalized heat protection composite fabric. For example, CN 111395018A discloses a expandable graphite modifier, its preparation method and application on heat protection fabric. The expandable graphite modifier is modified on the fabric by dipping, padding, baking, printing, dispensing, drying and baking to obtain a fabric with high heat protection performance. CN 105342043A discloses a new type of heat protection composite fabric for firefighters, which comprises a flame-retardant reflective heat insulation outer layer and a phase change comfort layer. The flame-retardant reflective heat insulation outer layer fabric is obtained by inserting a high-temperature-resistant nano reflective heat insulation coating on the aramid 1414 blended fabric base cloth, replacing the previous firefighter heat insulation fabric with surface sprayed metal aluminum film. CN 108221397B relates to a preparation method of a fireproof heat insulation metalized coating fabric, which comprises the following steps: after the flame-retardant base cloth is calendered and humidified, a flame-retardant polyurethane silver paste solution is coated on the surface of the base cloth by using a coating tester to obtain a coated base cloth, and the heat reflection of the heat insulation metalized coating is used to reduce the heat radiation of the skin surface.

[0005] The other way is to bond multiple single-layer fabrics (such as organic matter, knitted fabric, felt and non-woven fabric) or functional films by heat-resistant adhesive to form a multi-layer composite fabric. For example, CN112221027B discloses a flame-retardant heat insulation fabric for fire escape emergency, which is connected by adhesive bonding or hot melt reinforcement by three single-layer fabrics of hydrogel dressing layer, heat insulation non-woven fabric layer and flame-retardant non-woven fabric layer. CN107618225A provides a fireproof fabric for high-temperature operation, which comprises an outer fireproof heat insulation layer, an intermediate heat insulation fabric layer and an inner moisture-absorbing and breathable fabric layer, and the three layers are connected by heat-resistant adhesive. CN203945760U discloses a waterproof and warm-keeping composite fabric, which is laminated and connected by four fabric layers of fabric layer, first elastic layer, second elastic layer and high molecular film layer through PU oil adhesive or PUR hot melt adhesive.

[0006] The heat protection composite fabrics prepared by the above two existing technologies have the following technical defects:

[0007] Firstly, the film structure of the heat protection composite fabric obtained by coating a reflective heat insulation coating on the surface of the fabric base cloth or spraying a metal aluminum film on the surface of the fabric base cloth is unstable, and the film structure is easily damaged during the processing and wearing of the fabric, resulting in a decrease in the heat protection performance. At the same time, the heat protection fabric formed by coating or coating finishing on the surface of the fabric base cloth does not have windproof and waterproof functions, and has very poor air permeability, which is difficult to provide all-round effective protection to individuals.

[0008] Second, the thermal protection composite fabric formed by bonding multiple single-layer fabrics or films with hot melt adhesive. In the thermal bonding process, the amount of adhesive is difficult to control. If the amount is small, the bonding force between the layers is low, and it is difficult to form a stable composite film fabric. If the amount of hot melt adhesive is large, it is easy to cause glue penetration, affecting the style of the fabric, resulting in a significant increase in the overall unit area of the thermal protection composite film fabric, which cannot achieve lightweight and high performance. At the same time, the comfort performance indicators such as air permeability and moisture permeability decrease significantly.

[0009] Third, the thermal protection composite fabric formed by bonding multiple single-layer fabrics or films with hot melt adhesive. In actual production, it is difficult to achieve uniform distribution of the adhesive, resulting in uneven texture of the composite film fabric, and some areas have weak adhesion, and even there may be a protective "weak area".

[0010] Fourth, the thermal protection composite fabric formed by bonding multiple single-layer fabrics or films with hot melt adhesive. The current bonding method is surface bonding, that is, each layer of fabric or film is completely connected by hot melt adhesive or other adhesives to form a whole, resulting in a hard overall thermal protection composite film fabric with poor flexibility and difficulty in bending. The thermal protective clothing developed from such fabric is heavy, and the operation flexibility of the workers is poor, which seriously affects the work efficiency.

[0011] Fifth, when the workers wear the thermal protective clothing developed by the existing technology in a high temperature and high humidity environment, the barrier of the protective clothing leads to delayed heat dissipation, which easily causes human body heat imbalance, seriously affects the work efficiency of the workers, and even constitutes a life danger. Therefore, the thermal protection composite film fabric should have temperature regulation and buffering functions to ensure human body heat balance, protect the human body from thermal stress load, and prevent heat stroke.

[0012] It can be seen that the existing film-coated composite fabric has technical defects such as unstable film structure, no wind and rain protection function, overall weight, uneven texture, poor flexibility, and poor heat and humidity comfort. At the same time, the overall thermal protection level of the composite fabric needs to be improved. SUMMARY

[0013] In view of the above technical problems of the prior art, the present application first provides an intelligent temperature regulating and flame-retardant coaxial yarn, and the preparation method thereof comprises the following steps:

[0014] Step 1: Preparation of phase change flame-retardant filament: first, place the intelligent temperature regulating filament with a certain winding density in the plasma treatment device for treatment, then place the treated intelligent temperature regulating filament package in a high temperature and high pressure stirring reaction kettle, add a certain amount of mixture of composite flame retardant and crosslinking agent in the reaction kettle, set a certain stirring speed to make the intelligent temperature regulating filament package fully contact with the finishing agent, then dehydrate, and finally dry at a certain drying temperature to obtain the phase change flame-retardant filament.

[0015] Step 2: Firstly, the flame-retardant high-performance fiber mixture is sequentially subjected to oiling, pre-mixing, carding, drawing, and then the 3 temperature-adjusting phase-change flame-retardant filaments obtained in Step 1 and the 2 flame-retardant fiber rovings are spun into the intelligent temperature-adjusting flame-retardant coaxial yarn according to a certain arrangement.

[0016] The base material of the intelligent temperature-adjusting filament in Step 1 is one of acrylic, viscose, polyester, and nylon filaments;

[0017] In the plasma treatment in Step 1, the treatment pressure is 180-250 Pa, the treatment time is 4-8 min, and the treatment power is 20-35 W;

[0018] In the mixture of the composite flame retardant and the crosslinking agent in Step 1, the mass percentage of the composite flame retardant is 40%-60%, the mass percentage of the crosslinking agent is 5%-10%, and the rest is water, and the total mass percentage of the above components is 100%;

[0019] In the composite flame retardant in Step 1, the mass percentage of ammonium dihydrogen phosphate (MAP) is 40%-65%, the mass percentage of diammonium hydrogen phosphate (DAP) is 25%-45%, and the mass percentage of ammonium polyphosphate (APP) is 5%-25%, and the total mass percentage of the above components is 100%;

[0020] In the crosslinking agent in Step 1, the mass percentage of ammonium sulfate is 35%-75%, and the mass percentage of ammonium chloride is 25%-65%, and the total mass percentage of the above components is 100%

[0021] The volume density of the temperature-adjusting flame-retardant filaments in Step 1 wound on the hollow parallel pipe is 0.30-0.50 g / cm 3 ;

[0022] In Step 1, the stirring treatment temperature is 120-160℃, the stirring speed is 120-160 rpm, the dehydration time is 5-8 min, and the drying temperature is 180-200℃;

[0023] The high-performance flame-retardant fiber mixture in Step 2 is a mixture of two or more of flame-retardant viscose, modacrylic, aramid 1313, aramid 1414, polyphenylene sulfide fiber, and polyimide fiber (PI fiber);

[0024] Preferably, in the high-performance flame-retardant fiber mixture in Step 2, the mass percentage of flame-retardant viscose is 45%-55%, the mass percentage of modacrylic is 25%-35%, the mass percentage of aramid 1313 is 35%-55%, the mass percentage of aramid 1414 is 10%-35%, the mass percentage of polyphenylene sulfide fiber is 15%-35%, and the mass percentage of polyimide fiber is 45%-55%, and the total mass percentage of the components is 100%;

[0025] The arrangement mode of the temperature-regulating flame-retardant filaments and the flame-retardant fiber rovings in step 2 is, from left to right, one phase-change flame-retardant filament, one flame-retardant fiber roving, one phase-change flame-retardant filament, one flame-retardant fiber roving, and one phase-change flame-retardant filament.

[0026] The application also provides a flexible temperature-regulating heat protection fabric containing the above-mentioned intelligent temperature-regulating flame-retardant coaxial yarn, and a preparation method of the fabric includes the following steps:

[0027] Step 1): Preparation of the base fabric: the above-mentioned intelligent temperature-regulating flame-retardant coaxial yarn is used as warp and weft yarns, carbon-based conductive composite filaments are interwoven at equal intervals on the outer layer (front side) of the fabric, and flame-retardant hot-melt composite filaments are arranged at equal intervals on the inner layer (back side) of the fabric, and then the fabric is subjected to the processes of warping, sizing, reeding, weaving, and finishing to obtain the base fabric.

[0028] Step 2): Preparation of the film-coated composite fabric: the base fabric prepared in step 1) is subjected to the processes of desizing, dyeing, and tentering, and then is bonded with a nanometer waterproof and breathable film web format, and finally is rolled to form a flexible temperature-regulating heat protection film-coated composite fabric.

[0029] The linear density of the outer layer intelligent temperature-regulating flame-retardant coaxial yarn in step 1) is 23.62 tex to 29.53 tex.

[0030] The linear density of the inner layer intelligent temperature-regulating flame-retardant coaxial yarn in step 1) is 19.68 tex to 26.24 tex.

[0031] The linear density of the carbon-based conductive composite filaments in step 1) is 2.22 tex to 4.44 tex.

[0032] The fiber base material of the flame-retardant hot-melt composite filaments in step 1) is a polyester base or a nylon base.

[0033] The linear density of the flame-retardant hot-melt composite filaments in step 1) is 5.55 tex to 11.11 tex.

[0034] The melting point of the flame-retardant hot-melt composite filaments in step 1) is 110℃ to 130℃.

[0035] The fabric structure in step 1) is formed by the outer layer and the inner layer of warp and weft yarns through the interweaving and interlocking of the surface weft and the inner warp.

[0036] The planar pattern of the flame-retardant hot-melt composite filaments and the carbon-based conductive composite filaments formed on the inner and outer layers of the fabric in step 1) is a square, the side length of the square formed by the outer layer carbon-based conductive composite filaments is 5 to 10 mm, the side length of the square formed by the inner layer flame-retardant hot-melt composite filaments is 10 mm to 12 mm, and the two squares are distributed in a non-overlapping and overlapping manner.

[0037] The number of the flame-retardant hot-melt composite filaments in each cycle of the inner layer in step 1) is 2-4;

[0038] The fabric tissue structure of the outer layer in step 1) is plain weave or twill weave, and the fabric tissue structure of the inner layer is plain weave or varied twill weave;

[0039] The arrangement ratio of the inner and outer layer yarns in step 1) is 1:1-3:2;

[0040] The warp density of the fabric in step 1) is 535-582 per 10 cm, and the weft density is 465-504 per 10 cm;

[0041] The unit area mass of the base fabric in step 1) is 240-280 g / m 2 , and the unit area mass ratio of the inner and outer layer fabrics is 3:2;

[0042] The hot bonding temperature in step 2) is 130-150 DEG C;

[0043] The hot bonding form in step 2) is net form;

[0044] The nano waterproof and breathable film in step 2) is nano flame-retardant high-temperature-resistant ePTFE waterproof and breathable film;

[0045] The thickness of the nano waterproof and breathable film in step 2) is 0.20-0.40 mm;

[0046] The unit area mass of the nano waterproof and breathable film in step 2) is 20-40 g / m 2 ;

[0047] The unit area mass of the film-coated composite fabric in step 2) is 260-320 g / m 2 .

[0048] Compared with the prior art, the present application has the following advantages:

[0049] First, the lightweight flexible temperature-regulating thermal protective composite fabric provided by the present application creatively interweaves flame-retardant hot-melt composite filaments at equal distances on the reverse side of the fabric during the weaving and processing of the base fabric. The introduced flame-retardant hot-melt composite filaments can be used as an adhesive for the hot bonding of the base fabric and the waterproof and breathable film after being fused by lamination and heating, thereby avoiding the fabric weight increase caused by the additional coating of the adhesive in the prior art and realizing the "zero weight increase" of the adhesive during the processing of the film-coated composite fabric. Meanwhile, the distribution and quantity of the flame-retardant hot-melt composite filaments are determined during weaving, thereby realizing the accurate regulation of the adhesive content and coating position, solving the technical problems of glue penetration when the adhesive content is too high and insufficient bonding strength when the adhesive content is too low in the prior art, and avoiding the protective "weak area" caused by uneven distribution of the adhesive. The overall protective performance of the fabric is excellent and balanced.

[0050] Secondly, the flame-retardant hot melt composite filaments are equidistantly interwoven during weaving of the base cloth, and during thermal lamination, the grid-shaped flame-retardant hot melt composite filaments melt to form a grid bonding between the base cloth and the film, which solves the problems of hard texture and poor air permeability caused by surface bonding in the prior art while ensuring bonding firmness. The flexible design of the film composite fabric is realized, and the flexibility of the fabric is improved, which can be bent multiple times, and helps to improve the flexibility and convenience of the operator, thereby achieving the purpose of improving work efficiency.

[0051] Thirdly, the grid bonding forms a three-dimensional space between the base cloth and the film, and when the three-dimensional space contacts a high-temperature heat source, a three-dimensional array of air cavities is formed on the surface of the fabric due to the different thermal shrinkage rates of the film and the base cloth, the air cavities formed by the heat insulation layer of the captured air can delay the speed of heat transfer to the human body, so that the time for the human body to reach the secondary skin burn is prolonged, and the heat protection performance of the fabric is significantly improved.

[0052] Fourthly, the new hydrophilic active groups such as amino, carboxyl and hydroxyl are introduced into the intelligent temperature-regulating filaments of different fiber substrates by plasma treatment, and through the synergistic effect between different components of flame retardants, the chemical cross-linking reaction such as phosphorylation or sulfonation occurs under the action of cross-linking agents, the temperature-regulating filaments of acrylic, viscose, polyester and nylon substrates are flame-retardant finished, the intelligent temperature-regulating flame-retardant filaments are prepared, and the effective use of the intelligent temperature-regulating filaments in the heat protection fabric is realized. At the same time, due to the existence of the intelligent temperature-regulating flame-retardant filaments, on the one hand, the thermal stress generated by the clothing in the hot environment can be reduced, and the hygrothermal comfort performance of the heat protection fabric can be improved; on the other hand, the temperature mutation of the inner layer of the clothing can be inhibited, and the heat protection performance of the film-coated composite fabric can be enhanced.

[0053] Fifthly, the flame-retardant short fibers are uniformly distributed around the temperature-regulating filaments in the coaxial yarn structure, which effectively protects the phase change microcapsules distributed in the temperature-regulating filament substrate in an "island-in-sea" manner, so that the temperature-regulating function can effectively and durably play the intelligent temperature-regulating function. BRIEF DESCRIPTION OF DRAWINGS

[0054] Figure 1 Intelligent temperature-regulating flame-retardant coaxial yarn:

[0055] 1, 3, 5 - temperature-regulating flame-retardant filaments;

[0056] 2, 4 - flame-retardant fiber roving.

[0057] Figure 2 Lightweight flexible temperature-regulating heat protection composite fabric:

[0058] 6 - inner layer flame-retardant hot melt composite filaments;

[0059] 7 - outer layer carbon-based conductive composite filament;

[0060] 8 - flame retardant high temperature resistant ePTFE waterproof and breathable membrane;

[0061] 9 - three-dimensional array air cavity. DETAILED DESCRIPTION

[0062] The preferred embodiments of the present application are described below in conjunction with the accompanying drawings, it should be understood that the preferred embodiments described herein are only used to illustrate and explain the present application, and are not used to limit the present application.

[0063] Example 1:

[0064] A kind of intelligent temperature control flame-retardant coaxial yarn, its preparation method includes the following steps:

[0065] Step 1: preparation of phase change flame-retardant filament: first, the intelligent temperature control filament with a certain winding density is placed in the plasma treatment device for treatment, then the treated intelligent temperature control filament package is placed in a high temperature and high pressure stirring reactor, a certain amount of composite flame retardant and crosslinking agent mixture is added in the reactor, the intelligent temperature control filament package is fully contacted with the finishing agent by setting a certain stirring speed at a certain temperature, then dehydration treatment, and finally drying at a certain drying temperature to obtain phase change flame-retardant filament.

[0066] Step 2: first, the flame-retardant high-performance fiber mixture is sequentially subjected to oiling, pre-mixing, carding, drawing, and roving processes to form flame-retardant fiber roving, then the 3 temperature control phase change flame-retardant filaments obtained in step 1 and 2 flame-retardant fiber rovings are spun into intelligent temperature control flame-retardant coaxial yarn according to a certain arrangement.

[0067] The base material of the intelligent temperature control filament in step 1 is selected from acrylic fiber;

[0068] In step 1, the plasma treatment is performed at a pressure of 180 Pa for 6 min and a power of 35 W;

[0069] In step 1, the mixture of composite flame retardant and crosslinking agent contains 50% of composite flame retardant, 8% of crosslinking agent, and the rest is water, and the total mass fraction of the above components is 100%;

[0070] In step 1, the composite flame retardant contains 40% of ammonium dihydrogen phosphate (MAP), 35% of diammonium hydrogen phosphate (DAP), and 25% of ammonium polyphosphate (APP);

[0071] In step 1, the crosslinking agent contains 55% of ammonium sulfate and 45% of ammonium chloride;

[0072] The volume density of the temperature-regulating flame-retardant filament wound on the hollow parallel pipe in step 1 is 0.30 g / cm 3 ;

[0073] The stirring treatment temperature in step 1 is 120 DEG C, the stirring speed is 120 r / min, the dehydration time is 5 min, and the drying temperature is 180 DEG C;

[0074] The flame-retardant fiber mixture in step 2 comprises 45% of flame-retardant viscose, 25% of modacrylic, and 30% of aramid 1414;

[0075] The arrangement mode of the temperature-regulating flame-retardant filament and the flame-retardant fiber roving in step 2 is 1 temperature-regulating flame-retardant filament, 1 flame-retardant fiber roving, 1 temperature-regulating flame-retardant filament, 1 flame-retardant fiber roving, and 1 temperature-regulating flame-retardant filament from left to right.

[0076] Embodiment 2

[0077] A flexible temperature-regulating heat protection fabric containing the intelligent temperature-regulating flame-retardant coaxial yarn of embodiment 1, the preparation method of the fabric comprises the following steps:

[0078] Step 1): Preparation of base cloth: the intelligent temperature-regulating flame-retardant coaxial yarn prepared in embodiment 1 is used as warp and weft yarn, carbon-based conductive composite yarn is interwoven at equal intervals on the outer layer (front side) of the fabric, and flame-retardant hot melt composite filament is arranged at equal intervals on the inner layer (back side) of the fabric, and then the fabric is subjected to the processes of warping, sizing, reeding, weaving, and finishing to obtain the base cloth.

[0079] Step 2): Preparation of film-coated composite fabric: the base cloth prepared in step 3 is subjected to the processes of desizing, dyeing, and tentering, and then is bonded with a nanometer waterproof and breathable film web format, and finally is rolled to form a flexible temperature-regulating heat protection film-coated composite fabric.

[0080] The linear density of the outer layer intelligent temperature-regulating flame-retardant coaxial yarn in step 1 is 29.53 tex;

[0081] The linear density of the inner layer intelligent temperature-regulating flame-retardant coaxial yarn in step 1 is 23.62 tex;

[0082] The linear density of the carbon-based conductive composite yarn in step 1 is 2.22 tex;

[0083] The fiber base material of the flame-retardant hot melt composite filament in step 1 is polyester;

[0084] The linear density of the flame-retardant hot melt composite filament in step 1 is 11.11 tex;

[0085] The melting point of the flame-retardant hot melt composite filament in step 1 is 130 DEG C;

[0086] The fabric structure in step 1) is formed by interlacing the outer layer and the inner layer of warp and weft yarns through the surface weft and the inner warp;

[0087] The planar graph of the flame-retardant hot melt composite filament and the carbon-based conductive composite filament formed in the inner and outer layers of the fabric in step 1) is a square, the side length of the square formed by the outer layer of carbon-based conductive composite filament is 8 mm, the side length of the square formed by the inner layer of flame-retardant hot melt composite filament is 10 mm, and the two squares are distributed in a non-overlapping and overlapping manner;

[0088] The number of flame-retardant hot melt composite filaments in each cycle in the inner layer in step 1) is 3;

[0089] The fabric structure of the outer layer in step 1) is plain weave or twill weave, and the fabric structure of the inner layer is plain weave or variable twill weave;

[0090] The arrangement ratio of the inner and outer layer yarns in step 1) is 3:2;

[0091] The warp density of the fabric in step 1) is 535 roots / 10 cm, and the weft density is 465 roots / 10 cm;

[0092] The unit area mass of the base fabric in step 1) is 280 g / m 2 , and the unit area mass ratio of the inner and outer layer fabrics is 3:2;

[0093] The hot bonding temperature in step 2) is 150 DEG C;

[0094] The hot bonding form in step 2) is a mesh pattern;

[0095] The nano waterproof and breathable film in step 2) is a nano flame-retardant high-temperature-resistant ePTFE waterproof and breathable film;

[0096] The thickness of the nano waterproof and breathable film in step 2) is 0.20 mm;

[0097] The unit area mass of the nano waterproof and breathable film in step 2) is 20 g / m 2 ;

[0098] The unit area mass of the film-coated composite fabric in step 2) is 300 g / m 2 .

[0099] Example 3:

[0100] A kind of intelligent temperature regulating flame-retardant coaxial yarn, its preparation method includes the following steps:

[0101] Step 1: Preparation of phase change flame-retardant filament: First, the smart temperature-regulating filament with a certain winding density is placed in a plasma treatment device for treatment, and then the treated smart temperature-regulating filament package is placed in a high-temperature and high-pressure stirring reaction kettle. A certain amount of a mixture of a composite flame retardant and a crosslinking agent is added to the reaction kettle. The smart temperature-regulating filament package is fully contacted with the finishing agent at a certain temperature and a certain stirring speed. Then, dehydration treatment is performed, and finally, drying is performed at a certain drying temperature to obtain the phase change flame-retardant filament.

[0102] Step 2: First, the flame-retardant high-performance fiber mixture is sequentially subjected to oiling, pre-mixing, carding, drawing, and roving processes to form flame-retardant fiber roving. Then, the three temperature-regulating phase change flame-retardant filaments obtained in Step 1 and the two flame-retardant fiber rovings are spun into smart temperature-regulating flame-retardant coaxial yarn according to a certain arrangement.

[0103] The base material of the smart temperature-regulating filament in Step 1 is selected from acrylic fibers;

[0104] In Step 1, the plasma treatment is performed at a pressure of 250 Pa for 8 min and a power of 20 W.

[0105] In Step 1, the mixture of the composite flame retardant and the crosslinking agent contains 60% of the composite flame retardant, 10% of the crosslinking agent, and the rest is water. The total mass fraction of the above components is 100%.

[0106] In Step 1, the composite flame retardant contains 60% of ammonium dihydrogen phosphate (MAP), 25% of diammonium hydrogen phosphate (DAP), and 15% of ammonium polyphosphate (APP).

[0107] In Step 1, the crosslinking agent contains 35% of ammonium sulfate and 65% of ammonium chloride.

[0108] In Step 1, the volume density of the temperature-regulating flame-retardant filament wound on the hollow parallel pipe is 0.50 g / cm 3 ;

[0109] In Step 1, the stirring treatment temperature is 140°C, the stirring speed is 160 rpm, the dehydration time is 8 min, and the drying temperature is 200°C.

[0110] In Step 2, the high-performance flame-retardant fiber mixture contains 45% of flame-retardant viscose, 35% of aramid 1313, and 20% of polyphenylene sulfide.

[0111] In Step 2, the arrangement of the temperature-regulating flame-retardant filament and the flame-retardant fiber roving from left to right is one phase change flame-retardant filament, one flame-retardant fiber roving, one phase change flame-retardant filament, one flame-retardant fiber roving, and one phase change flame-retardant filament.

[0112] Example 4:

[0113] A flexible temperature-regulating thermal protective fabric containing the intelligent temperature-regulating flame-retardant coaxial yarn of Example 3, the preparation method of the fabric comprising the following steps:

[0114] Step 1): Preparation of base cloth: the intelligent temperature-regulating flame-retardant coaxial yarn prepared in Example 1 is used as warp and weft yarns, carbon-based conductive composite filaments are interwoven at equal intervals on the outer layer (front side) of the fabric, and flame-retardant hot melt composite filaments are arranged at equal intervals on the inner layer (back side) of the fabric, and then the fabric is subjected to beaming, sizing, reeding, weaving, and finishing to obtain the base cloth.

[0115] Step 2): Preparation of film-coated composite fabric: the base cloth prepared in Step 3 is subjected to desizing, dyeing, tentering, and other treatments, then is bonded with a nanometer waterproof and breathable film web format, and finally is rolled to form a flexible temperature-regulating thermal protective film-coated composite fabric.

[0116] The linear density of the outer layer intelligent temperature-regulating flame-retardant coaxial yarn in Step 1) is 23.62 tex;

[0117] The linear density of the inner layer intelligent temperature-regulating flame-retardant coaxial yarn in Step 1) is 19.68 tex;

[0118] The linear density of the carbon-based conductive composite filaments in Step 1) is 3.33 tex;

[0119] The fiber base material of the flame-retardant hot melt composite filaments in Step 1) is nylon-based;

[0120] The linear density of the flame-retardant hot melt composite filaments in Step 1) is 5.55 tex;

[0121] The melting point of the flame-retardant hot melt composite filaments in Step 1) is 110°C;

[0122] The fabric structure in Step 1) is formed by interweaving and joining the outer layer and inner layer warp and weft yarns through surface weft and inner warp;

[0123] The planar pattern of the flame-retardant hot melt composite filaments and carbon-based conductive composite filaments in Step 1) respectively formed on the inner and outer layers of the fabric is a square, the outer layer carbon-based conductive composite filaments form a square with a side length of 10 mm, the inner layer flame-retardant hot melt composite filaments form a square with a side length of 12 mm, and the two squares are distributed in a non-overlapping and overlapping manner;

[0124] The number of flame-retardant hot melt composite filaments in each cycle in Step 1) is 4;

[0125] The outer layer fabric structure in Step 1) is plain weave or twill weave, and the inner layer fabric structure is plain weave or variable twill weave;

[0126] The inner and outer layer yarn arrangement ratio in step 1) is 5:4;

[0127] The warp density of the fabric in step 1) is 582 ends / 10 cm, and the weft density is 492 ends / 10 cm;

[0128] The unit area mass of the base fabric in step 1) is 240 g / m 2 , and the unit area mass ratio of the inner and outer layer fabrics is 3:2;

[0129] The heat bonding temperature in step 2) is 130 DEG C;

[0130] The heat bonding form in step 2) is a mesh pattern;

[0131] The nano waterproof and breathable membrane in step 2) is a nano flame-retardant high-temperature-resistant ePTFE waterproof and breathable membrane;

[0132] The thickness of the nano waterproof and breathable membrane in step 2) is 0.30 mm;

[0133] The unit area mass of the nano waterproof and breathable membrane in step 2) is 30 g / m 2 ;

[0134] The unit area mass of the film-coated composite fabric in step 2) is 270 g / m 2 .

[0135] Example 5:

[0136] A kind of intelligent temperature regulating flame-retardant coaxial yarn, its preparation method includes the following steps:

[0137] Step 1: preparation of phase change flame-retardant filament: first, the intelligent temperature regulating filament of a certain winding density is placed in the plasma processing device to implement processing, then the treated intelligent temperature regulating filament package is placed in a high-temperature high-pressure stirring reactor, a certain amount of composite flame retardant and crosslinking agent mixture is added in the reactor, the intelligent temperature regulating filament package is fully contacted with the finishing agent by setting a certain stirring speed at a certain temperature, then dehydration treatment is carried out, and finally, the phase change flame-retardant filament is obtained by drying at a certain drying temperature.

[0138] Step 2: first, the flame-retardant high-performance fiber mixture is sequentially subjected to oiling, pre-mixing, carding, drawing, and roving processes to form flame-retardant fiber roving, then the three temperature regulating phase change flame-retardant filaments obtained in step 1 and two flame-retardant fiber rovings are spun into intelligent temperature regulating flame-retardant coaxial yarn according to a certain arrangement.

[0139] The base material of the intelligent temperature regulating filament in step 1 is selected as acrylic;

[0140] The plasma treatment in step 1 is performed at a pressure of 230 Pa, for 4 min, and at a power of 32 W;

[0141] The mixture of the composite flame retardant and the crosslinking agent in step 1 comprises 55% of the composite flame retardant, 8% of the crosslinking agent, and the rest is water, and the total mass fraction of the above components is 100%;

[0142] The composite flame retardant in step 1 comprises 50% of ammonium dihydrogen phosphate (MAP), 45% of diammonium hydrogen phosphate (DAP), and 5% of ammonium polyphosphate (APP);

[0143] The crosslinking agent in step 1 comprises 75% of ammonium sulfate and 25% of ammonium chloride;

[0144] The volume density of the temperature-regulating flame-retardant filament in step 1 wound on the hollow parallel pipe is 0.40 g / cm 3 ;

[0145] The stirring treatment in step 1 is performed at a temperature of 160°C, a stirring speed of 140 rpm, a dehydration time of 6 min, and a drying temperature of 180°C;

[0146] The mixture of high-performance flame-retardant fibers in step 2 comprises 35% of aramid 1313, 45% of polyimide, and 45% of aramid 1414;

[0147] The arrangement of the temperature-regulating flame-retardant filament and the flame-retardant fiber roving in step 2 from left to right is one temperature-regulating flame-retardant filament, one flame-retardant fiber roving, one temperature-regulating flame-retardant filament, one flame-retardant fiber roving, and one temperature-regulating flame-retardant filament.

[0148] Example 6:

[0149] A flexible temperature-regulating heat protection fabric containing the intelligent temperature-regulating flame-retardant coaxial yarn of Example 5, the preparation method of the fabric comprising the following steps:

[0150] Step 1): Preparation of the base fabric: the intelligent temperature-regulating flame-retardant coaxial yarn prepared in Example 1 is used as the warp and weft yarns, carbon-based conductive composite filaments are interwoven at equal intervals on the outer layer (front side) of the fabric, and flame-retardant hot melt composite filaments are arranged at equal intervals on the inner layer (back side) of the fabric, and then the fabric is subjected to beaming, sizing, reeding, weaving, and finishing to obtain the base fabric.

[0151] Step 2): Preparation of the film-coated composite fabric: the base fabric prepared in step 3 is subjected to desizing, dyeing, and tentering, and then is bonded with a nanometer waterproof and breathable film web format, and finally is rolled to form a flexible temperature-regulating heat protection film-coated composite fabric.

[0152] The linear density of the outer layer intelligent temperature-regulating flame-retardant coaxial yarn in step 1 is 26.24 tex;

[0153] The linear density of the inner layer intelligent temperature-regulating flame-retardant coaxial yarn in step 1) is 26.24 tex;

[0154] The linear density of the carbon-based conductive composite filament in step 1) is 4.44 tex;

[0155] The fiber base material of the flame-retardant hot melt composite filament in step 1) is nylon-based;

[0156] The linear density of the flame-retardant hot melt composite filament in step 1) is 8.33 tex;

[0157] The melting point of the flame-retardant hot melt composite filament in step 1) is 120℃;

[0158] The fabric organization structure in step 1) is formed by interweaving and interlocking the warp and weft yarns of the outer layer and the inner layer;

[0159] The planar graph formed by the flame-retardant hot melt composite filament and the carbon-based conductive composite filament in step 1) is a square, the outer layer carbon-based conductive composite filament forms a square with a side length of 5mm, the inner layer flame-retardant hot melt composite filament forms a square with a side length of 10mm, and the two squares are distributed in a non-overlapping and overlapping manner;

[0160] The number of flame-retardant hot melt composite filaments in each cycle of the inner layer in step 1) is 4;

[0161] The outer layer fabric organization structure in step 1) is plain weave or twill weave, and the inner layer fabric organization structure is plain weave or variable twill weave;

[0162] The arrangement ratio of the inner and outer layers of yarns in step 1) is 1:1;

[0163] The warp density of the fabric in step 1) is 543 roots / 10cm, and the weft density is 504 roots / 10cm;

[0164] The unit area mass of the base fabric in step 1) is 280g / m 2 , and the unit area mass ratio of the inner and outer layers of fabric is 3:2;

[0165] The heat bonding temperature in step 2) is 130℃;

[0166] The heat bonding form in step 2) is a mesh pattern;

[0167] The nano waterproof and breathable membrane in step 2) is a nano flame-retardant high-temperature-resistant ePTFE waterproof and breathable membrane;

[0168] The thickness of the nano waterproof and breathable membrane in step 2) is 0.40mm;

[0169] The unit area mass of the nano waterproof and breathable film in step 2) is 40 g / m 2 ;

[0170] The unit area mass of the film-coated composite fabric in step 2) is 320 g / m 2 .

[0171] Comparative Example 1:

[0172] The arrangement of the temperature-regulating and flame-retardant filaments and the flame-retardant fiber rovings from left to right is 1 temperature-regulating filament, 1 flame-retardant fiber roving, 1 temperature-regulating filament, 1 flame-retardant fiber roving, and 1 temperature-regulating filament, wherein the temperature-regulating filament does not undergo the flame-retardant treatment in step 1, i.e., only has the temperature-regulating function and does not have the flame-retardant function; the rest is the same as in Example 3.

[0173] Comparative Example 2:

[0174] A flexible temperature-regulating thermal protective fabric containing the intelligent temperature-regulating and flame-retardant coaxial yarn of Comparative Example 1, with the same process conditions as in Example 4.

[0175] Comparative Example 3:

[0176] The arrangement of the temperature-regulating and flame-retardant filaments and the flame-retardant fiber rovings from left to right is 1 temperature-regulating and flame-retardant filament, 1 temperature-regulating and flame-retardant filament, 1 temperature-regulating and flame-retardant filament, 1 temperature-regulating and flame-retardant filament, and 1 temperature-regulating and flame-retardant filament; the rest is the same as in Example 3.

[0177] Comparative Example 4:

[0178] A flexible temperature-regulating thermal protective fabric containing the intelligent temperature-regulating and flame-retardant coaxial yarn of Comparative Example 3, with the same process conditions as in Example 4.

[0179] Comparative Example 5:

[0180] The arrangement of the temperature-regulating and flame-retardant filaments and the flame-retardant fiber rovings from left to right is 1 flame-retardant fiber roving, 1 flame-retardant fiber roving, 1 flame-retardant fiber roving, 1 flame-retardant fiber roving, and 1 flame-retardant fiber roving; the rest is the same as in Example 3.

[0181] Comparative Example 6:

[0182] A flexible temperature-regulating thermal protective fabric containing the intelligent temperature-regulating and flame-retardant coaxial yarn of Comparative Example 5, with the same process conditions as in Example 4.

[0183] Comparative Example 7:

[0184] The composite flame retardant uses ammonium dihydrogen phosphate (MAP) accounting for 10%, diammonium phosphate (DAP) accounting for 20%, and ammonium polyphosphate (APP) accounting for 70%; the rest is the same as in Example 3.

[0185] Comparative Example 8:

[0186] A flexible temperature-regulating thermal protective fabric containing the intelligent temperature-regulating flame-retardant coaxial yarn of Comparative Example 7, the process conditions being the same as those of Example 4.

[0187] Comparative Example 9:

[0188] The composite flame retardant uses ammonium dihydrogen phosphate (MAP) accounting for 33.33%, diammonium hydrogen phosphate (DAP) accounting for 33.33%, and ammonium polyphosphate (APP) accounting for 33.33%; the rest is the same as Example 3.

[0189] Comparative Example 10:

[0190] A flexible temperature-regulating thermal protective fabric containing the intelligent temperature-regulating flame-retardant coaxial yarn of Comparative Example 9, the process conditions being the same as those of Example 4.

[0191] Comparative Example 11:

[0192] The flame retardant only uses ammonium dihydrogen phosphate (MAP); the rest is the same as Example 3.

[0193] Comparative Example 12:

[0194] A flexible temperature-regulating thermal protective fabric containing the intelligent temperature-regulating flame-retardant coaxial yarn of Comparative Example 11, the process conditions being the same as those of Example 4.

[0195] Comparative Example 13:

[0196] A flexible temperature-regulating thermal protective fabric containing the intelligent temperature-regulating flame-retardant coaxial yarn of Comparative Example 5, using face bonding to bond the base fabric and the waterproof and breathable film, and the rest of the process conditions being the same as those of Example 4.

[0197] The flexible temperature-regulating thermal protective fabrics prepared according to Examples 2 and 4, and Comparative Examples 2, 4, 6, 8, 10, 12, and 13 are tested according to standards GB / T 18318.1-2009 “Determination of the Bending Properties of Textiles Part 1: Inclined Plane Method”, FZ / T 60039-2013 “Peeling Strength Test Method for Coated Fabrics for Membrane Structures”, GB 8965.1-2020 “Protective Clothing Flame-Resistant Clothing”, and GB 38453-2019 “Protective Clothing Thermal Insulating Clothing”. The measured data of the physicochemical properties (bending stiffness, peeling strength), flame-retardant properties, and thermal insulation properties of the composite fabric are shown in Table 1.

[0198] Table 1: Test results of various indicators of lightweight flexible temperature-regulating thermal protective composite fabric

[0199]

[0200] By comparing and analyzing the test data of the composite fabric prepared in Example 4, Comparative Example 2, Comparative Example 4, Comparative Example 6, it can be seen that when the phase change temperature regulating filament does not have flame retardant (Comparative Example 2), the fabric has sustained combustion and smoldering phenomenon, and the flame retardant performance cannot meet the standard requirement (damage length > 100 mm), so it can be seen that the flame retardant performance must be given to the temperature regulating filament to meet the standard requirement; when all the coaxial yarns are phase change flame retardant filaments (Comparative Example 4), the damage length of the composite fabric is large, and the thermal stability cannot meet the standard requirement; when all the coaxial yarns are flame retardant filaments (Comparative Example 6), the thermal protective coefficient of the composite fabric is reduced by 30%, so it can be seen that when the coaxial yarns contain flame retardant temperature regulating filaments and flame retardant yarns at the same time, the overall performance of the flame retardant performance and the heat insulation performance of the composite fabric is better, so the various fibers in the coaxial yarns can significantly improve the flame retardant performance and the heat insulation performance of the fabric through synergistic effect.

[0201] By comparing and analyzing the test data of the composite fabric prepared in Example 4, Comparative Example 8, Comparative Example 10, Comparative Example 12, it can be seen that the specific composition of the flame retardant significantly affects the flame retardant and heat insulation performance of the composite fabric. When the components of the flame retardant are equal in mass (Comparative Example 10) or are single components (Comparative Example 12) or are not set according to the claim (Comparative Example 8), the flame retardant and heat insulation performance of the fabric is far from that of Example 4, so it can be seen that there is a flame retardant synergistic effect between the components of the flame retardant, and the content also affects the flame retardant and thermal protective performance of the composite fabric.

[0202] By comparing and analyzing the test data of the composite fabric prepared in Example 4, Comparative Example 6, Comparative Example 13, it can be seen that although the use of surface bonding can improve the peeling strength of the composite fabric, the bending strength of the fabric is increased by 213.6%, so it can be seen that the use of the mesh format bonding can significantly improve the flexibility of the composite fabric while ensuring the fastness of the composite fabric, and the thermal protective performance is slightly improved, so it can be seen that the light and flexible temperature regulating thermal protective composite fabric developed by the mesh format bonding of the present application can be used to develop high-performance thermal protective clothing with flexible operation.

[0203] The principles, steps and the like not explicitly described in the present application can be obtained by those skilled in the art through conventional technical means, and therefore will not be described. Obviously, those skilled in the art can make various modifications and variations to the present application without departing from the spirit and scope of the present application. Thus, if these modifications and variations of the present application fall within the scope of the claims of the present application and their equivalent technologies, the present application also intends to include these modifications and variations.

Claims

1. A process for the preparation of an intelligent temperature regulating flame retardant coaxial yarn characterized in that, It comprises the following steps: Step 1: Preparation of phase change flame-retardant filament: first, the intelligent temperature regulating filament is treated in a plasma treatment device, then the treated intelligent temperature regulating filament is placed in a high-temperature and high-pressure stirring reaction kettle, a mixture of composite flame retardant and crosslinking agent is added in the reaction kettle, stirring is carried out at a certain temperature, the stirring speed is set to make the intelligent temperature regulating filament cylinder yarn fully contact with the finishing agent, then dehydration treatment is carried out, and finally drying is carried out at a certain drying temperature to obtain the phase change flame-retardant filament, The base material of the intelligent temperature regulating filament in step 1 is one of acrylic, viscose, polyester and nylon filament; The plasma treatment in step 1 is carried out at a treatment pressure of 180-250 Pa, a treatment time of 4-8 min and a treatment power of 20-35 W; In the mixture of composite flame retardant and crosslinking agent in step 1, the mass percentage of composite flame retardant is 40-60%, the mass percentage of crosslinking agent is 5-10%, and the rest is water; In the composite flame retardant in step 1, ammonium dihydrogen phosphate (MAP) accounts for 40% ~ 65%, diammonium hydrogen phosphate (DAP) accounts for 25% ~ 45%, and ammonium polyphosphate (APP) accounts for 5% ~ 25%, and the total mass fraction of the above components is 100%; In the crosslinking agent in step 1, ammonium sulfate accounts for 35% ~ 75%, and ammonium chloride accounts for 25% ~ 65%, and the total mass fraction of the above components is 100% The volume density of the intelligent temperature regulating filament wound on the hollow parallel pipe in step 1 is 0.30-0.50 g / cm³; The treatment temperature of the stirring in step 1 is 120-160℃, the stirring speed is 120-160 revolutions / minute, the dehydration time is 5-8 min, and the drying temperature is 180-200℃; Step 2: First, the flame-retardant high-performance fiber mixture is sequentially subjected to oiling, pre-mixing, carding, drawing, and roving processes to form flame-retardant fiber roving, then 3 phase change flame-retardant filaments obtained in step 1 and 2 flame-retardant fiber rovings are spun into intelligent temperature regulating flame-retardant coaxial yarn according to a certain arrangement.

2. A process for the preparation of an intelligent temperature regulating flame retardant coaxial yarn as claimed in claim 1, wherein, The flame-retardant high-performance fiber mixture in step 2 is a mixture of two or more of flame-retardant viscose, modacrylic, aramid 1313, aramid 1414, polyphenylene sulfide fiber and polyimide fiber.

3. A method of making a smart temperature regulating flame resistant coaxial yarn according to claim 1 or 2, characterized in that, The arrangement of the phase change flame-retardant filament and the flame-retardant fiber roving in step 2 is 1 phase change flame-retardant filament, 1 flame-retardant fiber roving, 1 phase change flame-retardant filament, 1 flame-retardant fiber roving and 1 phase change flame-retardant filament from left to right.

4. The intelligent temperature regulating flame-retardant coaxial yarn prepared by the preparation method of any one of claims 1-3.

5. A method of making a flexible temperature-regulating thermal protective fabric, characterized in that, It comprises the following steps: Step 1): Preparation of base cloth: the intelligent temperature regulating flame-retardant coaxial yarn of claim 4 is used as warp and weft yarn, carbon-based conductive composite yarn is interwoven at equal intervals on the outer layer of the fabric, and flame-retardant hot melt composite filament is arranged at equal intervals on the inner layer of the fabric, and the fabric is subjected to warping, sizing, reeding, weaving, finishing and finishing in sequence to obtain the base cloth; Step 2): Preparation of the coated fabric: the base fabric prepared in step 1) is subjected to desizing, dyeing, and tentering treatment, then is web-format hot-bonded with the nano waterproof and breathable film, and finally is rolled to form the flexible temperature-regulating and thermal protective coated fabric.

6. The method of claim 5, wherein the flexible temperature-regulating thermal protective fabric is prepared by the steps of: The linear density of the intelligent temperature-regulating and flame-retardant coaxial yarn of the outer layer in step 1) is 23.62 tex to 29.53 tex; The linear density of the intelligent temperature-regulating and flame-retardant coaxial yarn of the inner layer in step 1) is 19.68 tex to 26.24 tex; The linear density of the carbon-based conductive composite filament in step 1) is 2.22 tex to 4.44 tex; The fiber base material of the flame-retardant hot-melt composite filament in step 1) is polyester-based or nylon-based; The linear density of the flame-retardant hot-melt composite filament in step 1) is 5.55 tex to 11.11 tex; The melting point of the flame-retardant hot-melt composite filament in step 1) is 110°C to 130°C; The fabric structure in step 1) is formed by interlacing and joining the warp yarns of the outer layer and the weft yarns of the inner layer through the surface weft and the inner warp; The planar graph formed by the flame-retardant hot-melt composite filament and the carbon-based conductive composite filament in step 1) is a square, the side length of the square formed by the carbon-based conductive composite filament in the outer layer is 5 to 10 mm, the side length of the square formed by the flame-retardant hot-melt composite filament in the inner layer is 10 mm to 12 mm, and the two squares are distributed in a non-overlapping and overlapping manner; The number of the flame-retardant hot-melt composite filament in each cycle of the inner layer in step 1) is 2 to 4; The fabric structure of the outer layer in step 1) is plain weave or twill weave, and the fabric structure of the inner layer is plain weave or variable twill weave; The arrangement ratio of the inner and outer layer yarns in step 1) is 1:1 to 3:2; The warp density of the fabric in step 1) is 535 to 582 per 10 cm, and the weft density is 465 to 504 per 10 cm; The unit area mass of the base cloth described in Step 1) is 240 to 280 g / m 2 The unit area mass ratio of the inner and outer fabrics is 3:

2.

7. The method of claim 5, wherein the flexible temperature-regulating thermal protective fabric is prepared by the steps of: The hot-bonding temperature in step 2) is 130°C to 150°C; The nano waterproof and breathable film in step 2) is a nano flame-retardant and high-temperature-resistant ePTFE waterproof and breathable film; The thickness of the nano waterproof and breathable film in step 2) is 0.20 to 0.40 mm; The unit area mass of the nano waterproof and breathable film described in step 2) is 20-40 g / m 2 ; The unit area mass of the film-coated composite fabric described in Step 2) is 260 to 320 g / m 2 .

8. A lightweight and flexible temperature-regulating and thermal protective composite fabric prepared by the preparation method according to any one of claims 5 to 7.

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