Flame-retardant high-temperature-resistant fabric and preparation method thereof

Abstract

The application discloses a kind of flame-retardant high-temperature resistant fabric and preparation method thereof, cloth is placed in pre-finishing liquid, two dip two roll, once drying, once baking, washing, plasma treatment, obtain pre-finishing cloth, then pre-finishing cloth is completely immersed in strengthening finishing liquid, heat impregnation, secondary drying, secondary baking, ammonia fumigation, washing, air dry, three times drying, immediately obtained.The pre-finishing liquid of the application is made by mixing polyacrylamide modified halloysite nanotube, nano zirconium oxide, tetrahydroxymethyl sulfate phosphorus, sodium dodecyl sulfate and water, the strengthening finishing liquid is made by mixing 1,2-dimethyl-3-hydroxyethyl imidazole bis (trifluoromethanesulfonyl) imidazole salt and 1-aminopropyl-3-methyl imidazole bis (trifluoromethanesulfonyl) imidazole salt, using them to carry out pre-finishing and strengthening finishing in turn, greatly improve the flame resistance and high-temperature resistance of fabric.

Description

A flame-retardant and high-temperature resistant fabric and its preparation method Technical Field

[0001] This invention belongs to the field of fabric preparation technology, specifically relating to a flame-retardant and high-temperature resistant fabric and its preparation method. Background Technology

[0002] With social progress, economic development, and the improvement of people's living standards, people have more diversified demands for functional textiles. Fire is a terrible disaster that can cause severe property damage and endanger human life. 50% of fires are caused by fiber materials, and 10% are caused by sparks generated by static electricity. Special fields such as automobiles, trains, airplanes, ships, seats, and mattresses have certain requirements for the flame retardancy and high-temperature resistance of fabrics. For example, JT / T1095-2016 "Flame Retardant Characteristics of Interior Materials for Operating Passenger Vehicles" stipulates an oxygen index ≥28.0%, while GB8624-2012 "Classification of Burning Performance of Building Materials and Products" and GB20286-2006 "Requirements and Marking for Burning Performance of Flame Retardant Products and Components in Public Places" stipulate an oxygen index ≥32.0%.

[0003] Most common fabrics on the market lack flame retardancy. A small amount is obtained by treating ordinary fabric with flame retardants, but this method produces fabrics with poor flame retardancy and lack high-temperature resistance. Fabrics obtained this way will slowly release or decompose under sealed, heated conditions, emitting a very unpleasant odor and potentially affecting human health, making them environmentally unfriendly. Furthermore, after multiple washes, a significant amount of flame-retardant components are lost, drastically reducing the flame-retardant effect until it disappears. In fact, the flame-retardant processing itself can damage the fabric's strength and reduce comfort, greatly limiting its widespread application.

[0004] Patent application CN113771454A discloses a flame-retardant composite fabric and its preparation method. The composite fabric is made by bonding an inner layer fabric and an outer layer fabric. The outer layer fabric is composed of an aerogel heat-insulating coating, a blended textile layer, and a flame-retardant heat-insulating coating. The blended textile layer is disposed between the aerogel heat-insulating coating and the flame-retardant heat-insulating coating, and the aerogel heat-insulating coating is disposed close to the inner layer fabric. The inner layer fabric is made of a blend of aramid 1313 fiber, pure cotton fiber, and activated carbon fiber. The blended textile layer is made of a blend of basalt fiber, cotton fiber, and polytetrafluoroethylene fiber. The outer layer fabric is obtained by coating the aerogel heat-insulating layer and the flame-retardant heat-insulating coating on both sides of the blended textile layer, and then the outer layer fabric and the inner layer fabric are laminated and bonded to obtain the composite fabric. This composite fabric mainly relies on aerogel insulation coating and flame-retardant insulation coating to achieve heat insulation and flame retardant effects. However, there is an unavoidable risk that repeated washing will cause the function to disappear. The flame-retardant insulation coating is obtained by directly mixing organosilicon resin, mica powder, hollow ceramic microspheres, chromium trioxide, etc., which makes it difficult to exert the maximum flame-retardant effect.

[0005] Patent application CN102965798A discloses a flame-retardant protective clothing fabric woven from flame-retardant yarns, wherein the flame-retardant yarns comprise the following fibers by weight: 50-60% wool fiber, 15-30% polyphenylene sulfide fiber, and 10-35% flame-retardant viscose fiber. This fabric achieves its flame-retardant properties solely through the flame-retardant viscose fiber, resulting in a generally poor flame-retardant effect and low high-temperature resistance. Summary of the Invention

[0006] To address the shortcomings of existing technologies, the present invention aims to provide a flame-retardant and high-temperature resistant fabric and its preparation method, which has good flame retardancy and high-temperature resistance.

[0007] To achieve the above objectives, the present invention adopts the following technical solution:

[0008] A method for preparing a flame-retardant and high-temperature resistant fabric involves immersing a pre-finishing fabric in a pre-treatment solution, performing two dips and two rolls, one drying, one baking, washing, and plasma treatment to obtain a pre-treated fabric. The pre-treated fabric is then completely immersed in a reinforcing finishing solution, heated and impregnated, dried a second time, baked a second time, fumigated with ammonia, washed, air-dried, and dried a third time to obtain the fabric. The pre-treatment solution is prepared by uniformly mixing the following raw materials in parts by weight: 8-10 parts polyacrylamide-modified halloysite nanotubes, 4-5 parts nano-zirconia, 3-4 parts tetramethylolphosphine sulfate, 1-2 parts sodium dodecyl sulfate, and 100 parts water. The reinforcing finishing solution is prepared by mixing the following raw materials in parts by weight: 30-40 parts 1,2-dimethyl-3-hydroxyethylimidazolium bis(trifluoromethanesulfonyl)imide salt and 70-80 parts 1-aminopropyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide salt.

[0009] Preferably, the greige fabric is obtained by blending and weaving cotton fibers and aramid fibers in a mass ratio of 10:2 to 3.

[0010] A further preferred method is as follows: cotton fibers are opened, cleaned, carded, combed, and pre-drawn to obtain combed cotton sliver; aramid fibers are opened, cleaned, carded, combed, and pre-drawn to obtain aramid cotton sliver; then the combed cotton sliver and aramid cotton sliver are blended, roving, spinning, and wound to obtain blended yarn; finally, the blended yarn is woven using a single-sided plain weave method, using 30S / 2 strands, with a warp density of 66 / 10cm, a weft density of 40 / 10cm, and a needle size of 12G.

[0011] Preferably, the process conditions for one drying step are: drying at 100-110℃ for 40-50 seconds; and the process conditions for one baking step are: baking at 150-160℃ for 25-30 seconds.

[0012] Preferably, the working gas for plasma treatment is argon at 100–200 sccm, nitrogen at 80–100 sccm, and oxygen at 200–220 sccm, with a gas discharge power of 3–4 kW and a treatment time of 2–3 minutes.

[0013] Preferably, the heat impregnation process conditions are: impregnation treatment at 110-120°C for 60-70 minutes under ultrasonic oscillation of 300-400W.

[0014] Preferably, the secondary drying process conditions are: drying at 110-120℃ for 60-70 seconds; the secondary baking process conditions are: baking at 160-170℃ for 100-120 seconds; and the air drying process conditions are: air drying at room temperature for 20-24 hours.

[0015] Preferably, the specific method for ammonia fumigation is as follows: the fabric after secondary baking is transferred to a vacuum reactor, and ammonia is flowed through the vacuum reactor at a rate of 400-500 L / min for 8-10 minutes at a temperature of 40-50°C, and then naturally cooled to room temperature.

[0016] Preferably, the process conditions for three drying cycles are: drying at 70-80℃ for 8-10 hours.

[0017] The preferred method for preparing the pretreatment solution is as follows: first, dissolve sodium dodecyl sulfate in water, then add nano-zirconia and tetramethyl phosphonic acid, stir and disperse evenly, finally add polyacrylamide to modify halloysite nanotubes, and then oscillate with ultrasonic waves at 300-400W for 50-60 minutes to obtain the solution, which is ready for immediate use.

[0018] Preferably, the polyacrylamide-modified halloysite nanotubes are prepared by the following method, based on parts by weight:

[0019] (A) First, dissolve 3-5 parts of pyridine in 10-12 parts of anhydrous ethanol, then add 0.8-1.2 parts of halloysite nanotubes, stir and heat to 65-75°C, keep warm and stir for 40-50 minutes, cool naturally to room temperature, centrifuge to collect the precipitate, wash, dry, and obtain pretreated halloysite nanotubes.

[0020] (B) Then, acrylic acid is prepared into an acrylic acid solution with a mass concentration of 15-20% using a 2-3 mol / L sodium hydroxide aqueous solution. 0.8-1.2 parts of acrylamide are prepared into an acrylamide solution with a mass concentration of 15-20% using water. 0.8-1.2 parts of the acrylic acid solution and the acrylamide solution are then mixed. Next, the obtained pretreated halloysite nanotubes are added and stirred until well mixed. Finally, 0.6-0.7 parts of sodium dodecyl sulfate and 0.6-0.7 parts of ammonium persulfate are added, and the mixture is stirred and heated to 70-80°C. The mixture is kept at this temperature and stirred for 3-4 hours. After naturally cooling to room temperature, it is dried to obtain the final product.

[0021] Preferably, the strengthening and finishing solution is obtained by mixing 1,2-dimethyl-3-hydroxyethylimidazolium bis(trifluoromethanesulfonyl)imide salt and 1-aminopropyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide salt and stirring at 400-500 r / min for 30-40 minutes.

[0022] A flame-retardant and high-temperature resistant fabric is obtained by the above preparation method.

[0023] Compared with the prior art, the present invention has the following beneficial effects:

[0024] This invention involves immersing the fabric in a pre-treatment solution, performing two dips and two rolls, one drying, one baking, washing, and plasma treatment to obtain a pre-treated fabric. The pre-treated fabric is then completely immersed in a reinforcing finishing solution, heated and impregnated, dried a second time, baked a second time, fumigated with ammonia, washed, air-dried, and dried a third time to obtain a flame-retardant and high-temperature resistant fabric. The pre-treatment solution is prepared by mixing polyacrylamide-modified halloysite nanotubes, nano-zirconia, tetramethylolphosphine sulfate, sodium dodecyl sulfate, and water. The reinforcing finishing solution is prepared by mixing 1,2-dimethyl-3-hydroxyethylimidazolium bis(trifluoromethanesulfonyl)imide salt and 1-aminopropyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide salt. Using these solutions sequentially for pre-treatment and reinforcing finishing significantly improves the fabric's flame retardancy and high-temperature resistance.

[0025] 1. The fabric of the present invention is made by blending and weaving cotton fiber and aramid fiber. Aramid fiber itself has high temperature resistance and flame retardancy, but its disadvantage is that it is expensive. Therefore, the present invention uses only a small amount of aramid fiber to blend with cotton fiber, so that the fabric has certain high temperature resistance and flame retardancy.

[0026] 2. This invention further improves the high temperature resistance and flame retardancy of the fabric through pre-treatment and reinforcement treatment.

[0027] The pre-finishing solution is prepared by mixing polyacrylamide-modified halloysite nanotubes, nano-zirconia, tetramethylolphosphine sulfate, sodium dodecyl sulfate, and water. Among these, nano-zirconia exhibits excellent high-temperature resistance, good stability, and small particle size. Filling the spaces between the fabric fibers, it significantly improves the product's high-temperature resistance, which in turn contributes to further improvements in flame retardancy. Tetramethylolphosphine sulfate possesses good flame retardancy, while halloysite nanotubes exhibit both high-temperature resistance and flame retardancy. Modifying the halloysite nanotubes with polyacrylamide further enhances their flame retardancy. Therefore, through the synergistic effect of polyacrylamide-modified halloysite nanotubes, nano-zirconia, and tetramethylolphosphine sulfate, the product's high-temperature resistance and flame retardancy are further improved.

[0028] The reinforcing finishing liquid is made by mixing 1,2-dimethyl-3-hydroxyethylimidazolium bis(trifluoromethanesulfonyl)imide salt and 1-aminopropyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide salt. These two ionic liquids have certain flame retardancy and can promote penetration and further bond the pre-finishing liquid components with the fabric fibers. The former contains hydroxyl groups and the latter contains amino groups, which can also strengthen the bonding force through hydrogen bonding, further improving the high temperature resistance and flame retardancy of the fabric.

[0029] 3. After the pre-treatment liquid treatment, plasma treatment is carried out. The plasma treatment promotes the combination of the components in the pre-treatment liquid with the fabric fibers, thereby improving the flame retardancy and high temperature resistance of the fabric.

[0030] 4. After the second baking, ammonia fumigation is performed. The specific method is as follows: the fabric after the second baking is transferred to a vacuum reactor, and ammonia gas is introduced to achieve fumigation. The ammonia gas penetrates into the fabric and forms a phosphorus-nitrogen flame retardant effect with tetramethylolphosphine sulfate, further improving the flame retardancy of the fabric. Detailed Implementation

[0031] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0032] Unless otherwise specified, all products in this invention were purchased through market channels.

[0033] Example 1

[0034] A method for preparing a flame-retardant and high-temperature resistant fabric involves immersing the pre-finished fabric in a pre-treatment solution, performing two dips and two rolls, one drying, one baking, washing, and plasma treatment to obtain a pre-treated fabric. The pre-treated fabric is then completely immersed in a reinforcing finishing solution, heated and impregnated, dried a second time, baked a second time, fumigated with ammonia, washed, air-dried, and dried a third time to obtain the fabric. The pre-treatment solution is prepared as follows: first, 1g of sodium dodecyl sulfate is dissolved in 100g of water; then, 4g of nano-zirconia and 3g of tetramethylolphosphine sulfate are added and stirred until evenly dispersed; finally, 8g of polyacrylamide-modified halloysite nanotubes are added, and the mixture is ultrasonically vibrated at 300W for 50 minutes to obtain the pre-treated fabric, ready for immediate use.

[0035] The strengthening and finishing solution is prepared by mixing 30g of 1,2-dimethyl-3-hydroxyethylimidazolium bis(trifluoromethanesulfonyl)imide salt and 70g of 1-aminopropyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide salt and stirring at 400r / min for 30 minutes.

[0036] The fabric is made by blending and weaving cotton fibers and aramid fibers in a mass ratio of 10:2.

[0037] The specific method is as follows: Cotton fibers are opened, cleaned, carded, combed, and pre-drawn to obtain combed cotton sliver; aramid fibers are opened, cleaned, carded, combed, and pre-drawn to obtain aramid cotton sliver; then the combed cotton sliver and aramid cotton sliver are blended, roving, spinning, and wound to obtain blended yarn; finally, the blended yarn is woven using a single-sided plain weave method, using 30S / 2 strands of yarn, with a warp density of 66 / 10cm, a weft density of 40 / 10cm, and a needle size of 12G.

[0038] The process conditions for one drying step are: drying at 100℃ for 40 seconds; the process conditions for one baking step are: baking at 150℃ for 25 seconds.

[0039] The working gases for plasma treatment are argon 100 sccm, nitrogen 80 sccm, and oxygen 200 sccm. The gas discharge power is 3 kW, and the treatment time is 2 minutes.

[0040] The heat impregnation process conditions are as follows: impregnation treatment at 110°C for 60 minutes under 300W ultrasonic oscillation.

[0041] The process conditions for secondary drying are: drying at 110℃ for 60 seconds; the process conditions for secondary baking are: baking at 160℃ for 100 seconds; and the process conditions for air drying are: air drying at room temperature for 20 hours.

[0042] The specific method for ammonia fumigation is as follows: after the fabric has been baked twice, it is transferred to a vacuum reactor. At 40°C, ammonia gas flows through the vacuum reactor at a rate of 400 L / min for 8 minutes, and then it is allowed to cool naturally to room temperature.

[0043] The process conditions for three drying cycles are: drying at 70℃ for 8 hours.

[0044] The polyacrylamide-modified halloysite nanotubes were prepared by the following method:

[0045] (A) First, dissolve 3g of pyridine in 10g of anhydrous ethanol, then add 0.8g of halloysite nanotubes, stir and heat to 65°C, keep warm and stir for 40 minutes, cool naturally to room temperature, centrifuge to collect the precipitate, wash and dry to obtain pretreated halloysite nanotubes.

[0046] (B) Then, acrylic acid was prepared into a 15% acrylic acid solution using a 2 mol / L sodium hydroxide aqueous solution, and 0.8 g of acrylamide was prepared into a 15% acrylamide solution using water. The 0.8 g acrylic acid solution and acrylamide solution were then mixed. The obtained pretreated halloysite nanotubes were then added and stirred until homogeneous. Finally, 0.6 g sodium dodecyl sulfate and 0.6 g ammonium persulfate were added, and the mixture was stirred and heated to 70°C. The mixture was kept at this temperature and stirred for 3 hours. After naturally cooling to room temperature, the mixture was dried to obtain the final product.

[0047] Example 2

[0048] A method for preparing a flame-retardant and high-temperature resistant fabric involves immersing the pre-finished fabric in a pre-treatment solution, performing two dips and two rolls, one drying, one baking, washing, and plasma treatment to obtain a pre-treated fabric. The pre-treated fabric is then completely immersed in a reinforcing finishing solution, heated and impregnated, dried a second time, baked a second time, fumigated with ammonia, washed, air-dried, and dried a third time to obtain the fabric. The pre-treatment solution is prepared as follows: first, 2g of sodium dodecyl sulfate is dissolved in 100g of water; then, 5g of nano-zirconia and 4g of tetramethylolphosphine sulfate are added and stirred until evenly dispersed; finally, 10g of polyacrylamide-modified halloysite nanotubes are added, and the mixture is ultrasonically vibrated at 400W for 60 minutes to obtain the pre-treated fabric, ready for immediate use.

[0049] The strengthening and finishing solution is obtained by mixing 40g of 1,2-dimethyl-3-hydroxyethylimidazolium bis(trifluoromethanesulfonyl)imide salt and 80g of 1-aminopropyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide salt, and stirring at 500r / min for 30-40 minutes.

[0050] The fabric is made by blending and weaving cotton fibers and aramid fibers in a mass ratio of 10:3.

[0051] The specific method is as follows: Cotton fibers are opened, cleaned, carded, combed, and pre-drawn to obtain combed cotton sliver; aramid fibers are opened, cleaned, carded, combed, and pre-drawn to obtain aramid cotton sliver; then the combed cotton sliver and aramid cotton sliver are blended, roving, spinning, and wound to obtain blended yarn; finally, the blended yarn is woven using a single-sided plain weave method, using 30S / 2 strands of yarn, with a warp density of 66 / 10cm, a weft density of 40 / 10cm, and a needle size of 12G.

[0052] The process conditions for one drying step are: drying at 110℃ for 50 seconds; the process conditions for one baking step are: baking at 160℃ for 30 seconds.

[0053] The working gases for plasma treatment are argon 200 sccm, nitrogen 100 sccm, and oxygen 220 sccm. The gas discharge power is 4 kW, and the treatment time is 3 minutes.

[0054] The heat impregnation process conditions are: impregnation treatment at 120°C for 70 minutes under 400W ultrasonic oscillation.

[0055] The process conditions for secondary drying are: drying at 120℃ for 70 seconds; the process conditions for secondary baking are: baking at 170℃ for 120 seconds; and the process conditions for air drying are: air drying at room temperature for 24 hours.

[0056] The specific method for ammonia fumigation is as follows: after the fabric has been baked twice, it is transferred to a vacuum reactor. At 50°C, ammonia gas flows through the vacuum reactor at a rate of 500 L / min for 10 minutes, and then it is allowed to cool naturally to room temperature.

[0057] The process conditions for three drying cycles are: drying at 80℃ for 10 hours.

[0058] The polyacrylamide-modified halloysite nanotubes were prepared by the following method:

[0059] (A) First, dissolve 5g of pyridine in 12g of anhydrous ethanol, then add 1.2g of halloysite nanotubes, stir and heat to 75°C, keep warm and stir for 50 minutes, cool naturally to room temperature, centrifuge to collect the precipitate, wash and dry to obtain pretreated halloysite nanotubes.

[0060] (B) Then, acrylic acid was prepared into a 20% acrylic acid solution using a 3 mol / L sodium hydroxide aqueous solution, and 1.2 g of acrylamide was prepared into a 20% acrylamide solution using water. The 1.2 g acrylic acid solution and acrylamide solution were then mixed. The obtained pretreated halloysite nanotubes were then added and stirred until homogeneous. Finally, 0.7 g sodium dodecyl sulfate and 0.7 g ammonium persulfate were added, and the mixture was stirred and heated to 80°C. The mixture was kept at this temperature and stirred for 4 hours. After naturally cooling to room temperature, the mixture was dried to obtain the final product.

[0061] Example 3

[0062] A method for preparing a flame-retardant and high-temperature resistant fabric involves immersing the pre-finished fabric in a pre-treatment solution, performing two dips and two rolls, one drying, one baking, washing, and plasma treatment to obtain a pre-treated fabric. The pre-treated fabric is then completely immersed in a reinforcing finishing solution, heated and impregnated, dried a second time, baked a second time, fumigated with ammonia, washed, air-dried, and dried a third time to obtain the fabric. The pre-treatment solution is prepared as follows: first, 1g of sodium dodecyl sulfate is dissolved in 100g of water; then, 5g of nano-zirconia and 3g of tetramethylolphosphine sulfate are added and stirred until evenly dispersed; finally, 10g of polyacrylamide-modified halloysite nanotubes are added, and the mixture is ultrasonically vibrated at 300W for 60 minutes to obtain the pre-treated fabric, ready for immediate use.

[0063] The strengthening and finishing solution is prepared by mixing 30g of 1,2-dimethyl-3-hydroxyethylimidazolium bis(trifluoromethanesulfonyl)imide salt and 80g of 1-aminopropyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide salt, and stirring at 400r / min for 40 minutes.

[0064] The fabric is made by blending and weaving cotton fibers and aramid fibers in a mass ratio of 10:2.

[0065] The specific method is as follows: Cotton fibers are opened, cleaned, carded, combed, and pre-drawn to obtain combed cotton sliver; aramid fibers are opened, cleaned, carded, combed, and pre-drawn to obtain aramid cotton sliver; then the combed cotton sliver and aramid cotton sliver are blended, roving, spinning, and wound to obtain blended yarn; finally, the blended yarn is woven using a single-sided plain weave method, using 30S / 2 strands of yarn, with a warp density of 66 / 10cm, a weft density of 40 / 10cm, and a needle size of 12G.

[0066] The process conditions for one drying step are: drying at 110℃ for 40 seconds; the process conditions for one baking step are: baking at 160℃ for 25 seconds.

[0067] The working gases for plasma treatment are argon 200 sccm, nitrogen 80 sccm, and oxygen 220 sccm. The gas discharge power is 3 kW, and the treatment time is 3 minutes.

[0068] The heat impregnation process conditions are: impregnation treatment at 120°C for 60 minutes under 300W ultrasonic oscillation.

[0069] The process conditions for secondary drying are: drying at 120℃ for 60 seconds; the process conditions for secondary baking are: baking at 170℃ for 100 seconds; and the process conditions for air drying are: air drying at room temperature for 24 hours.

[0070] The specific method for ammonia fumigation is as follows: after the fabric has been baked twice, it is transferred to a vacuum reactor. At 40°C, ammonia is flowed through the vacuum reactor at a rate of 500 L / min for 8 minutes. The mixture is then allowed to cool naturally to room temperature.

[0071] The process conditions for three drying cycles are: drying at 80℃ for 8 hours.

[0072] The polyacrylamide-modified halloysite nanotubes were prepared by the following method:

[0073] (A) First, dissolve 5g of pyridine in 10g of anhydrous ethanol, then add 1.2g of halloysite nanotubes, stir and heat to 65°C, keep warm and stir for 50 minutes, cool naturally to room temperature, centrifuge to collect the precipitate, wash and dry to obtain pretreated halloysite nanotubes.

[0074] (B) Then, acrylic acid was prepared into a 20% acrylic acid solution using a 2 mol / L sodium hydroxide aqueous solution, and 0.8 g of acrylamide was prepared into a 20% acrylamide solution using water. The 0.8 g acrylic acid solution and acrylamide solution were then mixed. Next, the obtained pretreated halloysite nanotubes were added and stirred until homogeneous. Finally, 0.7 g sodium dodecyl sulfate and 0.6 g ammonium persulfate were added, and the mixture was stirred and heated to 80°C. The mixture was kept at this temperature and stirred for 3 hours. After naturally cooling to room temperature, the mixture was dried to obtain the final product.

[0075] Example 4

[0076] A method for preparing a flame-retardant and high-temperature resistant fabric involves immersing the pre-finished fabric in a pre-treatment solution, performing two dips and two rolls, one drying, one baking, washing, and plasma treatment to obtain a pre-treated fabric. The pre-treated fabric is then completely immersed in a reinforcing finishing solution, heated and impregnated, dried a second time, baked a second time, fumigated with ammonia, washed, air-dried, and dried a third time to obtain the fabric. The pre-treatment solution is prepared as follows: first, 1.5g of sodium dodecyl sulfate is dissolved in 100g of water; then, 4.5g of nano-zirconia and 3.5g of tetramethylolphosphine sulfate are added and stirred until evenly dispersed; finally, 9g of polyacrylamide-modified halloysite nanotubes are added, and the mixture is ultrasonically vibrated at 400W for 55 minutes to obtain the pre-treated fabric, ready for immediate use.

[0077] The strengthening and finishing solution is obtained by mixing 35g of 1,2-dimethyl-3-hydroxyethylimidazolium bis(trifluoromethanesulfonyl)imide salt and 75g of 1-aminopropyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide salt, and stirring at 500r / min for 35 minutes.

[0078] The fabric is made by blending and weaving cotton fibers and aramid fibers in a mass ratio of 10:2.5.

[0079] The specific method is as follows: Cotton fibers are opened, cleaned, carded, combed, and pre-drawn to obtain combed cotton sliver; aramid fibers are opened, cleaned, carded, combed, and pre-drawn to obtain aramid cotton sliver; then the combed cotton sliver and aramid cotton sliver are blended, roving, spinning, and wound to obtain blended yarn; finally, the blended yarn is woven using a single-sided plain weave method, using 30S / 2 strands of yarn, with a warp density of 66 / 10cm, a weft density of 40 / 10cm, and a needle size of 12G.

[0080] The process conditions for one drying step are: drying at 105℃ for 45 seconds; the process conditions for one baking step are: baking at 155℃ for 28 seconds.

[0081] The working gases for plasma treatment are argon 150 sccm, nitrogen 90 sccm, and oxygen 210 sccm. The gas discharge power is 3.5 kW, and the treatment time is 2.5 minutes.

[0082] The heat impregnation process conditions are: impregnation treatment at 115°C for 65 minutes under 400W ultrasonic oscillation.

[0083] The process conditions for secondary drying are: drying at 115℃ for 65 seconds; the process conditions for secondary baking are: baking at 165℃ for 110 seconds; and the process conditions for air drying are: air drying at room temperature for 22 hours.

[0084] The specific method for ammonia fumigation is as follows: after the fabric has been baked twice, it is transferred to a vacuum reactor. At 45°C, ammonia gas flows through the vacuum reactor at a rate of 500 L / min for 9 minutes, and then it is allowed to cool naturally to room temperature.

[0085] The process conditions for three drying cycles are: drying at 75℃ for 9 hours.

[0086] The polyacrylamide-modified halloysite nanotubes were prepared by the following method:

[0087] (A) First, dissolve 4g of pyridine in 11g of anhydrous ethanol, then add 1g of halloysite nanotubes, stir and heat to 70°C, keep warm and stir for 45 minutes, cool naturally to room temperature, centrifuge to collect the precipitate, wash and dry to obtain pretreated halloysite nanotubes.

[0088] (B) Then, acrylic acid was prepared into an 18% acrylic acid solution using a 3 mol / L sodium hydroxide aqueous solution. 1 g of acrylamide was prepared into an 18% acrylamide solution using water. The acrylic acid solution and acrylamide solution were then mixed. The obtained pretreated halloysite nanotubes were then added and stirred until homogeneous. Finally, 0.65 g of sodium dodecyl sulfate and 0.65 g of ammonium persulfate were added. The mixture was stirred and heated to 75°C and kept at this temperature for 3.5 hours. After naturally cooling to room temperature, the mixture was dried to obtain the final product.

[0089] Comparative Example 1

[0090] A method for preparing a fabric involves placing a pre-finished fabric in a pre-treatment solution, subjecting it to two dips and two rolls, one drying, one baking, and washing to obtain a pre-treated fabric. The pre-treated fabric is then completely immersed in a reinforcing finishing solution, heated for impregnation, dried a second time, baked a second time, fumigated with ammonia, washed, air-dried, and dried a third time to obtain the fabric. The pre-treatment solution is prepared as follows: first, 1g of sodium dodecyl sulfate is dissolved in 100g of water; then, 4g of nano-zirconia and 3g of tetramethylolphosphine sulfate are added and stirred until evenly dispersed; finally, 8g of polyacrylamide-modified halloysite nanotubes are added, and the mixture is ultrasonically vibrated at 300W for 50 minutes to obtain the pre-treated fabric, ready for immediate use.

[0091] The strengthening and finishing solution is prepared by mixing 30g of 1,2-dimethyl-3-hydroxyethylimidazolium bis(trifluoromethanesulfonyl)imide salt and 70g of 1-aminopropyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide salt and stirring at 400r / min for 30 minutes.

[0092] The fabric is made by blending and weaving cotton fibers and aramid fibers in a mass ratio of 10:2.

[0093] The specific method is as follows: Cotton fibers are opened, cleaned, carded, combed, and pre-drawn to obtain combed cotton sliver; aramid fibers are opened, cleaned, carded, combed, and pre-drawn to obtain aramid cotton sliver; then the combed cotton sliver and aramid cotton sliver are blended, roving, spinning, and wound to obtain blended yarn; finally, the blended yarn is woven using a single-sided plain weave method, using 30S / 2 strands of yarn, with a warp density of 66 / 10cm, a weft density of 40 / 10cm, and a needle size of 12G.

[0094] The process conditions for one drying step are: drying at 100℃ for 40 seconds; the process conditions for one baking step are: baking at 150℃ for 25 seconds.

[0095] The heat impregnation process conditions are as follows: impregnation treatment at 110°C for 60 minutes under 300W ultrasonic oscillation.

[0096] The process conditions for secondary drying are: drying at 110℃ for 60 seconds; the process conditions for secondary baking are: baking at 160℃ for 100 seconds; and the process conditions for air drying are: air drying at room temperature for 20 hours.

[0097] The specific method for ammonia fumigation is as follows: after the fabric has been baked twice, it is transferred to a vacuum reactor. At 40°C, ammonia gas flows through the vacuum reactor at a rate of 400 L / min for 8 minutes, and then it is allowed to cool naturally to room temperature.

[0098] The process conditions for three drying cycles are: drying at 70℃ for 8 hours.

[0099] The polyacrylamide-modified halloysite nanotubes were prepared by the following method:

[0100] (A) First, dissolve 3g of pyridine in 10g of anhydrous ethanol, then add 0.8g of halloysite nanotubes, stir and heat to 65°C, keep warm and stir for 40 minutes, cool naturally to room temperature, centrifuge to collect the precipitate, wash and dry to obtain pretreated halloysite nanotubes.

[0101] (B) Then, acrylic acid was prepared into a 15% acrylic acid solution using a 2 mol / L sodium hydroxide aqueous solution, and 0.8 g of acrylamide was prepared into a 15% acrylamide solution using water. The 0.8 g acrylic acid solution and acrylamide solution were then mixed. The obtained pretreated halloysite nanotubes were then added and stirred until homogeneous. Finally, 0.6 g sodium dodecyl sulfate and 0.6 g ammonium persulfate were added, and the mixture was stirred and heated to 70°C. The mixture was kept at this temperature and stirred for 3 hours. After naturally cooling to room temperature, the mixture was dried to obtain the final product.

[0102] Comparative Example 2

[0103] A method for preparing a fabric involves placing a pre-finished fabric in a pre-treatment solution, performing two dips and two rolls, one drying, one baking, washing, and plasma treatment to obtain a pre-treated fabric. The pre-treated fabric is then completely immersed in a reinforcing finishing solution, heated and impregnated, dried a second time, baked a second time, fumigated with ammonia, washed, air-dried, and dried a third time to obtain the fabric. The pre-treatment solution is prepared as follows: first, 1g of sodium dodecyl sulfate is dissolved in 100g of water, then 4g of nano-zirconia and 3g of tetramethylolphosphine sulfate are added, and the mixture is stirred and dispersed evenly to obtain the pre-treated fabric, ready for immediate use.

[0104] The strengthening and finishing solution is prepared by mixing 30g of 1,2-dimethyl-3-hydroxyethylimidazolium bis(trifluoromethanesulfonyl)imide salt and 70g of 1-aminopropyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide salt and stirring at 400r / min for 30 minutes.

[0105] The fabric is made by blending and weaving cotton fibers and aramid fibers in a mass ratio of 10:2.

[0106] The specific method is as follows: Cotton fibers are opened, cleaned, carded, combed, and pre-drawn to obtain combed cotton sliver; aramid fibers are opened, cleaned, carded, combed, and pre-drawn to obtain aramid cotton sliver; then the combed cotton sliver and aramid cotton sliver are blended, roving, spinning, and wound to obtain blended yarn; finally, the blended yarn is woven using a single-sided plain weave method, using 30S / 2 strands of yarn, with a warp density of 66 / 10cm, a weft density of 40 / 10cm, and a needle size of 12G.

[0107] The process conditions for one drying step are: drying at 100℃ for 40 seconds; the process conditions for one baking step are: baking at 150℃ for 25 seconds.

[0108] The working gases for plasma treatment are argon 100 sccm, nitrogen 80 sccm, and oxygen 200 sccm. The gas discharge power is 3 kW, and the treatment time is 2 minutes.

[0109] The heat impregnation process conditions are as follows: impregnation treatment at 110°C for 60 minutes under 300W ultrasonic oscillation.

[0110] The process conditions for secondary drying are: drying at 110℃ for 60 seconds; the process conditions for secondary baking are: baking at 160℃ for 100 seconds; and the process conditions for air drying are: air drying at room temperature for 20 hours.

[0111] The specific method for ammonia fumigation is as follows: after the fabric has been baked twice, it is transferred to a vacuum reactor. At 40°C, ammonia gas flows through the vacuum reactor at a rate of 400 L / min for 8 minutes, and then it is allowed to cool naturally to room temperature.

[0112] The process conditions for three drying cycles are: drying at 70℃ for 8 hours.

[0113] Test case

[0114] The high temperature resistance and flame retardancy of the fabrics obtained in Examples 1-4 and Comparative Examples 1 and 2 were investigated respectively, and the results are shown in Table 1.

[0115] High temperature resistance: Refer to GB / T13767-92 "Determination of heat resistance of textiles" to determine the maximum temperature that the fabric can withstand.

[0116] Flame retardancy: The flame retardancy of the fabric was investigated with reference to GB / T5454-1997 "Test for Burning Performance of Textiles - Oxygen Index Method" and GB / T5455-2014 "Determination of Vertical Damage Length, Smoldering and Afterflame Time of Textiles".

[0117] Table 1. Performance Evaluation Results

[0118]

[0119] As shown in Table 1, the fabrics obtained in Examples 1 to 4 have excellent high temperature resistance and flame retardancy, which can meet high fire protection requirements.

[0120] Comparative Example 1 omitted plasma treatment, and Comparative Example 2 omitted polyacrylamide-modified halloysite nanotubes. The resulting fabrics showed significantly worse high-temperature resistance and flame retardancy, indicating that plasma treatment is beneficial to improving the high-temperature resistance and flame retardancy of the fabrics. Polyacrylamide-modified halloysite nanotubes, along with other components, synergistically improve the high-temperature resistance and flame retardancy of the fabrics.

[0121] The present invention has been illustrated through the above embodiments, but the present invention is not limited to the above embodiments, that is, it does not mean that the present invention must rely on the above embodiments to be implemented. Those skilled in the art should understand that any improvements to the present invention, equivalent substitutions of individual raw materials in the product of the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

Claims

1. A method for preparing a flame-retardant and high-temperature resistant fabric, characterized in that, The pre-finished fabric is placed in a pre-treatment solution, dipped and rolled twice, dried once, baked once, washed, and plasma-treated to obtain a pre-treated fabric. Then, the pre-treated fabric is completely immersed in a reinforcing finishing solution, heated and impregnated, dried a second time, baked a second time, fumigated with ammonia, washed, air-dried, and dried a third time to obtain the fabric. The pre-treatment solution is prepared by uniformly mixing the following raw materials in parts by weight: 8-10 parts polyacrylamide-modified halloysite nanotubes, 4-5 parts nano-zirconia, and tetramethylolsulfonic acid. Phosphorus 3-4 parts, sodium dodecyl sulfate 1-2 parts, water 100 parts; the strengthening finishing liquid is prepared by mixing the following raw materials in parts by weight: 30-40 parts of 1,2-dimethyl-3-hydroxyethylimidazolium bis(trifluoromethanesulfonyl)imide salt, 70-80 parts of 1-aminopropyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide salt; wherein, the grey fabric is obtained by blending and weaving cotton fiber and aramid fiber in a mass ratio of 10:2-3; wherein, the specific method of ammonia fumigation is: secondary baking... After drying, the fabric is transferred to a vacuum reactor. Ammonia gas is introduced into the reactor at 40-50°C at a rate of 400-500 L / min for 8-10 minutes, and then the mixture is allowed to cool naturally to room temperature. The pre-finishing solution is prepared as follows: sodium dodecyl sulfate is dissolved in water, followed by the addition of nano-zirconia and tetramethyl phosphonic acid, which are stirred and dispersed evenly. Finally, polyacrylamide-modified halloysite nanotubes are added, and the mixture is ultrasonically vibrated at 300-400 W for 50-60 minutes to obtain the solution, which is ready for immediate use. The strengthening and finishing solution is obtained by mixing 1,2-dimethyl-3-hydroxyethylimidazolium bis(trifluoromethanesulfonyl)imide salt and 1-aminopropyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide salt and stirring at 400-500 r / min for 30-40 minutes; wherein, the working gas for plasma treatment is argon 100-200 sccm, nitrogen 80-100 sccm, and oxygen 200-220 sccm, the gas discharge power is 3-4 kW, and the treatment time is 2-3 minutes.

2. The preparation method according to claim 1, characterized in that, The specific preparation method of the greige fabric is as follows: cotton fibers are opened, cleaned, carded, combed, and pre-drawn to obtain combed cotton sliver; aramid fibers are opened, cleaned, carded, combed, and pre-drawn to obtain aramid cotton sliver; then the combed cotton sliver and aramid cotton sliver are blended, roving, spinning, and wound to obtain blended yarn; finally, the blended yarn is woven using a single-sided plain weave method, using 30S / 2 strands, with a warp density of 66 / 10cm, a weft density of 40 / 10cm, and a needle size of 12G.

3. The preparation method according to claim 1, characterized in that, The process conditions for a single drying are: drying at 100-110℃ for 40-50 seconds; the process conditions for a single baking are: baking at 150-160℃ for 25-30 seconds.

4. The preparation method according to claim 1, characterized in that, The process conditions for heat impregnation are: impregnation treatment at 110-120℃ for 60-70 minutes under ultrasonic oscillation of 300-400W.

5. The preparation method according to claim 1, characterized in that, The process conditions for secondary drying are: drying at 110-120℃ for 60-70 seconds; the process conditions for secondary baking are: baking at 160-170℃ for 100-120 seconds; and the process conditions for air drying are: air drying at room temperature for 20-24 hours.

6. A flame-retardant and high-temperature resistant fabric, obtained by the preparation method described in any one of claims 1 to 5.

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