A flame-retardant fiber fireproof and heat-insulating knitted composite cotton and its preparation process

Abstract

The present invention relates to the technical field of composite layer structures, and particularly relates to a flame-retardant fiber fireproof and heat-insulating knitted composite cotton and a preparation process thereof. The knitted composite cotton includes a knitted cotton matrix layer, fiber layers are fixedly arranged on both the upper surface and the lower surface of the knitted cotton matrix layer, both fiber layers are woven by polyester fibers and spandex fibers, resin layers are fixedly arranged on the outer surfaces of both fiber layers, and the resin layers are formed by molding and curing with a resin composite agent. The knitted composite cotton of the present invention is composed of a knitted cotton matrix layer, two upper and lower fiber layers, and two upper and lower resin layers. The resin body in the resin composite agent is formulated with bisphenol A epoxy resin, dicyandiamide curing agent, 1-benzyl-2-methylimidazole, and silane coupling agent KH560 to form a base liquid. Glass microspheres and magnesium hydroxide flame retardant added as functional auxiliaries, and at the same time, modified glass fibers and reinforcing effect modifiers coordinate with each other to jointly enhance the effect. The obtained knitted composite cotton has excellent heat insulation and flame-retardant fireproof properties.

Description

Technical Field

[0001] The present invention relates to the technical field of composite cotton structures, and particularly relates to a flame-retardant fiber fireproof and heat-insulating knitted composite cotton and a preparation process thereof. Background Art

[0002] Fabrics play a great role in human life. In addition to directly using fiber fabrics, they can also be processed into composite materials in combination with resin matrices. Moreover, due to their high strength and high modulus characteristics, fiber-reinforced composite materials have been widely used in the engineering field.

[0003] For the existing knitted composite materials, in order to improve the heat-insulating performance of the products, it is easy to cause a decline in the flame-retardant and fireproof performance of the products. It is very difficult to coordinately improve the heat-insulating, flame-retardant and fireproof properties of the products. At the same time, the corrosion resistance and immersion stability of the products are poor, which limits the use efficiency of the products. Summary of the Invention

[0004] Aiming at the defects of the existing technology, the purpose of the present invention is to provide a flame-retardant fiber fireproof and heat-insulating knitted composite cotton and a preparation process thereof, so as to solve the problems put forward in the above background art.

[0005] The present invention adopts the following technical solutions to solve the technical problems:

[0006] The present invention provides a flame-retardant fiber fireproof and heat-insulating knitted composite cotton. The knitted composite cotton includes a knitted cotton matrix layer. Fiber layers are fixedly arranged on both the upper surface and the lower surface of the knitted cotton matrix layer. Both fiber layers are woven from polyester fiber and spandex fiber according to a weight ratio of 1:1.

[0007] Resin layers are fixedly arranged on the outer surfaces of both fiber layers away from the knitted cotton matrix layer. The resin layers are formed by molding and curing with a resin composite agent. The molding and curing temperature is 130 - 135 °C, the molding pressure is 10 Mpa, and the molding time is 12 h.

[0008] Preferably, the preparation method of the knitted cotton matrix layer is as follows:

[0009] Knit 35 - 40 parts of 100S / 2 cotton yarn and 30 - 35 parts of 30D spandex yarn into a cotton fabric by weight. Then immerse the cotton fabric in a sufficient amount of sodium hydroxide solution with a mass fraction of 5% for alkali washing treatment. After the treatment, wash with water and dry to obtain the knitted cotton matrix layer.

[0010] Preferably, the resin composite agent includes the following raw materials in parts by weight:

[0011] 10 - 15 parts of modified glass fiber, 5 - 8 parts of glass microspheres, 4 - 7 parts of magnesium hydroxide flame retardant, 6 - 10 parts of reinforcement modifier, and 45 - 55 parts of resin body.

[0012] Preferably, the resin body is prepared from bisphenol A epoxy resin, dicyandiamide curing agent, 1-benzyl-2-methylimidazole, and silane coupling agent KH560 in a weight ratio of 50:10:3:2.

[0013] Preferably, the preparation method of the modified glass fiber is as follows:

[0014] S01: First, place the glass fiber in a sufficient amount of hydrogen peroxide solution with a mass fraction of 5-8% and stir well, then wash and dry it to obtain dried glass fiber; place the dried glass fiber in a proton irradiation chamber for irradiation for 20-30 min with an irradiation power of 350-400 W, and after the irradiation ends, obtain irradiated glass fiber;

[0015] S02: By weight, add 4-6 parts of kaolin powder and 1-3 parts of sodium silicate solution to 5-8 parts of phosphate buffer solution, and then add 2-4 parts of boron nitride and stir evenly to obtain the first additive solution;

[0016] By weight, add 3-5 parts of silicon carbide whiskers and 2-4 parts of sodium carboxymethylcellulose to 5-8 parts of chitosan solution and stir evenly to obtain the second additive solution;

[0017] S03: Mix the first additive solution and the second additive solution in a weight ratio of 5:3, perform ball milling treatment at a ball milling speed of 1500 r / min for 2 h, and after the ball milling ends, obtain the modified solution;

[0018] S04: Add the irradiated glass fiber to a modified solution that is 4-7 times the total weight of the irradiated glass fiber and perform stirring modification treatment. After the stirring ends, filter and dry to obtain the modified glass fiber.

[0019] Preferably, the mass fraction of the sodium silicate solution is 4-6%; the pH value of the phosphate buffer solution is 5.5; the mass fraction of the chitosan solution is 3-5%.

[0020] Preferably, the stirring speed of the stirring modification treatment is 550-650 r / min and the stirring time is 30 min.

[0021] Preferably, the preparation method of the reinforcement modifier is as follows:

[0022] S11: Preheat the flaky talc at 55-60 °C for 1 h, then immerse the preheated flaky talc in a lanthanum chloride solution that is 3-5 times the total weight of the preheated flaky talc and perform stirring treatment at a stirring speed of 500-700 r / min for 2 h. After the stirring ends, filter and dry to obtain the flaky talc agent doped with lanthanum;

[0023] S12: Mix the lanthanum-doped flaky talc agent and the intensity-adjusting and efficiency-supplementing liquid in a weight ratio of 5:3, perform ball milling treatment. The ball milling speed is 1000 - 1500 r / min, ball mill for 1 h. After the ball milling is completed, perform suction filtration and drying to obtain the intensity-adjusting and efficiency-strengthening agent.

[0024] Preferably, the mass fraction of the lanthanum chloride solution is 3 - 6%.

[0025] Preferably, the intensity-adjusting and efficiency-supplementing liquid comprises the following raw materials in parts by weight:

[0026] 3 - 4 parts of nano-aluminum oxide, 4 - 6 parts of sodium lignosulfonate solution, 2 - 3 parts of hydroxyapatite, 1 - 2 parts of yttrium oxide, and 1 - 2 parts of sodium alginate solution.

[0027] Preferably, the mass fraction of the sodium lignosulfonate solution is 5 - 8%; the mass fraction of the sodium alginate solution is 3 - 6%.

[0028] The present invention also provides a preparation process for a flame-retardant fiber fireproof and heat-insulating knitted composite cotton, comprising the following steps:

[0029] Step 1: Prepare a knitted cotton matrix layer;

[0030] Step 2: Prepare a fiber layer, and arrange the fiber layer on the upper surface and the lower surface of the knitted cotton matrix layer;

[0031] Step 3: Prepare a resin composite agent, and arrange a resin layer on the outer surface of the fiber layer away from the knitted cotton matrix layer, thus obtaining the flame-retardant fiber fireproof and heat-insulating knitted composite cotton.

[0032] Compared with the prior art, the present invention has the following beneficial effects:

[0033] The knitted composite cotton of the present invention is composed of a knitted cotton matrix layer, two upper and lower fiber layers, and two upper and lower resin layers. The knitted cotton matrix layer is knitted by cotton yarn and spandex yarn. The resin body in the resin composite is formulated with bisphenol A epoxy resin, dicyandiamide curing agent, 1-benzyl-2-methylimidazole, and silane coupling agent KH560 to form a base liquid. Glass microspheres and magnesium hydroxide flame retardant are added as functional aids. At the same time, modified glass fiber and reinforcing agent are coordinated and synergistically enhanced, resulting in the knitted composite cotton having excellent heat preservation and flame retardancy, and the coordination and improvement of the two. At the same time, the corrosion resistance and immersion stability of the product are remarkable. The modified glass fiber is improved by oxidizing and activating glass fiber with hydrogen peroxide solution, and then through proton irradiation, coordinated and optimized improvement. At the same time, it is stirred and improved with a modified liquid to coordinate and improve the glass fiber and optimize the product performance. The first additive liquid and the second additive liquid in the modified liquid are adjusted and improved by ball milling with each other. The first additive liquid is adjusted with kaolin powder, sodium silicate solution, phosphate buffer solution, and boron nitride. The lamellar kaolin is mixed with raw materials such as sodium silicate solution and boron nitride in the system to optimize the performance stability of the system. At the same time, the second additive liquid is obtained by stirring silicon carbide whiskers, sodium carboxymethylcellulose, and chitosan solution evenly. In the system with whisker-shaped silicon carbide whiskers, the interfacial property of the system raw materials is further enhanced. Thus, the modified liquid obtained by the mutual cooperation of the first additive liquid and the second additive liquid improves the glass fiber, and further improves the performance of the product. The reinforcing agent is based on flaky talc powder and is further improved by ball milling with a strengthening and reinforcing liquid. Nano-aluminum oxide in the strengthening and reinforcing liquid is coordinated with hydroxyapatite to flaky talc powder. At the same time, sodium lignosulfonate solution, yttrium oxide, and sodium alginate solution are added and blended for adjustment. Through the mutual cooperation and adjustment of raw materials, the reinforcing effect of the obtained reinforcing agent and modified glass fiber is enhanced, and the performance of the product is further improved. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] Figure 1 It is a layered structure diagram of the present invention. DETAILED DESCRIPTION OF THE INVENTION

[0035] The following combines specific embodiments to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative work fall within the protection scope of the present invention.

[0036] Such as Figure 1As shown in the figure, a flame-retardant fiber fireproof and heat-insulating knitted composite cotton of this embodiment, the knitted composite cotton includes a knitted cotton matrix layer 1, and fiber layers 2 are fixedly arranged on both the upper surface and the lower surface of the knitted cotton matrix layer 1 (by fixing methods such as hot pressing and sewing). Both fiber layers 2 are woven from polyester fiber and spandex fiber according to a weight ratio of 1:1;

[0037] Resin layers 3 are fixedly arranged on the outer surfaces of both fiber layers 2 away from the knitted cotton matrix layer 1. The resin layers 3 are formed by molding and curing with a resin composite agent. The molding and curing temperature is 130 - 135 °C, the molding pressure is 10 Mpa, and the molding time is 12 h.

[0038] The preparation method of the knitted cotton matrix layer of this embodiment is as follows:

[0039] Knit 35 - 40 parts of 100S / 2 cotton yarn and 30 - 35 parts of 30D spandex yarn into a cotton fabric by weight, then immerse the cotton fabric in a sufficient amount of 5% sodium hydroxide solution for alkali washing treatment. After the treatment is completed, wash with water and dry to obtain the knitted cotton matrix layer.

[0040] The resin composite agent of this embodiment includes the following raw materials by weight:

[0041] 10 - 15 parts of modified glass fiber, 5 - 8 parts of glass microspheres, 4 - 7 parts of magnesium hydroxide flame retardant, 6 - 10 parts of reinforcement modifier, 45 - 55 parts of resin body; the resin body is prepared from bisphenol A epoxy resin, dicyandiamide curing agent, 1 - benzyl - 2 - methylimidazole, and silane coupling agent KH560 according to a weight ratio of 50:10:3:2.

[0042] The preparation method of the modified glass fiber of this embodiment is as follows:

[0043] S01: First, place the glass fiber in a sufficient amount of 5 - 8% hydrogen peroxide solution and stir evenly. Then wash with water and dry to obtain dry glass fiber; place the dry glass fiber in a proton irradiation chamber for irradiation for 20 - 30 min, with an irradiation power of 350 - 400 W. After the irradiation is completed, obtain the irradiated glass fiber;

[0044] S02: Add 4 - 6 parts of kaolin powder and 1 - 3 parts of sodium silicate solution by weight to 5 - 8 parts of phosphate buffer solution, and then add 2 - 4 parts of boron nitride and stir evenly to obtain the first additive solution;

[0045] Add 3 - 5 parts of silicon carbide whiskers and 2 - 4 parts of carboxymethyl cellulose sodium by weight to 5 - 8 parts of chitosan solution and stir evenly to obtain the second additive solution;

[0046] S03: Mix the first additive solution and the second additive solution according to a weight ratio of 5:3, and perform ball milling treatment at a ball milling speed of 1500 r / min for 2 h. After the ball milling is completed, a modified solution is obtained.

[0047] S04: Add the irradiated glass fiber into a modified solution that is 4 - 7 times the total weight of the irradiated glass fiber, and perform stirring and modification treatment. After the stirring is completed, perform suction filtration and drying to obtain modified glass fiber.

[0048] In this example, the mass fraction of the sodium silicate solution is 4 - 6%; the pH value of the phosphate buffer solution is 5.5; the mass fraction of the chitosan solution is 3 - 5%.

[0049] In this example, the stirring speed for the stirring and modification treatment is 550 - 650 r / min, and the stirring is performed for 30 min.

[0050] The preparation method of the reinforcement adjusting agent in this example is as follows:

[0051] S11: Preheat the flaky talc at 55 - 60 °C for 1 h, and then immerse the preheated flaky talc into a lanthanum chloride solution that is 3 - 5 times the total weight of the preheated flaky talc, and perform stirring treatment at a stirring speed of 500 - 700 r / min for 2 h. After the stirring is completed, perform suction filtration and drying to obtain the flaky talc agent doped with lanthanum.

[0052] S12: Mix the flaky talc agent doped with lanthanum and the strength adjusting and reinforcing liquid according to a weight ratio of 5:3, and perform ball milling treatment at a ball milling speed of 1000 - 1500 r / min for 1 h. After the ball milling is completed, perform suction filtration and drying to obtain the reinforcement adjusting agent.

[0053] In this example, the mass fraction of the lanthanum chloride solution is 3 - 6%.

[0054] The strength adjusting and reinforcing liquid in this example includes the following raw materials in parts by weight:

[0055] 3 - 4 parts of nano - alumina, 4 - 6 parts of lignosulfonate solution, 2 - 3 parts of hydroxyapatite, 1 - 2 parts of yttrium oxide, and 1 - 2 parts of sodium alginate solution.

[0056] In this example, the mass fraction of the lignosulfonate solution is 5 - 8%; the mass fraction of the sodium alginate solution is 3 - 6%.

[0057] The preparation process of a flame - retardant fiber fire - proof and heat - insulating knitted composite cotton in this example includes the following steps:

[0058] Step 1: Prepare the knitted cotton matrix layer 1;

[0059] Step 2: Prepare the fiber layer 2, and set the fiber layer 2 on the upper and lower surfaces of the knitted cotton matrix layer 1.

[0060] Step 3: Prepare the resin composite agent. A resin layer 3 is provided on the outer surface of the fiber layer 2 away from the knitted cotton matrix layer 1, and thus the flame-retardant fiber fireproof and heat-insulating knitted composite cotton is obtained.

[0061] Example 1: As Figure 1 shown, a flame-retardant fiber fireproof and heat-insulating knitted composite cotton, the knitted composite cotton includes a knitted cotton matrix layer 1, fiber layers 2 are fixedly provided on both the upper surface and the lower surface of the knitted cotton matrix layer 1, and both fiber layers 2 are woven from polyester fiber and spandex fiber according to a weight ratio of 1:1;

[0062] Resin layers 3 are fixedly provided on the outer surfaces of both fiber layers 2 away from the knitted cotton matrix layer 1, and the resin layer 3 is formed by molding and curing with a resin composite agent. The molding and curing temperature is 130 °C, the molding pressure is 10 Mpa, and the molding time is 12 h.

[0063] The preparation method of the knitted cotton matrix layer in this example is as follows:

[0064] Knitting 35 parts of 100S / 2 cotton yarn and 30 parts of 30D spandex yarn into a cotton fabric according to weight parts, and then immersing the cotton fabric in a sufficient amount of sodium hydroxide solution with a mass fraction of 5% for alkali washing treatment. After the treatment is completed, washing with water and drying to obtain the knitted cotton matrix layer.

[0065] The resin composite agent in this example includes the following raw materials in weight parts:

[0066] 10 parts of modified glass fiber, 5 parts of glass microspheres, 4 parts of magnesium hydroxide flame retardant, 6 parts of reinforcement modifier, 45 parts of resin body; the resin body is prepared from bisphenol A epoxy resin, dicyandiamide curing agent, 1-benzyl-2-methylimidazole, and silane coupling agent KH560 according to a weight ratio of 50:10:3:2.

[0067] The preparation method of the modified glass fiber in this example is as follows:

[0068] S01: First, place the glass fiber in a sufficient amount of hydrogen peroxide solution with a mass fraction of 5% and stir evenly, then wash with water and dry to obtain dry glass fiber; place the dry glass fiber in a proton irradiation chamber for irradiation for 20 min, with an irradiation power of 350 W. After the irradiation is completed, obtain the irradiated glass fiber;

[0069] S02: Add 4 parts of kaolin powder and 1 part of sodium silicate solution to 5 parts of phosphate buffer solution according to weight parts, and then add 2 parts of boron nitride and stir evenly to obtain the first additive solution;

[0070] Add 3 parts of silicon carbide whiskers and 2 parts of carboxymethyl cellulose sodium to 5 parts of chitosan solution according to weight parts and stir evenly to obtain the second additive solution;

[0071] S03: Mix the first additive solution and the second additive solution according to a weight ratio of 5:3, and perform ball milling treatment at a ball milling speed of 1500 r / min for 2 h. After the ball milling is completed, a modified solution is obtained.

[0072] S04: Add the irradiated glass fiber to a modified solution that is 4 times the total weight of the irradiated glass fiber, and perform stirring and modification treatment. After the stirring is completed, perform suction filtration and drying to obtain modified glass fiber.

[0073] In this embodiment, the mass fraction of the sodium silicate solution is 4%; the pH value of the phosphate buffer solution is 5.5; the mass fraction of the chitosan solution is 3%.

[0074] In this embodiment, the stirring speed for the stirring and modification treatment is 550 r / min, and the stirring time is 30 min.

[0075] The preparation method of the strengthening and toughening agent in this embodiment is as follows:

[0076] S11: Preheat the flaky talc at 55 °C for 1 h, and then immerse the preheated flaky talc in a lanthanum chloride solution that is 3 times the total weight of the preheated flaky talc, and perform stirring treatment at a stirring speed of 500 r / min for 2 h. After the stirring is completed, perform suction filtration and drying to obtain the flaky talc agent doped with lanthanum.

[0077] S12: Mix the flaky talc agent doped with lanthanum and the strengthening and toughening liquid according to a weight ratio of 5:3, and perform ball milling treatment at a ball milling speed of 1000 r / min for 1 h. After the ball milling is completed, perform suction filtration and drying to obtain the strengthening and toughening agent.

[0078] In this embodiment, the mass fraction of the lanthanum chloride solution is 3%.

[0079] The strengthening and toughening liquid in this embodiment includes the following raw materials in parts by weight:

[0080] 3 parts of nano-aluminum oxide, 4 parts of sodium lignosulfonate solution, 2 parts of hydroxyapatite, 1 part of yttrium oxide, and 1 part of sodium alginate solution.

[0081] In this embodiment, the mass fraction of the sodium lignosulfonate solution is 5%; the mass fraction of the sodium alginate solution is 3%.

[0082] The preparation process of a flame-retardant fiber fireproof and heat-insulating knitted composite cotton in this embodiment includes the following steps:

[0083] Step 1: Prepare the knitted cotton matrix layer 1;

[0084] Step 2: Prepare the fiber layer 2, and set the fiber layer 2 on the upper surface and the lower surface of the knitted cotton matrix layer 1;

[0085] Step 3. Prepare the resin composite: Mix the modified glass fiber, glass microspheres, magnesium hydroxide flame retardant, reinforcement modifier, and resin body evenly to obtain the resin composite; form a resin layer 3 on the outer surface of the fiber layer 2 away from the knitted cotton matrix layer 1 by resin composite molding and curing, and then the flame-retardant fiber fireproof and heat-insulating knitted composite cotton is obtained.

[0086] Example 2: As Figure 1 shown, a flame-retardant fiber fireproof and heat-insulating knitted composite cotton, the knitted composite cotton includes a knitted cotton matrix layer 1, fiber layers 2 are fixedly arranged on both the upper surface and the lower surface of the knitted cotton matrix layer 1, and both fiber layers 2 are woven by polyester fiber and spandex fiber according to a weight ratio of 1:1;

[0087] Resin layers 3 are fixedly arranged on the outer surfaces of both fiber layers 2 away from the knitted cotton matrix layer 1, and the resin layers 3 are formed by resin composite molding and curing, the molding and curing temperature is 135 °C, the molding pressure is 10 Mpa, and the molding time is 12 h.

[0088] The preparation method of the knitted cotton matrix layer in this example is:

[0089] Knit 40 parts of 100S / 2 cotton yarn and 35 parts of 30D spandex yarn into a cotton fabric by weight, then immerse the cotton fabric in a sufficient amount of 5% sodium hydroxide solution for alkali washing treatment, after the treatment is over, wash with water and dry to obtain the knitted cotton matrix layer.

[0090] The resin composite in this example includes the following raw materials by weight:

[0091] 15 parts of modified glass fiber, 8 parts of glass microspheres, 7 parts of magnesium hydroxide flame retardant, 10 parts of reinforcement modifier, 55 parts of resin body; the resin body is prepared by mixing bisphenol A epoxy resin, dicyandiamide curing agent, 1-benzyl-2-methylimidazole, and silane coupling agent KH560 according to a weight ratio of 50:10:3:2.

[0092] The preparation method of the modified glass fiber in this example is:

[0093] S01: First place the glass fiber in a sufficient amount of 8% hydrogen peroxide solution and stir evenly, then wash with water and dry to obtain dry glass fiber; place the dry glass fiber in a proton irradiation chamber for irradiation for 30 min, the irradiation power is 400 W, and after the irradiation is over, obtain the irradiated glass fiber;

[0094] S02: Add 6 parts of kaolin powder and 3 parts of sodium silicate solution to 8 parts of phosphate buffer solution by weight, and then add 4 parts of boron nitride and stir evenly to obtain the first additive solution;

[0095] Add 5 parts of silicon carbide whiskers and 4 parts of sodium carboxymethylcellulose by weight to 8 parts of chitosan solution, and stir evenly to obtain the second additive solution;

[0096] S03: Mix and ball-mill the first additive solution and the second additive solution according to a weight ratio of 5:3. The ball-milling speed is 1500 r / min, and ball-mill for 2 h. After the ball-milling is completed, obtain the modified solution;

[0097] S04: Add the irradiated glass fiber to 7 times the total weight of the irradiated glass fiber of the modified solution and stir for modification treatment. After the stirring is completed, filter and dry to obtain the modified glass fiber.

[0098] In this example, the mass fraction of the sodium silicate solution is 6%; the pH value of the phosphate buffer solution is 5.5; the mass fraction of the chitosan solution is 5%.

[0099] In this example, the stirring speed for the stirring modification treatment is 650 r / min, and stir for 30 min.

[0100] The preparation method of the strengthening and toughening agent in this example is as follows:

[0101] S11: Preheat the flaky talc at 60 °C for 1 h, and then immerse the preheated flaky talc in 5 times the total weight of the preheated flaky talc of the lanthanum chloride solution and stir for treatment. The stirring speed is 700 r / min, and stir for 2 h. After the stirring is completed, filter and dry to obtain the flaky talc agent doped with lanthanum;

[0102] S12: Mix and ball-mill the flaky talc agent doped with lanthanum and the strengthening and toughening liquid according to a weight ratio of 5:3. The ball-milling speed is 1500 r / min, and ball-mill for 1 h. After the ball-milling is completed, filter and dry to obtain the strengthening and toughening agent.

[0103] In this example, the mass fraction of the lanthanum chloride solution is 6%.

[0104] The strengthening and toughening liquid in this example includes the following raw materials in parts by weight:

[0105] 4 parts of nano-aluminum oxide, 6 parts of sodium lignosulfonate solution, 3 parts of hydroxyapatite, 2 parts of yttrium oxide and 2 parts of sodium alginate solution.

[0106] In this example, the mass fraction of the sodium lignosulfonate solution is 8%; the mass fraction of the sodium alginate solution is 6%.

[0107] The preparation process of a flame-retardant fiber fireproof and heat-insulating knitted composite cotton in this example includes the following steps:

[0108] Step 1: Prepare the knitted cotton matrix layer 1;

[0109] Step 2: Prepare the fiber layer 2, and arrange the fiber layer 2 on the upper surface and the lower surface of the knitted cotton matrix layer 1;

[0110] Step 3: Prepare the resin composite agent: Mix the modified glass fiber, glass microbeads, magnesium hydroxide flame retardant, reinforcement modifier and resin body evenly to obtain the resin composite agent; On the outer surface of the fiber layer 2 away from the knitted cotton matrix layer 1, form a resin layer 3 by molding and curing with the resin composite agent, and thus obtain the flame-retardant fiber fireproof and heat-insulating knitted composite cotton.

[0111] Example 3: As Figure 1 shown, a flame-retardant fiber fireproof and heat-insulating knitted composite cotton, the knitted composite cotton includes a knitted cotton matrix layer 1, fiber layers 2 are fixedly arranged on both the upper surface and the lower surface of the knitted cotton matrix layer 1, and both fiber layers 2 are woven from polyester fiber and spandex fiber according to a weight ratio of 1:1;

[0112] Resin layers 3 are fixedly arranged on the outer surfaces of both fiber layers 2 away from the knitted cotton matrix layer 1, the resin layer 3 is formed by molding and curing with the resin composite agent, the molding and curing temperature is 132 °C, the molding pressure is 10 Mpa, and the molding time is 12 h.

[0113] The preparation method of the knitted cotton matrix layer in this example is:

[0114] Knitting 37.5 parts of 100S / 2 cotton yarn and 32.5 parts of 30D spandex yarn by weight into a cotton fabric, then immersing the cotton fabric in a sufficient amount of sodium hydroxide solution with a mass fraction of 5% for alkali washing treatment, after the treatment is completed, washing with water and drying to obtain the knitted cotton matrix layer.

[0115] The resin composite agent in this example includes the following raw materials by weight:

[0116] 12.5 parts of modified glass fiber, 6.5 parts of glass microbeads, 5.5 parts of magnesium hydroxide flame retardant, 8 parts of reinforcement modifier, 50 parts of resin body; The resin body is prepared from bisphenol A epoxy resin, dicyandiamide curing agent, 1-benzyl-2-methylimidazole and silane coupling agent KH560 according to a weight ratio of 50:10:3:2.

[0117] The preparation method of the modified glass fiber in this example is:

[0118] S01: First place the glass fiber in a sufficient amount of hydrogen peroxide solution with a mass fraction of 6.5% and stir evenly, then wash with water and dry to obtain the dried glass fiber; Place the dried glass fiber in a proton irradiation chamber for irradiation for 25 min, the irradiation power is 375 W, and after the irradiation is completed, obtain the irradiated glass fiber;

[0119] S02: Add 5 parts of kaolin powder and 2 parts of sodium silicate solution by weight to 6.5 parts of phosphate buffer solution, and then add 3 parts of boron nitride and stir evenly to obtain the first additive solution;

[0120] Add 4 parts of silicon carbide whiskers and 3 parts of sodium carboxymethylcellulose by weight to 6.5 parts of chitosan solution and stir evenly to obtain the second additive solution;

[0121] S03: Mix and ball-mill the first additive solution and the second additive solution according to a weight ratio of 5:3. The ball-milling speed is 1500 r / min and the ball-milling time is 2 h. After the ball-milling is completed, a modified solution is obtained;

[0122] Add the irradiated glass fiber to 5.5 times the total weight of the irradiated glass fiber of the modified solution and stir for modification. After the stirring is completed, filter and dry to obtain the modified glass fiber.

[0123] In this embodiment, the mass fraction of the sodium silicate solution is 5%; the pH value of the phosphate buffer solution is 5.5; the mass fraction of the chitosan solution is 4%.

[0124] In this embodiment, the stirring speed for the stirring modification treatment is 600 r / min and the stirring time is 30 min.

[0125] The preparation method of the reinforcement adjusting agent in this embodiment is as follows:

[0126] S11: Preheat the flaky talc at 57.5 °C for 1 h, and then immerse the preheated flaky talc in 4 times the total weight of the preheated flaky talc of the lanthanum chloride solution and stir. The stirring speed is 600 r / min and the stirring time is 2 h. After the stirring is completed, filter and dry to obtain the flaky talc agent doped with lanthanum;

[0127] S12: Mix and ball-mill the flaky talc agent doped with lanthanum and the strength adjustment and reinforcement liquid according to a weight ratio of 5:3. The ball-milling speed is 1250 r / min and the ball-milling time is 1 h. After the ball-milling is completed, filter and dry to obtain the reinforcement adjusting agent.

[0128] In this embodiment, the mass fraction of the lanthanum chloride solution is 4.5%.

[0129] The strength adjustment and reinforcement liquid in this embodiment includes the following raw materials by weight:

[0130] 3.5 parts of nano-aluminum oxide, 5 parts of sodium lignosulfonate solution, 2.5 parts of hydroxyapatite, 1.5 parts of yttrium oxide and 1.5 parts of sodium alginate solution.

[0131] In this embodiment, the mass fraction of the sodium lignosulfonate solution is 6.5%; the mass fraction of the sodium alginate solution is 4.5%.

[0132] The preparation process of a flame-retardant fiber fireproof and heat-insulating knitted composite cotton in this embodiment includes the following steps:

[0133] Step 1: Prepare the knitted cotton matrix layer 1;

[0134] Step 2: Prepare the fiber layer 2, and set the fiber layer 2 on the upper and lower surfaces of the knitted cotton matrix layer 1;

[0135] Step 3: Prepare the resin composite agent: Mix the modified glass fiber, glass microbeads, magnesium hydroxide flame retardant, reinforcement effect modifier, and resin body evenly to obtain the resin composite agent; Form a resin layer 3 on the outer surface of the fiber layer 2 away from the knitted cotton matrix layer 1 by resin composite agent molding and curing, and then the flame-retardant fiber fireproof and heat-insulating knitted composite cotton is obtained.

[0136] Comparative Example 1:

[0137] It is different from Example 3 in that the modified glass fiber is not added.

[0138] Comparative Example 2:

[0139] It is different from Example 3 in that the S01 treatment is not adopted in the preparation of the modified glass fiber.

[0140] Comparative Example 3:

[0141] It is different from Example 3 in that the modified liquid treatment is not adopted in the preparation of the modified glass fiber.

[0142] Comparative Example 4:

[0143] It is different from Example 3 in that the reinforcement effect modifier is not added.

[0144] Comparative Example 5:

[0145] It is different from Example 3 in that the S01 step treatment is not adopted in the preparation of the reinforcement effect modifier.

[0146] Comparative Example 6:

[0147] It is different from Example 3 in that the strengthening and reinforcing effect liquid treatment is not adopted in the preparation of the reinforcement effect modifier.

[0148] Comparative Example 7:

[0149] It is different from Example 3 in that nano-aluminum oxide and hydroxyapatite are not added to the strengthening and reinforcing effect liquid.

[0150] Comparative Example 8:

[0151] It is different from Example 3 in that yttrium oxide and sodium alginate solution are not added to the strengthening and reinforcing effect liquid.

[0152] The products of Examples 1 to 3 and Comparative Examples 1 to 8 were subjected to thermal insulation and flame retardancy tests under normal conditions. At the same time, the products were immersed in water for 12 hours, and then placed under 2% hydrochloric acid mist conditions for 12 hours, and then placed under 5% hydrochloric acid mist conditions for 12 hours, and then tested for thermal insulation and flame retardancy under corrosion resistance and immersion conditions. The test results are shown in Table 1.

[0153] Table 1 Product performance test results of Examples 1 to 3 and Comparative Examples 1 to 8:

[0154]

[0155] It can be seen from Comparative Examples 1-8 and Examples 1-3 that the product of Example 3 has excellent thermal conductivity and limiting oxygen index, and the thermal insulation and flame retardancy of the product can be improved in a coordinated manner. At the same time, the product has significant corrosion resistance and performance stability under water immersion conditions;

[0156] When neither modified glass fiber nor any of the conditioning and strengthening agents are added to the product, the performance of the product shows a significant trend of deterioration. When the two are used in combination, the product performance is most significant.

[0157] When S01 treatment and modifying liquid treatment are not used in the preparation of modified glass fiber, the performance of the product tends to deteriorate, especially when the modifying liquid treatment is not used, the performance of the product deteriorates significantly;

[0158] The preparation of the tonic strengthening agent does not use the S01 step, the preparation of the tonic strengthening agent does not use the tonic strengthening liquid, the tonic strengthening liquid does not add nano-alumina and hydroxyapatite, and the tonic strengthening liquid does not add yttrium oxide and sodium alginate solution. The performance of the products has a tendency to deteriorate to varying degrees. Only the tonic strengthening agent obtained by the specific method of the present invention has the most significant product performance effect. Other methods are not as obvious as the present invention.

[0159] At the same time, the inventors of the present invention also found that the preparation of the modified liquid has a great influence on the product performance. Based on this, the present invention further explores the influence of the preparation of the modified liquid on the product performance.

[0160] Experimental Example 1:

[0161] The only difference from Example 3 is that the first additive liquid is not added in the preparation of the modified liquid.

[0162] Experimental Example 2:

[0163] The only difference from Example 3 is that no kaolin powder or sodium silicate solution is added to the first additive solution.

[0164] Experimental Example 3:

[0165] The only difference from Example 3 is that boron nitride is not added to the first additive solution, and water is used instead of the phosphate buffer solution.

[0166] Experimental Example 4:

[0167] The only difference from Example 3 is that the second additive solution is not added during the preparation of the modified solution.

[0168] Experimental Example 5:

[0169] The only difference from Example 3 is that silicon carbide whiskers are not added to the second additive solution.

[0170] Experimental Example 6:

[0171] The only difference from Example 3 is that sodium carboxymethylcellulose is not added to the second additive solution, and water is used instead of the chitosan solution.

[0172] The products of Experimental Examples 1 - 6 were subjected to heat preservation and flame retardancy tests under normal conditions. At the same time, the products were immersed in water for 12 h, then placed in a hydrochloric acid mist with a mass fraction of 2% for 12 h, and then placed in a hydrochloric acid mist with a mass fraction of 5% for 12 h to conduct corrosion resistance and heat preservation and flame retardancy tests under immersion conditions. The test results are shown in Table 2.

[0173] Table 2 Performance test results of the products of Experimental Examples 1 - 6:

[0174]

[0175] It can be seen from Experimental Examples 1 - 6 that when the first additive solution or the second additive solution is not added during the preparation of the modified solution, the performance of the product changes. Among the factors for preparing the modified solution, the performance deterioration is the most obvious. Secondly, when kaolin powder and sodium silicate solution are not added to the first additive solution, when boron nitride is not added to the first additive solution and water is used instead of the phosphate buffer solution, and when silicon carbide whiskers and sodium carboxymethylcellulose are not added to the second additive solution and water is used instead of the chitosan solution, the performance of the product shows a deteriorating trend. Only the modified solution obtained by combining the first additive solution and the second additive solution using the specific method of the present invention has the most significant performance effect, and the effect of using other methods instead is not as significant as that of the present invention.

[0176] For those skilled in the art, it is obvious that the present invention is not limited to the details of the above - described exemplary embodiments, and can be implemented in other specific forms without departing from the spirit or basic characteristics of the present invention. Therefore, in any aspect, the embodiments should be regarded as exemplary and non - restrictive. The scope of the present invention is defined by the appended claims rather than the above description. Therefore, all changes falling within the meaning and scope of the equivalent elements of the claims are intended to be encompassed within the present invention.

[0177] In addition, it should be understood that although this specification is described according to embodiments, not every embodiment only contains an independent technical solution. This narrative way of the specification is only for clarity. Those skilled in the art should regard the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. A flame retardant fiber fireproof heat insulation knitted composite cotton, characterized in that: The invention comprises a knitted cotton base layer (1), wherein a fiber layer (2) is fixedly provided on the upper surface and the lower surface of the knitted cotton base layer (1), and the two fiber layers (2) are woven by polyester fiber and spandex fiber in a weight ratio of 1:1; a resin layer (3) is fixedly provided on the outer surfaces of the two fiber layers (2) away from the knitted cotton base layer (1), and the resin layer (3) is formed by molding and curing a resin composite agent, wherein the molding and curing temperature is 130-135° C., the molding pressure is 10 MPa, and the molding time is 12 hours; The resin composite comprises the following raw materials in parts by weight: 10-15 parts of modified glass fiber, 5-8 parts of glass microspheres, 4-7 parts of magnesium hydroxide flame retardant, 6-10 parts of strengthening agent, 45-55 parts of resin; The resin body is prepared by using bisphenol A epoxy resin, dicyandiamide curing agent, 1-benzyl-2-methylimidazole, and silane coupling agent KH560 in a weight ratio of 50:10:3:2; The preparation method of the modified glass fiber is: S01: placing the glass fiber in a sufficient amount of a hydrogen peroxide solution with a mass fraction of 5-8%, stirring and mixing well, then washing and drying to obtain dry glass fiber; placing the dry glass fiber in a proton irradiation box for irradiation for 20-30 minutes, with an irradiation power of 350-400W, and completing the irradiation to obtain irradiated glass fiber; S02: adding 4-6 parts of kaolin powder and 1-3 parts of sodium silicate solution to 5-8 parts of phosphate buffer solution by weight, and then adding 2-4 parts of boron nitride, stirring evenly, to obtain a first addition solution; Add 3-5 parts of silicon carbide whiskers and 2-4 parts of sodium carboxymethyl cellulose to 5-8 parts of chitosan solution by weight, and stir evenly to obtain a second additive solution; S03: The first additive liquid and the second additive liquid were mixed in a weight ratio of 5:3, and ball-milled at a speed of 1500 r / min for 2 h to obtain a modified liquid; S04: adding the irradiated glass fiber to a modification liquid of 4-7 times the total weight of the irradiated glass fiber, stirring and modifying the fiber, filtering and drying after the stirring is completed, to obtain the modified glass fiber; The preparation method of the tonic agent is as follows: S11: preheating the flaky talc at 55-60° C. for 1 h, then immersing the preheated flaky talc in a lanthanum chloride solution 3-5 times the total weight of the preheated flaky talc, stirring at a stirring speed of 500-700 r / min, stirring for 2 h, and after the stirring is completed, filtering and drying to obtain a flaky talc agent doped with lanthanum; S12: mixing the lanthanum-doped talc and the strength-regulating and tonic liquid in a weight ratio of 5:3, and subjecting the mixture to ball milling at a speed of 1000-1500 r / min for 1 h. After the ball milling is completed, filtering and drying are performed to obtain the strength-regulating and tonic agent; The strength-regulating and tonic liquid comprises the following raw materials in parts by weight: 3-4 parts of nano-alumina, 4-6 parts of sodium lignin sulfonate solution, 2-3 parts of hydroxyapatite, 1-2 parts of yttrium oxide and 1-2 parts of sodium alginate solution.

2. The flame retardant fiber fireproof heat preservation knitted composite cotton according to claim 1, characterized in that: The mass fraction of the sodium silicate solution is 4-6%; the pH value of the phosphate buffer solution is 5.5; and the mass fraction of the chitosan solution is 3-5%.

3. The flame retardant fiber fireproof heat preservation knitted composite cotton according to claim 1, characterized in that: The stirring speed of the stirring modification treatment is 550-650r / min, and the stirring is 30min.

4. The flame retardant fiber fireproof heat preservation knitted composite cotton according to claim 1, characterized in that: The mass fraction of the lanthanum chloride solution is 3-6%.

5. The flame retardant fiber fireproof heat preservation knitted composite cotton according to claim 1, characterized in that: The mass fraction of the sodium lignin sulfonate solution is 5-8%; the mass fraction of the sodium alginate solution is 3-6%.

6. The flame retardant fiber fireproof heat preservation knitted composite cotton according to claim 1, characterized in that: The preparation method of the knitted cotton substrate layer is: 35-40 parts by weight of 100S / 2 cotton yarn and 30-35 parts by weight of 30D spandex yarn are knitted into cotton fabric, and then the cotton fabric is immersed in a sufficient amount of 5% by weight sodium hydroxide solution for alkali washing. After the treatment, the fabric is washed with water and dried to obtain a knitted cotton base layer.

7. A process for preparing a flame-retardant fiber fireproof heat-insulating knitted composite cotton, used for preparing a flame-retardant fiber fireproof heat-insulating knitted composite cotton as claimed in any one of claims 1 to 6, characterized in that: The following steps are involved: Step 1: preparing a knitted cotton base layer (1); Step 2: preparing a fiber layer (2), and arranging the fiber layer (2) on the upper surface and the lower surface of the knitted cotton base layer (1); Step three: prepare a resin composite, and arrange a resin layer (3) on the outer surface of the fiber layer (2) away from the knitted cotton base layer (1), so as to obtain a flame retardant fiber fireproof heat-insulating knitted composite cotton.

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