Moisture-absorbing and antibacterial layered composite fabric and preparation method thereof

Abstract

The application relates to the technical field of multilayer composite fabrics, and discloses a moisture-absorbing and antibacterial layered composite fabric and a preparation method thereof. The preparation method comprises the following steps: antibacterial type nylon fibers are prepared by melt spinning of polyamide and an antibacterial agent; the antibacterial type nylon fibers, cotton fibers and profiled section nylon fibers are blended and then knitted to obtain a rough inner layer fabric; the antibacterial type nylon fibers and modified cotton fibers are blended and then knitted to obtain a rough surface layer fabric; the rough surface layer fabric and the rough inner layer fabric are respectively immersed in finishing liquid to obtain a surface layer fabric and an inner layer fabric, and the moisture-absorbing and antibacterial layered composite fabric is obtained by compounding the surface layer fabric and the inner layer fabric. The composite fabric has excellent antibacterial performance and good moisture absorption performance.

Description

Technical Field

[0001] The present invention relates to the technical field of multi-layer fabrics, and in particular to a moisture-absorbing and antibacterial layered composite fabric and a preparation method thereof. Background Art

[0002] At present, people have high requirements for the functionality and wearing comfort of fabrics, so it is necessary to improve the hydrophilicity, hygroscopicity and antibacterial properties of fabrics. Antibacterial fabrics can be classified according to their development direction into natural antibacterial fiber fabrics, newly developed fiber fabrics, artificial antibacterial fiber fabrics and antibacterial agent-finished fabrics. Among them, antibacterial agent-finished fabrics are fabrics that are post-finished and the antibacterial agent is attached to the fabric by different methods to obtain antibacterial fabrics. The fabrics obtained by this method have good antibacterial properties, but the antibacterial effect will decrease after several uses and washings.

[0003] Existing technologies, such as Chinese patent CN113386410A, disclose a multifunctional health-care knitted fabric and a preparation method thereof. The knitted fabric comprises modified holy hemp fiber, heating fiber, negative ion fiber and modified mugwort fiber as the inner layer, and modified kapok fiber, nylon fiber and regenerated cellulose fiber as the outer layer. The obtained knitted fabric has antibacterial, antibacterial and deodorizing properties. However, the antibacterial effect of the prepared fabric is mainly provided by the fiber and the finishing liquid containing antibacterial substances. After washing, the finishing agent on the surface of the fabric easily falls off, which reduces the antibacterial ability of the fabric and affects the long-term use of the fabric. Summary of the Invention

[0004] The purpose of the present invention is to overcome the deficiencies of the prior art and provide a hygroscopic and antibacterial layered composite fabric and a preparation method thereof, wherein the composite fabric has excellent antibacterial properties and good hygroscopic properties.

[0005] In order to achieve the above object, the technical solution adopted by the present invention is as follows:

[0006] A method for preparing a moisture-absorbing and antibacterial layered composite fabric comprises the following steps:

[0007] Step 1: mixing polyamide and an antibacterial agent, melt spinning, cooling and drawing, and chopping to obtain antibacterial nylon fiber;

[0008] The antibacterial agent is prepared by the following steps:

[0009] S11, mixing nano-hydroxyapatite with a silver nitrate aqueous solution, reacting, filtering, washing, and drying after the reaction is completed to obtain silver-loaded hydroxyapatite;

[0010] S12, dissolving 3-aminopyridine, triethylamine, and acetonitrile, adding trimesoyl chloride solution dropwise, reacting after the addition is complete, filtering, washing, and drying to obtain amidated pyridine;

[0011] The amidated pyridine and ethanol are mixed and dissolved, and silver-loaded hydroxyapatite is added to react. After the reaction is completed, the mixture is filtered, washed, and dried to obtain an antibacterial agent.

[0012] Step 2: blending the antibacterial nylon fiber, cotton fiber, and special-section nylon fiber to obtain an inner layer blended yarn; blending the antibacterial nylon fiber with the modified cotton fiber to obtain an outer layer blended yarn; and weaving the inner layer blended yarn and the outer layer blended yarn using a circular knitting machine to obtain an inner layer fabric rough product and an outer layer fabric rough product, respectively;

[0013] The modified cotton fiber is prepared by the following steps:

[0014] S21, mixing cotton fiber with an aqueous sodium periodate solution, reacting, filtering, washing, and drying after the reaction is complete to obtain formaldehyde-treated cotton fiber;

[0015] S22, mixing an amino-terminated hyperbranched polymer, 2,3-epoxypropyltrimethylammonium chloride, and water, reacting the mixture to obtain an antibacterial finishing solution, mixing the formaldehyde-modified cotton fiber with the antibacterial finishing solution, and continuing the reaction. After the reaction is completed, filtering, washing, and drying the mixture to obtain a modified cotton fiber;

[0016] Step 3: The rough surface fabric product and the rough lining fabric product are respectively immersed in the finishing liquid, and after the immersion is completed, they are dried and baked to obtain the surface fabric and the lining fabric respectively;

[0017] The finishing liquid is prepared by the following steps:

[0018] S31, N,N,N',N'-tetramethyl-1,6-hexanediamine acetate, polyetheramine, isopropyl alcohol, and 1,3-bis(3-glycidyloxypropyl)tetramethyldisiloxane are uniformly mixed and reacted. After the reaction is completed, the solvent isopropyl alcohol is removed by rotary evaporation to obtain a quaternized polyetheramine;

[0019] S32, adding the first catalyst to the quaternized polyetheramine and mixing evenly, adding nylon 66 salt, reacting, adding adipic acid and the second catalyst after the reaction is completed, continuing the reaction, evacuating the mixture, and keeping the mixture warm to react, and obtaining a finishing agent after the reaction is completed; mixing the finishing agent with water to obtain a finishing liquid;

[0020] Step 4: Compound the surface layer fabric and the inner layer fabric to obtain a moisture-absorbing and antibacterial layered composite fabric.

[0021] Preferably, in step one, the mass ratio of polyamide to antibacterial agent is 100:1-2; the melt spinning operation includes: melt extrusion through a twin-screw melt spinning machine, the melting section temperature is 260-270°C, and the spinning speed is 700-1000m / min; the specifications of the antibacterial nylon fiber are: fineness of 60-70D and average length of 39mm.

[0022] Preferably, in step 1 S11: the mass ratio of nano-hydroxyapatite to silver nitrate aqueous solution is 1:8-10, the silver nitrate aqueous solution is 0.1 mol / L silver nitrate aqueous solution; and the reaction conditions are: reaction at 80-90° C. for 16-20 hours.

[0023] Preferably, in S12 of step 1, the mass ratio of 3-aminopyridine, triethylamine, acetonitrile, and trimesoyl chloride solution is 3.7-3.9:5-5.5:16-20:43-45; the trimesoyl chloride solution is a 6.2-6.5 wt% trimesoyl chloride solution, and the solvent is dichloromethane; the trimesoyl chloride solution is added dropwise at a temperature of 0-5° C. for 20-30 minutes; when preparing amidated pyridine, the reaction conditions are: stirring the reaction at room temperature for 48-52 hours.

[0024] Preferably, the detergent used in the washing operation includes: saturated sodium bicarbonate aqueous solution, water, ethyl acetate in sequence, and ethyl acetate includes ethyl acetate at a temperature of -5-0°C.

[0025] Preferably, in step 1 S12, the mass ratio of amidated pyridine, ethanol, and silver-loaded hydroxyapatite is 8-10:480-550:5; when preparing the antibacterial agent, the reaction conditions are: reaction at a temperature of 60-70° C. for 20-24 hours.

[0026] Preferably, in the step 2, when preparing the inner layer blended yarn, the mass ratio of the antibacterial nylon fiber, the cotton fiber, and the special-shaped cross-section nylon fiber is 10-20:30:10-20, and the yarn count of the inner layer blended yarn is 60-70S in British count; when preparing the surface layer blended yarn, the mass ratio of the antibacterial nylon fiber to the modified cotton fiber is 1:1-2, and the yarn count of the surface layer blended yarn is 40-50S in British count; the gram weight of the inner layer fabric rough product is 100-120g / m 2 ; The surface fabric weight is 80-100g / m 2 .

[0027] Preferably, the antibacterial nylon fiber used to prepare the rough surface fabric product is the same as the antibacterial nylon fiber used to prepare the rough inner fabric product.

[0028] Preferably, in step 2 S21: the mass ratio of cotton fiber to sodium periodate aqueous solution is 1:20-30, and the sodium periodate aqueous solution is 0.1 mol / L sodium periodate aqueous solution; and the reaction conditions are: in a light-proof environment, at a temperature of 40-60° C. for 4-6 hours.

[0029] Preferably, in step 2 S22: the mass ratio of the amino-terminated hyperbranched polymer, 2,3-epoxypropyltrimethylammonium chloride, and water is 10:2-3:480-520; the reaction conditions are: stirring and reacting at a temperature of 70-80°C for 5-10 minutes; the mass ratio of the formaldehyde-modified cotton fiber to the antibacterial finishing liquid is 1:20-30; and the continued reaction conditions are: continuing the reaction at a temperature of 60-80°C for 45-60 minutes.

[0030] Preferably, in the step 3, in the dipping operation, the bath ratio is 20-30:1; the dipping operation includes: dipping at a temperature of 40-50° C. for 50-60 min, two dippings and two rollings, and the rolling rate is 78-82%.

[0031] Preferably, in S31 of step three, the molar ratio of N,N,N',N'-tetramethyl-1,6-hexanediamine acetate, polyetheramine, isopropyl alcohol, and 1,3-bis(3-glycidyloxypropyl)tetramethyldisiloxane is 1:2.5-3:3-4:2; and the reaction conditions are: reaction at 80-90° C. for 3-5 hours.

[0032] Furthermore, N,N,N',N'-tetramethyl-1,6-hexanediamine acetate is prepared by mixing N,N,N',N'-tetramethyl-1,6-hexanediamine and acetic acid in a molar ratio of 1:2 and stirring at room temperature for 1 hour.

[0033] Preferably, in step three S32: the mass ratio of quaternized polyetheramine, nylon 66 salt, adipic acid, the first catalyst, and the second catalyst is 80-90:23-26:14-15:1-1.1:0.5-0.6, and both the first catalyst and the second catalyst are phosphorous acid.

[0034] Preferably, in step 3 S32: the first catalyst is added to the quaternized polyetheramine under a nitrogen atmosphere at a temperature of 210-220° C.; the reaction is carried out under a nitrogen atmosphere at a temperature of 220-230° C. for 3-4 hours; the reaction is continued under a nitrogen atmosphere at a temperature of 230-240° C. for 3-4 hours; the heat preservation reaction is carried out under a vacuum degree of 10 Pa and a temperature of 235-240° C. for 1-2 hours; and the mass ratio of the finishing agent to water is 1-1.5:10.

[0035] Preferably, a hygroscopic and antibacterial layered composite fabric is prepared by the method for preparing the hygroscopic and antibacterial layered composite fabric as described above.

[0036] Compared with the prior art, the present invention has the following beneficial effects:

[0037] The invention prepares antibacterial nylon fibers with antibacterial properties by melt-blending an antibacterial agent with polyamide, spinning the fibers, blending the fibers with cotton fibers and special-section nylon fibers, and knitting the fibers to prepare a crude inner fabric product; blending the antibacterial nylon fibers with modified cotton fibers grafted with quaternary ammonium salts, and knitting the resulting crude surface fabric product; and respectively immersing the crude surface fabric product and the crude inner fabric product in a finishing liquid containing a quaternary ammonium salt structure and a polyether polyamide block copolymer to improve the antibacterial ability and hygroscopic performance of the prepared surface fabric and the prepared inner fabric. The two fibers are composited to obtain a hygroscopic antibacterial layered composite fabric having excellent antibacterial properties and good hygroscopic properties.

[0038] The present invention uses an ion exchange method to mix nano-hydroxyapatite with a silver nitrate aqueous solution to cause an ion exchange reaction, so that silver ions replace part of calcium ions and enter the lattice structure of the hydroxyapatite. The obtained silver-loaded hydroxyapatite has excellent antibacterial ability as an antibacterial material. 3-aminopyridine and trimesoyl chloride undergo an amidation reaction to prepare an amidated pyridine having an amide bond and a polypyridine ring structure. The amidated pyridine is mixed with the silver-loaded hydroxyapatite for reaction. The pyridine ring structure of the amidated pyridine can act as a ligand to undergo a coordination reaction with the silver ions in the silver-loaded hydroxyapatite to form a coordination bond. The amidated pyridine is loaded on the surface of the silver-loaded hydroxyapatite as a surface modifier. The prepared antibacterial agent has an amide structure and can be connected with the amide group in the polyamide substrate of the nylon fiber through molecular forces during melt spinning. The antibacterial agent has good compatibility with the polyamide. The antibacterial nylon fiber obtained after melt spinning has long-lasting antibacterial ability.

[0039] The present invention prepares a crude inner fabric product by blending antibacterial nylon fiber with cotton fiber and special-section nylon fiber through knitting; and prepares a crude outer fabric product by blending antibacterial nylon fiber with modified cotton fiber through knitting; wherein the modified cotton fiber is prepared by oxidizing cotton fiber with a sodium periodate aqueous solution to generate aldehyde-modified cotton fiber, and then mixing and reacting the aldehyde-modified cotton fiber with an antibacterial finishing liquid containing an amino-terminated hyperbranched polymer and 2,3-epoxypropyltrimethylammonium chloride. The amino-terminated hyperbranched polymer in the antibacterial finishing agent can not only undergo a ring-opening reaction with 2,3-epoxypropyltrimethylammonium chloride to generate a quaternary ammonium salt structure having an antibacterial functional group, but can also undergo a Schiff base reaction with the aldehyde-modified cotton fiber to generate a Schiff base bond having antibacterial properties, thereby improving the antibacterial properties of the prepared modified cotton fiber.

[0040] The invention comprises the following steps: mixing N,N,N',N'-tetramethyl-1,6-hexanediamine acetate, polyetheramine and 1,3-bis(3-glycidyloxypropyl)tetramethyldisiloxane to undergo a ring-opening reaction to prepare a quaternized polyetheramine having a siloxane segment and a quaternary ammonium salt structure; using the quaternized polyetheramine as a polyether component, polycondensing it with nylon 66 salt and adipic acid to obtain a finishing agent having a polyether segment, a polyamide structure and a quaternary ammonium salt antibacterial group; and padding a surface layer fabric crude product and an inner layer fabric crude product with a finishing liquid. During the padding treatment, the surfaces of the cotton fibers and modified cotton fibers in the fabric have active groups, which can form hydrogen bonds with the finishing agent; the polyamide structure in the finishing agent can form a eutectic with the nylon fibers in the fabric, and the polyether component in the finishing agent improves the hydrophilic and hygroscopic properties of the fabric, and the washability, antibacterial ability and moisture absorption capacity of the fabric are improved; the surface fabric and the inner fabric are compounded to obtain a hygroscopic and antibacterial layered composite fabric with excellent antibacterial properties and good moisture absorption properties. BRIEF DESCRIPTION OF THE DRAWINGS

[0041] Figure 1 This is a process flow chart for preparing the moisture-absorbing and antibacterial layered composite fabric in the present invention;

[0042] Figure 2 Schematic diagram of the structure of the moisture-absorbing and antibacterial layered composite fabric prepared in the present invention;

[0043] Figure 3 It is a histogram of the antibacterial rates of the layered composite fabrics prepared in the examples and comparative examples of the present invention in the performance tests;

[0044] Figure 4 It is a histogram of the water absorption rate of the layered composite fabrics prepared in the examples and comparative examples of the present invention in the performance test;

[0045] Figure 5 It is a histogram of the drip diffusion time of the layered composite fabrics prepared in the examples and comparative examples of the present invention in the performance test;

[0046] In the picture:

[0047] 1. Surface fabric; 2. Lining fabric. DETAILED DESCRIPTION

[0048] The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only 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 ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0049] Example 1

[0050] This embodiment discloses a method for preparing a moisture-absorbing and antibacterial layered composite fabric, comprising the following steps:

[0051] Step 1: polyamide and antibacterial agent are mixed in a mass ratio of 100:1, melt-extruded through a twin-screw melt spinning machine, the melting section temperature is 260°C, and the spinning speed is 700 m / min. The fibers are cooled, drawn, and chopped to obtain antibacterial nylon fibers with a fineness of 60D and an average length of 39 mm;

[0052] The antibacterial agent is prepared by the following steps:

[0053] S11, mixing nanohydroxyapatite with a 0.1 mol / L silver nitrate aqueous solution in a mass ratio of 1:9, reacting at 85° C. for 18 h. After the reaction is complete, filtering, taking the filter cake, washing it with water 6 times the mass of the filter cake, and drying it at 55° C. for 26 h to obtain silver-loaded hydroxyapatite;

[0054] S12, 3-aminopyridine, triethylamine, and acetonitrile were mixed and dissolved, and 6.2 wt% trimesoyl chloride solution was added dropwise at 0°C for 20 min. After the addition was complete, the mixture was stirred and reacted at room temperature for 48 h. After the reaction was completed, the mixture was filtered, and the filter cake was washed with saturated sodium bicarbonate aqueous solution (5 times the mass of the filter cake), water, and ethyl acetate in that order, and dried at 40°C for 24 h to obtain amidated pyridine;

[0055] The mass ratio of 3-aminopyridine, triethylamine, acetonitrile and trimesoyl chloride solution is 3.7:5:16:43; the solvent of trimesoyl chloride solution is dichloromethane; and the ethyl acetate is ethyl acetate at a temperature of -5°C.

[0056] The amidated pyridine and ethanol were mixed and dissolved, and silver-loaded hydroxyapatite was added, with the mass ratio of amidated pyridine, ethanol, and silver-loaded hydroxyapatite being 8:480:5. The mixture was reacted at 60°C for 24 hours. After the reaction was completed, the mixture was filtered, and the filter cake was taken. The filter cake was washed with water 5 times the mass of the filter cake, and dried at 40°C for 24 hours to obtain an antibacterial agent.

[0057] Step 2: blend the antibacterial nylon fiber, cotton fiber, and special-section nylon fiber in a mass ratio of 10:30:20 to obtain an inner layer blended yarn with a yarn count of 60S in the imperial system; blend the antibacterial nylon fiber and the modified cotton fiber in a mass ratio of 1:1 to obtain a surface layer blended yarn with a yarn count of 40S in the imperial system; weave the inner layer blended yarn and the surface layer blended yarn respectively using a knitting circular machine to obtain a gram weight of 100g / m 2 The inner layer fabric is coarse and weighs 80g / m 2 Surface fabric crude product; the antibacterial nylon fiber used to prepare the surface fabric crude product is the same as the antibacterial nylon fiber used to prepare the inner layer fabric crude product;

[0058] The modified cotton fiber is prepared by the following steps:

[0059] S21, mixing cotton fiber with a 0.1 mol / L sodium periodate aqueous solution at a mass ratio of 1:25, reacting the mixture in a dark environment at 50° C. for 5 h. After the reaction is completed, filtering the mixture, taking the filter cake, washing the mixture with water 6 times the mass of the filter cake until neutral, and drying the mixture at 45° C. for 19 h to obtain formaldehyde-modified cotton fiber;

[0060] S22, the amino-terminated hyperbranched polymer, 2,3-epoxypropyltrimethylammonium chloride, and water were mixed in a mass ratio of 10:2:480, stirred and reacted at 70°C for 10 minutes, and after the reaction, an antibacterial finishing liquid was obtained, and the formaldehyde-modified cotton fiber and the antibacterial finishing liquid were mixed in a mass ratio of 1:20, and the reaction was continued at 60°C for 60 minutes. After the reaction was completed, the filter cake was taken, and water 5 times the mass of the filter cake was added for washing, and dried at 60°C for 16 hours to obtain modified cotton fiber;

[0061] Step 3, the surface fabric crude product and the inner layer fabric crude product are immersed in the finishing liquid respectively, with a bath ratio of 20:1, immersed at 40°C for 60 minutes, double-immersed and double-rolled, with a rolling rate of 78%. After the impregnation, dry at 80°C for 5 minutes and bake at 160°C for 60 seconds to obtain the surface fabric and the inner layer fabric respectively;

[0062] The finishing liquid is prepared by the following steps:

[0063] S31, N,N,N',N'-tetramethyl-1,6-hexanediamine acetate, polyetheramine, isopropyl alcohol, and 1,3-bis(3-glycidyloxypropyl)tetramethyldisiloxane are uniformly mixed in a molar ratio of 1:3:3:2, and the mixture is reacted at 80°C for 5 hours. After the reaction is completed, the solvent isopropyl alcohol is removed by rotary evaporation at 50°C to obtain a quaternized polyetheramine;

[0064] Wherein, N,N,N',N'-tetramethyl-1,6-hexanediamine acetate is prepared by mixing N,N,N',N'-tetramethyl-1,6-hexanediamine and acetic acid at a molar ratio of 1:2 and stirring at room temperature for 1 hour;

[0065] S32. In a nitrogen atmosphere, the first catalyst is added to the quaternized polyetheramine at a temperature of 210° C. and mixed evenly. Nylon 66 salt is added, and the mixture is reacted in a nitrogen atmosphere at a temperature of 220° C. for 4 h. After the reaction is completed, adipic acid and a second catalyst are added, and the mixture is reacted at a temperature of 230° C. for another 4 h. After the reaction is completed, the mixture is evacuated, and the mixture is kept in a vacuum of 10 Pa and a temperature of 235° C. for 2 h. After the reaction is completed, a finishing agent is obtained; the finishing agent is mixed with water at a mass ratio of 1:10 to obtain a finishing liquid.

[0066] The mass ratio of the quaternized polyetheramine, nylon 66 salt, adipic acid, the first catalyst, and the second catalyst is 80:23:14:1:0.5, and both the first catalyst and the second catalyst are phosphorous acid;

[0067] Step 4: Lay the surface fabric and the inner fabric together, align the layers, and sew the surface fabric and the inner fabric together using a multi-layer fabric quilting machine using pure cotton sewing thread to obtain a moisture-absorbing and antibacterial layered composite fabric.

[0068] Example 2

[0069] This embodiment discloses a method for preparing a moisture-absorbing and antibacterial layered composite fabric, comprising the following steps:

[0070] Step 1: polyamide and antibacterial agent are mixed in a mass ratio of 100:1.3, melt-extruded through a twin-screw melt spinning machine, the melting section temperature is 265° C., and the spinning speed is 800 m / min. The fibers are cooled, drawn, and chopped to obtain antibacterial nylon fibers with a fineness of 65D and an average length of 39 mm.

[0071] The antibacterial agent is prepared by the following steps:

[0072] S11, the preparation of silver-loaded hydroxyapatite is the same as that in Example 1;

[0073] S12, 3-aminopyridine, triethylamine, and acetonitrile were mixed and dissolved, and 6.3 wt% trimesoyl chloride solution was added dropwise at 2°C for 25 min. After the addition was complete, the mixture was stirred and reacted at room temperature for 50 h. After the reaction was completed, the mixture was filtered, and the filter cake was washed with saturated sodium bicarbonate aqueous solution (5 times the mass of the filter cake), water, and ethyl acetate in that order, and dried at 45°C for 21 h to obtain amidated pyridine;

[0074] The mass ratio of 3-aminopyridine, triethylamine, acetonitrile, and trimesoyl chloride solution is 3.75:5.2:17:43.5; the solvent of the trimesoyl chloride solution is dichloromethane; and the ethyl acetate is ethyl acetate at a temperature of -5°C.

[0075] The amidated pyridine and ethanol were mixed and dissolved, and silver-loaded hydroxyapatite was added, with the mass ratio of amidated pyridine, ethanol, and silver-loaded hydroxyapatite being 8.5:500:5. The mixture was reacted at 65°C for 22 hours. After the reaction was completed, the mixture was filtered, and the filter cake was taken out. The filter cake was washed with water 5 times the mass of the filter cake, and dried at 45°C for 23 hours to obtain an antibacterial agent.

[0076] Step 2: blend the antibacterial nylon fiber, cotton fiber, and special-section nylon fiber in a mass ratio of 12:30:18 to obtain an inner layer blended yarn with a yarn count of 65S in the imperial system; blend the antibacterial nylon fiber and modified cotton fiber in a mass ratio of 1:1.3 to obtain a surface layer blended yarn with a yarn count of 45S in the imperial system; the inner layer blended yarn and the surface layer blended yarn are woven separately using a knitting circular machine to obtain yarns with a gram weight of 105g / m 2 The inner layer fabric is coarse and weighs 85g / m 2 Surface fabric crude product; the antibacterial nylon fiber used to prepare the surface fabric crude product is the same as the antibacterial nylon fiber used to prepare the inner layer fabric crude product;

[0077] The modified cotton fiber is prepared by the following steps:

[0078] S21, the preparation of aldehyde-modified cotton fiber is the same as that in Example 1;

[0079] S22, the amino-terminated hyperbranched polymer, 2,3-epoxypropyltrimethylammonium chloride, and water were mixed in a mass ratio of 10:2.3:500, and stirred at 75°C for 8 minutes. After the reaction, an antibacterial finishing liquid was obtained, and the formaldehyde-modified cotton fiber and the antibacterial finishing liquid were mixed in a mass ratio of 1:22, and the reaction was continued at 70°C for 50 minutes. After the reaction was completed, the filter cake was taken, and water 6 times the mass of the filter cake was added for washing, and the filter cake was dried at 65°C for 14 hours to obtain a modified cotton fiber;

[0080] Step 3, the surface fabric crude product and the inner layer fabric crude product are immersed in the finishing liquid respectively, with a bath ratio of 25:1, immersed at 45°C for 55 minutes, double-immersed and double-rolled, with a rolling rate of 79%. After the impregnation, dry at 85°C for 4.5 minutes and bake at 165°C for 55 seconds to obtain the surface fabric and the inner layer fabric respectively;

[0081] The finishing liquid is prepared by the following steps:

[0082] S31, N,N,N',N'-tetramethyl-1,6-hexanediamine acetate, polyetheramine, isopropyl alcohol, and 1,3-bis(3-glycidyloxypropyl)tetramethyldisiloxane are uniformly mixed in a molar ratio of 1:2.6:3.3:2, and the mixture is reacted at 85°C for 4 hours. After the reaction is completed, the solvent isopropyl alcohol is removed by rotary evaporation at 55°C to obtain a quaternized polyetheramine;

[0083] Wherein, the preparation of N,N,N',N'-tetramethyl-1,6-hexanediamine acetate is the same as that in Example 1;

[0084] S32. In a nitrogen atmosphere, the first catalyst was added to the quaternized polyetheramine at a temperature of 215° C., and the mixture was evenly mixed. Nylon 66 salt was added, and the mixture was reacted in a nitrogen atmosphere at a temperature of 220° C. for 3.5 hours. After the reaction was completed, adipic acid and a second catalyst were added, and the mixture was reacted at a temperature of 230° C. for another 3.5 hours. After the reaction was completed, the mixture was evacuated, and the mixture was kept in a vacuum of 10 Pa and a temperature of 235° C. for 1.5 hours. After the reaction was completed, a finishing agent was obtained; the finishing agent was mixed with water at a mass ratio of 1.2:10 to obtain a finishing liquid.

[0085] The mass ratio of the quaternized polyetheramine, nylon 66 salt, adipic acid, the first catalyst, and the second catalyst is 83:24:14.3:1:0.5, and both the first catalyst and the second catalyst are phosphorous acid;

[0086] Step 4: Lay the surface fabric and the inner fabric together, align the layers, and sew the surface fabric and the inner fabric together using a multi-layer fabric quilting machine using pure cotton sewing thread to obtain a moisture-absorbing and antibacterial layered composite fabric.

[0087] Example 3

[0088] This embodiment discloses a method for preparing a moisture-absorbing and antibacterial layered composite fabric, comprising the following steps:

[0089] Step 1: polyamide and antibacterial agent are mixed in a mass ratio of 100:1.5, melt-extruded through a twin-screw melt spinning machine, the melting section temperature is 265° C., spinning is performed at a spinning speed of 900 m / min, cooled and drawn, and chopped to obtain antibacterial nylon fiber with a fineness of 65D and an average length of 39 mm;

[0090] The antibacterial agent is prepared by the following steps:

[0091] S11, the preparation of silver-loaded hydroxyapatite is the same as that in Example 1;

[0092] S12, 3-aminopyridine, triethylamine, and acetonitrile were mixed and dissolved, and 6.4 wt% trimesoyl chloride solution was added dropwise at 2°C for 25 min. After the addition was complete, the mixture was stirred and reacted at room temperature for 50 h. After the reaction was completed, the mixture was filtered, and the filter cake was washed with saturated sodium bicarbonate aqueous solution (6 times the mass of the filter cake), water, and ethyl acetate in that order, and dried at 45°C for 21 h to obtain amidated pyridine;

[0093] The mass ratio of 3-aminopyridine, triethylamine, acetonitrile and trimesoyl chloride solution is 3.8:5.3:18:44; the solvent of trimesoyl chloride solution is dichloromethane; and the ethyl acetate is ethyl acetate at a temperature of -2°C.

[0094] The amidated pyridine and ethanol were mixed and dissolved, and silver-loaded hydroxyapatite was added, with the mass ratio of amidated pyridine, ethanol, and silver-loaded hydroxyapatite being 9:510:5. The mixture was reacted at 65°C for 22 hours. After the reaction was completed, the mixture was filtered, and the filter cake was taken. The filter cake was washed with water 6 times the mass of the filter cake, and dried at 45°C for 23 hours to obtain an antibacterial agent.

[0095] Step 2: blend the antibacterial nylon fiber, cotton fiber, and special-section nylon fiber in a mass ratio of 15:30:15 to obtain an inner layer blended yarn with a yarn count of 65S in the imperial system; blend the antibacterial nylon fiber and modified cotton fiber in a mass ratio of 1:1.5 to obtain a surface layer blended yarn with a yarn count of 45S in the imperial system; the inner layer blended yarn and the surface layer blended yarn are woven separately using a knitting circular machine to obtain yarns with a gram weight of 110g / m 2 The inner layer fabric is coarse and weighs 90g / m 2 Surface fabric crude product; the antibacterial nylon fiber used to prepare the surface fabric crude product is the same as the antibacterial nylon fiber used to prepare the inner layer fabric crude product;

[0096] The modified cotton fiber is prepared by the following steps:

[0097] S21, the preparation of aldehyde-modified cotton fiber is the same as that in Example 1;

[0098] S22, the amino-terminated hyperbranched polymer, 2,3-epoxypropyltrimethylammonium chloride, and water were mixed in a mass ratio of 10:2.5:500, and stirred at 75°C for 8 minutes. After the reaction, an antibacterial finishing liquid was obtained, and the formaldehyde-modified cotton fiber and the antibacterial finishing liquid were mixed in a mass ratio of 1:25, and the reaction was continued at 70°C for 50 minutes. After the reaction was completed, the filter cake was taken, and water 6 times the mass of the filter cake was added for washing, and the filter cake was dried at 65°C for 14 hours to obtain a modified cotton fiber;

[0099] Step 3, the surface fabric crude product and the lining fabric crude product are immersed in the finishing liquid respectively, with a bath ratio of 25:1, immersed at 45°C for 55 minutes, double-immersed and double-rolled, with a rolling rate of 80%. After the impregnation, dry at 85°C for 4.5 minutes and bake at 165°C for 55 seconds to obtain the surface fabric and the lining fabric respectively;

[0100] The finishing liquid is prepared by the following steps:

[0101] S31, N,N,N',N'-tetramethyl-1,6-hexanediamine acetate, polyetheramine, isopropyl alcohol, and 1,3-bis(3-glycidyloxypropyl)tetramethyldisiloxane are uniformly mixed in a molar ratio of 1:2.8:3.5:2, and the mixture is reacted at 85°C for 4 hours. After the reaction is completed, the solvent isopropyl alcohol is removed by rotary evaporation at 55°C to obtain a quaternized polyetheramine;

[0102] Wherein, the preparation of N,N,N',N'-tetramethyl-1,6-hexanediamine acetate is the same as that in Example 1;

[0103] S32. In a nitrogen atmosphere, the first catalyst was added to the quaternized polyetheramine at 215° C., and the mixture was evenly mixed. Nylon 66 salt was added, and the mixture was reacted in a nitrogen atmosphere at 225° C. for 3.5 hours. After the reaction was completed, adipic acid and the second catalyst were added, and the mixture was reacted at 235° C. for 3.5 hours. After the reaction was completed, the mixture was evacuated, and the mixture was kept in a vacuum of 10 Pa and at 238° C. for 1.5 hours. After the reaction was completed, a finishing agent was obtained; the finishing agent was mixed with water at a mass ratio of 1.3:10 to obtain a finishing liquid.

[0104] The mass ratio of quaternized polyetheramine, nylon 66 salt, adipic acid, the first catalyst, and the second catalyst is 85:25.5:14.5:1.05:0.55, and both the first catalyst and the second catalyst are phosphorous acid;

[0105] Step 4: Lay the surface fabric and the inner fabric together, align the layers, and sew the surface fabric and the inner fabric together using a multi-layer fabric quilting machine using pure cotton sewing thread to obtain a moisture-absorbing and antibacterial layered composite fabric.

[0106] Example 4

[0107] This embodiment discloses a method for preparing a moisture-absorbing and antibacterial layered composite fabric, comprising the following steps:

[0108] Step 1: polyamide and antibacterial agent are mixed in a mass ratio of 100:1.8, melt-extruded through a twin-screw melt spinning machine, the melting section temperature is 265° C., and the spinning speed is 1000 m / min. The fibers are cooled, drawn, and chopped to obtain antibacterial nylon fibers with a fineness of 70D and an average length of 39 mm;

[0109] The antibacterial agent is prepared by the following steps:

[0110] S11, the preparation of silver-loaded hydroxyapatite is the same as that in Example 1;

[0111] S12, 3-aminopyridine, triethylamine, and acetonitrile were mixed and dissolved, and 6.5 wt% trimesoyl chloride solution was added dropwise at 2°C for 25 min. After the addition was complete, the mixture was stirred and reacted at room temperature for 50 h. After the reaction was completed, the mixture was filtered, and the filter cake was washed with 8 times the mass of the filter cake, water, and ethyl acetate in sequence, and dried at 45°C for 21 h to obtain amidated pyridine;

[0112] The mass ratio of 3-aminopyridine, triethylamine, acetonitrile, and trimesoyl chloride solution is 3.85:5.4:19:44.5; the solvent of the trimesoyl chloride solution is dichloromethane; and the ethyl acetate is ethyl acetate at a temperature of -2°C.

[0113] The amidated pyridine and ethanol were mixed and dissolved, and silver-loaded hydroxyapatite was added, with the mass ratio of amidated pyridine, ethanol, and silver-loaded hydroxyapatite being 9.5:510:5. The mixture was reacted at 65°C for 22 hours. After the reaction was completed, the mixture was filtered, the filter cake was taken, and water 8 times the mass of the filter cake was added for washing, and the mixture was dried at 45°C for 23 hours to obtain an antibacterial agent.

[0114] Step 2: blend the antibacterial nylon fiber, cotton fiber, and special-section nylon fiber in a mass ratio of 18:30:12 to obtain an inner layer blended yarn with a yarn count of 65S in the imperial system; blend the antibacterial nylon fiber and modified cotton fiber in a mass ratio of 1:1.8 to obtain a surface layer blended yarn with a yarn count of 45S in the imperial system; the inner layer blended yarn and the surface layer blended yarn are woven separately using a knitting circular machine to obtain a gram weight of 115g / m 2 The inner layer fabric is coarse and weighs 95g / m 2 Surface fabric crude product; the antibacterial nylon fiber used to prepare the surface fabric crude product is the same as the antibacterial nylon fiber used to prepare the inner layer fabric crude product;

[0115] The modified cotton fiber is prepared by the following steps:

[0116] S21, the preparation of aldehyde-modified cotton fiber is the same as that in Example 1;

[0117] S22, the amino-terminated hyperbranched polymer, 2,3-epoxypropyltrimethylammonium chloride, and water were mixed in a mass ratio of 10:2.8:500, and stirred at 75 ° C for 8 minutes. After the reaction, an antibacterial finishing liquid was obtained, and the formaldehyde-modified cotton fiber and the antibacterial finishing liquid were mixed in a mass ratio of 1:28, and the reaction was continued at 70 ° C for 50 minutes. After the reaction was completed, the filter cake was taken, and 8 times the mass of the filter cake was added for washing, and dried at 65 ° C for 14 hours to obtain modified cotton fiber;

[0118] Step 3, the surface fabric crude product and the inner layer fabric crude product are immersed in the finishing liquid respectively, with a bath ratio of 25:1, immersed at 50°C for 55 minutes, double-immersed and double-rolled, with a rolling rate of 81%. After the impregnation, dry at 85°C for 5 minutes and bake at 165°C for 55 seconds to obtain the surface fabric and the inner layer fabric respectively;

[0119] The finishing liquid is prepared by the following steps:

[0120] S31, N,N,N',N'-tetramethyl-1,6-hexanediamine acetate, polyetheramine, isopropyl alcohol, and 1,3-bis(3-glycidyloxypropyl)tetramethyldisiloxane are uniformly mixed in a molar ratio of 1:2.9:3.5:2, and the mixture is reacted at 85°C for 4 hours. After the reaction is completed, the solvent isopropyl alcohol is removed by rotary evaporation at 55°C to obtain a quaternized polyetheramine;

[0121] Wherein, the preparation of N,N,N',N'-tetramethyl-1,6-hexanediamine acetate is the same as that in Example 1;

[0122] S32. In a nitrogen atmosphere, the first catalyst was added to the quaternized polyetheramine at 220° C., and the mixture was evenly mixed. Nylon 66 salt was added, and the mixture was reacted in a nitrogen atmosphere at 230° C. for 3.5 hours. After the reaction was completed, adipic acid and the second catalyst were added, and the mixture was reacted at 240° C. for 3.5 hours. After the reaction was completed, the mixture was evacuated, and the mixture was kept in a vacuum of 10 Pa and at 240° C. for 1.5 hours. After the reaction was completed, a finishing agent was obtained; the finishing agent was mixed with water at a mass ratio of 1.4:10 to obtain a finishing liquid.

[0123] The mass ratio of the quaternized polyetheramine, nylon 66 salt, adipic acid, the first catalyst, and the second catalyst is 88:25:14.8:1.1:0.6, and both the first catalyst and the second catalyst are phosphorous acid;

[0124] Step 4: Lay the surface fabric and the inner fabric together, align the layers, and sew the surface fabric and the inner fabric together using a multi-layer fabric quilting machine using pure cotton sewing thread to obtain a moisture-absorbing and antibacterial layered composite fabric.

[0125] Example 5

[0126] This embodiment discloses a method for preparing a moisture-absorbing and antibacterial layered composite fabric, comprising the following steps:

[0127] Step 1: polyamide and antibacterial agent are mixed in a mass ratio of 100:2, melt-extruded through a twin-screw melt spinning machine, the melting section temperature is 270°C, and the spinning speed is 1000 m / min. The fibers are cooled, drawn, and chopped to obtain antibacterial nylon fibers with a fineness of 70D and an average length of 39 mm;

[0128] The antibacterial agent is prepared by the following steps:

[0129] S11, the preparation of silver-loaded hydroxyapatite is the same as that in Example 1;

[0130] S12, 3-aminopyridine, triethylamine, and acetonitrile were mixed and dissolved, and 6.5 wt% trimesoyl chloride solution was added dropwise at 5°C for 30 min. After the addition was complete, the mixture was stirred and reacted at room temperature for 52 h. After the reaction was completed, the mixture was filtered, and the filter cake was washed with 8 times the mass of the filter cake, saturated sodium bicarbonate aqueous solution, water, and ethyl acetate in sequence, and dried at 50°C for 18 h to obtain amidated pyridine;

[0131] The mass ratio of 3-aminopyridine, triethylamine, acetonitrile and trimesoyl chloride solution is 3.9:5.5:20:45; the solvent of trimesoyl chloride solution is dichloromethane; and the ethyl acetate is ethyl acetate at a temperature of 0°C.

[0132] The amidated pyridine and ethanol were mixed and dissolved, and silver-loaded hydroxyapatite was added, with the mass ratio of amidated pyridine, ethanol, and silver-loaded hydroxyapatite being 10:550:5. The mixture was reacted at 70°C for 20 hours. After the reaction was completed, the mixture was filtered, and the filter cake was taken out. The filter cake was washed with water 8 times the mass of the filter cake, and dried at 50°C for 22 hours to obtain an antibacterial agent.

[0133] Step 2: blend the antibacterial nylon fiber, cotton fiber, and special-section nylon fiber in a mass ratio of 20:30:10 to obtain an inner layer blended yarn with a yarn count of 70S in the imperial system; blend the antibacterial nylon fiber and modified cotton fiber in a mass ratio of 1:2 to obtain a surface layer blended yarn with a yarn count of 50S in the imperial system; weave the inner layer blended yarn and the surface layer blended yarn respectively using a knitting circular machine to obtain a gram weight of 120g / m 2 The inner layer fabric is coarse and weighs 100g / m 2 Surface fabric crude product; the antibacterial nylon fiber used to prepare the surface fabric crude product is the same as the antibacterial nylon fiber used to prepare the inner layer fabric crude product;

[0134] The modified cotton fiber is prepared by the following steps:

[0135] S21, the preparation of aldehyde-modified cotton fiber is the same as that in Example 1;

[0136] S22, the amino-terminated hyperbranched polymer, 2,3-epoxypropyltrimethylammonium chloride, and water were mixed in a mass ratio of 10:3:520, stirred and reacted at 80°C for 5 minutes, and after the reaction, an antibacterial finishing liquid was obtained, and the formaldehyde-modified cotton fiber and the antibacterial finishing liquid were mixed in a mass ratio of 1:30, and the reaction was continued at 80°C for 45 minutes. After the reaction was completed, the filter cake was taken, and water 8 times the mass of the filter cake was added for washing, and dried at 70°C for 12 hours to obtain modified cotton fiber;

[0137] Step 3, the surface fabric crude product and the lining fabric crude product are immersed in the finishing liquid respectively, with a bath ratio of 30:1, immersed at 50°C for 50 minutes, double-immersed and double-rolled, with a rolling rate of 82%. After the impregnation, dry at 90°C for 4 minutes and bake at 170°C for 50 seconds to obtain the surface fabric and the lining fabric respectively;

[0138] The finishing liquid is prepared by the following steps:

[0139] S31, N,N,N',N'-tetramethyl-1,6-hexanediamine acetate, polyetheramine, isopropyl alcohol, and 1,3-bis(3-glycidyloxypropyl)tetramethyldisiloxane are uniformly mixed in a molar ratio of 1:2.5:4:2, and the mixture is reacted at 90°C for 3 hours. After the reaction is completed, the solvent isopropyl alcohol is removed by rotary evaporation at 60°C to obtain a quaternized polyetheramine;

[0140] Wherein, the preparation of N,N,N',N'-tetramethyl-1,6-hexanediamine acetate is the same as that in Example 1;

[0141] S32, adding the first catalyst to the quaternized polyetheramine in a nitrogen atmosphere at 220° C. and mixing evenly, adding nylon 66 salt, and reacting in a nitrogen atmosphere at 230° C. for 3 h. After the reaction is completed, adding adipic acid and the second catalyst, and continuing to react at 240° C. for 3 h. After the reaction is completed, evacuating the mixture, and keeping the mixture at a vacuum degree of 10 Pa and a temperature of 240° C. for 1 h. After the reaction is completed, obtaining a finishing agent; mixing the finishing agent with water at a mass ratio of 1.5:10 to obtain a finishing liquid;

[0142] The mass ratio of the quaternized polyetheramine, nylon 66 salt, adipic acid, the first catalyst, and the second catalyst is 90:26:15:1.1:0.6, and both the first catalyst and the second catalyst are phosphorous acid;

[0143] Step 4: Lay the surface fabric and the inner fabric together, align the layers, and sew the surface fabric and the inner fabric together using a multi-layer fabric quilting machine using pure cotton sewing thread to obtain a moisture-absorbing and antibacterial layered composite fabric.

[0144] Comparative Example 1

[0145] This comparative example discloses a method for preparing a layered composite fabric, comprising the following steps:

[0146] Step 1: melt-extrude the polyamide through a twin-screw melt spinning machine at a melting section temperature of 260° C. and a spinning speed of 700 m / min, cool and stretch, and chop to obtain nylon fibers with a fineness of 60D and an average length of 39 mm;

[0147] Step 2: Blend nylon fiber, cotton fiber, and special-section nylon fiber in a mass ratio of 10:30:20 to obtain an inner layer blended yarn with a yarn count of 60S in the imperial system; blend nylon fiber and modified cotton fiber in a mass ratio of 1:1 to obtain a surface layer blended yarn with a yarn count of 40S in the imperial system; weave the inner layer blended yarn and the surface layer blended yarn respectively using a knitting circular machine to obtain a gram weight of 100g / m 2 The inner layer fabric is coarse and weighs 80g / m 2 Surface fabric crude product; the nylon fiber used to prepare the surface fabric crude product is the same as the nylon fiber used to prepare the inner fabric crude product;

[0148] The modified cotton fiber is prepared by the following steps:

[0149] S21, the preparation of aldehyde-modified cotton fiber is the same as that in Example 1;

[0150] S22, the amino-terminated hyperbranched polymer, 2,3-epoxypropyltrimethylammonium chloride, and water were mixed in a mass ratio of 10:2:480, stirred and reacted at 70°C for 10 minutes, and after the reaction, an antibacterial finishing liquid was obtained, and the formaldehyde-modified cotton fiber and the antibacterial finishing liquid were mixed in a mass ratio of 1:20, and the reaction was continued at 60°C for 60 minutes. After the reaction was completed, the filter cake was taken, and water 5 times the mass of the filter cake was added for washing, and dried at 60°C for 16 hours to obtain modified cotton fiber;

[0151] Step 3, the surface fabric crude product and the inner layer fabric crude product are immersed in the finishing liquid respectively, with a bath ratio of 20:1, immersed at 40°C for 60 minutes, double-immersed and double-rolled, with a rolling rate of 78%. After the impregnation, dry at 80°C for 5 minutes and bake at 160°C for 60 seconds to obtain the surface fabric and the inner layer fabric respectively;

[0152] The finishing liquid is prepared by the following steps:

[0153] S31, N,N,N',N'-tetramethyl-1,6-hexanediamine acetate, polyetheramine, isopropyl alcohol, and 1,3-bis(3-glycidyloxypropyl)tetramethyldisiloxane are uniformly mixed in a molar ratio of 1:3:3:2, and the mixture is reacted at 80°C for 5 hours. After the reaction is completed, the solvent isopropyl alcohol is removed by rotary evaporation at 50°C to obtain a quaternized polyetheramine;

[0154] Wherein, the preparation of N,N,N',N'-tetramethyl-1,6-hexanediamine acetate is the same as that in Example 1;

[0155] S32. In a nitrogen atmosphere, the first catalyst is added to the quaternized polyetheramine at a temperature of 210° C. and mixed evenly. Nylon 66 salt is added, and the mixture is reacted in a nitrogen atmosphere at a temperature of 220° C. for 4 h. After the reaction is completed, adipic acid and a second catalyst are added, and the mixture is reacted at a temperature of 230° C. for another 4 h. After the reaction is completed, the mixture is evacuated, and the mixture is kept in a vacuum of 10 Pa and a temperature of 235° C. for 2 h. After the reaction is completed, a finishing agent is obtained; the finishing agent is mixed with water at a mass ratio of 1:10 to obtain a finishing liquid.

[0156] The mass ratio of the quaternized polyetheramine, nylon 66 salt, adipic acid, the first catalyst, and the second catalyst is 80:23:14:1:0.5, and both the first catalyst and the second catalyst are phosphorous acid;

[0157] Step 4: Lay the surface fabric and the inner fabric together, align the layers, and use pure cotton sewing thread to sew the surface fabric and the inner fabric together through a multi-layer fabric quilting machine to obtain a layered composite fabric.

[0158] Comparative Example 2

[0159] This comparative example discloses a method for preparing a layered composite fabric, comprising the following steps:

[0160] Step 1: polyamide and antibacterial agent are mixed in a mass ratio of 100:1, melt-extruded through a twin-screw melt spinning machine, the melting section temperature is 260°C, and the spinning speed is 700 m / min. The fibers are cooled, drawn, and chopped to obtain antibacterial nylon fibers with a fineness of 60D and an average length of 39 mm;

[0161] The antibacterial agent is prepared by the following steps:

[0162] S11, the preparation of silver-loaded hydroxyapatite is the same as that in Example 1;

[0163] S12, 3-aminopyridine, triethylamine, and acetonitrile were mixed and dissolved, and 6.2 wt% trimesoyl chloride solution was added dropwise at 0°C for 20 min. After the addition was complete, the mixture was stirred and reacted at room temperature for 48 h. After the reaction was completed, the mixture was filtered, and the filter cake was washed with saturated sodium bicarbonate aqueous solution (5 times the mass of the filter cake), water, and ethyl acetate in that order, and dried at 40°C for 24 h to obtain amidated pyridine;

[0164] The mass ratio of 3-aminopyridine, triethylamine, acetonitrile and trimesoyl chloride solution is 3.7:5:16:43; the solvent of trimesoyl chloride solution is dichloromethane; and the ethyl acetate is ethyl acetate at a temperature of -5°C.

[0165] The amidated pyridine and ethanol were mixed and dissolved, and silver-loaded hydroxyapatite was added, with the mass ratio of amidated pyridine, ethanol, and silver-loaded hydroxyapatite being 8:480:5. The mixture was reacted at 60°C for 24 hours. After the reaction was completed, the mixture was filtered, and the filter cake was taken. The filter cake was washed with water 5 times the mass of the filter cake, and dried at 40°C for 24 hours to obtain an antibacterial agent.

[0166] Step 2: blend the antibacterial nylon fiber, cotton fiber, and special-section nylon fiber in a mass ratio of 10:30:20 to obtain an inner layer blended yarn with a yarn count of 60S in the imperial system; blend the antibacterial nylon fiber and cotton fiber in a mass ratio of 1:1 to obtain a surface layer blended yarn with a yarn count of 40S in the imperial system; weave the inner layer blended yarn and the surface layer blended yarn respectively using a knitting circular machine to obtain a gram weight of 100g / m 2 The inner layer fabric weight is 80g / m 2 Surface fabric; the antibacterial nylon fiber used to prepare the surface fabric is the same as the antibacterial nylon fiber used to prepare the inner fabric;

[0167] Step 3: Lay the surface fabric and the inner fabric together, align the layers, and use pure cotton sewing thread to sew the surface fabric and the inner fabric together through a multi-layer fabric quilting machine to obtain a layered composite fabric.

[0168] In the above embodiments and comparative examples: polyamide is from Baling Petrochemical Company, product name PA6 BL3240H; nanohydroxyapatite is from Wuhan Lanabai Pharmaceutical Chemical Co., Ltd., with a particle size of 50 nm and CAS number: 1306-06-5; trimesoyl chloride is from AlfaAesar, CAS number: 4422-95-1; cotton fiber is long-staple cotton with an average fiber length of 38 mm; special-shaped cross-section nylon fiber is from Nantong Yiheng New Materials Technology Co., Ltd., with a specification of hollow cross-section nylon staple fiber, a fineness of 1.5D, and an average fiber length of 38 mm; amino-terminated hyperbranched polymer is from Xi'an Qiyue Biotechnology Co., Ltd., product name amino-terminated hyperbranched polymer HBP-NH2, with an average molecular weight of 7500; 2,3-cyclohexane Oxypropyltrimethylammonium chloride was obtained from Shanghai Aladdin Biochemical Technology Co., Ltd., CAS No.: 3033-77-0; N,N,N',N'-tetramethyl-1,6-hexanediamine was obtained from Shanghai MacLean Biochemical Technology Co., Ltd., CAS No.: 111-18-2; polyetheramine was obtained from Shanghai MacLean Biochemical Technology Co., Ltd., product name: polyetheramine 600; 1,3-bis(3-glycidyloxypropyl)tetramethyldisiloxane was obtained from Shanghai Aladdin Biochemical Technology Co., Ltd., CAS No.: 126-80-7; nylon 66 salt was obtained from Guangdong Wengjiang Chemical Reagent Co., Ltd., product name: AH salt, CAS No.: 3323-53-3.

[0169] Test example

[0170] The performance of the layered composite fabrics prepared in Examples 1-5 and Comparative Examples 1-2 was tested. The specific test results are shown in Table 1:

[0171] Table 1

[0172]

[0173] The tests of various indicators in Table 1 are based on the following standards: the antibacterial rate is determined by referring to GB / T20944.3-2008 "Evaluation of antibacterial properties of textiles Part 3: Oscillation method", in which Escherichia coli is selected as the bacterial species; the water absorption rate, drip diffusion time, and wicking height are all determined by GB / T21655.1-2008 "Evaluation of moisture absorption and quick-drying properties of textiles Part 1: Single combination test method".

[0174] According to the test results in Table 1, it can be seen that the hygroscopic and antibacterial layered composite fabric prepared by the present invention has excellent antibacterial properties and good hygroscopic properties.

[0175] The present invention prepares silver-loaded hydroxyapatite with excellent antibacterial ability, and mixes it with amidated pyridine for reaction. The pyridine ring structure of the amidated pyridine can act as a ligand to undergo a coordination reaction with silver ions in the silver-loaded hydroxyapatite to form a coordination bond, so that the amidated pyridine is loaded on the surface of the silver-loaded hydroxyapatite as a surface modifier. The prepared antibacterial agent has an amide structure and can be interconnected with the amide groups in the nylon fiber substrate polyamide through molecular forces during melt spinning. The antibacterial agent has good compatibility with the polyamide, and the antibacterial nylon fiber prepared after melt spinning has long-lasting antibacterial ability. In comparative example 1, no antibacterial agent is added to the nylon fiber, and the antibacterial performance of the fabric is reduced. Therefore, the antibacterial rate of comparative example 1 is lower than that of the embodiment.

[0176] The modified cotton fiber of the present invention is prepared by mixing and reacting aldehyde-modified cotton fiber with an antibacterial finishing liquid containing an amino-terminated hyperbranched polymer and 2,3-epoxypropyltrimethylammonium chloride. The amino-terminated hyperbranched polymer in the antibacterial finishing agent can not only undergo a ring-opening reaction with 2,3-epoxypropyltrimethylammonium chloride to generate a quaternary ammonium salt structure with an antibacterial functional group, but also undergo a Schiff base reaction with the aldehyde-modified cotton fiber to generate a Schiff base bond with antibacterial properties, so the antibacterial property of the prepared modified cotton fiber is improved. The quaternary ammonium polyetheramine is used as a polyether component and is polycondensed with nylon 66 salt and adipic acid to obtain a modified cotton fiber having polyether segments, polyamide segments and polyamide groups. A finishing agent with an amine structure and a quaternary ammonium salt antibacterial group; when the fabric is padded, the cotton fiber and the modified cotton fiber in the fabric have active groups on their surfaces, which can form hydrogen bonds with the finishing agent; the polyamide structure in the finishing agent can form a eutectic with the nylon fiber in the fabric, and the polyether component in the finishing agent improves the hydrophilic and hygroscopic properties of the fabric, thereby improving the antibacterial and hygroscopic properties of the fabric; in comparative example 2, the cotton fiber is not modified, and the surface and inner layers of the fabric are not impregnated with the finishing liquid, lacking the modified cotton fiber and the effect of improving the antibacterial and hygroscopic properties of the finishing agent fabric, so the antibacterial rate and hygroscopic properties of comparative example 2 are lower than those of the embodiment.

[0177] While embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions, and variations may be made to these embodiments without departing from the principles and spirit of the invention, and that the scope of the invention is defined by the appended claims and their equivalents.

Claims

1. A method for preparing a hygroscopic and antibacterial layered composite fabric, characterized in that: The following steps are involved: Step 1: mixing polyamide and an antibacterial agent, melt spinning, cooling and drawing, and chopping to obtain antibacterial nylon fiber; The antibacterial agent is prepared by the following steps: 3-aminopyridine, triethylamine, and acetonitrile are mixed and dissolved, and a trimesoyl chloride solution is added dropwise. After the addition is complete, the mixture is reacted. After the reaction is complete, the mixture is filtered, washed, and dried to obtain an amidated pyridine. The amidated pyridine is mixed and dissolved with ethanol, and silver-loaded hydroxyapatite is added. The mixture is reacted. After the reaction is complete, the mixture is filtered, washed, and dried to obtain an antibacterial agent. Step 2: mixing the cotton fiber with a 0.1 mol / L sodium periodate aqueous solution at a mass ratio of 1:20-30, reacting the mixture in a dark environment at a temperature of 40-60° C. for 4-6 hours. After the reaction is complete, filtering, washing, and drying the mixture to obtain formaldehyde-modified cotton fiber; The amino-terminated hyperbranched polymer, 2,3-epoxypropyltrimethylammonium chloride, and water are mixed in a mass ratio of 10:2-3:480-520, stirred and reacted at 70-80°C for 5-10 minutes, and after the reaction is completed, an antibacterial finishing liquid is obtained. The formaldehyde-modified cotton fiber and the antibacterial finishing liquid are mixed in a mass ratio of 1:20-30, and the reaction is continued at 60-80°C for 45-60 minutes. After the reaction is completed, the modified cotton fiber is filtered, washed, and dried to obtain the modified cotton fiber. The antibacterial nylon fiber, cotton fiber and special-section nylon fiber are blended to obtain an inner layer blended yarn; the antibacterial nylon fiber is blended with modified cotton fiber to obtain an outer layer blended yarn; the inner layer blended yarn and the outer layer blended yarn are knitted separately to obtain an inner layer fabric rough product and an outer layer fabric rough product respectively; Step 3: The rough surface fabric product and the rough lining fabric product are respectively immersed in the finishing liquid, and after the immersion is completed, they are dried and baked to obtain the surface fabric and the lining fabric respectively; The finishing liquid is prepared by the following steps: N,N,N',N'-tetramethyl-1,6-hexanediamine acetate, polyetheramine, isopropyl alcohol, and 1,3-bis(3-glycidyloxypropyl)tetramethyldisiloxane are uniformly mixed and reacted. After the reaction is completed, the solvent isopropyl alcohol is removed by rotary evaporation to obtain a quaternized polyetheramine; The first catalyst is added to the quaternized polyetheramine and mixed evenly, and nylon 66 salt is added to react. After the reaction is completed, adipic acid and the second catalyst are added and the reaction is continued. After the reaction is completed, vacuum is evacuated and the temperature is kept to react. After the reaction is completed, a finishing agent is obtained; the finishing agent is mixed with water to obtain a finishing liquid. Step 4: Compound the surface layer fabric and the inner layer fabric to obtain a moisture-absorbing and antibacterial layered composite fabric.

2. The method for preparing a hygroscopic and antibacterial layered composite fabric according to claim 1, characterized in that: In step 1, the mass ratio of polyamide to antibacterial agent is 100:1-2; the melt spinning operation includes: melt extrusion through a twin-screw melt spinning machine, the melting section temperature is 260-270°C, and the spinning speed is 700-1000m / min; the specifications of the antibacterial nylon fiber are: fineness of 60-70D and average length of 39mm.

3. The method for preparing a moisture-absorbing and antibacterial layered composite fabric according to claim 1, characterized in that: In the preparation of the antibacterial agent in step 1: The mass ratio of 3-aminopyridine, triethylamine, acetonitrile, and trimesoyl chloride solution is 3.7-3.9:5-5.5:16-20:43-45; the trimesoyl chloride solution is a 6.2-6.5 wt% trimesoyl chloride solution, and the solvent is dichloromethane. The trimesoyl chloride solution is added dropwise at 0-5°C for 20-30 minutes. When preparing the amidated pyridine, the reaction is stirred at room temperature for 48-52 hours. The mass ratio of amidated pyridine, ethanol and silver-loaded hydroxyapatite is 8-10:480-550:5; when preparing the antibacterial agent, the reaction conditions are: reacting at a temperature of 60-70° C. for 20-24 hours.

4. The method for preparing a hygroscopic and antibacterial layered composite fabric according to claim 1, characterized in that: In the preparation of the antibacterial agent in step 1, the silver-loaded hydroxyapatite is prepared by the following steps: The nano-hydroxyapatite is mixed with a silver nitrate aqueous solution, reacted, filtered, washed, and dried after the reaction is completed to obtain silver-loaded hydroxyapatite; The mass ratio of nano-hydroxyapatite to silver nitrate aqueous solution is 1:8-10, and the silver nitrate aqueous solution is 0.1 mol / L silver nitrate aqueous solution; and the reaction conditions are: reaction at a temperature of 80-90° C. for 16-20 hours.

5. The method for preparing a moisture-absorbing and antibacterial layered composite fabric according to claim 1, characterized in that: In the step 2, when preparing the inner layer blended yarn, the mass ratio of the antibacterial nylon fiber, the cotton fiber, and the special-section nylon fiber is 10-20:30:10-20, and the yarn count of the inner layer blended yarn is 60-70S in British count; when preparing the surface layer blended yarn, the mass ratio of the antibacterial nylon fiber to the modified cotton fiber is 1:1-2, and the yarn count of the surface layer blended yarn is 40-50S in British count; the gram weight of the inner layer fabric rough product is 100-120g / m 2 ; The surface fabric weight is 80-100g / m 2 The antibacterial nylon fiber used to prepare the surface fabric crude product is the same as the antibacterial nylon fiber used to prepare the inner fabric crude product.

6. The method for preparing a moisture-absorbing and antibacterial layered composite fabric according to claim 1, characterized in that: In the step 3, in the dipping operation, the bath ratio is 20-30:1; the dipping operation includes: dipping at a temperature of 40-50° C. for 50-60 minutes, two dippings and two rollings, and the rolling rate is 78-82%.

7. The method for preparing a moisture-absorbing and antibacterial layered composite fabric according to claim 1, characterized in that: In step 3, when preparing the finishing liquid: The molar ratio of N,N,N',N'-tetramethyl-1,6-hexanediamine acetate, polyetheramine, isopropyl alcohol, and 1,3-bis(3-glycidyloxypropyl)tetramethyldisiloxane is 1:2.5-3:3-4:2; when preparing the quaternized polyetheramine, the reaction conditions are: reaction at a temperature of 80-90° C. for 3-5 hours; The mass ratio of quaternized polyetheramine, nylon 66 salt, adipic acid, the first catalyst, and the second catalyst is 80-90:23-26:14-15:1-1.1:0.5-0.6, and both the first catalyst and the second catalyst are phosphorous acid. The first catalyst is added to the quaternized polyetheramine under a nitrogen atmosphere at a temperature of 210-220° C. When preparing the finishing agent, the reaction conditions are as follows: reacting at a temperature of 220-230° C. under a nitrogen atmosphere for 3-4 hours; continuing the reaction conditions are as follows: continuing the reaction at a temperature of 230-240° C. under a nitrogen atmosphere for 3-4 hours; and maintaining the reaction temperature for 1-2 hours under a vacuum degree of 10 Pa and a temperature of 235-240° C.; and the mass ratio of the finishing agent to water is 1-1.5:

10.

8. A hygroscopic and antibacterial layered composite fabric prepared by the method for preparing a hygroscopic and antibacterial layered composite fabric according to any one of claims 1 to 7.

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