Moisture-absorbing antibacterial layered composite fabric and preparation method thereof
By mixing antibacterial agent with polyamide, antibacterial nylon fiber is prepared, and blended with cotton fiber and modified cotton fiber to knit into a layered fabric, the problem of degradation of antibacterial effect of existing antibacterial fabrics is solved, and the long-term antibacterial effect of the fabric is achieved and moisture absorption properties.
Patent Information
- Application Number
- CN202411571324.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-06
- Publication Date
- 2025-02-14
- Estimated Expiration
- 2044-11-06
AI Technical Summary
After multiple use and washing of existing antibacterial fabrics, their antibacterial effect will decrease, making it difficult to maintain long-term antibacterial properties.
Antibacterial nylon fibers are prepared by mixing antibacterial agents with polyamide, melt-spinning, and blending them with cotton fibers and modified cotton fibers, knitted into a layered fabric, and finally treated in an impregnation finishing solution to improve antibacterial and hygroscopic properties.
The prepared hygroscopic antibacterial layered composite fabric has excellent antibacterial properties and good hygroscopic properties, and can maintain a high effect after multiple uses and washing.
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Figure CN119427864A_ABST
Abstract
Description
Technical Field
[0001] The 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 the development direction into natural antibacterial fiber fabrics, new developed fiber fabrics, artificial antibacterial fiber fabrics and antibacterial agent finished fabrics. Among them, antibacterial agent finished fabrics are post-finishing treatments of fabrics, 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 after several uses and washings, the antibacterial effect will decrease.
[0003] Prior art, such as Chinese patent CN113386410A, discloses a multifunctional health-care knitted fabric and a preparation method thereof, wherein modified holy hemp fiber, heating fiber, negative ion fiber and modified wormwood fiber are used as the inner layer, and modified kapok fiber, nylon fiber and regenerated cellulose fiber are used as the outer layer. The obtained knitted fabric has antibacterial, antibacterial and deodorizing properties. However, in the prepared fabric, the antibacterial effect is mainly provided by the fiber and the finishing liquid containing antibacterial substances. After washing, the finishing agent on the surface of the fabric is easy to fall 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. 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 antibacterial agent, melt spinning, cooling and drawing, and chopping to obtain antibacterial nylon fiber;
[0008] Wherein, 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 in a mixed solution, adding trimesoyl chloride solution dropwise, reacting after the addition is complete, filtering, washing and drying after the reaction is complete 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; weaving the inner layer blended yarn and the outer layer blended yarn respectively using a circular knitting machine to obtain an inner layer fabric rough product and an outer layer fabric rough product respectively;
[0013] Wherein, the modified cotton fiber is prepared by the following steps:
[0014] S21, mixing cotton fiber with sodium periodate aqueous solution, reacting, filtering, washing, and drying after the reaction is completed to obtain aldehyde-modified cotton fiber;
[0015] S22, mixing the amino-terminated hyperbranched polymer, 2,3-epoxypropyltrimethylammonium chloride and water, reacting, and obtaining an antibacterial finishing liquid after the reaction is completed, mixing the aldehyde-modified cotton fiber with the antibacterial finishing liquid, and continuing the reaction, and filtering, washing and drying after the reaction is completed to obtain modified cotton fiber;
[0016] Step 3, respectively immersing the rough surface fabric product and the rough lining fabric product in the finishing liquid, and after the immersion is completed, drying and baking to obtain the surface fabric product and the lining fabric product respectively;
[0017] Wherein, the finishing liquid is prepared by the following steps:
[0018] S31, N,N,N',N'-tetramethyl-1,6-hexanediamine acetate, polyetheramine, isopropanol, and 1,3-bis(3-glycidyloxypropyl)tetramethyldisiloxane are uniformly mixed and reacted, and after the reaction is completed, the solvent isopropanol is removed by rotary evaporation to obtain a quaternized polyetheramine;
[0019] S32, adding the first catalyst to the quaternary ammonium 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 for reaction, 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 the 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 spinning is carried out at a spinning speed of 700-1000m / min; the specifications of the antibacterial nylon fiber are: fineness is 60-70D, and the average length is 39mm.
[0022] Preferably, in S11 of step 1: 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: reacting at a temperature of 80-90° C. for 16-20 hours.
[0023] Preferably, in S12 of the 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 6.2-6.5wt% trimesoyl chloride solution, and the solvent is dichloromethane; the dripping condition of the trimesoyl chloride solution is: dripping at a temperature of 0-5°C for 20-30min; when preparing the amidated pyridine, the reaction conditions are: stirring the reaction at room temperature for 48-52h.
[0024] Preferably, the detergent used in the washing operation includes: saturated sodium bicarbonate aqueous solution, water, ethyl acetate in sequence, and the ethyl acetate includes ethyl acetate at a temperature of -5-0°C.
[0025] Preferably, in S12 of step 1, 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 20-24h.
[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-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 weight of the rough surface fabric 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 S21 of step 2: 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: reacting in a light-proof environment at a temperature of 40-60° C. for 4-6 hours.
[0029] Preferably, in S22 of step 2: 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 and 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 three: 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%.
[0031] Preferably, in S31 of step three: the molar ratio of N,N,N',N'-tetramethyl-1,6-hexanediamine acetate, polyetheramine, isopropanol, and 1,3-bis(3-glycidyloxypropyl)tetramethyldisiloxane is 1:2.5-3:3-4:2; and the reaction conditions are: reacting at a temperature of 80-90°C for 3-5h.
[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 S32 of step three, 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 S32 of the step three: the conditions for adding the first catalyst are: adding the first catalyst to the quaternized polyetheramine in a nitrogen atmosphere at a temperature of 210-220°C; the reaction conditions are: reacting for 3-4 hours in a nitrogen atmosphere at a temperature of 220-230°C; the conditions for continuing the reaction are: continuing the reaction for 3-4 hours in a nitrogen atmosphere at a temperature of 230-240°C; the insulation reaction conditions are: insulation reaction for 1-2 hours at a vacuum degree of 10Pa and a temperature of 235-240°C; 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, and then blending the fibers with cotton fibers and special-section nylon fibers, knitting, and preparing a rough inner fabric product; blending the antibacterial nylon fibers with modified cotton fibers grafted with quaternary ammonium salts, and knitting to obtain a rough surface fabric product; respectively impregnating the rough surface fabric product and the rough inner fabric product with a finishing liquid containing a quaternary ammonium salt structure and a polyether polyamide block copolymer, so that the antibacterial ability and hygroscopic performance of the prepared surface fabric and the inner fabric are improved; and the two are composited to obtain a hygroscopic antibacterial layered composite fabric with excellent antibacterial performance and good hygroscopic performance.
[0038] The invention uses an ion exchange method to mix nano hydroxyapatite with a silver nitrate aqueous solution to undergo an ion exchange reaction, so that silver ions replace part of calcium ions and enter the lattice structure of the hydroxyapatite, and 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, and the amidated pyridine is mixed with the silver-loaded hydroxyapatite for reaction, and the pyridine ring structure of the amidated pyridine can be used as a ligand to undergo a coordination reaction with the 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, and the obtained antibacterial agent has an amide structure, so that it can be connected with the amide group in the nylon fiber substrate polyamide through molecular forces during melt spinning, and the antibacterial agent has good compatibility with the polyamide, and the antibacterial nylon fiber obtained after melt spinning has long-lasting antibacterial ability;
[0039] The invention prepares a rough inner fabric by knitting antibacterial nylon fiber with cotton fiber and special-section nylon fiber; and prepares a rough surface fabric by knitting antibacterial nylon fiber with modified cotton fiber; wherein the modified cotton fiber is prepared by oxidizing cotton fiber with sodium periodate aqueous solution to generate aldehyde-modified cotton fiber, and then mixing and reacting 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 property, so that the antibacterial property of the prepared modified cotton fiber is improved;
[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, thereby obtaining a quaternized polyetheramine having a siloxane segment and a quaternary ammonium salt structure; using the quaternized polyetheramine as a polyether component, polycondensing the quaternary polyetheramine with nylon 66 salt and adipic acid, thereby obtaining a finishing agent having a polyether segment, a polyamide structure and a quaternary ammonium salt antibacterial group; and respectively padding a surface layer fabric crude product and an inner layer fabric crude product with a finishing liquid. During the padding treatment, the cotton fibers and modified cotton fibers 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 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 hygroscopicity of the fabric are improved; the surface fabric and the lining fabric are compounded to obtain a hygroscopic and antibacterial layered composite fabric with excellent antibacterial properties and good hygroscopicity. BRIEF DESCRIPTION OF THE DRAWINGS
[0041] Figure 1 It is a process flow chart for preparing the moisture-absorbing and antibacterial layered composite fabric in the present invention;
[0042] Figure 2 It is a schematic structural diagram of the moisture-absorbing and antibacterial layered composite fabric prepared in the present invention;
[0043] Figure 3 It is a bar graph of the antibacterial rate of the layered composite fabrics prepared in the embodiments and comparative examples of the present invention in the performance test;
[0044] Figure 4 It is a bar graph of water absorption rate of the layered composite fabrics prepared in the embodiments and comparative examples of the present invention in performance tests;
[0045] Figure 5 It is a bar graph of the drip diffusion time of the layered composite fabrics prepared in the embodiments and comparative examples of the present invention in the performance test;
[0046] In the figure:
[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 of 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., spinning is performed at a spinning speed of 700 m / min, cooled and drawn, and chopped to obtain an antibacterial nylon fiber with a fineness of 60D and an average length of 39 mm;
[0052] Wherein, the antibacterial agent is prepared by the following steps:
[0053] S11, mixing nano-hydroxyapatite with 0.1 mol / L silver nitrate aqueous solution at a mass ratio of 1:9, reacting at 85° C. for 18 h, filtering after the reaction, taking the filter cake, adding water 6 times the mass of the filter cake for washing, and drying at 55° C. for 26 h to obtain silver-loaded hydroxyapatite;
[0054] S12, 3-aminopyridine, triethylamine and acetonitrile were mixed and dissolved, 6.2 wt% trimesoyl chloride solution was added dropwise at 0°C for 20 min. After the addition was completed, the mixture was stirred at room temperature for 48 h. After the reaction was completed, the mixture was filtered, the filter cake was taken, 5 times the mass of the filter cake was washed with saturated sodium bicarbonate aqueous solution, water and ethyl acetate, and the mixture was 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 ethyl acetate is ethyl acetate at a temperature of -5°C;
[0056] Mix and dissolve amidated pyridine and ethanol, add silver-loaded hydroxyapatite, the mass ratio of amidated pyridine, ethanol and silver-loaded hydroxyapatite is 8:480:5, react at 60°C for 24 hours, filter and take the filter cake after the reaction is completed, add water 5 times the mass of the filter cake for washing, and dry 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 British 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 British 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 fabric crude product;
[0058] Wherein, the modified cotton fiber is prepared by the following steps:
[0059] S21, mixing cotton fiber with 0.1 mol / L sodium periodate aqueous solution at a mass ratio of 1:25, reacting in a light-proof environment at 50° C. for 5 h, filtering and taking the filter cake after the reaction, washing it with water 6 times the mass of the filter cake until it is neutral, and drying it at 45° C. for 19 h to obtain aldehyde-modified cotton fiber;
[0060] S22, the amino-terminated hyperbranched polymer, 2,3-epoxypropyltrimethylammonium chloride, and water are mixed in a mass ratio of 10:2:480, and stirred for reaction at 70°C for 10 minutes. After the reaction is completed, an antibacterial finishing liquid is obtained, and the formaldehyde-modified cotton fiber and the antibacterial finishing liquid are mixed in a mass ratio of 1:20, and the reaction is continued at 60°C for 60 minutes. After the reaction is completed, the filter is filtered, the filter cake is taken, and water 5 times the mass of the filter cake is added for washing, and the filter cake is dried at 60°C for 16 hours to obtain modified cotton fiber;
[0061] Step 3, the rough surface fabric and the rough lining fabric are immersed in the finishing liquid respectively, the bath ratio is 20:1, immersed at 40°C for 60 minutes, double-immersed and double-rolled, the rolling rate is 78%, after the immersion, dried at 80°C for 5 minutes, baked at 160°C for 60 seconds, to obtain the surface fabric and the lining fabric respectively;
[0062] Wherein, the finishing liquid is prepared by the following steps:
[0063] S31, N,N,N',N'-tetramethyl-1,6-hexanediamine acetate, polyetheramine, isopropanol, and 1,3-bis(3-glycidyloxypropyl)tetramethyldisiloxane are uniformly mixed in a molar ratio of 1:3:3:2, and reacted at 80°C for 5h. After the reaction is completed, the solvent isopropanol 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 in a molar ratio of 1:2 and stirring at room temperature for 1 hour;
[0065] S32, in a nitrogen atmosphere, at a temperature of 210° C., adding the first catalyst to the quaternary ammonium polyetheramine and mixing evenly, adding nylon 66 salt, reacting in a nitrogen atmosphere at a temperature of 220° C. for 4 hours, after the reaction is completed, adding adipic acid and the second catalyst, continuing to react at a temperature of 230° C. for 4 hours, after the reaction is completed, evacuating, and keeping the temperature at a vacuum degree of 10 Pa and a temperature of 235° C. for 2 hours, after the reaction is completed, obtaining a finishing agent; mixing the finishing agent with water at a mass ratio of 1:10 to obtain a finishing liquid;
[0066] The mass ratio of 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: fit 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 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, spinning is performed at a spinning speed of 800m / min, cooling and drawing, and short-cutting to obtain antibacterial nylon fiber with a fineness of 65D and an average length of 39mm;
[0071] Wherein, 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, 6.3 wt% of trimesoyl chloride solution was added dropwise at 2°C for 25 min. After the addition was completed, 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 taken. A saturated sodium bicarbonate aqueous solution, water and ethyl acetate with a weight of 5 times the weight of the filter cake were added in turn for washing, and the mixture was 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 trimesoyl chloride solution is dichloromethane; ethyl acetate is ethyl acetate at a temperature of -5°C;
[0075] Mix and dissolve amidated pyridine and ethanol, add silver-loaded hydroxyapatite, the mass ratio of amidated pyridine, ethanol and silver-loaded hydroxyapatite is 8.5:500:5, react at 65°C for 22h, filter after the reaction, take the filter cake, add water 5 times the mass of the filter cake for washing, and dry at 45°C for 23h 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 blended yarn with a yarn count of 65S in British system; blend the antibacterial nylon fiber and the modified cotton fiber in a mass ratio of 1:1.3 to obtain a surface blended yarn with a yarn count of 45S in British system; weave the inner blended yarn and the surface blended yarn using a knitting circular machine to obtain a gram weight of 105 g / 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 fabric crude product;
[0077] Wherein, 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 are mixed in a mass ratio of 10:2.3:500, and stirred at 75°C for 8 minutes. After the reaction is completed, an antibacterial finishing liquid is obtained, and the formaldehyde-modified cotton fiber and the antibacterial finishing liquid are mixed in a mass ratio of 1:22, and the reaction is continued at 70°C for 50 minutes. After the reaction is completed, the filter is filtered, and the filter cake is taken, and water 6 times the mass of the filter cake is added for washing, and dried at 65°C for 14 hours to obtain modified cotton fiber;
[0080] Step 3, the rough surface fabric and the rough lining fabric are immersed in the finishing liquid respectively, the bath ratio is 25:1, immersed at 45°C for 55 minutes, double-immersed and double-rolled, the rolling rate is 79%, after the immersion, dried at 85°C for 4.5 minutes, baked at 165°C for 55 seconds, to obtain the surface fabric and the lining fabric respectively;
[0081] Wherein, the finishing liquid is prepared by the following steps:
[0082] S31, N,N,N',N'-tetramethyl-1,6-hexanediamine acetate, polyetheramine, isopropanol, and 1,3-bis(3-glycidyloxypropyl)tetramethyldisiloxane are uniformly mixed in a molar ratio of 1:2.6:3.3:2, and reacted at 85°C for 4 hours. After the reaction is completed, the solvent isopropanol is removed by rotary evaporation at 55°C to obtain a quaternary ammonium 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, at a temperature of 215°C, adding the first catalyst to the quaternary ammonium polyetheramine and mixing evenly, adding nylon 66 salt, reacting in a nitrogen atmosphere at a temperature of 220°C for 3.5 hours, after the reaction is completed, adding adipic acid and the second catalyst, continuing to react at a temperature of 230°C for 3.5 hours, after the reaction is completed, evacuating, and keeping the temperature at a vacuum degree of 10Pa and a temperature of 235°C for 1.5 hours, after the reaction is completed, obtaining a finishing agent; mixing the finishing agent with water at a mass ratio of 1.2:10 to obtain a finishing liquid;
[0085] The mass ratio of 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: fit 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 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] Wherein, 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, 6.4 wt% of trimesoyl chloride solution was added dropwise at 2°C for 25 min. After the addition was completed, 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 taken. A saturated sodium bicarbonate aqueous solution, water and ethyl acetate with a weight of 6 times the weight of the filter cake were added in turn for washing, and the mixture was 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; ethyl acetate is ethyl acetate at a temperature of -2°C;
[0094] Mix and dissolve amidated pyridine and ethanol, add silver-loaded hydroxyapatite, the mass ratio of amidated pyridine, ethanol and silver-loaded hydroxyapatite is 9:510:5, react at 65°C for 22h, filter and take the filter cake after the reaction is completed, add water 6 times the mass of the filter cake for washing, and dry at 45°C for 23h 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 blended yarn with a yarn count of 65S in British system; blend the antibacterial nylon fiber and the modified cotton fiber in a mass ratio of 1:1.5 to obtain a surface blended yarn with a yarn count of 45S in British system; weave the inner blended yarn and the surface blended yarn using a knitting circular machine to obtain a gram weight of 110 g / m 2 The inner layer fabric is rough 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 fabric crude product;
[0096] Wherein, 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 are mixed in a mass ratio of 10:2.5:500, and stirred at 75°C for 8 minutes. After the reaction is completed, an antibacterial finishing liquid is obtained, and the formaldehyde-modified cotton fiber and the antibacterial finishing liquid are mixed in a mass ratio of 1:25, and the reaction is continued at 70°C for 50 minutes. After the reaction is completed, the filter is filtered, and the filter cake is taken, and water 6 times the mass of the filter cake is added for washing, and dried at 65°C for 14 hours to obtain modified cotton fiber;
[0099] Step 3, the rough surface fabric and the rough lining fabric are immersed in the finishing liquid respectively, the bath ratio is 25:1, immersed at 45°C for 55 minutes, double-immersed and double-rolled, the rolling rate is 80%, after the immersion, dried at 85°C for 4.5 minutes, baked at 165°C for 55 seconds, to obtain the surface fabric and the lining fabric respectively;
[0100] Wherein, the finishing liquid is prepared by the following steps:
[0101] S31, N,N,N',N'-tetramethyl-1,6-hexanediamine acetate, polyetheramine, isopropanol, and 1,3-bis(3-glycidyloxypropyl)tetramethyldisiloxane are uniformly mixed in a molar ratio of 1:2.8:3.5:2, and reacted at 85°C for 4 hours. After the reaction is completed, the solvent isopropanol 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, at a temperature of 215° C., adding the first catalyst to the quaternary ammonium polyetheramine and mixing evenly, adding nylon 66 salt, reacting in a nitrogen atmosphere at a temperature of 225° C. for 3.5 hours, after the reaction is completed, adding adipic acid and the second catalyst, continuing to react at a temperature of 235° C. for 3.5 hours, after the reaction is completed, evacuating, and keeping the temperature at a vacuum degree of 10 Pa and a temperature of 238° C. for 1.5 hours, after the reaction is completed, obtaining a finishing agent; mixing the finishing agent 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: fit 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 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, spinning is performed at a spinning speed of 1000m / min, cooling and drawing, and short-cutting to obtain antibacterial nylon fiber with a fineness of 70D and an average length of 39mm;
[0109] Wherein, 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, 6.5 wt% trimesoyl chloride solution was added dropwise at 2°C for 25 min. After the addition was completed, 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 taken. A saturated sodium bicarbonate aqueous solution, water and ethyl acetate in an amount 8 times the mass of the filter cake were added in turn for washing, and the mixture was 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 trimesoyl chloride solution is dichloromethane; ethyl acetate is ethyl acetate at a temperature of -2°C;
[0113] Mix and dissolve amidated pyridine and ethanol, add silver-loaded hydroxyapatite, the mass ratio of amidated pyridine, ethanol and silver-loaded hydroxyapatite is 9.5:510:5, react at 65°C for 22h, filter and take the filter cake after the reaction is completed, add water 8 times the mass of the filter cake for washing, and dry at 45°C for 23h 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 blended yarn with a yarn count of 65S in British system; blend the antibacterial nylon fiber and the modified cotton fiber in a mass ratio of 1:1.8 to obtain a surface blended yarn with a yarn count of 45S in British system; weave the inner blended yarn and the surface blended yarn using a knitting circular machine to obtain a gram weight of 115g / m 2 The inner layer fabric is rough 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 fabric crude product;
[0115] Wherein, 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 are mixed in a mass ratio of 10:2.8:500, and stirred at 75°C for 8 minutes. After the reaction is completed, an antibacterial finishing liquid is obtained, and the formaldehyde-modified cotton fiber and the antibacterial finishing liquid are mixed in a mass ratio of 1:28, and the reaction is continued at 70°C for 50 minutes. After the reaction is completed, the filter is filtered, and the filter cake is taken, and water 8 times the mass of the filter cake is added for washing, and dried at 65°C for 14 hours to obtain modified cotton fiber;
[0118] Step 3, the rough surface fabric and the rough lining fabric are immersed in the finishing liquid respectively, the bath ratio is 25:1, immersed at 50°C for 55 minutes, double-immersed and double-rolled, the rolling rate is 81%, after the immersion, dried at 85°C for 5 minutes, baked at 165°C for 55 seconds, to obtain the surface fabric and the lining fabric respectively;
[0119] Wherein, the finishing liquid is prepared by the following steps:
[0120] S31, N,N,N',N'-tetramethyl-1,6-hexanediamine acetate, polyetheramine, isopropanol, and 1,3-bis(3-glycidyloxypropyl)tetramethyldisiloxane are uniformly mixed in a molar ratio of 1:2.9:3.5:2, and reacted at 85°C for 4 hours. After the reaction is completed, the solvent isopropanol is removed by rotary evaporation at 55°C to obtain a quaternary ammonium 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, at a temperature of 220° C., adding the first catalyst to the quaternary ammonium polyetheramine and mixing evenly, adding nylon 66 salt, reacting in a nitrogen atmosphere at a temperature of 230° C. for 3.5 hours, after the reaction is completed, adding adipic acid and the second catalyst, continuing to react at a temperature of 240° C. for 3.5 hours, after the reaction is completed, evacuating, and keeping the temperature at a vacuum degree of 10 Pa and a temperature of 240° C. for 1.5 hours, after the reaction is completed, obtaining a finishing agent; mixing the finishing agent with water at a mass ratio of 1.4:10 to obtain a finishing liquid;
[0123] The mass ratio of 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: fit 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 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, spinning is performed at a spinning speed of 1000m / min, cooling and drawing, and short-cutting to obtain antibacterial nylon fiber with a fineness of 70D and an average length of 39mm;
[0128] Wherein, 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, 6.5 wt% trimesoyl chloride solution was added dropwise at 5°C for 30 min. After the addition was completed, the mixture was stirred at room temperature for 52 h. After the reaction was completed, the mixture was filtered and the filter cake was taken. A saturated sodium bicarbonate aqueous solution, water and ethyl acetate in an amount 8 times the mass of the filter cake were added in turn for washing, and the mixture was 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; ethyl acetate is ethyl acetate at a temperature of 0°C;
[0132] Mix and dissolve amidated pyridine and ethanol, add silver-loaded hydroxyapatite, the mass ratio of amidated pyridine, ethanol and silver-loaded hydroxyapatite is 10:550:5, react at 70°C for 20h, filter and take the filter cake after the reaction is completed, add water 8 times the mass of the filter cake for washing, and dry at 50°C for 22h 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 blended yarn with a yarn count of 70S in British system; blend the antibacterial nylon fiber and the modified cotton fiber in a mass ratio of 1:2 to obtain a surface blended yarn with a yarn count of 50S in British system; weave the inner blended yarn and the surface blended yarn using a large circular knitting machine to obtain a gram weight of 120g / m 2 The inner layer fabric is rough 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 fabric crude product;
[0134] Wherein, 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 are mixed in a mass ratio of 10:3:520, stirred and reacted at 80°C for 5 minutes, and after the reaction is completed, an antibacterial finishing liquid is obtained, and the formaldehyde-modified cotton fiber and the antibacterial finishing liquid are mixed in a mass ratio of 1:30, and the reaction is continued at 80°C for 45 minutes. After the reaction is completed, the filter is filtered, and the filter cake is taken, and water 8 times the mass of the filter cake is added for washing, and dried at 70°C for 12 hours to obtain modified cotton fiber;
[0137] Step 3, the rough surface fabric and the rough lining fabric are immersed in the finishing liquid respectively, the bath ratio is 30:1, immersed at 50°C for 50 minutes, double-immersed and double-rolled, the rolling rate is 82%, after the immersion, dried at 90°C for 4 minutes, baked at 170°C for 50 seconds, to obtain the surface fabric and the lining fabric respectively;
[0138] Wherein, the finishing liquid is prepared by the following steps:
[0139] S31, N,N,N',N'-tetramethyl-1,6-hexanediamine acetate, polyetheramine, isopropanol, and 1,3-bis(3-glycidyloxypropyl)tetramethyldisiloxane are uniformly mixed in a molar ratio of 1:2.5:4:2, and reacted at 90°C for 3h. After the reaction is completed, the solvent isopropanol 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, in a nitrogen atmosphere, at a temperature of 220° C., adding the first catalyst to the quaternary ammonium polyetheramine and mixing evenly, adding nylon 66 salt, reacting in a nitrogen atmosphere at a temperature of 230° C. for 3 hours, after the reaction is completed, adding adipic acid and the second catalyst, continuing to react at a temperature of 240° C. for 3 hours, after the reaction is completed, evacuating, and keeping the temperature at a vacuum degree of 10 Pa and a temperature of 240° C. for 1 hour, 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 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: fit 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 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, with the melting section temperature at 260° C., spin at 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 British 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 British system; weave the inner layer blended yarn and the surface layer blended yarn 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] Wherein, 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 are mixed in a mass ratio of 10:2:480, and stirred for reaction at 70°C for 10 minutes. After the reaction is completed, an antibacterial finishing liquid is obtained, and the formaldehyde-modified cotton fiber and the antibacterial finishing liquid are mixed in a mass ratio of 1:20, and the reaction is continued at 60°C for 60 minutes. After the reaction is completed, the filter is filtered, the filter cake is taken, and water 5 times the mass of the filter cake is added for washing, and the filter cake is dried at 60°C for 16 hours to obtain modified cotton fiber;
[0151] Step 3, the rough surface fabric and the rough lining fabric are immersed in the finishing liquid respectively, the bath ratio is 20:1, immersed at 40°C for 60 minutes, double-immersed and double-rolled, the rolling rate is 78%, after the immersion, dried at 80°C for 5 minutes, baked at 160°C for 60 seconds, to obtain the surface fabric and the lining fabric respectively;
[0152] Wherein, the finishing liquid is prepared by the following steps:
[0153] S31, N,N,N',N'-tetramethyl-1,6-hexanediamine acetate, polyetheramine, isopropanol, and 1,3-bis(3-glycidyloxypropyl)tetramethyldisiloxane are uniformly mixed in a molar ratio of 1:3:3:2, and reacted at 80°C for 5h. After the reaction is completed, the solvent isopropanol 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, at a temperature of 210° C., adding the first catalyst to the quaternary ammonium polyetheramine and mixing evenly, adding nylon 66 salt, reacting in a nitrogen atmosphere at a temperature of 220° C. for 4 hours, after the reaction is completed, adding adipic acid and the second catalyst, continuing to react at a temperature of 230° C. for 4 hours, after the reaction is completed, evacuating, and keeping the temperature at a vacuum degree of 10 Pa and a temperature of 235° C. for 2 hours, after the reaction is completed, obtaining a finishing agent; mixing the finishing agent with water at a mass ratio of 1:10 to obtain a finishing liquid;
[0156] The mass ratio of 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: fit 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., spinning is performed at a spinning speed of 700 m / min, cooling and drawing, and short-cutting to obtain antibacterial nylon fiber with a fineness of 60D and an average length of 39 mm;
[0161] Wherein, 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, 6.2 wt% trimesoyl chloride solution was added dropwise at 0°C for 20 min. After the addition was completed, 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 taken. A saturated sodium bicarbonate aqueous solution, water and ethyl acetate with a weight of 5 times the weight of the filter cake were added in turn for washing, and the mixture was 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 ethyl acetate is ethyl acetate at a temperature of -5°C;
[0165] Mix and dissolve amidated pyridine and ethanol, add silver-loaded hydroxyapatite, the mass ratio of amidated pyridine, ethanol and silver-loaded hydroxyapatite is 8:480:5, react at 60°C for 24 hours, filter and take the filter cake after the reaction is completed, add water 5 times the mass of the filter cake for washing, and dry 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 British 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 British 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: fit 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 comes from Baling Petrochemical Company, product name PA6 BL3240H; nanohydroxyapatite comes from Wuhan Lanabai Pharmaceutical Chemical Co., Ltd., with a particle size of 50 nm and CAS number: 1306-06-5; trimesoyl chloride comes 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 comes 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 comes from Xi'an Qiyue Biotechnology Co., Ltd., product name amino-terminated hyperbranched polymer HBP-NH 2 , average molecular weight 7500; 2,3-epoxypropyltrimethylammonium chloride comes from Shanghai Aladdin Biochemical Technology Co., Ltd., CAS No.: 3033-77-0; N,N,N',N'-tetramethyl-1,6-hexanediamine comes from Shanghai MacLean Biochemical Technology Co., Ltd., CAS No.: 111-18-2; polyetheramine comes from Shanghai MacLean Biochemical Technology Co., Ltd., product name polyetheramine 600; 1,3-bis(3-glycidyloxypropyl)tetramethyldisiloxane comes from Shanghai Aladdin Biochemical Technology Co., Ltd., CAS No.: 126-80-7; nylon 66 salt comes 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, and the specific test results are shown in Table 1:
[0171] Table 1
[0172]
[0173] The detection of each index in Table 1 is 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 bacteria; 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] It can be seen from the test results in Table 1 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 coordinate with the 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 connected with the amide group 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, so 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 property, so that the antibacterial property of the prepared modified cotton fiber is improved. The quaternary ammonium polyetheramine is used as a polyether component and polycondensed with nylon 66 salt and adipic acid to obtain a modified cotton fiber having a polyether segment, a polyacrylic acid segment and a polyacrylic acid segment. A finishing agent with an amine structure and a quaternary ammonium salt antibacterial group; when the fabric is subjected to padding treatment, 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 hygroscopic properties of the fabric, and the antibacterial ability and hygroscopic ability of the fabric are improved; in comparative example 2, the cotton fiber is not modified, and the surface layer and the inner layer of the fabric are not impregnated with the finishing liquid, lacking the modified cotton fiber and the effect of improving the antibacterial property and hygroscopic property of the finishing agent fabric, so the antibacterial rate and hygroscopic property of comparative example 2 are lower than those of the embodiment.
[0177] Although 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 the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present 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 antibacterial agent, melt spinning, cooling and drawing, and chopping to obtain antibacterial nylon fiber; Wherein, the antibacterial agent is prepared by the following steps: Mix and dissolve 3-aminopyridine, triethylamine and acetonitrile, dropwise add trimesoyl chloride solution, react after the dropwise addition is complete, filter, wash and dry after the reaction is complete to obtain amidated pyridine; mix and dissolve amidated pyridine with ethanol, add silver-loaded hydroxyapatite, react, filter, wash and dry after the reaction is complete to obtain an antibacterial agent; 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; knitting the inner layer blended yarn and the outer layer blended yarn separately to obtain an inner layer fabric rough product and an outer layer fabric rough product respectively; Step 3, respectively immersing the rough surface fabric product and the rough lining fabric product in the finishing liquid, and after the immersion is completed, drying and baking to obtain the surface fabric product and the lining fabric product respectively; 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 the 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 spinning is performed at a spinning speed of 700-1000m / min; the specifications of the antibacterial nylon fiber are: fineness is 60-70D, and the average length is 39mm.
3. 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 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 6.2-6.5wt% trimesoyl chloride solution, and the solvent is dichloromethane; the dripping condition of the trimesoyl chloride solution is: dripping at a temperature of 0-5°C for 20-30min; when preparing the amidated pyridine, the reaction condition is: stirring the reaction at room temperature for 48-52h; 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 20-24h.
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 the 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; the reaction conditions are: reacting at a temperature of 80-90° C. for 16-20 hours.
5. The method for preparing a hygroscopic 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 weight of the rough surface fabric is 80-100g / m 2 The antibacterial nylon fiber used to prepare the rough surface fabric is the same as the antibacterial nylon fiber used to prepare the rough inner fabric.
6. The method for preparing a hygroscopic and antibacterial layered composite fabric according to claim 1, characterized in that: In the step 2, the modified cotton fiber is prepared by the following steps: The cotton fiber is mixed with a sodium periodate aqueous solution, reacted, filtered, washed, and dried after the reaction is completed to obtain the aldehyde-modified cotton fiber; 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; the reaction conditions are: reacting in a light-proof environment at a temperature of 40-60° C. for 4-6 hours; The amino-terminated hyperbranched polymer, 2,3-epoxypropyltrimethylammonium chloride and water are mixed and reacted. After the reaction is completed, an antibacterial finishing liquid is obtained. The formaldehyde-modified cotton fiber and the antibacterial finishing liquid are mixed and continued to react. After the reaction is completed, the modified cotton fiber is filtered, washed and dried to obtain the modified cotton fiber. 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 70-80°C for 5-10 minutes; the mass ratio of the formaldehyde-modified cotton fiber and the antibacterial finishing liquid is 1:20-30; and the continued reaction conditions are: continuing the reaction at 60-80°C for 45-60 minutes.
7. The method for preparing a hygroscopic 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%.
8. The method for preparing a hygroscopic and antibacterial layered composite fabric according to claim 1, characterized in that: In step 3, the finishing liquid is prepared by the following steps: N,N,N',N'-tetramethyl-1,6-hexanediamine acetate, polyetheramine, isopropanol, and 1,3-bis(3-glycidyloxypropyl)tetramethyldisiloxane are uniformly mixed and reacted. After the reaction is completed, the solvent isopropanol is removed by rotary evaporation to obtain a quaternary ammonium polyetheramine; The first catalyst is added to the quaternary ammonium 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 to continue the reaction. After the reaction is completed, vacuum is evacuated and the reaction is kept warm. After the reaction is completed, a finishing agent is obtained; the finishing agent is mixed with water to obtain a finishing liquid.
9. The method for preparing a hygroscopic and antibacterial layered composite fabric according to claim 8, characterized in that: In the preparation of the finishing solution: The molar ratio of N,N,N',N'-tetramethyl-1,6-hexanediamine acetate, polyetheramine, isopropanol, and 1,3-bis(3-glycidyloxypropyl)tetramethyldisiloxane is 1:2.5-3:3-4:2; when preparing the quaternary ammonium polyetheramine, the reaction conditions are: reacting at a temperature of 80-90°C for 3-5h; The mass ratio of quaternary ammonium 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 the first catalyst and the second catalyst are both phosphorous acid; the first catalyst is added under the condition of adding the first catalyst to the quaternary ammonium polyetheramine at a temperature of 210-220°C in a nitrogen atmosphere; when preparing the finishing agent, the reaction conditions are as follows: reacting for 3-4 hours at a temperature of 220-230°C in a nitrogen atmosphere; the continued reaction conditions are as follows: continuing the reaction for 3-4 hours at a temperature of 230-240°C in a nitrogen atmosphere; the heat preservation reaction conditions are as follows: heat preservation reaction for 1-2 hours at a vacuum degree of 10Pa and a temperature of 235-240°C; the mass ratio of the finishing agent to water is 1-1.5:
10.
10. A hygroscopic and antibacterial layered composite fabric prepared by the method for preparing a hygroscopic and antibacterial layered composite fabric as claimed in any one of claims 1 to 9.
Citation Information
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