Antibacterial waterproof multilayer non-woven fabric and preparation process thereof

Abstract

The invention discloses an antibacterial waterproof multilayer non-woven fabric and a preparation process thereof, and relates to the technical field of non-woven fabrics. The antibacterial property and hydrophobicity of the organosilicon long-chain quaternary ammonium salt are compounded with the chitosan, the non-woven fabric is endowed with softness and antibacterial property, then the organosilicon long-chain quaternary ammonium salt is mixed with the nano ZnO to form a coordinate bond, the adhesive force of the nano ZnO on the surface of the non-woven fabric is enhanced, the nano ZnO is not prone to falling off, hydroxyl in the quaternized chitosan and carbonyl in spandex form hydrogen bonding, and the antibacterial property of the non-woven fabric is improved. The mechanical strength of the non-woven fabric is enhanced; the preparation method comprises the following steps: introducing vinyl into long-chain silane, and then copolymerizing with octadecyl methacrylate and the like to obtain a waterproof emulsion; the vinyl can permeate into the fibers to form crosslinking, the organic silicon has umbrella-shaped molecular arrangement, a more uniform and compact waterproof film can be formed on the surface of the non-woven fabric, moisture permeation is effectively prevented, and the waterproof performance of the non-woven fabric is improved.

Description

Technical Field

[0001] The present invention relates to the technical field of non-woven fabrics, and specifically to an antibacterial and waterproof multi-layer non-woven fabric and its preparation process. Background Art

[0002] Non-woven fabrics are also known as non-woven cloth, needle-punched cotton, needle-punched non-woven fabrics, etc., which are made of polyester, nylon or polypropylene fibers, and can be made into different hardnesses and thicknesses according to different requirements. Due to the characteristics of non-woven fabrics such as moisture-proof, light, breathable, non-toxic, odorless, inexpensive and easy to obtain, recyclable, etc., they are widely used in different industries, such as medical, clothing, sound insulation, heat insulation, etc.

[0003] Antibacterial and waterproof non-woven fabrics are widely used in the medical and health fields. In the prior art, the functions of single-layer non-woven fabrics are relatively single and the mechanical properties are poor.

[0004] Therefore, we propose an antibacterial and waterproof multi-layer non-woven fabric and its preparation process. Summary of the Invention

[0005] The purpose of the present invention is to provide an antibacterial and waterproof multi-layer non-woven fabric and its preparation process to solve the problems raised in the prior art.

[0006] To achieve the above purpose, the present invention provides the following technical solution: an antibacterial and waterproof multi-layer non-woven fabric, including an antibacterial layer, a waterproof layer and a skin-friendly layer, the antibacterial layer is located between the skin-friendly layer and the waterproof layer, forming a three-layer structure of skin-friendly layer - antibacterial layer - waterproof layer;

[0007] The antibacterial layer is obtained by impregnating non-woven fabric in an antibacterial solution; the waterproof layer is obtained by impregnating non-woven fabric in a waterproof emulsion;

[0008] The skin-friendly layer is a cotton spunlace non-woven fabric.

[0009] Further, the antibacterial solution includes the following components: chitosan, dimethyloctadecyl [3-(trimethoxysilyl)propyl] ammonium chloride, phenol;

[0010] The waterproof emulsion includes the following components: vinyltriethoxysilane, cetyltrimethoxysilane, octadecyl methacrylate, 2-hydroxyethyl acrylate, butyl acrylate, methyl methacrylate.

[0011] A preparation process of an antibacterial and waterproof multi-layer non-woven fabric includes the following steps:

[0012] Step (1): Put the non-woven fabric into the antibacterial solution, impregnate and finish, and bake to obtain the antibacterial layer. Put the non-woven fabric into the waterproof emulsion, impregnate and finish, and bake to obtain the waterproof layer;

[0013] Step (2): Level the skin-friendly layer, antibacterial layer and waterproof layer, and perform ultrasonic lamination to form a three-layer structure of skin-friendly layer - antibacterial layer - waterproof layer, obtaining the antibacterial and waterproof multi-layer non-woven fabric.

[0014] Further, in step (1), the bath ratio of the non-woven fabric to the antibacterial solution is 1:(5 - 8);

[0015] The bath ratio of the non-woven fabric to the waterproof emulsion is 1:(5 - 8).

[0016] Further, in step (1), the process conditions for impregnation finishing are: temperature 45 - 65°C, time 40 - 60 min;

[0017] The process conditions for baking are: temperature 100 - 150°C, time 1 - 3 min.

[0018] Further, in step (2), the process conditions for ultrasonic lamination are: frequency 1 - 3 KHz, amplitude 40 - 80%.

[0019] Further, the non-woven fabric is made by blending spandex fiber and polyester fiber, and the specific process is as follows:

[0020] Lay the polyester fiber and spandex fiber evenly in a mass ratio of 1:1 to obtain a composite fiber web, and then perform needle punching reinforcement to obtain the non-woven fabric.

[0021] Further, the needle punching density is 10000 - 15000 punches / m 2 ;

[0022] The obtained non-woven fabric has a gram weight of 55 - 75 g / m 2 , and a thickness of 1.0 - 2.0 mm.

[0023] Further, the antibacterial solution is prepared by the following process:

[0024] S1: Mix nano-ZnO (zinc oxide) with deionized water and perform ultrasonic dispersion to obtain a nano-ZnO dispersion;

[0025] S2: Mix chitosan, deionized water and isopropanol to obtain a mixture, heat it in a water bath, add NaOH (sodium hydroxide) solution, stir evenly, then add dimethyloctadecyl [3-(trimethoxysilyl)propyl] ammonium chloride, stir and react, adjust the pH to neutral, add phenol solution, heat up and react, and then add the nano-ZnO dispersion to obtain the antibacterial solution.

[0026] Further, in S1, the mass ratio of nano-ZnO to deionized water is 1:(50 - 100).

[0027] Further, in S1, the process conditions for ultrasonic dispersion are: power 200 - 400 w, time 0.5 - 1 h.

[0028] Further, in S2, the ratio of chitosan, deionized water and isopropanol is 1 g:(5 - 15) mL:(10 - 20) mL;

[0029] The mass ratio of the mixture, NaOH solution, dimethyloctadecyl[3-(trimethoxysilyl)propyl]ammonium chloride, phenol solution and nano-ZnO dispersion is 1:(0.05 - 0.1):(0.5 - 1):(0.1 - 0.3):(0.05 - 0.15).

[0030] Further, in S2, the process conditions for water bath heating are: temperature 65 - 85°C, time 0.5 - 1 h;

[0031] The process conditions for stirring reaction are: rotation speed 50 - 80 r / min, time 24 - 48 h;

[0032] The process conditions for heating-up reaction are: temperature 40 - 60°C, time 12 - 24 h.

[0033] Further, in S2, the phenol solution is prepared by the following process:

[0034] Dissolve phenol in absolute ethanol, cool down to 0°C, and add EDC (ethyl-(3-dimethylaminopropyl)carbodiimide) to obtain the phenol solution.

[0035] Further, the volume ratio of phenol, absolute ethanol and EDC is 1:(30 - 50):(0.1 - 0.5).

[0036] In the above technical solution, dimethyloctadecyl[3-(trimethoxysilyl)propyl]ammonium chloride reacts with chitosan to generate quaternized chitosan. Dimethyloctadecyl[3-(trimethoxysilyl)propyl]ammonium chloride has good antibacterial properties, the long-chain alkyl group has certain hydrophobic properties, the silicon element endows the fabric with softness, and chitosan has good antibacterial properties, adsorption capacity and biocompatibility. Therefore, compounding it with quaternary ammonium salt can further improve its antibacterial properties and adhesion; then phenolic hydroxyl groups are introduced onto the quaternized chitosan. The phenolic hydroxyl groups and quaternary ammonium groups act synergistically to significantly enhance the antibacterial property, and the introduction of phenolic hydroxyl groups expands the antibacterial spectrum and increases the antibacterial range; nano-ZnO can form a layer of barrier on the surface of the non-woven fabric to further improve its antibacterial property. Quaternized chitosan can form coordination bonds with nano-ZnO to enhance the adhesion of nano-ZnO on the surface of the non-woven fabric and make it not easy to fall off;

[0037] In addition, the hydroxyl groups in quaternized chitosan form hydrogen bond bonding with the carbonyl groups in spandex and form cross-linking with the molecular chains of spandex, enhancing the mechanical strength of the non-woven fabric.

[0038] Further, the waterproof emulsion is prepared by the following process:

[0039] Step A: Mix deionized water, dodecylbenzenesulfonic acid, and sodium dodecylsulfonate, heat and stir in an oil bath, then add octamethylcyclotetrasiloxane, vinyltriethoxysilane, and cetyltrimethoxysilane, stir evenly, and carry out a heat preservation reaction to obtain a double-bond-containing silicone emulsion;

[0040] Step B: Mix deionized water, octadecyl methacrylate, 2-hydroxyethyl acrylate, butyl acrylate, methyl methacrylate, azobisisobutyronitrile, and DNS-86 (1-allyloxy-3-(4-nonylphenol)-2-propanol polyoxyethylene (10) ether ammonium sulfate), and homogenize for 20 - 30 min to obtain a mixed emulsion;

[0041] Step C: Mix deionized water, the mixed emulsion, and nano-SiO₂, carry out ultrasonic dispersion, dropwise add the double-bond-containing silicone emulsion within 2 h, and carry out a heat preservation reaction to obtain a waterproof emulsion.

[0042] Further, in Step A, the mass ratio of deionized water, dodecylbenzenesulfonic acid, sodium dodecylsulfonate, octamethylcyclotetrasiloxane, vinyltriethoxysilane, and cetyltrimethoxysilane is 10:(0.1 - 0.3):(0.05 - 0.1):(1 - 3):(0.1 - 0.3):(0.1 - 0.3).

[0043] Further, in Step A, the process conditions for heating and stirring in an oil bath are: temperature 65 - 75 °C, time 20 - 30 min, and rotation speed 250 - 350 r / min.

[0044] Further, in Step A, the process conditions for the heat preservation reaction are: temperature 65 - 75 °C, time 3 - 4 h.

[0045] Further, in Step B, the mass ratio of deionized water, octadecyl methacrylate, 2-hydroxyethyl acrylate, butyl acrylate, methyl methacrylate, azobisisobutyronitrile, and DNS-86 is 10:(1.5 - 2):(0.06 - 0.1):(1 - 3):(1 - 3):(0.03 - 0.05):(0.01 - 0.03).

[0046] Further, in Step C, the mass ratio of deionized water, the mixed emulsion, nano-SiO₂, and the double-bond-containing silicone emulsion is 10:(3 - 5):(0.1 - 0.3):(0.5 - 1).

[0047] Further, in Step C, the process conditions for ultrasonic dispersion are: power 200 - 400 w, time 0.5 - 1 h.

[0048] In the above technical solution, by introducing vinyl into the long-chain silane, an organosilicon containing double bonds is obtained, and then copolymerized with octadecyl methacrylate, etc. to obtain a waterproof emulsion; vinyl has hydrophobicity and can crosslink with the main chain of the long-chain silane to form a network structure, reducing the water penetration rate. Vinyl is not easily decomposed at high temperatures, has good stability, can form chemical bonds with the hydroxyl groups in spandex fibers, enhancing its adhesion to non-woven fabrics and making it not easy to fall off. Organosilicon has a "umbrella-shaped" molecular arrangement, which can form a more uniform and dense waterproof film on the surface of the non-woven fabric, effectively preventing water penetration while maintaining the breathability of the non-woven fabric;

[0049] Nano-SiO 2 The surface contains silanol groups, which can undergo a condensation reaction with the carboxyl and hydroxyl groups in the mixed emulsion to form Si-O-C bonds, enhancing the interfacial bonding and the mechanical properties of the non-woven fabric. And nano-SiO 2 can fill the micropores of the acrylate coating, reduce the water molecule penetration path, improve the denseness, and further improve the waterproof property of the non-woven fabric.

[0050] Compared with the prior art, the beneficial effects of the present invention are:

[0051] 1. By reacting dimethyloctadecyl [3-(trimethoxysilyl)propyl] ammonium chloride with chitosan to generate quaternized chitosan. Dimethyloctadecyl [3-(trimethoxysilyl)propyl] ammonium chloride has good antibacterial properties, the long-chain alkyl group has certain hydrophobic properties, and silicon also endows the fabric with softness. Chitosan has good antibacterial properties, adsorption capacity and biocompatibility. When it is compounded with quaternary ammonium salts, its antibacterial property and adhesion are further improved; then phenolic hydroxyl groups are introduced onto the quaternized chitosan. The phenolic hydroxyl groups and the quaternary ammonium groups act synergistically to significantly enhance the antibacterial property, and the introduction of phenolic hydroxyl groups expands the antibacterial spectrum and increases the antibacterial range;

[0052] Nano-ZnO can form a barrier on the surface of the non-woven fabric to further improve its antibacterial property. Quaternized chitosan can form a coordination bond with nano-ZnO, enhancing the adhesion of nano-ZnO on the surface of the non-woven fabric and making it not easy to fall off; in addition, the hydroxyl groups in quaternized chitosan form hydrogen bond bonding with the carbonyl groups in spandex and form crosslinking with the spandex molecular chain, enhancing the mechanical strength of the non-woven fabric.

[0053] 2. By introducing vinyl into long-chain silanes, organosilicon containing double bonds was obtained, and then copolymerized with octadecyl methacrylate, etc. to obtain a waterproof emulsion; vinyl has hydrophobicity and can crosslink with the main chain of long-chain silanes to form a network structure, reducing the water penetration rate. Vinyl is not easily decomposed at high temperatures, has good stability, can form chemical bonds with the hydroxyl groups in spandex fibers, enhancing its adhesion to non-woven fabrics and making it not easy to fall off. Organosilicon has an "umbrella-shaped" molecular arrangement, which can form a more uniform and dense waterproof film on the surface of non-woven fabrics, effectively preventing water penetration while maintaining the breathability of non-woven fabrics; nano-SiO 2 The surface contains silanol groups, which can undergo a condensation reaction with carboxyl and hydroxyl groups in the mixed emulsion to form Si-O-C bonds, enhancing the interfacial bonding and the mechanical properties of non-woven fabrics. Moreover, nano-SiO 2 can fill the micropores of acrylate coatings, reduce the water molecule penetration path, improve the density, and further improve the waterproof property of non-woven fabrics.

[0054] 3. The skin-friendly layer, antibacterial layer, and waterproof layer are bonded by ultrasonic pressing, avoiding the delamination of non-woven fabrics during use and the decrease in the breathability of non-woven fabrics caused by the use of adhesives; at the same time, a pressing mold with a grid is used to form grid-like units on the non-woven fabrics, further improving the mechanical strength of non-woven fabrics. Specific Embodiments

[0055] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only a 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 those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

[0056] In the following specific embodiments,

[0057] The skin-friendly layer is a cotton spunlace non-woven fabric, product number TY0246, sourced from Dongguan Tuoyuan Composite Technology Co., Ltd.;

[0058] Spandex fiber, 40D, sourced from Wuxi Sanjiang New Material Fiber Co., Ltd.;

[0059] Polyester fiber, 75D, sourced from Jiangsu Sanlian New Material Co., Ltd.;

[0060] Phenol, CAS No. 108-95-2, sourced from Jinan Qichen Chemical Co., Ltd.;

[0061] Absolute ethanol, CAS No. 64-17-5, sourced from Shanghai Kelong Chemical Co., Ltd.;

[0062] EDC, CAS No. 1892-57-5, sourced from Wuhan Smartbio Technology Co., Ltd.;

[0063] Nano-ZnO, CAS No. 1314-13-2, 50 nm, sourced from Fujian Ruisen New Materials Co., Ltd.;

[0064] Chitosan, CAS No. 9012-76-4, sourced from Guangdong Mingcheng Biotechnology Co., Ltd.;

[0065] Isopropyl alcohol, CAS No. 67-63-0, sourced from Nanjing Reagent;

[0066] NaOH solution, mass fraction 40%, CAS No. 1310-73-2, sourced from Nanjing Reagent;

[0067] Dimethyloctadecyl[3-(trimethoxysilyl)propyl]ammonium chloride, CAS No. 27668-52-6, sourced from Hubei Xinyuhong Biomedical Technology Co., Ltd.;

[0068] Dodecylbenzenesulfonic acid, CAS No. 27176-87-0, sourced from Shanghai Richu Biotechnology Co., Ltd.;

[0069] Sodium dodecyl sulfate, CAS No. 2386-53-0, sourced from Nanjing Reagent;

[0070] Octamethylcyclotetrasiloxane, CAS No. 556-67-2, sourced from Shandong Qiyun Chemical Technology Co., Ltd.;

[0071] Vinyltriethoxysilane, CAS No. 78-08-0, sourced from Nanjing Ron Silicon Materials Co., Ltd.;

[0072] Hexadecyltrimethoxysilane, CAS No. 16415-12-6, sourced from Wuhan Lanabai Pharmaceutical and Chemical Co., Ltd.;

[0073] Octadecyl methacrylate, CAS No. 32360-05-7, sourced from Jinan Yunuo Chemical Co., Ltd.;

[0074] 2-Hydroxyethyl acrylate, CAS No. 818-61-1, sourced from Shandong Chuangying Chemical Co., Ltd.;

[0075] Methyl methacrylate, CAS No. 80-62-6, sourced from Shandong Chuangying Chemical Co., Ltd.;

[0076] Butyl acrylate, CAS No. 141-32-2, sourced from Shandong Kejian Chemical Co., Ltd.;

[0077] 2,2'-Azobis(2-methylpropionitrile), CAS No. 78-67-1, sourced from Jinan Weizhen Chemical Co., Ltd.;

[0078] DNS-86, with CAS number 184719-88-8, is sourced from Guangzhou Shanghe Chemical Technology Co., Ltd.;

[0079] Antibacterial agent, model JF-5570, is sourced from Shandong Shoucheng Chemical Co., Ltd.;

[0080] Waterproofing agent, model TY4-1G, is sourced from Dongguan Taiyang New Material Technology Co., Ltd.

[0081] Example 1: A preparation process of an antibacterial and waterproof multi-layer non-woven fabric includes the following steps:

[0082] (1) Preparation of the antibacterial solution:

[0083] Dissolve phenol in absolute ethanol, cool down to 0°C, and add EDC to obtain a phenol solution; the volume ratio of phenol, absolute ethanol, and EDC is 1:50:0.1;

[0084] S1: Mix nano-ZnO and deionized water at a mass ratio of 1:100, and perform ultrasonic dispersion to obtain a nano-ZnO dispersion; S2: Mix chitosan, deionized water, and isopropanol in a ratio of 1 g:15 mL:20 mL to obtain a mixture, heat it in a water bath at 85°C for 1 h, add NaOH solution, stir evenly, then add dimethyloctadecyl [3-(trimethoxysilyl)propyl] ammonium chloride, stir and react at a rotation speed of 80 r / min for 48 h, adjust the pH to neutral, add the phenol solution, raise the temperature to 60°C and react for 24 h, and then add the nano-ZnO dispersion to obtain an antibacterial solution; in S1, the process conditions for ultrasonic dispersion are: power 400 w, time 1 h; in S2, the mass ratio of the mixture, NaOH solution, dimethyloctadecyl [3-(trimethoxysilyl)propyl] ammonium chloride, phenol solution, and nano-ZnO dispersion is 1:0.1:1:0.1:0.15;

[0085] (2) Preparation of the waterproof emulsion:

[0086] Step A: Mix deionized water, dodecylbenzenesulfonic acid, and sodium dodecylsulfonate, heat and stir in an oil bath, then add octamethylcyclotetrasiloxane, vinyltriethoxysilane, and cetyltrimethoxysilane, stir evenly, and keep the temperature at 75°C for 4 h to obtain a double-bond-containing silicone emulsion; Step B: Mix deionized water, stearyl methacrylate, 2-hydroxyethyl acrylate, butyl acrylate, methyl methacrylate, azobisisobutyronitrile, and DNS-86 in a mass ratio of 10:2:0.1:3:3:0.05:0.03, and homogenize for 30 min to obtain a mixed emulsion; Step C: Mix deionized water, the mixed emulsion, and nano-SiO 2Mix, disperse with ultrasonic at a power of 400 w for 1 h, add the double-bonded silicone emulsion dropwise within 2 h, and keep the temperature for reaction to obtain a waterproof emulsion; in step A, the mass ratio of deionized water, dodecylbenzenesulfonic acid, sodium dodecylsulfonate, octamethylcyclotetrasiloxane, vinyltriethoxysilane and cetyltrimethoxysilane is 10: 0.3: 0.1: 3: 0.3: 0.3; in step A, the process conditions of oil bath heating and stirring are: temperature 75 °C, time 30 min, rotation speed 350 r / min; in step C, the mass ratio of deionized water, mixed emulsion, hyperbranched nano-SiO 2 to the double-bonded silicone emulsion is 10: 5: 0.3: 1;

[0087] (3) Preparation of non-woven fabric:

[0088] Lay the polyester fiber and spandex fiber evenly according to the mass ratio of 1:1 to obtain a composite fiber web, and then carry out needling reinforcement to obtain a non-woven fabric; the needling density is 15000 needles / m 2 ; the gram weight of the obtained non-woven fabric is 75 g / m 2 , and the thickness is 2.0 mm;

[0089] (4) Preparation of multi-layer non-woven fabric:

[0090] Step (1): Put the non-woven fabric into the antibacterial solution, impregnate and finish, and bake to obtain an antibacterial layer. Put the non-woven fabric into the waterproof emulsion, impregnate and finish, and bake to obtain a waterproof layer; Step (2): Lay the skin-friendly layer, antibacterial layer and waterproof layer flat, and carry out ultrasonic pressing to form a three-layer structure of skin-friendly layer - antibacterial layer - waterproof layer to obtain an antibacterial and waterproof multi-layer non-woven fabric; in step (1), the process conditions of impregnation and finishing are: temperature 65 °C, time 60 min; the process conditions of baking are: temperature 150 °C, time 3 min; in step (1), the bath ratio of the non-woven fabric to the antibacterial solution is 1:8; the bath ratio of the non-woven fabric to the waterproof emulsion is 1:8; in step (2), the process conditions of ultrasonic pressing are: frequency 3 KHz, amplitude 80%.

[0091] Example 2: A preparation process of an antibacterial and waterproof multi-layer non-woven fabric, comprising the following steps:

[0092] (1) Preparation of antibacterial solution:

[0093] Dissolve phenol in absolute ethanol, cool down to 0 °C, and add EDC to obtain a phenol solution; the volume ratio of phenol, absolute ethanol and EDC is 1: 40: 0.25;

[0094] S1: Mix nano-ZnO and deionized water at a mass ratio of 1:75, and disperse them by ultrasonic wave to obtain a nano-ZnO dispersion; S2: Mix chitosan, deionized water and isopropanol at a ratio of 1 g:10 mL:15 mL to obtain a mixture. Heat it in a water bath at 75 °C for 0.7 h, add NaOH solution, stir evenly, then add dimethyloctadecyl [3-(trimethoxysilyl)propyl] ammonium chloride, stir and react at a speed of 65 r / min for 36 h, adjust the pH to neutral, add phenol solution, raise the temperature to 50 °C and react for 18 h, and then add the nano-ZnO dispersion to obtain an antibacterial solution; In S1, the technological conditions of ultrasonic dispersion are: power 300 w, time 0.7 h; In S2, the mass ratio of the mixture, NaOH solution, dimethyloctadecyl [3-(trimethoxysilyl)propyl] ammonium chloride, phenol solution and nano-ZnO dispersion is 1:0.07:0.7:0.2:0.1;

[0095] (2) Preparation of waterproof emulsion:

[0096] Step A: Mix deionized water, dodecylbenzenesulfonic acid and sodium dodecylsulfonate, heat and stir in an oil bath, then add octamethylcyclotetrasiloxane, vinyltriethoxysilane and cetyltrimethoxysilane, stir evenly, and keep the temperature at 70 °C for 3.5 h to obtain a double-bond-containing silicone emulsion; Step B: Mix deionized water, octadecyl methacrylate, 2-hydroxyethyl acrylate, butyl acrylate, methyl methacrylate, azobisisobutyronitrile and DNS-86 at a mass ratio of 10:1.7:0.08:2:2:0.04:0.02, and homogenize for 25 min to obtain a mixed emulsion; Step C: Mix deionized water, the mixed emulsion and nano-SiO 2 Mix them, disperse them by ultrasonic wave at a power of 300 w for 0.7 h, dropwise add the double-bond-containing silicone emulsion within 2 h, and keep the temperature for reaction to obtain a waterproof emulsion; In Step A, the mass ratio of deionized water, dodecylbenzenesulfonic acid, sodium dodecylsulfonate, octamethylcyclotetrasiloxane, vinyltriethoxysilane and cetyltrimethoxysilane is 10:0.2:0.07:2:0.2:0.2; In Step A, the technological conditions of oil bath heating and stirring are: temperature 70 °C, time 25 min, speed 300 r / min; In Step C, the mass ratio of deionized water, the mixed emulsion, hyperbranched nano-SiO 2 and the double-bond-containing silicone emulsion is 10:4:0.2:0.7;

[0097] (3) Preparation of non-woven fabric:

[0098] Evenly lay a web of polyester fiber and spandex fiber at a mass ratio of 1:1 to obtain a composite fiber web, and then carry out needle punching reinforcement to obtain a non-woven fabric; The needle punching density is 13000 needles / m 2 ; The gram weight of the obtained non-woven fabric is 65 g / m 2, with a thickness of 1.5 mm;

[0099] (4) Preparation of multi-layer non-woven fabric:

[0100] Step (1): Put the non-woven fabric into the antibacterial solution, impregnate and finish, then bake to obtain the antibacterial layer. Put the non-woven fabric into the waterproof emulsion, impregnate and finish, then bake to obtain the waterproof layer; Step (2): Lay the skin-friendly layer, antibacterial layer and waterproof layer flat, and perform ultrasonic lamination to form a three-layer structure of skin-friendly layer - antibacterial layer - waterproof layer, obtaining the antibacterial and waterproof multi-layer non-woven fabric; In step (1), the process conditions for impregnation and finishing are: temperature 55 °C, time 50 min; the process conditions for baking are: temperature 130 °C, time 2 min; In step (1), the bath ratio of the non-woven fabric to the antibacterial solution is 1:6; the bath ratio of the non-woven fabric to the waterproof emulsion is 1:6; In step (2), the process conditions for ultrasonic lamination are: frequency 3 KHz, amplitude 60%.

[0101] Example 3: A preparation process of an antibacterial and waterproof multi-layer non-woven fabric, including the following steps:

[0102] (1) Preparation of antibacterial solution:

[0103] Dissolve phenol in absolute ethanol, cool down to 0 °C, and add EDC to obtain a phenol solution; the volume ratio of phenol, absolute ethanol to EDC is 1:30:0.1;

[0104] S1: Mix nano-ZnO and deionized water according to a mass ratio of 1:50, and perform ultrasonic dispersion to obtain a nano-ZnO dispersion; S2: Mix chitosan, deionized water and isopropanol in a ratio of 1 g:5 mL:10 mL to obtain a mixture, heat it in a water bath at 65 °C for 0.5 h, add NaOH solution, stir evenly, then add dimethyloctadecyl [3-(trimethoxysilyl)propyl] ammonium chloride, stir and react at a rotation speed of 50 r / min for 24 h, adjust the pH to neutral, add the phenol solution, raise the temperature to 40 °C and react for 12 h, then add the nano-ZnO dispersion to obtain the antibacterial solution; In S1, the process conditions for ultrasonic dispersion are: power 200 w, time 0.5 h; In S2, the mass ratio of the mixture, NaOH solution, dimethyloctadecyl [3-(trimethoxysilyl)propyl] ammonium chloride, phenol solution to nano-ZnO dispersion is 1:0.05:0.5:0.3:0.05;

[0105] (2) Preparation of waterproof emulsion:

[0106] Step A: Mix deionized water, dodecylbenzenesulfonic acid, and sodium dodecylsulfonate, heat and stir in an oil bath, then add octamethylcyclotetrasiloxane, vinyltriethoxysilane, and cetyltrimethoxysilane, stir evenly, and keep the reaction at 65 °C for 3 h to obtain a double-bond-containing silicone emulsion; Step B: Mix deionized water, stearyl methacrylate, 2-hydroxyethyl acrylate, butyl acrylate, methyl methacrylate, azobisisobutyronitrile, and DNS-86 according to a mass ratio of 10:1.5:0.06:1:1:0.03:0.01, and homogenize for 20 min to obtain a mixed emulsion; Step C: Mix deionized water, the mixed emulsion, and nano-SiO 2 and ultrasonically disperse at a power of 200 w for 0.5 h, and add the double-bond-containing silicone emulsion dropwise within 2 h, then keep the reaction to obtain a waterproof emulsion; In Step A, the mass ratio of deionized water, dodecylbenzenesulfonic acid, sodium dodecylsulfonate, octamethylcyclotetrasiloxane, vinyltriethoxysilane, and cetyltrimethoxysilane is 10:0.1:0.05:1:0.1:0.1; In Step A, the process conditions for oil bath heating and stirring are: temperature 65 °C, time 20 min, rotation speed 250 r / min; In Step C, the mass ratio of deionized water, the mixed emulsion, hyperbranched nano-SiO 2 and the double-bond-containing silicone emulsion is 10:3:0.1:0.5;

[0107] (3) Preparation of non-woven fabric:

[0108] Evenly lay the polyester fiber and spandex fiber in a mass ratio of 1:1 to obtain a composite fiber web, and then carry out needle punching reinforcement to obtain a non-woven fabric; The needle punching density is 10000 needles / m 2 ; The gram weight of the obtained non-woven fabric is 55 g / m 2 , and the thickness is 1.0 mm;

[0109] (4) Preparation of multi-layer non-woven fabric:

[0110] Step (1): Put the non-woven fabric into an antibacterial solution, impregnate and finish, and bake to obtain an antibacterial layer. Put the non-woven fabric into a waterproof emulsion, impregnate and finish, and bake to obtain a waterproof layer; Step (2): Lay the skin-friendly layer, antibacterial layer, and waterproof layer flat and carry out ultrasonic lamination to form a three-layer structure of skin-friendly layer - antibacterial layer - waterproof layer to obtain an antibacterial and waterproof multi-layer non-woven fabric; In Step (1), the process conditions for impregnation and finishing are: temperature 45 °C, time 40 min; The process conditions for baking are: temperature 100 °C, time 1 min; In Step (1), the bath ratio of the non-woven fabric to the antibacterial solution is 1:5; The bath ratio of the non-woven fabric to the waterproof emulsion is 1:5; In Step (2), the process conditions for ultrasonic lamination are: frequency 3 KHz, amplitude 40%.

[0111] Comparative Example 1: Compared with Example 1, replace the antibacterial solution with a commercially available antibacterial agent, and keep the other conditions unchanged.

[0112] Comparative Example 2: Compared with Example 1, the waterproof emulsion was replaced with a commercially available waterproofing agent, and the other conditions remained unchanged.

[0113] Comparative Example 3: Compared with Example 1, the antibacterial solution was replaced with a commercially available antibacterial agent, and at the same time the waterproof emulsion was replaced with a commercially available waterproofing agent, and the other conditions remained unchanged.

[0114] Experiment: Take the non-woven fabrics in Examples 1 to 3 and Comparative Examples 1 to 3, and conduct various performance tests on them;

[0115] Antibacterial performance test: According to "GB / T20944.3-2008", the antibacterial performance of the non-woven fabric was detected;

[0116] Waterproof performance test: Referring to GB / T 4745—2012 "Textiles - Determination of waterproof performance - Spray test", the waterproof performance of the non-woven fabric was tested;

[0117] Mechanical property test: Cut the non-woven fabrics in Examples 1 to 3 and Comparative Examples 1 to 3 into samples of 10 cm × 20 cm, use a universal testing machine to conduct mechanical property tests, the test speed is 10 mm / min, and the average value is taken after testing each sample 3 times;

[0118] The following table shows the test results of each performance of the non-woven fabric;

[0119]

[0120] Based on the data in the above table, the following conclusions can be obtained:

[0121] Comparing the non-woven fabrics obtained in Examples 1 to 3 with those in Comparative Examples 1 to 3, the test results show that

[0122] Compared with Example 1, in Comparative Example 1, the antibacterial solution was replaced with a commercially available antibacterial agent, and its antibacterial ability and elongation at break decreased significantly, and the antibacterial rate decreased more after washing. The reason is that the commercially available antibacterial agent has a weak adhesion ability to the non-woven fabric and cannot form cross-links with the fibers, reducing the mechanical properties of the non-woven fabric;

[0123] Compared with Example 1, in Comparative Example 2, the waterproof emulsion was replaced with a commercially available waterproofing agent, and its waterproof grade and elongation at break decreased significantly. The reason is that the commercially available waterproofing agent does not contain vinyl and nano-SiO 2 , the cross-linking ability with the fibers decreased, and there was a lack of nano-particles to fill the micropores, and the waterproof film was not dense enough, resulting in a decrease in the waterproof grade;

[0124] Compared with Example 1, in Comparative Example 3, the antibacterial solution was replaced with a commercially available antibacterial agent, and at the same time, the waterproof emulsion was replaced with a commercially available waterproof agent. The antibacterial performance, waterproof performance and elongation at break all decreased significantly, indicating that the process and material settings of the present application can promote the improvement of the antibacterial, waterproof and mechanical properties of non-woven fabrics.

[0125] For those skilled in the art, it is obvious that the present invention is not limited to the details of the above exemplary embodiments, and the present invention can be implemented in other specific forms without departing from the spirit or basic characteristics of the present invention. Therefore, from any point of view, the embodiments should be regarded as exemplary and non-limiting. The scope of the present invention is defined by the appended claims rather than the above description. Therefore, all changes falling within the meaning and scope of the equivalent elements of the claims are intended to be included in the present invention.

Claims

1. An antibacterial and waterproof multi-layer non-woven fabric, characterized in that: It includes an antibacterial layer, a waterproof layer and a skin-friendly layer, wherein the antibacterial layer is located between the skin-friendly layer and the waterproof layer to form a three-layer structure of skin-friendly layer-antibacterial layer-waterproof layer; The antibacterial layer is obtained by dipping the non-woven fabric in an antibacterial solution; the waterproof layer is obtained by dipping the non-woven fabric in a waterproof emulsion; The skin-friendly layer is made of pure cotton spunlace nonwoven fabric.

2. The antibacterial and waterproof multi-layer nonwoven fabric according to claim 1, characterized in that: The antibacterial solution comprises the following components: chitosan, dimethyloctadecyl[3-(trimethoxysilyl)propyl]ammonium chloride, and phenol; The waterproof emulsion comprises the following components: vinyl triethoxysilane, hexadecyl trimethoxysilane, octadecyl methacrylate, hydroxyethyl acrylate, butyl acrylate and methyl methacrylate.

3. A process for preparing an antibacterial and waterproof multi-layer non-woven fabric, characterized in that: The following steps are involved: Step (1): placing the non-woven fabric in an antibacterial solution, dipping and finishing, and baking to obtain an antibacterial layer; placing the non-woven fabric in a waterproof emulsion, dipping and finishing, and baking to obtain a waterproof layer; Step (2): Flatten the skin-friendly layer, the antibacterial layer and the waterproof layer, and perform ultrasonic pressing to form a three-layer structure of skin-friendly layer-antibacterial layer-waterproof layer to obtain an antibacterial and waterproof multi-layer non-woven fabric.

4. The process for preparing an antibacterial and waterproof multi-layer nonwoven fabric according to claim 3, characterized in that: The antibacterial solution is prepared by the following process: S1: Mixing nano ZnO with deionized water and performing ultrasonic dispersion to obtain nano ZnO dispersion; S2: Chitosan, deionized water and isopropanol are mixed to obtain a mixture, heated in a water bath, NaOH solution is added, stirred evenly, dimethyloctadecyl[3-(trimethoxysilyl)propyl]ammonium chloride is added, stirred to react, the pH is adjusted to neutral, phenol solution is added, the temperature is raised to react, and nano ZnO dispersion is added to obtain an antibacterial solution.

5. The process for preparing an antibacterial and waterproof multi-layer nonwoven fabric according to claim 3, characterized in that: The waterproof emulsion is prepared by the following process: Step A: deionized water, dodecylbenzenesulfonic acid and sodium dodecylsulfonate are mixed, heated in an oil bath and stirred, and then octamethylcyclotetrasiloxane, vinyltriethoxysilane and hexadecyltrimethoxysilane are added, stirred evenly, and kept warm for reaction to obtain a double bond-containing organosilicon emulsion; Step B: Mix octadecyl methacrylate, hydroxyethyl acrylate, butyl acrylate, methyl methacrylate, azobisisobutyronitrile and DNS-86, and homogenize for 20 to 30 minutes to obtain a mixed emulsion; Step C: Deionized water, mixed emulsion and nano-SiO2 are mixed, ultrasonically dispersed, double-bond organic silicon emulsion is added dropwise within 2 hours, and the mixture is heated to react to obtain a waterproof emulsion.

6. The process for preparing an antibacterial and waterproof multi-layer nonwoven fabric according to claim 3, characterized in that: The non-woven fabric is made by blending spandex fiber and polyester fiber, and the specific process is as follows: Polyester fiber and spandex fiber are evenly laid in a mass ratio of 1:1 to obtain a composite fiber web, which is then reinforced by needle punching to obtain a non-woven fabric.

7. The process for preparing an antibacterial and waterproof multi-layer nonwoven fabric according to claim 3, characterized in that: In step (1), the process conditions for impregnation finishing are: temperature 45-65° C., time 40-60 min; The baking process conditions are: temperature 100-150°C, time 1-3 minutes.

8. The process for preparing an antibacterial and waterproof multi-layer nonwoven fabric according to claim 3, characterized in that: In step (2), the process conditions of ultrasonic pressing are: frequency 1 to 3 kHz, amplitude 40 to 80%.

9. The process for preparing an antibacterial and waterproof multi-layer nonwoven fabric according to claim 4, characterized in that: In S1, the mass ratio of nano ZnO to deionized water is 1:(50-100); In S2, the ratio of chitosan, deionized water, and isopropanol is 1 g: (5-15) mL: (10-20) mL; The mass ratio of the mixed agent, NaOH solution, dimethyloctadecyl[3-(trimethoxysilyl)propyl]ammonium chloride, phenol solution and nano ZnO dispersion is 1:(0.05-0.1):(0.5-1):(0.1-0.3):(0.05-0.15).

10. The process for preparing an antibacterial and waterproof multi-layer nonwoven fabric according to claim 6, characterized in that: The acupuncture density is 10000-15000 punctures / m 2 ; The nonwoven fabric has a grammage of 55-75 g / m 2 , thickness is 1.0~2.0mm.

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