Antibacterial anti-mite fabric suitable for processing bedding articles and preparation method of antibacterial anti-mite fabric
By modifying chitosan with silane and coating it with zinc oxide, a stable three-dimensional network structure is formed, which solves the shortcomings of existing antibacterial and anti-mite fabrics in terms of washability, safety and softness and comfort, and achieves stable antibacterial and anti-mite effect and soft hand feel.
Patent Information
- Application Number
- CN202511888616.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-15
- Publication Date
- 2026-02-10
AI Technical Summary
Existing antibacterial and anti-mite fabrics are inadequate in terms of washability, material safety, and softness and comfort, making it difficult to maintain the stability of both highly effective antibacterial and anti-mite effects.
A finishing method using silane-modified chitosan and zinc oxide coating was adopted. A stable three-dimensional network structure was formed through electrostatic adsorption and cross-linking. Combined with the synergistic antibacterial system of chitosan and zinc oxide, the chemical bonding strength of the fiber surface and the uniform distribution of the finishing solution were improved.
It significantly improves the antibacterial and anti-mite properties of the fabric, enhances its washability and safety, while maintaining a soft and comfortable feel and reducing the chance of microbial adhesion.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of fabric processing technology, specifically to an antibacterial and anti-mite fabric suitable for bedding processing and its preparation method. Background Technology
[0002] With increasing health awareness and stricter hygiene standards for home textiles, the demand for bedding with antibacterial and anti-mite functions is growing rapidly. To achieve these effects, fabrics are mostly finished with functional finishing agents that have bio-inhibitory properties. Commonly used antibacterial components include quaternary ammonium salts, chitosan derivatives, metal ions, and organic antibacterial agents. Anti-mite finishing often uses pyrethroid agents, plant extracts, fatty acid esters, and other active ingredients. To improve the bonding stability between the finishing agent and the fiber, common modification methods include: using resin-based crosslinking agents to build a network structure on the fiber surface, using cationic modification to improve fiber adsorption performance, using microencapsulation to achieve slow release and wash resistance, and using plasma treatment or ozone treatment to improve fiber surface activity. These methods enhance antibacterial and anti-mite functions to a certain extent, leading to the gradual maturation of the functional bedding market.
[0003] Currently, although antibacterial and anti-mite fabric technology is relatively mature, it still has many shortcomings. First, the washing durability of quaternary ammonium salts, organic antibacterial agents, and pyrethroid agents is generally poor. They are easily migrated or detached during washing and friction, leading to a rapid decline in antibacterial and anti-mite effects. This is because these finishing agents mostly rely on physical adsorption or weak bond binding, making it difficult for them to remain stable for a long time. Second, although metal antibacterial agents such as silver ions and copper ions have good antibacterial properties, they are expensive, prone to aggregation leading to poor dispersibility, and may even cause discoloration and pose safety hazards such as skin sensitivity. In addition, although microcapsule encapsulation can prolong the finishing effect, it can easily cause the fabric to feel stiff and reduce breathability. Moreover, the processing technology is complex and expensive. Although plasma or ozone treatment can improve the surface activity of fibers, the equipment investment is large, the uniformity of treatment is limited, and there is potential damage to some fibers.
[0004] Overall, existing technologies generally struggle to balance high-efficiency antibacterial properties, mite prevention, washability, material safety, and softness and comfort, limiting their effectiveness and stability in long-term use of bedding. Therefore, a solution is proposed. Summary of the Invention
[0005] The purpose of this invention is to provide an antibacterial and anti-mite fabric suitable for bedding processing and its preparation method, in order to solve the technical problem that the antibacterial and anti-mite properties of fabrics in the prior art need to be further improved.
[0006] The objective of this invention can be achieved through the following technical solution: a method for preparing an antibacterial and anti-mite fabric suitable for bedding processing, comprising the following steps:
[0007] S1. Place silane-modified chitosan and deionized water in a reaction vessel and stir. Add an aqueous acetic acid solution and stir at room temperature for 30-50 minutes to obtain the chitosan component.
[0008] S2. Place the coated zinc oxide, deionized water and fatty alcohol polyoxyethylene ether in a reaction vessel, stir evenly, add chitosan component, polyethylene glycol diglycidyl ether and softener, stir for 15-30 minutes to obtain antibacterial and anti-mite finishing liquid.
[0009] The preparation reaction principle of the antibacterial and anti-mite finishing solution is as follows:
[0010] During the reaction, silane-modified chitosan is placed in deionized water and stirred to swell. The acidity of the system is adjusted by adding acetic acid aqueous solution dropwise to completely dissolve the chitosan and form a clear and transparent chitosan component. In step S2, coated zinc oxide, deionized water and fatty alcohol polyoxyethylene ether are mixed in a reaction vessel to fully disperse the zinc oxide particles in the aqueous phase. The stability and wettability are improved by using nonionic surfactants. Then, the chitosan component is added, along with polyethylene glycol diglycidyl ether as a crosslinking agent and softener. The antibacterial and anti-mite finishing liquid is obtained by stirring for a short time.
[0011] S3. Place sodium hydroxide, wetting agent, stabilizer and deionized water in a reaction vessel, add the base fabric for impregnation, heat the reaction vessel to 80-90℃, impregnate for 30-60min, and then perform post-treatment to obtain the pretreated base fabric.
[0012] The reaction principle for preparing the pretreated base fabric is as follows:
[0013] In order to improve the bonding ability between the base fabric and the finishing agent during the reaction process, sodium hydroxide, wetting agent, stabilizer and deionized water are mixed to prepare an alkaline pretreatment bath. The base fabric is immersed in the bath at 80-90℃ for 30-60 minutes. The sizing, oil and impurities on the fiber surface are removed by alkaline boiling, so that the hydroxyl groups in the base fabric are exposed and can more easily adsorb the subsequent functional finishing liquid, thus obtaining the pretreated base fabric.
[0014] S4. The pretreated substrate is immersed in an antibacterial and anti-mite finishing solution and subjected to double immersion and double rolling. The post-treatment yields an antibacterial and anti-mite fabric.
[0015] The reaction principle for preparing antibacterial and anti-mite fabrics is as follows:
[0016] During the reaction, the hydroxyl groups on the surface of the pretreated base fabric, after alkali treatment, are exposed and their hydrophilicity is enhanced, giving it good wetting and adsorption capabilities for antibacterial and anti-mite finishing liquid. Chitosan cationic segments are adsorbed onto the fiber surface and inside the pores through electrostatic interactions, hydrogen bonds, and van der Waals forces. At the same time, zinc oxide coated with an organic shell is embedded into the polymer network. Double dip and double squeegee further penetrate and replenish the finishing liquid inside the fiber, ensuring the uniform amount and distribution of functional components. In the subsequent drying stage, the epoxy groups in polyethylene glycol diglycidyl ether undergo ring-opening addition reactions with the hydroxyl groups on the fiber, the hydroxyl groups on the chitosan molecules, and the amino groups under heating conditions to form ether bonds, constructing a three-dimensional cross-linked network of base fabric fiber-chitosan-crosslinking agent. Meanwhile, the silane-modified silane on the chitosan is hydrolyzed to generate silanol, which then condenses with the hydroxyl groups on the fiber to form Si-OC bonds, and condenses with each other to form a local Si-O-Si network structure, significantly improving the chemical bonding strength between the chitosan film layer and the fiber surface.
[0017] Further, in step S1, the ratio of the amount of silane-modified chitosan, deionized water, and acetic acid aqueous solution is 8-10g:300-500mL:25-35mL, and the concentration of the acetic acid aqueous solution is 0.5-1.0mol / L; in step S2, the ratio of the amount of the coating zinc oxide, deionized water, fatty alcohol polyoxyethylene ether, chitosan component, polyethylene glycol diglycidyl ether, and softener is 4-6g:900-1100mL:1-3g:8-10g:3-5g:15-20g, and the softener is an amino-modified silicone emulsion;
[0018] Further, in step S3, the ratio of sodium hydroxide, wetting agent, stabilizer and deionized water is 2-4g:1-3g:3-5g:800-1000mL, the impregnation ratio is 1:28-32, the base fabric is cotton fabric, the wetting agent is isomeric tridecyl alcohol polyoxyethylene ether, the stabilizer is silicone oil Goon836, and the post-treatment step includes: after the reaction is completed, removing excess alkali solution from the base fabric by rolling, and drying the base fabric in an oven at a temperature of 90-100℃ for 4-6 hours to obtain a pretreated base fabric;
[0019] Furthermore, in step S4, the roll-off rate of the double dip and double roll is 60-80%, the dip ratio is 1:30-32, and the post-treatment step includes: after the reaction is completed, the substrate is dried in an oven at a temperature of 90-100℃ for 4-6 hours to obtain an antibacterial and anti-mite fabric.
[0020] Furthermore, the silane-modified chitosan is prepared by the following steps:
[0021] A1. Chitosan, deionized water and acetic acid are placed in a reaction vessel under nitrogen atmosphere protection and stirred at room temperature for 2-4 hours. Sodium hydroxide aqueous solution is added to adjust the pH of the system to 4.5-5.5. Chloroacetic acid is added and reacted at room temperature for 2-4 hours. Carboxylated chitosan is obtained after post-treatment.
[0022] A2. Carboxylated chitosan, ethanol, and deionized water were placed in a reaction vessel, and an aqueous acetic acid solution was added to adjust the pH of the system to 4.5-5.5. A silane coupling agent solution was added dropwise, and the reaction was carried out at room temperature for 3-6 hours. The silane-modified chitosan was obtained after post-treatment.
[0023] The reaction principle for preparing silane-modified chitosan is as follows:
[0024] During the reaction, chitosan dissolves in a weakly acidic environment. Chloroacetic acid undergoes nucleophilic substitution with the amino and hydroxyl groups on the chitosan molecular chain under pH 4.5-5.5 conditions, introducing carboxyl groups to obtain carboxylated chitosan with multiple functional groups such as amino, carboxyl, and hydroxyl groups. Subsequently, in A2, the silane coupling agent hydrolyzes in an ethanol-water system to generate active Si-OH groups, which undergo condensation reactions with the hydroxyl and amino groups on the carboxylated chitosan chain under weakly acidic conditions to form stable Si-OC or local Si-O-Si bonds, allowing the silane groups to be grafted onto the surface of the chitosan molecules, resulting in silane-modified chitosan.
[0025] Further, in step A1, the ratio of chitosan, deionized water, acetic acid and chloroacetic acid is 8-10g:400-600mL:1-3mL:5-10g, the concentration of sodium hydroxide aqueous solution is 10-20wt%, and the post-treatment steps include: after the reaction is completed, adding 1-3wt% sodium hydroxide aqueous solution to adjust the pH of the reaction solution to neutral, after the precipitate is formed, filtering, washing the filter cake with deionized water 2-4 times, transferring it to an oven at a temperature of 50-60℃, drying it to constant weight, and obtaining carboxylated chitosan;
[0026] Further, in step A2, the ratio of carboxylated chitosan, ethanol, deionized water, and silane coupling agent solution is 8-10g:150-200mL:20-40mL:2-4mL. The silane coupling agent solution is a 50-70wt% γ-methacryloxypropyltrimethoxysilane ethanol solution, and the concentration of the acetic acid aqueous solution is 0.5-1.0mol / L. The post-treatment steps include: after the reaction is completed, wait for the reaction to cool to room temperature, filter, wash the filter cake 2-4 times with deionized water and ethanol, transfer it to an oven at 50-60℃, and dry it to constant weight to obtain silane-modified chitosan.
[0027] Furthermore, the coated zinc oxide is prepared by the following steps:
[0028] B1. Place zinc oxide, deionized water and ethanol in a reaction vessel and stir. Add ammonia water and stir at room temperature for 1-2 hours. Post-treatment yields activated zinc oxide.
[0029] B2. Place acrylic acid, butyl acrylate and 1,4-butanediol diacrylate in a reaction vessel and stir until homogeneous to obtain a mixed monomer;
[0030] B3. Place activated zinc oxide in a reaction vessel and stir. Slowly add mixed monomers and ammonium persulfate solution. Heat the reaction vessel to 50-60℃ and keep it at that temperature for 0.5-1h. Post-process to obtain coated zinc oxide.
[0031] The reaction principle for preparing coated zinc oxide is as follows:
[0032] During the reaction, zinc oxide, deionized water, and ethanol are placed together in a reaction vessel. Ammonia is introduced under stirring to allow the system to react in an alkaline environment for 1-2 hours, causing partial formation of -OH or Zn-NH3 on the surface of the zinc oxide particles. + The coordination structure is obtained to obtain activated zinc oxide. In step B2, acrylic acid, butyl acrylate and 1,4-butanediol diacrylate are added to the reactor in proportion and stirred to obtain a mixed monomer system. In step B3, activated zinc oxide is added to the reactor, and the mixed monomers and ammonium persulfate solution are slowly added under stirring conditions. The ammonium persulfate decomposes under heating conditions to generate active free radicals, which can initiate the in-situ polymerization of acrylic monomers on the surface of zinc oxide to form a polymer shell containing carboxyl or hydroxyl groups, thus obtaining organic layer modified coated zinc oxide.
[0033] Further, in step B1, the ratio of zinc oxide, deionized water, ethanol and ammonia is 2-4g:40-60mL:15-30mL:1-2mL, and the concentration of ammonia is 25-30wt%. The post-processing steps include: after the reaction is completed, the mixture is filtered, the filter cake is washed 2-4 times with deionized water and ethanol, transferred to an oven at 50-60℃, and dried to constant weight to obtain activated zinc oxide.
[0034] Furthermore, in step B2, the weight ratio of acrylic acid, butyl acrylate, and 1,4-butanediol diacrylate is 2-3:6-7:0.3-0.5;
[0035] Further, in step B3, the ratio of activated zinc oxide, mixed monomers, and ammonium persulfate solution is 10-12g:3-5g:1-2mL, and the ammonium persulfate solution is a 50-70wt% aqueous solution of ammonium persulfate. The post-processing steps include: after the reaction is completed, the mixture is filtered, the filter cake is washed 2-4 times with deionized water and ethanol, transferred to an oven at 50-60℃, dried to constant weight, and ground through a 200-mesh sieve to obtain coated zinc oxide.
[0036] The present invention also proposes an antibacterial and anti-mite fabric suitable for bedding processing, which is prepared by the above-mentioned preparation method of an antibacterial and anti-mite fabric suitable for bedding processing.
[0037] The present invention has the following beneficial effects:
[0038] 1. This invention involves treating zinc oxide with ammonia to obtain surface active sites, followed by in-situ polymerization with acrylic monomers at high temperature to coat the zinc oxide, thus obtaining coated zinc oxide. Zinc oxide itself possesses broad-spectrum antibacterial and anti-mite capabilities, which are achieved by releasing Zn... 2+ It generates reactive oxygen species and disrupts the cell membrane structure of microorganisms, exhibiting a sustained inhibitory effect on bacteria, fungi, and common dust mites. Furthermore, the coated zinc oxide obtained through activation-monomer coating-polymerization curing yields finer particles and better dispersibility. The surface coating layer enhances the stability of the particles in the aqueous phase and finishing system, allowing for more complete and uniform adsorption to the fiber interface during impregnation and finishing, achieving a higher effective loading capacity. Secondly, the acrylic acid, butyl acrylate, and crosslinking monomers in the coating layer can form a flexible and fiber-friendly polymer shell structure on the fiber surface, effectively strengthening the bond between zinc oxide and the fiber. After being jointly fixed onto the fiber surface by the chitosan component and epoxy crosslinking agent, the zinc oxide forms a more stable three-dimensional network, making it less likely to migrate and fall off during washing. This improves the antibacterial and anti-mite properties of the fabric. At the same time, the zinc oxide coating and chitosan can form a synergistic antibacterial system. The cationic properties of chitosan promote the fixation of the zinc oxide coating on the fiber surface. Meanwhile, the zinc oxide coating supplements the weak areas of chitosan against mold and mites, making the overall antibacterial and anti-mite performance reach a higher level. When applied to bedding, it can effectively reduce bacterial growth, reduce mite survival rate, and improve the hygiene, safety, and skin-friendliness of the product.
[0039] 2. In this invention, carboxylated chitosan is further subjected to a hydrolysis grafting reaction with γ-methacryloxypropyltrimethoxysilane under acidic conditions to obtain silane-modified chitosan. Chitosan itself possesses cationic and natural antibacterial properties. Its amino structure can electrostatically adsorb onto bacterial cell walls and disrupt cell membranes. Carboxylation improves the water solubility and reactivity of chitosan, enabling it to form a more stable and uniform dispersion system in the finishing solution, which is beneficial for penetrating into the fiber structure during impregnation and finishing. The silane groups can undergo hydrolysis under acidic conditions to produce active ingredients. The siloxane contains siloxane and can form Si-OC bonds with the hydroxyl groups on the surface of cellulose fibers. During the drying and curing stage, a siloxane condensation reaction occurs to generate a dense cross-linked network, which firmly fixes the chitosan to the fiber surface. This gives the fabric excellent wash resistance and overall antibacterial and anti-mite properties. The siloxane segments are flexible and hydrophobic, and can form a composite film with certain hydrophobicity and smoothness on the fiber surface. This makes the finished fabric softer to the touch and improves surface hydrophobicity, reducing the chance of microbial adhesion, thereby further enhancing the antibacterial and anti-mite effects.
[0040] 3. In this invention, the base fabric is further impregnated at high temperature in an aqueous solution containing sodium hydroxide, a nonionic surfactant, and silicone oil to complete the cleaning, swelling, activation, and pre-softening treatments, resulting in a pretreated base fabric. Sodium hydroxide at high temperatures can effectively saponify oils, waxes, and sizing residues on the fiber surface, deeply cleaning the fiber surface and eliminating barriers that hinder the adsorption of finishing agents. Simultaneously, alkaline treatment causes moderate swelling of cellulose, opening the microporous structure of the fiber surface, exposing more hydroxyl groups, and increasing the binding sites for subsequent chitosan, epoxy crosslinking agents, and coated zinc oxide. Furthermore, isomeric tridecyl alcohol polyoxyethylene ether, as a highly efficient nonionic surfactant... Surfactants further emulsify impurities and enhance fiber hydrophilicity, allowing the finishing solution to penetrate the fiber more evenly. This ensures a stable and consistent application of antibacterial and anti-mite components. The silicone oil Goon836 in the pretreatment system forms a preliminary lubricating film on the fiber surface during cleaning, reducing fiber hardening caused by alkali treatment. This lays the foundation for the softness and skin-friendliness of the final finished product. The pretreated base fabric has increased liquid absorption, surface energy, and fully exposed active sites, allowing the chitosan membrane and coated zinc oxide to be more firmly and evenly fixed to the fiber surface, thereby significantly enhancing the antibacterial and anti-mite effects and wash resistance. Detailed Implementation
[0041] The technical solution of the present invention will be clearly and completely described below with reference to the embodiments. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0042] The chitosan used in this invention was purchased from Shandong Gushuo Biotechnology Co., Ltd., and the standard implemented is the national standard, with an effective ingredient content of 85%.
[0043] The zinc oxide used in this invention was purchased from Ningbo Luofei Nanotechnology Co., Ltd., and its particle size is 50-100nm.
[0044] The fatty alcohol polyoxyethylene ether used in this invention was purchased from Zhengzhou Xutai Chemical Co., Ltd., with an HLB value of 12.5 and a molecular weight of 582.81.
[0045] The amino-modified organosilicon emulsion used in this invention was purchased from Dongguan Taiyang New Material Technology Co., Ltd., model number TYW-129. The product is a hydrophilic softener and the execution standard is SO14000.
[0046] The isomeric tridecyl alcohol polyoxyethylene ether used in this invention was purchased from Greenlink (Jining) Chemical Technology Co., Ltd., model number 1307.
[0047] The silicone oil Goon836 used in this invention was purchased from Jining Fangyu Chemical Co., Ltd., and its model is Goon836.
[0048] The cotton fabric used in this invention was purchased from Huang Gongbing Fabric Shop in China Textile City, Keqiao District, Shaoxing City. The yarn count is 21*21Ne, the fabric structure is twill, and the composition is 100% cotton.
[0049] Example 1
[0050] This embodiment provides a method for preparing zinc oxide-coated antibacterial and anti-mite fabrics suitable for bedding processing, comprising the following steps:
[0051] Step I: Preparation of activated zinc oxide
[0052] Weigh 20g of zinc oxide, 400mL of deionized water and 150mL of ethanol and place them in a reaction vessel and stir. Add 10mL of 25wt% ammonia water and stir at room temperature for 1h. After the reaction is complete, filter the mixture and wash the filter cake twice with deionized water and ethanol. Transfer the cake to an oven at 50℃ and dry it to constant weight to obtain activated zinc oxide.
[0053] Step II: Preparation of mixed monomers
[0054] Weigh out 20g of acrylic acid, 60g of butyl acrylate and 3g of 1,4-butanediol diacrylate and place them in a reaction vessel. Stir well to obtain a mixed monomer.
[0055] Step III: Preparation of coated zinc oxide
[0056] Weigh 100g of activated zinc oxide and place it in a reaction vessel and stir. Slowly add 30g of mixed monomers and 10mL of 50wt% ammonium persulfate aqueous solution. Heat the reaction vessel to 50℃ and keep it at that temperature for 0.5h. After the reaction is complete, filter the mixture. Wash the filter cake twice with deionized water and ethanol. Transfer it to an oven at 50℃ and dry it to constant weight. Grind it through a 200-mesh sieve to obtain coated zinc oxide.
[0057] Example 2
[0058] This embodiment provides a method for preparing zinc oxide-coated antibacterial and anti-mite fabrics suitable for bedding processing, comprising the following steps:
[0059] Step I: Preparation of activated zinc oxide
[0060] Weigh out 30g of zinc oxide, 500mL of deionized water and 220mL of ethanol and place them in a reaction vessel and stir. Add 15mL of 27wt% ammonia water and stir at room temperature for 1.5h. After the reaction is complete, filter the mixture and wash the filter cake three times with deionized water and ethanol. Transfer the cake to an oven at 55℃ and dry it to constant weight to obtain activated zinc oxide.
[0061] Step II: Preparation of mixed monomers
[0062] Weigh out 25g of acrylic acid, 65g of butyl acrylate and 4g of 1,4-butanediol diacrylate and place them in a reaction vessel. Stir until homogeneous to obtain a mixed monomer.
[0063] Step III: Preparation of coated zinc oxide
[0064] Weigh 110g of activated zinc oxide and place it in a reaction vessel and stir. Slowly add 40g of mixed monomers and 15mL of 60wt% ammonium persulfate aqueous solution. Heat the reaction vessel to 55℃ and keep it at that temperature for 1h. After the reaction is complete, filter the mixture. Wash the filter cake three times with deionized water and ethanol. Transfer it to an oven at 55℃ and dry it to constant weight. Grind it through a 200-mesh sieve to obtain coated zinc oxide.
[0065] Example 3
[0066] This embodiment provides a method for preparing zinc oxide-coated antibacterial and anti-mite fabrics suitable for bedding processing, comprising the following steps:
[0067] Step I: Preparation of activated zinc oxide
[0068] Weigh 40g of zinc oxide, 600mL of deionized water and 300mL of ethanol and place them in a reaction vessel and stir. Add 20mL of 30wt% ammonia water and stir at room temperature for 2 hours. After the reaction is complete, filter the mixture and wash the filter cake 4 times with deionized water and ethanol. Transfer the cake to an oven at 60℃ and dry it to constant weight to obtain activated zinc oxide.
[0069] Step II: Preparation of mixed monomers
[0070] Weigh out 30g of acrylic acid, 70g of butyl acrylate and 5g of 1,4-butanediol diacrylate and place them in a reaction vessel. Stir until homogeneous to obtain a mixed monomer.
[0071] Step III: Preparation of coated zinc oxide
[0072] Weigh 120g of activated zinc oxide and place it in a reaction vessel and stir. Slowly add 50g of mixed monomers and 20mL of 70wt% ammonium persulfate aqueous solution. Heat the reaction vessel to 60℃ and keep it at that temperature for 1h. After the reaction is complete, filter the mixture. Wash the filter cake four times with deionized water and ethanol. Transfer it to an oven at 60℃ and dry it to constant weight. Grind it through a 200-mesh sieve to obtain coated zinc oxide.
[0073] Example 4
[0074] This embodiment provides a method for preparing silane-modified chitosan for antibacterial and anti-mite fabrics suitable for bedding processing, including the following steps:
[0075] Step ①: Preparation of carboxylated chitosan
[0076] Weigh out 80g of chitosan, 4000mL of deionized water and 10mL of acetic acid and place them in a reaction vessel under nitrogen atmosphere protection. Stir at room temperature for 2h, add 10wt% sodium hydroxide aqueous solution to adjust the pH of the system to 4.5, add 50g of chloroacetic acid, and react at room temperature for 2h. After the reaction is complete, add 1wt% sodium hydroxide aqueous solution to adjust the pH of the reaction solution to neutral. After the precipitate is formed, filter it, wash the filter cake twice with deionized water, transfer it to an oven at 50℃ and dry it to constant weight to obtain carboxylated chitosan.
[0077] Step ②: Preparation of silane-modified chitosan
[0078] Weigh out 80g of carboxylated chitosan, 1500mL of ethanol and 200mL of deionized water and place them in a reaction vessel. Add 0.5mol / L acetic acid aqueous solution to adjust the pH of the system to 4.5. Add 20mL of 50wt% γ-methacryloxypropyltrimethoxysilane ethanol solution dropwise. React at room temperature for 3h. After the reaction is complete, wait for the reaction to cool to room temperature, filter, wash the filter cake twice with deionized water and ethanol, transfer it to an oven at 50℃ and dry it to constant weight to obtain silane-modified chitosan.
[0079] Example 5
[0080] This embodiment provides a method for preparing silane-modified chitosan for antibacterial and anti-mite fabrics suitable for bedding processing, including the following steps:
[0081] Step ①: Preparation of carboxylated chitosan
[0082] Weigh 90g of chitosan, 5000mL of deionized water, and 20mL of acetic acid and place them in a reaction vessel under nitrogen atmosphere protection. Stir at room temperature for 3h, add 15wt% sodium hydroxide aqueous solution to adjust the pH of the system to 5, add 75g of chloroacetic acid, and react at room temperature for 3h. After the reaction is complete, add 2wt% sodium hydroxide aqueous solution to adjust the pH of the reaction solution to neutral. After the precipitate is formed, filter it, wash the filter cake three times with deionized water, transfer it to an oven at 55℃, and dry it to constant weight to obtain carboxylated chitosan.
[0083] Step ②: Preparation of silane-modified chitosan
[0084] Weigh 90g of carboxylated chitosan, 1750mL of ethanol and 300mL of deionized water and place them in a reaction vessel. Add 0.75mol / L acetic acid aqueous solution to adjust the pH of the system to 5. Add 30mL of 60wt% γ-methacryloxypropyltrimethoxysilane ethanol solution. React at room temperature for 4.5h. After the reaction is complete, wait for the reaction to cool to room temperature, filter, wash the filter cake three times with deionized water and ethanol, transfer it to an oven at 55℃ and dry it to constant weight to obtain silane-modified chitosan.
[0085] Example 6
[0086] This embodiment provides a method for preparing silane-modified chitosan for antibacterial and anti-mite fabrics suitable for bedding processing, including the following steps:
[0087] Step ①: Preparation of carboxylated chitosan
[0088] Weigh 100g of chitosan, 6000mL of deionized water, and 30mL of acetic acid and place them in a reaction vessel under nitrogen atmosphere protection. Stir at room temperature for 4 hours. Add 20wt% sodium hydroxide aqueous solution to adjust the pH of the system to 5.5. Add 100g of chloroacetic acid and react at room temperature for 4 hours. After the reaction is complete, add 3wt% sodium hydroxide aqueous solution to adjust the pH of the reaction solution to neutral. After the precipitate is formed, filter it. Wash the filter cake 4 times with deionized water and transfer it to an oven at 60℃ to dry to constant weight to obtain carboxylated chitosan.
[0089] Step ②: Preparation of silane-modified chitosan
[0090] Weigh 100g of carboxylated chitosan, 2000mL of ethanol and 400mL of deionized water and place them in a reaction vessel. Add 1.0mol / L acetic acid aqueous solution to adjust the pH of the system to 5.5. Add 40mL of 70wt% γ-methacryloxypropyltrimethoxysilane ethanol solution dropwise. React at room temperature for 6h. After the reaction is complete, wait for the reaction to cool to room temperature, filter, wash the filter cake 4 times with deionized water and ethanol, transfer it to an oven at 60℃ and dry it to constant weight to obtain silane-modified chitosan.
[0091] Example 7
[0092] This embodiment provides a method for preparing an antibacterial and anti-mite fabric suitable for bedding processing, including the following steps:
[0093] Step 1: Preparation of chitosan component
[0094] Weigh 80g of the silane-modified chitosan prepared in Example 4 and 3000mL of deionized water and place them in a reaction vessel and stir. Add 250mL of 0.5mol / L acetic acid aqueous solution and stir at room temperature for 30min to obtain the chitosan component.
[0095] Step 2: Prepare antibacterial and anti-mite finishing solution
[0096] Weigh out 40g of coated zinc oxide prepared in Example 1, 9000mL of deionized water and 10g of fatty alcohol polyoxyethylene ether and place them in a reaction vessel. Stir well, add 80g of chitosan component, 30g of polyethylene glycol diglycidyl ether and 150g of amino-modified organosilicon emulsion, and stir for 15min to obtain antibacterial and anti-mite finishing solution.
[0097] Step 3: Preparation of pretreated base fabric
[0098] Weigh out 20g of sodium hydroxide, 10g of isomeric tridecyl alcohol polyoxyethylene ether, 30g of silicone oil Goon836, and 8000mL of deionized water and place them in a reaction vessel. Add the base fabric for impregnation. Heat the reaction vessel to 80℃ and impregnate for 30min at an impregnation ratio of 1:28. After the reaction is complete, remove the excess alkali solution from the base fabric by rolling. Dry the base fabric in an oven at 90℃ for 4h to obtain the pretreated base fabric.
[0099] Step 4: Prepare antibacterial and anti-mite fabric
[0100] Weigh the pretreated substrate into the antibacterial and anti-mite finishing solution, and perform double immersion and double rinsing with a 60% roll-in rate and an impregnation ratio of 1:30. After the reaction is completed, dry the substrate in an oven at 90℃ for 4 hours to obtain the antibacterial and anti-mite fabric.
[0101] Example 8
[0102] This embodiment provides a method for preparing an antibacterial and anti-mite fabric suitable for bedding processing, including the following steps:
[0103] Step 1: Preparation of chitosan component
[0104] Weigh 90g of the silane-modified chitosan prepared in Example 5 and 4000mL of deionized water and place them in a reaction vessel and stir. Add 300mL of 0.75mol / L acetic acid aqueous solution and stir at room temperature for 40min to obtain the chitosan component.
[0105] Step 2: Prepare antibacterial and anti-mite finishing solution
[0106] Weigh out 50g of coated zinc oxide prepared in Example 2, 10000mL of deionized water and 20g of fatty alcohol polyoxyethylene ether and place them in a reaction vessel. Stir well, add 90g of chitosan component, 40g of polyethylene glycol diglycidyl ether and 175g of amino-modified organosilicon emulsion, and stir for 22min to obtain antibacterial and anti-mite finishing solution.
[0107] Step 3: Preparation of pretreated base fabric
[0108] Weigh out 30g of sodium hydroxide, 20g of isomeric tridecyl alcohol polyoxyethylene ether, 40g of silicone oil Goon836, and 9000mL of deionized water and place them in a reaction vessel. Add the base fabric for impregnation. Heat the reaction vessel to 85℃ and impregnate for 45min at an impregnation ratio of 1:30. After the reaction is complete, remove excess alkali solution from the base fabric by rolling. Dry the base fabric in an oven at 95℃ for 5h to obtain the pretreated base fabric.
[0109] Step 4: Prepare antibacterial and anti-mite fabric
[0110] Weigh the pretreated substrate into the antibacterial and anti-mite finishing solution, and perform double dip and double tread at a 70% roll-in rate and an impregnation ratio of 1:31. After the reaction is complete, dry the substrate in an oven at 95℃ for 5 hours to obtain the antibacterial and anti-mite fabric.
[0111] Example 9
[0112] This embodiment provides a method for preparing an antibacterial and anti-mite fabric suitable for bedding processing, including the following steps:
[0113] Step 1: Preparation of chitosan component
[0114] Weigh 100g of the silane-modified chitosan prepared in Example 6 and 5000mL of deionized water and place them in a reaction vessel and stir. Add 350mL of 1.0mol / L acetic acid aqueous solution and stir at room temperature for 50min to obtain the chitosan component.
[0115] Step 2: Prepare antibacterial and anti-mite finishing solution
[0116] Weigh out 60g of coated zinc oxide prepared in Example 3, 11000mL of deionized water and 30g of fatty alcohol polyoxyethylene ether and place them in a reaction vessel. Stir well, add 100g of chitosan component, 50g of polyethylene glycol diglycidyl ether and 200g of amino-modified organosilicon emulsion, and stir for 30min to obtain antibacterial and anti-mite finishing solution.
[0117] Step 3: Preparation of pretreated base fabric
[0118] Weigh out 40g of sodium hydroxide, 30g of isomeric tridecyl alcohol polyoxyethylene ether, 50g of silicone oil Goon836, and 10000mL of deionized water and place them in a reaction vessel. Add the base fabric for impregnation. Heat the reaction vessel to 90℃ and impregnate for 60min at an impregnation ratio of 1:32. After the reaction is complete, remove excess alkali solution from the base fabric by rolling. Dry the base fabric in an oven at 100℃ for 6h to obtain the pretreated base fabric.
[0119] Step 4: Prepare antibacterial and anti-mite fabric
[0120] Weigh the pretreated substrate into the antibacterial and anti-mite finishing solution, and perform double immersion and double rinsing with an 80% roll-in rate and an impregnation ratio of 1:32. After the reaction is completed, dry the substrate in an oven at 100℃ for 6 hours to obtain the antibacterial and anti-mite fabric.
[0121] Comparative Example 1
[0122] The difference between this comparative example and Example 9 is that the chitosan component was omitted when preparing the antibacterial and anti-mite finishing solution in step (2).
[0123] Comparative Example 2
[0124] The difference between this comparative example and Example 9 is that, in step (2) when preparing the antibacterial and anti-mite finishing liquid, zinc oxide is used in an equal amount instead of coated zinc oxide.
[0125] Comparative Example 3
[0126] The difference between this comparative example and Example 9 is that, in step (4) when preparing the antibacterial and anti-mite fabric, the pre-treated base fabric is replaced with an equal amount of base fabric.
[0127] Performance testing:
[0128] The tensile properties of the antibacterial and anti-mite fabrics prepared in Examples 7-9 and Comparative Examples 1-3 were tested in accordance with the standard GB / T 3923.1-2013 "Textiles - Tensile properties of fabrics - Part 1: Determination of breaking strength and elongation at break (strip method)".
[0129] The antibacterial properties of the antibacterial and anti-mite fabrics prepared in Examples 7-9 and Comparative Examples 1-3 were tested in accordance with the standard GB / T 20944.2-2007 "Evaluation of antibacterial properties of textiles - Part 2: Absorption method".
[0130] The antibacterial and anti-mite fabrics prepared in Examples 7-9 and Comparative Examples 1-3 were tested for their repellency and inhibition rates against mites in accordance with the standard GB / T 24253-2009 "Evaluation of anti-mite performance of textiles". The specific data are shown in Table 1.
[0131] Table 1 - Performance Test Data for Each Sample
[0132]
[0133] Data Analysis:
[0134] Comparative analysis of the data in Table 1 reveals that the antibacterial and anti-mite fabric prepared by this invention has a warp tensile strength of 398 N and a weft tensile strength of 356 N. It exhibits a mite repellency rate of 89.6%, an inhibition rate of 95.1%, and an inhibition rate of 99.6% against Staphylococcus aureus and 99.1% against Escherichia coli. All these data are superior to those of the comparative example.
[0135] The antibacterial and anti-mite fabric of this invention is produced by in-situ polymerization of zinc oxide activated with ammonia and acrylic monomers initiated by ammonium persulfate, forming coated zinc oxide with good dispersibility and fiber affinity, thus improving the stability and fabric fastness of the antibacterial components. Subsequently, chitosan is carboxylated and silane modified to give it good water solubility, film-forming ability, and the ability to form chemical bonds with fibers. In subsequent finishing, it not only provides its own antibacterial properties but also acts as a bonding layer to stabilize inorganic antibacterial particles. At the same time, the base fabric is pretreated with alkali, surfactant, and silicone oil to remove oil stains and enhance fiber hydrophilicity and exposure of active sites, allowing the finishing solution to fully penetrate and uniformly adsorb. Finally, the pretreated base fabric is double-dipped and double-rolled in a finishing solution containing coated zinc oxide, silane chitosan, epoxy crosslinking agent, and silicone softener, and dried at a moderate temperature to form a dense, uniform, and washable functional composite film layer, giving the fabric excellent antibacterial and anti-mite properties while maintaining good mechanical properties and wearing comfort.
[0136] The preferred embodiments of the present invention disclosed above are merely illustrative of the invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the invention to specific implementations. Clearly, many modifications and variations can be made based on the content of this specification. This specification selects and specifically describes these embodiments to better explain the principles and practical applications of the invention, thereby enabling those skilled in the art to better understand and utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims
1. A method for preparing an antibacterial and anti-mite fabric suitable for bedding processing, characterized in that, Includes the following steps: S1. Place silane-modified chitosan and deionized water in a reaction vessel and stir. Add an aqueous acetic acid solution and stir at room temperature for 30-50 minutes to obtain the chitosan component. S2. Place the coated zinc oxide, deionized water and fatty alcohol polyoxyethylene ether in a reaction vessel, stir evenly, add chitosan component, polyethylene glycol diglycidyl ether and softener, stir for 15-30 minutes to obtain antibacterial and anti-mite finishing liquid. S3. Place sodium hydroxide, wetting agent, stabilizer and deionized water in a reaction vessel, add the base fabric for impregnation, heat the reaction vessel to 80-90℃, impregnate for 30-60min, and then perform post-treatment to obtain the pretreated base fabric. S4. The pretreated substrate is immersed in an antibacterial and anti-mite finishing solution and subjected to double immersion and double rolling. The post-treatment yields an antibacterial and anti-mite fabric.
2. The method for preparing an antibacterial and anti-mite fabric suitable for bedding processing according to claim 1, characterized in that, In step S1, the ratio of the amount of silane-modified chitosan, deionized water, and acetic acid aqueous solution is 8-10g:300-500mL:25-35mL, and the concentration of the acetic acid aqueous solution is 0.5-1.0mol / L; in step S2, the ratio of the amount of the coating zinc oxide, deionized water, fatty alcohol polyoxyethylene ether, chitosan component, polyethylene glycol diglycidyl ether, and softener is 4-6g:900-1100mL:1-3g:8-10g:3-5g:15-20g.
3. The method for preparing an antibacterial and anti-mite fabric suitable for bedding processing according to claim 1, characterized in that, In step S3, the ratio of sodium hydroxide, wetting agent, stabilizer and deionized water is 2-4g:1-3g:3-5g:800-1000mL, and the impregnation ratio is 1:28-32; in step S4, the roll residue of the double dip and double roll is 60-80%, and the impregnation ratio is 1:30-32.
4. The method for preparing an antibacterial and anti-mite fabric suitable for bedding processing according to claim 1, characterized in that, The silane-modified chitosan was prepared by the following steps: A1. Chitosan, deionized water and acetic acid are placed in a reaction vessel under nitrogen atmosphere protection and stirred at room temperature for 2-4 hours. Sodium hydroxide aqueous solution is added to adjust the pH of the system to 4.5-5.
5. Chloroacetic acid is added and reacted at room temperature for 2-4 hours. Carboxylated chitosan is obtained after post-treatment. A2. Carboxylated chitosan, ethanol, and deionized water were placed in a reaction vessel, and an aqueous acetic acid solution was added to adjust the pH of the system to 4.5-5.
5. A silane coupling agent solution was added dropwise, and the reaction was carried out at room temperature for 3-6 hours. The silane-modified chitosan was obtained after post-treatment.
5. The method for preparing an antibacterial and anti-mite fabric suitable for bedding processing according to claim 4, characterized in that, In step A1, the ratio of chitosan, deionized water, acetic acid, and chloroacetic acid is 8-10g:400-600mL:1-3mL:5-10g, and the concentration of sodium hydroxide aqueous solution is 10-20wt%. In step A2, the ratio of carboxylated chitosan, ethanol, deionized water, and silane coupling agent solution is 8-10g:150-200mL:20-40mL:2-4mL, the silane coupling agent solution is a 50-70wt% γ-methacryloyloxypropyltrimethoxysilane ethanol solution, and the concentration of acetic acid aqueous solution is 0.5-1.0mol / L.
6. The method for preparing an antibacterial and anti-mite fabric suitable for bedding processing according to claim 1, characterized in that, The coated zinc oxide is prepared by the following steps: B1. Place zinc oxide, deionized water and ethanol in a reaction vessel and stir. Add ammonia water and stir at room temperature for 1-2 hours. Post-treatment yields activated zinc oxide. B2. Place acrylic acid, butyl acrylate and 1,4-butanediol diacrylate in a reaction vessel and stir until homogeneous to obtain a mixed monomer; B3. Place activated zinc oxide in a reaction vessel and stir. Slowly add mixed monomers and ammonium persulfate solution. Heat the reaction vessel to 50-60℃ and keep it at that temperature for 0.5-1h. Post-process to obtain coated zinc oxide.
7. The method for preparing an antibacterial and anti-mite fabric suitable for bedding processing according to claim 6, characterized in that, In step B1, the ratio of zinc oxide, deionized water, ethanol, and ammonia is 2-4g:40-60mL:15-30mL:1-2mL, and the concentration of ammonia is 25-30wt%. In step B2, the weight ratio of acrylic acid, butyl acrylate, and 1,4-butanediol diacrylate is 2-3:6-7:0.3-0.
5. In step B3, the ratio of activated zinc oxide, mixed monomers, and ammonium persulfate solution is 10-12g:3-5g:1-2mL, and the ammonium persulfate solution is a 50-70wt% aqueous solution of ammonium persulfate.
8. An antibacterial and anti-mite fabric suitable for bedding processing, characterized in that, The antibacterial and anti-mite fabric suitable for bedding processing is prepared by the preparation method of the antibacterial and anti-mite fabric suitable for bedding processing as described in any one of claims 1-7.