A processing method for antibacterial children's clothing fabric

Abstract

The present invention relates to the technical field of clothing fabrics, and provides a processing method for antibacterial children's clothing fabrics, which solves the problem that traditional dyeing and finishing processes easily cause short fiber fluff to stand up on the fabric surface, affecting the feel of the fabric and interfering with the effect of subsequent antibacterial finishing. The method comprises the following steps: (1) pretreatment; (2) dyeing; (3) post-treatment: refilling the water washing tank with water, adding glacial acetic acid, adjusting the pH value to 6.0-6.8, raising the temperature to 55°C, adding polishing enzyme, reacting for 20-30 minutes, then adding soaping agent, running for 5-10 minutes, raising the temperature to 90-95°C for soaping, keeping the temperature for 10-15 minutes, draining, and rinsing the grey fabric; and (4) antibacterial finishing and shaping.

Description

Technical Field

[0001] The present invention relates to the technical field of clothing fabrics, and in particular to a processing method of antibacterial children's clothing fabrics. Background Art

[0002] Infants and children are naturally active and enjoy being outdoors, so their everyday clothing can sometimes become a breeding ground for bacteria. Ordinary textile fabrics lack antimicrobial properties, and under suitable conditions of temperature, humidity, and nutrients, microorganisms can rapidly grow and multiply. Compared to adults, infants and children are less able to resist external pathogens. The growth of microorganisms not only creates odor but can also cause bacterial infections, posing a threat to human health. Consequently, children's clothing labeled as antimicrobial has become an increasingly popular choice among parents in recent years.

[0003] Currently, antimicrobial textile fabrics are produced primarily through two methods. The first is the functional fiber method. Antimicrobial fibers are produced through co-spinning or composite spinning, and various textile fabrics are then made from these fibers. The antimicrobial textile fabrics produced by this method have long-lasting antimicrobial effects and excellent wash resistance, but they are technically demanding, difficult to manufacture, and require high levels of antimicrobial agents, making the production of antimicrobial fibers more challenging. The second method is the post-finishing method. Fabrics are impregnated, padded, or coated with a solution or resin containing an antimicrobial agent, and then evaporated by high-temperature baking or other methods to deposit a layer of insoluble or slightly soluble antimicrobial agent on the fabric. This process is generally performed in the final stages of dyeing and finishing. The post-finishing method offers a simple process and a wide range of antimicrobial agents to choose from. Therefore, the majority of currently used antimicrobial textile fabrics are produced through post-finishing methods.

[0004] The traditional dyeing and finishing process is: pre-treatment → polishing → dyeing → post-treatment. For example, Chinese patent number CN201010585103.0 discloses a low-temperature dyeing process for pure cotton fabric, which includes the following steps:

[0005] (1) Low-temperature pretreatment: Add a scouring bath auxiliary to the dye liquor, adjust the temperature to 40-60°C, and continue the reaction for 15-30 minutes; (2) Polishing: Adjust the temperature to 35-60°C and the pH value to 5.5-6, add 0.2-0.5% of the fabric weight of neutral polishing enzyme, and continue the reaction for 15-20 minutes; (3) Low-temperature dyeing: Adjust the temperature to 35-45°C, and add low-temperature reactive dye, sodium sulfate, soda ash, and liquid caustic soda in sequence at regular time intervals to react. The above low-temperature dyeing process has the advantages of simple process, low pollution, and low energy consumption.

[0006] Conventional cotton fabric polishing is performed using an acidic polishing enzyme under acidic conditions to improve surface finish and reduce pilling. This polishing process must be performed separately after pretreatment and not in the same bath as the dyeing process. Furthermore, given the impact of enzyme activity on fabric strength, it is necessary to add alkali or inactivate the enzyme at high temperatures after polishing. Chang Xiangzhen et al. (Chang Xiangzhen, Zhang Xin et al. One-bath Production Practice of Enzyme Polishing and Dyeing of Knitted Fabrics [J]. 2010, 4:31-32.) used a neutral polishing enzyme to perform the polishing and dyeing processes in a single bath. The resulting polishing results are comparable to those achieved with conventional acidic polishing enzymes, while eliminating a separate polishing step. This process minimizes fabric strength damage and quality loss, significantly reduces energy costs such as water, electricity, and steam, and improves production efficiency.

[0007] The purpose of polishing is to use enzymes to remove the fuzz from the fabric surface, ensuring a smooth surface and a pleasant feel. However, the two aforementioned methods require the fabric to circulate in the polishing vat for a long time after polishing. Friction against the vat walls, the cloth-lifting wheel, and the cloth-steering rack causes short fibers to rise again. This not only affects the fabric's feel but also allows microorganisms to attach to these fibers, absorbing waste products from the human sweat glands and spleen, and rapidly multiplying, reducing the effectiveness of the antimicrobial finishing process. Summary of the Invention

[0008] Therefore, in response to the above content, the present invention provides a processing method for antibacterial children's clothing fabrics to solve the problem that traditional dyeing and finishing processes easily cause short fiber fuzz to stand up on the fabric surface, affecting the feel of the fabric and interfering with the effect of subsequent antibacterial finishing.

[0009] To achieve the above object, the present invention is achieved through the following technical solutions:

[0010] A method for processing antibacterial children's clothing fabric comprises the following steps:

[0011] (1) Pretreatment

[0012] After the grey cloth is put into the vat, water is added and the temperature is raised to 40-50℃. High-efficiency energy-saving bath agent and degreasing agent are added. After running for 5 minutes, the temperature is raised to 70℃. Then hydrogen peroxide is added and the temperature is raised to 110℃. The temperature is kept for 20-40 minutes. Then the temperature is lowered to 78℃ and the water is drained. After washing, glacial acetic acid is added to adjust the pH value to 6.0-7.0. Deoxygenase is added and the temperature is raised to 50℃ for deoxidation. The residual oxygen content is less than 0.5mg, which is qualified.

[0013] (2) Dyeing

[0014] Adjust the temperature to 40-50℃, add reactive dye to the vat, then add sodium sulfate, add the material for 15 minutes, react for 10 minutes, then add soda ash, add the soda ash twice, the first time is 1 / 10, add the material for 20 minutes, react for 5 minutes, adjust the pH value to 7.5-8.5, the second time is 9 / 10, add the material for 25 minutes, react for 10 minutes, adjust the pH value to 10.5-11.5, then heat to 60℃, keep warm for 30-40 minutes, and drain;

[0015] (3) Post-processing

[0016] After washing, refill the tank with water, add glacial acetic acid, adjust the pH value to 6.0-6.8, heat to 55℃, add polishing enzyme, react for 20-30min, then add soaping agent, run for 5-10min, heat to 90-95℃ for soaping, keep warm for 10-15min, finally cool to 78℃, drain, and rinse the grey cloth with clean water;

[0017] (4) Antibacterial finishing and shaping

[0018] Add water, antibacterial finishing agent, penetrant, and sodium laureth sulfate to the trough of the setting machine, and stir evenly to form an antibacterial finishing liquid, wherein the addition amount of the penetrant in the antibacterial finishing liquid is 1.0-2.0 g / L, the addition amount of sodium laureth sulfate is 1.5-3.5 g / L, and the addition amount of the antibacterial finishing agent is 2.0-3.0% of the mass of the grey cloth;

[0019] The grey cloth passes through the trough, double dip and double rolling, and the rolling rate is maintained at 80-90%;

[0020] Finally, the grey fabric passes through a setting machine oven and is set and dried at 150-170°C to obtain the antibacterial children's clothing fabric.

[0021] A further improvement is that the concentrations of the auxiliary agents in step (1) are: 2.0-2.5 g / L of high-efficiency energy-saving bath agent, 1.0-3.0 g / L of hydrogen peroxide, 2.0-3.0 g / L of degreasing agent, and 0.12-0.18 g / L of deoxidase.

[0022] A further improvement is that in step (2), the amount of sodium sulfate added is 25-30 g / L, and the amount of soda ash added is 10-15 g / L.

[0023] A further improvement is that the reactive dye consists of reactive red BES, reactive yellow 3RE and reactive military blue XL-3G. Based on 100% of the mass of the grey cloth, the added mass of each component in the reactive dye is: reactive red BES 0.5-1.0%, reactive yellow 3RE 0.2-1.5%, and reactive military blue XL-3G 0.18-0.24%.

[0024] A further improvement is that the concentrations of the auxiliary agents in step (3) are: polishing enzyme 1.0-1.5 g / L, soaping agent 1.0-2.0 g / L.

[0025] A further improvement is that the antibacterial finishing agent comprises the following raw materials in parts by weight: 12-25 parts of antibacterial microcapsules, 6-12 parts of modified nano zinc oxide, and 8-15 parts of terminal carboxyl quaternary ammonium salt; the antibacterial microcapsules are prepared by interfacial polymerization using a composite essential oil as a core material; the composite essential oil comprises the following components in the following mass fractions: 20-28% of artemisia essential oil, 22-30% of Sichuan bergamot essential oil, 30-40% of cypress leaf essential oil, and 10-18% of Sichuan sunflower essential oil.

[0026] A further improvement is that the modified nano zinc oxide is prepared by the following method: nano zinc oxide is added to a reactor filled with water, ultrasonically dispersed for 20-40 minutes, then vinyl trimethoxyethoxy silane is added, the temperature is raised to 50-60°C, stirred and reacted for 6-10 hours, then an initiator is added to the reactor, the temperature is raised to 70-80°C, 2-ethyl isocyanate is added dropwise, and the reaction is carried out for 3-6 hours. After the reaction is completed, the modified nano zinc oxide is obtained by centrifugation, washing, and drying.

[0027] A further improvement is that the mass ratio of the nano zinc oxide, vinyl trimethoxyethoxysilane, initiator, and 2-isocyanate acrylate is 1-3:1:0.02-0.08:0.5-0.8.

[0028] A further improvement is that the antibacterial microcapsules are prepared according to the following method:

[0029] a. The composite essential oil and diphenylmethane diisocyanate were added to the toluene solvent and stirred to mix to obtain an oil phase;

[0030] b. Add the emulsifier and dispersant to water and stir to mix to obtain an aqueous phase;

[0031] c. The oil phase obtained in the above step is mixed with the aqueous phase and homogenized to obtain an emulsion, wherein the mass ratio of the oil phase to the aqueous phase is 1:2-4, the mass fraction of the composite essential oil in the oil phase is 35-50%, the mass fraction of diphenylmethane diisocyanate is 25-35%, the mass fraction of the emulsifier in the aqueous phase is 2-4%, and the mass fraction of the dispersant is 1-3%;

[0032] d. Add a 35-55% aqueous solution of aliphatic polyether diamine to the emulsion, raise the temperature to 55-65°C after the addition, stir and react for 2-3h, filter after the reaction, wash with water, and dry to obtain antibacterial microcapsules.

[0033] A further improvement is that the mass ratio of the aliphatic polyether diamine to diphenylmethane diisocyanate is 2-4:1. The molecular weight of the aliphatic polyether diamine is in the range of 400-900, and the mass ratio of the two increases with the increase of the molecular weight of the aliphatic polyether diamine.

[0034] A further improvement is that the carboxyl-terminated quaternary ammonium salt is prepared according to the following method: first, acrylamide is added to a reaction kettle containing acetone, N,N-dimethylethylenediamine is slowly added dropwise, and the reaction is stirred at room temperature for 20-30 hours. After the reaction is completed, distillation is carried out under reduced pressure to obtain intermediate I, wherein the mass ratio of N,N-dimethylethylenediamine to acrylamide is 1:2-3; then intermediate I is dissolved in dimethyl sulfoxide, alkyl halide is added, and the reaction is carried out at 80-100°C for 2-4 days. After the reaction is completed, The method comprises the following steps: treating the intermediate II, wherein the structural formula of the alkyl halide is RX, X is any one of Cl, Br, and I, R represents a C4-C8 alkyl group, and the molar ratio of the intermediate I to the alkyl halide is 1:2.4-3.6; then dissolving succinic anhydride in chloroform and adding the solution dropwise to the reactor containing the intermediate II, reacting at 55-65° C. for 4-8 hours, filtering, washing, and drying after the reaction to obtain a carboxyl-terminated quaternary ammonium salt, and the molar ratio of the intermediate II to succinic anhydride is 1:2.5-4.

[0035] By adopting the above technical solution, the beneficial effects of the present invention are:

[0036] 1. In traditional dyeing and finishing processes, the greige fabric spends a long time circulating in the drum, causing friction between the greige fabric surface and the drum wall, cloth lifting wheel, and cloth swing frame, resulting in relatively severe fuzzing on the fabric surface. The production process proposed in this invention reduces the friction time of the greige fabric in the drum, resulting in less fuzzing on the fabric surface, and a smoother and more pleasant feel.

[0037] 2. In traditional processes, additives such as dyes, sodium sulfate, and alkali can affect the activity of the polishing enzyme, reducing its activity. This can lead to increased polishing enzyme usage and poor polishing results. The present invention adjusts the pH to a specific value after dyeing, and then directly adds the polishing enzyme for polishing. This maximizes performance without being affected by any chemical additives. After polishing, the temperature is directly raised and soaping is performed in the same bath, saving costs. Analysis shows that processing one ton of grey cloth can save approximately 51% in water consumption, over 27% in electricity consumption, and over 11% in steam consumption, with savings reaching as high as 52%.

[0038] 3. Antibacterial finishing is performed on the grey cloth using an antibacterial finishing liquid, which gives the fabric excellent antibacterial and anti-wrinkle effects, and it still has good antibacterial properties after multiple washings. The main component of the antibacterial finishing liquid is an antibacterial finishing agent, which includes the following raw materials: antibacterial microcapsules, modified nano zinc oxide, and end-carboxyl quaternary ammonium salts. Nano zinc oxide has a strong inhibitory or killing effect on many pathogenic bacteria, but its particles have high surface energy and are prone to agglomeration. If directly applied, it is easy to cause less and uneven distribution on the fiber surface of cotton fabrics, affecting the antibacterial effect. The present application performs surface modification on nano zinc oxide, and grafts vinyl trimethoxyethoxysilane on the surface of nano zinc oxide particles through dehydration condensation. The steric hindrance effect of the long organic chain of vinyl trimethoxyethoxysilane is utilized to hinder the agglomeration between particles and improve the dispersion uniformity of nano zinc oxide. Then, -NCO groups are introduced into the structure, which can react with the hydroxyl groups on the cotton fabric, thereby enhancing the bonding force between the modified nano zinc oxide and the fabric, so that the modified nano zinc oxide can adhere to the cotton fabric for a long time, thereby improving the antibacterial and washable properties of the fabric.

[0039] The present invention dissolves two wall material reaction monomers with different hydrophilicity in the water phase and the oil phase respectively, and a polymerization reaction occurs at the interface between the water and oil phases to form a polyurea shell, in which the core material composite essential oil is coated. The prepared antibacterial microcapsules have a relatively uniform particle size distribution and a good sustained-release effect, effectively preventing the volatilization loss of the essential oil and improving the antibacterial durability of the fabric. Some amino groups in the aliphatic polyether diamine react with the -NCO group of diphenylmethane diisocyanate to form long polyurea chains, and the unreacted amino groups form hydrogen bonds with the hydroxyl groups on the cotton fabric, thereby improving the adhesion to the cotton fabric. The various components in the composite essential oil have a synergistic effect, and the combined effect improves the antibacterial effect of the fabric. DETAILED DESCRIPTION

[0040] The following will describe the implementation methods of the present invention in detail with reference to specific embodiments, so that the implementation process of how the present invention applies technical means to solve technical problems and achieve technical effects can be fully understood and implemented accordingly.

[0041] Unless otherwise specified, the techniques used in the examples are conventional techniques well known to those skilled in the art, and the reagents and products used are all commercially available. The sources, trade names, and, where necessary, the components of the reagents used are indicated when they first appear.

[0042] Example 1

[0043] A method for processing antibacterial children's clothing fabric comprises the following steps:

[0044] (1) Pretreatment

[0045] After the grey cloth is put into the vat, water is added and the temperature is raised to 40℃. High-efficiency energy-saving bath agent and degreasing agent are added. After running for 5 minutes, the temperature is raised to 70℃. Then hydrogen peroxide is added and the temperature is raised to 110℃. The temperature is kept for 20 minutes. Then the temperature is lowered to 78℃ and the water is drained. After washing, glacial acetic acid is added to adjust the pH value to 6.0-7.0. Deoxygenase is added and the temperature is raised to 50℃ for deoxidation. The residual oxygen content is less than 0.5mg, which is qualified.

[0046] The concentrations of the additives are: high-efficiency energy-saving bath agent 2.0 g / L, hydrogen peroxide 1.0 g / L, degreasing agent 2.0 g / L, deoxidase 0.12 g / L;

[0047] (2) Dyeing

[0048] Adjust the temperature to 40℃, add reactive dye to the vat, then add sodium sulfate, add the material for 15 minutes, react for 10 minutes, then add soda ash, add the soda ash twice, the first time is 1 / 10, add the material for 20 minutes, react for 5 minutes, adjust the pH value to 7.5-8.5, the second time is 9 / 10, add the material for 25 minutes, react for 10 minutes, adjust the pH value to 10.5-11.5, then heat to 60℃, keep warm for 30 minutes, and drain;

[0049] The reactive dye is composed of reactive red BES, reactive yellow 3RE and reactive military blue XL-3G. Based on 100% of the mass of the grey cloth, the added mass of each component in the reactive dye is: reactive red BES 0.5%, reactive yellow 3RE 1.5%, reactive military blue XL-3G 0.18%, the added amount of sodium sulfate is 25g / L, and the total added amount of soda ash is 10g / L;

[0050] (3) Post-processing

[0051] After washing, refill the tank with water, add glacial acetic acid, adjust the pH value to 6.0-6.8, heat to 55℃, add polishing enzyme, react for 20 minutes, then add soaping agent, run for 5 minutes, heat to 90℃ for soaping, keep warm for 15 minutes, and finally cool to 78℃, drain and rinse the grey cloth with clean water;

[0052] The concentrations of the additives are: polishing enzyme 1.0 g / L, soaping agent 1.0 g / L;

[0053] (4) Antibacterial finishing and shaping

[0054] Add water, antibacterial finishing agent, penetrant JFC-M, and sodium laureth sulfate to the trough of the setting machine, and stir evenly to form an antibacterial finishing liquid, wherein the addition amount of penetrant JFC-M in the antibacterial finishing liquid is 1.0 g / L, the addition amount of sodium laureth sulfate is 1.5 g / L, and the addition amount of the antibacterial finishing agent is 3.0% of the mass of the grey fabric;

[0055] The grey cloth passes through the trough, double dip and double rolling, and the rolling rate is maintained at 80-90%;

[0056] Finally, the grey fabric is passed through a setting machine oven and dried at 150°C to obtain the antibacterial children's clothing fabric.

[0057] The antibacterial finishing agent comprises the following raw materials in parts by weight: 12 parts of antibacterial microcapsules, 6 parts of modified nano zinc oxide, and 8 parts of terminal carboxyl quaternary ammonium salt. The modified nano zinc oxide is prepared by the following method: adding nano zinc oxide into a reactor filled with water, ultrasonically dispersing for 20 minutes, then adding vinyl trimethoxyethoxy silane, heating to 50° C., stirring and reacting for 10 hours, then adding benzoyl peroxide into the reactor, heating to 70° C., dropwise adding 2-isocyanate ethyl acrylate, reacting for 3 hours, and after the reaction is completed, centrifuging, washing, and drying to obtain the modified nano zinc oxide. The mass ratio of the nano zinc oxide, vinyl trimethoxyethoxy silane, benzoyl peroxide, and 2-isocyanate ethyl acrylate is 1:1:0.02:0.5.

[0058] The antibacterial microcapsules were prepared by the following method:

[0059] a. The composite essential oil and diphenylmethane diisocyanate were added to the toluene solvent and stirred to mix to obtain an oil phase, wherein the composite essential oil comprises the following mass fractions of the components: 20% artemisia essential oil, 30% Sichuan Buddha's hand essential oil, 40% cypress leaf essential oil, 10% Sichuan sunflower essential oil;

[0060] b. Add polyvinyl alcohol and dispersant to water and stir to mix to obtain an aqueous phase;

[0061] c. The oil phase obtained in the above step is mixed with the aqueous phase and homogenized to obtain an emulsion, wherein the mass ratio of the oil phase to the aqueous phase is 1:2, the mass fraction of the composite essential oil in the oil phase is 35%, the mass fraction of diphenylmethane diisocyanate is 25%, the mass fraction of polyvinyl alcohol in the aqueous phase is 2%, and the mass fraction of the dispersant is 1%;

[0062] d. Add a 35% aqueous solution of aliphatic polyether diamine to the emulsion, raise the temperature to 55°C after the addition, stir and react for 2 hours, filter after the reaction, wash with water, and dry to obtain antibacterial microcapsules.

[0063] The aliphatic polyether diamine is ED-600 water-soluble aliphatic diamine produced by Huntsman, and the mass ratio of the aliphatic polyether diamine to diphenylmethane diisocyanate is 3:1.

[0064] The carboxyl-terminated quaternary ammonium salt is prepared according to the following method: first, acrylamide is added to a reaction kettle containing acetone, N,N-dimethylethylenediamine is slowly added dropwise, and the reaction is stirred at room temperature for 20 hours. After the reaction is completed, the reaction is carried out under reduced pressure and distilled to obtain intermediate I, wherein the mass ratio of N,N-dimethylethylenediamine to acrylamide is 1:2; then, intermediate I is dissolved in dimethyl sulfoxide, 1-chlorobutane is added, and the reaction is carried out at 80°C for 4 days. After the reaction is completed, the reaction is post-treated to obtain intermediate II, wherein the molar ratio of intermediate I to 1-chlorobutane is 1:2.4; then, succinic anhydride is dissolved in chloroform and added dropwise to the reaction kettle containing intermediate II, and the reaction is carried out at 55°C for 4 hours. After the reaction is completed, the reaction is filtered, washed, and dried to obtain the carboxyl-terminated quaternary ammonium salt, wherein the molar ratio of intermediate II to succinic anhydride is 1:2.5.

[0065] Conventional quaternary ammonium salt compounds cannot form covalent bonds with cotton fabric fibers, resulting in poor antibacterial and wash-resistant properties. After repeated washing, the antibacterial function rapidly weakens and eventually disappears. The present invention uses acrylamide and N,N-dimethylethylenediamine as raw materials, sequentially performing a Michael addition reaction, a quaternization reaction, and an amidation reaction to produce a carboxyl-terminated quaternary ammonium salt. The carboxyl groups in the carboxyl-terminated quaternary ammonium salt molecules can undergo a cross-linking reaction with the hydroxyl groups on the cotton fabric, strengthening the bonding strength with the cotton fabric and thereby improving the antibacterial and wash-resistant properties of the fabric. Furthermore, the cross-linking reaction can enhance the connectivity between adjacent molecular chains in the cotton fiber, limiting the mutual slippage of adjacent molecular chains, thereby improving the wrinkle resistance of the fabric.

[0066] Comparative Example 1

[0067] This comparative example adopts a traditional dyeing and finishing process, which differs from Example 1 in that: polishing enzyme is not added in step (3), and polishing is performed before the dyeing process in step (2). The specific steps are: draining the water after the pre-treatment, refilling the water tank, heating it to 55°C, adding the polishing enzyme, running it for 30 minutes, taking samples to check the effect of the cloth after polishing, and if it meets the requirements, heating it to 80°C, inactivating the polishing enzyme for 10 minutes, and draining the water;

[0068] Comparative Example 2

[0069] This comparative example also adopts the traditional dyeing and finishing process (polishing and dyeing in the same bath), and the difference from Example 1 is that: no polishing enzyme is added in step (3), and the polishing enzyme is added before adding the reactive dye in step (2). After adding the sodium sulfate and reacting for 10 minutes, the temperature is raised to 55°C, the reaction is carried out for 30 minutes, and then soda ash is added.

[0070] The production costs of processing 1 ton of grey cloth using the dyeing and finishing processes of Example 1 and Comparative Examples 1-2 are compared, and the results are shown in Table 1.

[0071] Table 1

[0072] Water consumption / t Power consumption / KW·h <![CDATA[Steam consumption / m 3 > Example 1 7.2 0.70 0.358 Comparative Example 1 3.5 0.68 0.192 Comparative Example 2 3.5 0.49 0.170

[0073] As shown in Table 1, compared with the traditional dyeing and finishing process, the dyeing and finishing process of the present invention has a lower comprehensive cost for processing one ton of cloth, saves about 51% of water consumption, saves more than 27% of electricity consumption, saves more than 11% of steam consumption, and can reach up to 52%.

[0074] The fabrics prepared in Example 1 and Comparative Examples 1-2 were subjected to performance testing, and the test results are shown in Table 2.

[0075] Table 2

[0076] Test items Example 1 Comparative Example 1 Comparative Example 2 Test Method Pilling / Grade 4 3-4 3-4 GB / T4802.2-2008 Bursting strength / N 383 360 373 GB / T19976-2005

[0077] As shown in Table 2, compared with the traditional dyeing and finishing process, the fabric prepared by the present invention is smooth and has a good hand feel, has only slight pilling on the surface, and has better bursting strength.

[0078] Example 2

[0079] A method for processing antibacterial children's clothing fabric comprises the following steps:

[0080] (1) Pretreatment

[0081] After the grey cloth is put into the vat, water is added and the temperature is raised to 45℃. High-efficiency energy-saving bath agent and degreasing agent are added. After running for 5 minutes, the temperature is raised to 70℃. Then hydrogen peroxide is added and the temperature is raised to 110℃. The temperature is kept for 30 minutes. Then the temperature is lowered to 78℃ and the water is drained. After washing, glacial acetic acid is added to adjust the pH value to 6.0-7.0. Deoxygenase is added and the temperature is raised to 50℃ for deoxidation. The residual oxygen content is less than 0.5mg, which is qualified.

[0082] The concentrations of the additives are: high-efficiency energy-saving bath agent 2.2g / L, hydrogen peroxide 2.0g / L, degreasing agent 2.5g / L, deoxidase 0.15g / L;

[0083] (2) Dyeing

[0084] Adjust the temperature to 45°C, add reactive dye to the vat, then add sodium sulfate, add the material for 15 minutes, react for 10 minutes, then add soda ash, add the soda ash twice, the first time is 1 / 10, add the material for 20 minutes, react for 5 minutes, adjust the pH value to 7.5-8.5, the second time is 9 / 10, add the material for 25 minutes, react for 10 minutes, adjust the pH value to 10.5-11.5, then heat to 60°C, keep warm for 35 minutes, and drain;

[0085] The reactive dye is composed of reactive red BES, reactive yellow 3RE and reactive military blue XL-3G. Based on 100% of the mass of the grey cloth, the added mass of each component in the reactive dye is: reactive red BES 0.8%, reactive yellow 3RE 0.9%, reactive military blue XL-3G 0.21%, the added amount of sodium sulfate is 28g / L, and the total added amount of soda ash is 12g / L;

[0086] (3) Post-processing

[0087] After washing, refill the tank with water, add glacial acetic acid, adjust the pH value to 6.0-6.8, heat to 55℃, add polishing enzyme, react for 25 minutes, then add soaping agent, run for 8 minutes, heat to 92℃ for soaping, keep warm for 12 minutes, and finally cool to 78℃, drain and rinse the grey cloth with clean water;

[0088] The concentrations of the additives are: polishing enzyme 1.2 g / L, soaping agent 1.5 g / L;

[0089] (4) Antibacterial finishing and shaping

[0090] Add water, antibacterial finishing agent, penetrant, and sodium laureth sulfate to the trough of the setting machine and stir evenly to form an antibacterial finishing liquid, wherein the addition amount of penetrant in the antibacterial finishing liquid is 1.5 g / L, the addition amount of sodium laureth sulfate is 2.5 g / L, and the addition amount of the antibacterial finishing agent is 2.5% of the mass of the grey cloth;

[0091] The grey cloth passes through the trough, double dip and double rolling, and the rolling rate is maintained at 80-90%;

[0092] Finally, the grey fabric is passed through a setting machine oven and dried at 160°C to obtain the antibacterial children's clothing fabric.

[0093] The antibacterial finishing agent comprises the following raw materials in parts by weight: 18 parts of antibacterial microcapsules, 9 parts of modified nano zinc oxide, and 12 parts of terminal carboxyl quaternary ammonium salt. The modified nano zinc oxide is prepared by the following method: adding nano zinc oxide into a reactor filled with water, ultrasonically dispersing for 30 minutes, then adding vinyl trimethoxyethoxysilane, heating to 55° C., stirring and reacting for 8 hours, then adding azobisisobutyronitrile into the reactor, heating to 75° C., adding 2-ethyl isocyanate of acrylic acid dropwise, reacting for 5 hours, and after the reaction is completed, centrifuging, washing, and drying to obtain the modified nano zinc oxide. The mass ratio of the nano zinc oxide, vinyl trimethoxyethoxysilane, azobisisobutyronitrile, and 2-ethyl isocyanate of acrylic acid is 2:1:0.05:0.6.

[0094] The carboxyl-terminated quaternary ammonium salt is prepared according to the following method: first, acrylamide is added to a reaction kettle containing acetone, N,N-dimethylethylenediamine is slowly added dropwise, and the mixture is stirred and reacted at room temperature for 25 hours. After the reaction is completed, the mixture is distilled under reduced pressure to obtain intermediate I, wherein the mass ratio of N,N-dimethylethylenediamine to acrylamide is 1:2.5; then, intermediate I is dissolved in dimethyl sulfoxide, bromohexane is added, and the mixture is reacted at 90°C for 3 days. After the reaction is completed, the mixture is post-treated to obtain intermediate II, wherein the molar ratio of intermediate I to bromohexane is 1:3; then, succinic anhydride is dissolved in chloroform and added dropwise to the reaction kettle containing intermediate II, and the mixture is reacted at 60°C for 6 hours. After the reaction is completed, the mixture is filtered, washed, and dried to obtain the carboxyl-terminated quaternary ammonium salt, wherein the molar ratio of intermediate II to succinic anhydride is 1:3.

[0095] The antibacterial microcapsules were prepared by the following method:

[0096] a. The composite essential oil and diphenylmethane diisocyanate were added to the toluene solvent and stirred to mix to obtain an oil phase, wherein the composite essential oil comprises the following mass fractions of the components: 24% artemisia essential oil, 22% Sichuan Buddha's hand essential oil, 36% cypress leaf essential oil, 18% Sichuan sunflower essential oil;

[0097] b. Add emulsifier OP-10 and dispersant to water and stir to mix to obtain an aqueous phase;

[0098] c. The oil phase obtained in the above step is mixed with the aqueous phase and homogenized to obtain an emulsion, wherein the mass ratio of the oil phase to the aqueous phase is 1:2-4, the mass fraction of the composite essential oil in the oil phase is 45%, the mass fraction of diphenylmethane diisocyanate is 30%, the mass fraction of the emulsifier OP-10 in the aqueous phase is 3%, and the mass fraction of the dispersant is 2%;

[0099] d. A 45% aqueous solution of aliphatic polyether diamine was added dropwise to the emulsion. After addition, the temperature was raised to 60°C and stirred for 2.5 hours. After the reaction, the mixture was filtered, washed with water, and dried to obtain antibacterial microcapsules. The aliphatic polyether diamine was polyetheramine D-400, produced by Wuhan Huaxiang Kejie Biotechnology Co., Ltd., with a mass ratio of 2:1 to diphenylmethane diisocyanate.

[0100] Example 3

[0101] A method for processing antibacterial children's clothing fabric comprises the following steps:

[0102] (1) Pretreatment

[0103] After the grey cloth is put into the vat, water is added and the temperature is raised to 50℃. High-efficiency energy-saving bath agent and degreasing agent are added. After running for 5 minutes, the temperature is raised to 70℃. Then hydrogen peroxide is added and the temperature is raised to 110℃. The temperature is kept for 40 minutes. Then the temperature is lowered to 78℃ and the water is drained. After washing, glacial acetic acid is added to adjust the pH value to 6.0-7.0. Deoxygenase is added and the temperature is raised to 50℃ for deoxidation. The residual oxygen content is less than 0.5mg, which is qualified.

[0104] The concentrations of the additives are: high-efficiency energy-saving bath agent 2.5g / L, hydrogen peroxide 3.0g / L, degreasing agent 3.0g / L, deoxidase 0.18g / L;

[0105] (2) Dyeing

[0106] Adjust the temperature to 50℃, add reactive dye into the vat, then add sodium sulfate, add the material for 15 minutes, react for 10 minutes, then add soda ash, add the soda ash twice, the first time is 1 / 10, add the material for 20 minutes, react for 5 minutes, adjust the pH value to 7.5-8.5, the second time is 9 / 10, add the material for 25 minutes, react for 10 minutes, adjust the pH value to 10.5-11.5, then heat to 60℃, keep warm for 40 minutes, and drain;

[0107] The reactive dye is composed of reactive red BES, reactive yellow 3RE and reactive military blue XL-3G. Based on 100% of the mass of the grey cloth, the added mass of each component in the reactive dye is: reactive red BES 1.0%, reactive yellow 3RE 0.2%, reactive military blue XL-3G 0.24%, the added amount of sodium sulfate is 30g / L, and the total added amount of soda ash is 15g / L;

[0108] (3) Post-processing

[0109] After washing, refill the tank with water, add glacial acetic acid, adjust the pH value to 6.0-6.8, heat to 55℃, add polishing enzyme, react for 30 minutes, then add soaping agent, run for 10 minutes, heat to 95℃ for soaping, keep warm for 10 minutes, and finally cool to 78℃, drain and rinse the grey cloth with clean water;

[0110] The concentrations of the additives are: polishing enzyme 1.5 g / L, soaping agent 2.0 g / L;

[0111] (4) Antibacterial finishing and shaping

[0112] Add water, antibacterial finishing agent, penetrant, and sodium laureth sulfate to the trough of the setting machine and stir evenly to form an antibacterial finishing liquid, wherein the addition amount of penetrant in the antibacterial finishing liquid is 2.0 g / L, the addition amount of sodium laureth sulfate is 3.5 g / L, and the addition amount of the antibacterial finishing agent is 2.0% of the mass of the grey cloth;

[0113] The grey cloth passes through the trough, double dip and double rolling, and the rolling rate is maintained at 80-90%;

[0114] Finally, the grey fabric is passed through a setting machine oven and dried at 170°C to obtain the antibacterial children's clothing fabric.

[0115] The antibacterial finishing agent comprises the following raw materials in parts by weight: 25 parts of antibacterial microcapsules, 12 parts of modified nano zinc oxide, and 15 parts of terminal carboxyl quaternary ammonium salt. The modified nano zinc oxide is prepared by the following method: adding nano zinc oxide into a reactor filled with water, ultrasonically dispersing for 40 minutes, then adding vinyl trimethoxyethoxy silane, heating to 60° C., stirring and reacting for 6 hours, then adding lauroyl peroxide into the reactor, heating to 80° C., dropwise adding 2-isocyanate acrylate, reacting for 6 hours, and centrifuging, washing, and drying after the reaction is completed to obtain the modified nano zinc oxide. The mass ratio of the nano zinc oxide, vinyl trimethoxyethoxy silane, lauroyl peroxide, and 2-isocyanate acrylate is 3:1:0.08:0.8.

[0116] The carboxyl-terminated quaternary ammonium salt is prepared according to the following method: first, acrylamide is added to a reaction kettle containing acetone, N,N-dimethylethylenediamine is slowly added dropwise, and the mixture is stirred and reacted at room temperature for 30 hours. After the reaction is completed, the mixture is distilled under reduced pressure to obtain intermediate I, wherein the mass ratio of N,N-dimethylethylenediamine to acrylamide is 1:3; then, intermediate I is dissolved in dimethyl sulfoxide, 1-bromooctane is added, and the mixture is reacted at 100° C. for 2 days. After the reaction is completed, the mixture is post-treated to obtain intermediate II, wherein the molar ratio of intermediate I to 1-bromooctane is 1:3.6; then, succinic anhydride is dissolved in chloroform and added dropwise to the reaction kettle containing intermediate II, and the mixture is reacted at 65° C. for 8 hours. After the reaction is completed, the mixture is filtered, washed, and dried to obtain the carboxyl-terminated quaternary ammonium salt, wherein the molar ratio of intermediate II to succinic anhydride is 1:4.

[0117] The antibacterial microcapsules were prepared by the following method:

[0118] a. The composite essential oil and diphenylmethane diisocyanate were added to the toluene solvent and stirred to mix to obtain an oil phase, wherein the composite essential oil comprises the following mass fractions of the components: 28% artemisia essential oil, 27% Sichuan Buddha's hand essential oil, 30% cypress leaf essential oil, 15% Sichuan sunflower essential oil;

[0119] b. Add Tween-80 and dispersant to water and stir to mix to obtain an aqueous phase;

[0120] c. The oil phase obtained in the above step is mixed with the aqueous phase and homogenized to obtain an emulsion, wherein the mass ratio of the oil phase to the aqueous phase is 1:4, the mass fraction of the composite essential oil in the oil phase is 50%, the mass fraction of diphenylmethane diisocyanate is 35%, the mass fraction of Tween-80 in the aqueous phase is 4%, and the mass fraction of the dispersant is 3%;

[0121] d. Add 55% mass concentration of aliphatic polyether diamine aqueous solution to the emulsion, raise the temperature to 65 ° C after the addition, stir and react for 3 hours, filter after the reaction, wash with water, and dry to obtain antibacterial microcapsules.

[0122] The aliphatic polyether diamine is CAED-900 polyether amine produced by Yangzhou Chenhua New Materials Co., Ltd., and the mass ratio of the aliphatic polyether diamine to diphenylmethane diisocyanate is 4:1.

[0123] Example 4

[0124] The processing method is basically the same as that of Example 3, except that no carboxyl-terminated quaternary ammonium salt is added to the antibacterial finishing agent, and other components are increased proportionally.

[0125] Example 5

[0126] The processing method is basically the same as that of Example 3, except that the artemisia essential oil is omitted from the core material component of the antibacterial microcapsule, and the contents of the remaining three essential oils are increased proportionally.

[0127] Example 6

[0128] The processing method is basically the same as that of Example 3, except that Sichuan bergamot essential oil is omitted from the core material component of the antibacterial microcapsule, and the contents of the remaining three essential oils are increased proportionally.

[0129] Example 7

[0130] The processing method is basically the same as that of Example 3, except that the cypress leaf essential oil is omitted from the core material component of the antibacterial microcapsule, and the contents of the remaining three essential oils are increased proportionally.

[0131] Example 8

[0132] The processing method is basically the same as that of Example 3, except that the sunflower oil is omitted from the core material component of the antibacterial microcapsule, and the contents of the remaining three essential oils are increased proportionally.

[0133] Example 9

[0134] The processing method is basically the same as that of Example 3, except that all the core components of the antibacterial microcapsules are replaced with artemisia essential oil.

[0135] Example 10

[0136] The processing method is basically the same as that of Example 3, except that all the core components of the antibacterial microcapsules are replaced with thyme essential oil.

[0137] The antibacterial and wrinkle resistance properties of the children's clothing fabrics prepared in the above examples were tested, and the results are shown in Table 3. The antibacterial performance was determined by measuring the antibacterial rate according to the GB / T 20944.2-2007 standard method, and the wrinkle recovery angle according to the GB / T 3819-1997 standard method.

[0138] Table 3

[0139]

[0140] Among the various components of the composite essential oil, the antibacterial activity of mugwort essential oil is the highest. If the composite essential oil is all prepared with mugwort essential oil (i.e., embodiment 9), it is reasonable to expect that the fabric antibacterial rate prepared by embodiment 9 is better than embodiment 3, but the test results provided in table 3 are just the opposite, which shows that there is a certain correlation between the four components, which improves the antibacterial properties of the product. When ensuring that the total amount of addition remains unchanged, a certain essential oil component is omitted, and the remaining three essential oil components are increased in proportion (i.e., embodiment 5-8). The test results show that the antibacterial rate of the fabric prepared by embodiment 5-8 is not as good as embodiment 3, which shows that the four essential oil components have a synergistic promotion effect, and lacking any one of them will cause antibacterial performance to decline. The inventor further extends, and the total mass of the composite essential oil remains unchanged, omitting two of the essential oil components, and the remaining two essential oil components are increased in proportion. The test results show that antibacterial performance is not as good as embodiment 5-8, which further shows that the four natural plant essential oil components have a synergistic promotion effect. Thyme essential oil has high antibacterial activity and its antibacterial property is far superior to the four natural plant essential oils used in this application. When it is applied to the core material of the antibacterial microcapsule (ie, Example 10), it is reasonable to expect that the antibacterial rate of the fabric prepared in Example 10 is better than that in Example 3, but the actual test results show that the antibacterial effect is comparable, indicating that the compound use of Artemisia argyi essential oil, Sichuan Buddha's hand essential oil, cypress leaf essential oil, and Sichuan sunflower essential oil can produce a synergistic promotion effect and achieve an antibacterial effect of 1+1>2. The inventor further extended it and replaced any one of the four natural plant essential oils with thyme essential oil of equal mass, with the total mass remaining unchanged. The antibacterial performance test results are as follows: the antibacterial effect of the prepared fabric is not as good as that in Example 3, indicating that there is a synergistic effect between the four natural plant essential oils. If any one of them is replaced, the antibacterial rate will decline to a certain extent. However, there is no synergistic antibacterial effect between thyme essential oil and other essential oils or the synergistic antibacterial effect is relatively weak.

[0141] The above records are merely examples of the technical content of this invention. Any modifications and changes made by a person familiar with this technology using this invention are within the patent scope claimed by this invention, and are not limited to those disclosed in the examples.

Claims

1. A method for processing antibacterial children's clothing fabric, characterized by: The following steps are involved: (1) Pretreatment After the grey cloth is put into the vat, water is added and the temperature is raised to 40-50℃. High-efficiency energy-saving bath agent and degreasing agent are added. After running for 5 minutes, the temperature is raised to 70℃. Then hydrogen peroxide is added and the temperature is raised to 110℃. The temperature is kept for 20-40 minutes. Then the temperature is lowered to 78℃ and the water is drained. After washing, glacial acetic acid is added to adjust the pH value to 6.0-7.

0. Deoxygenase is added and the temperature is raised to 50℃ for deoxidation. The residual oxygen content is less than 0.5mg, which is qualified. (2) Dyeing Adjust the temperature to 40-50℃, add reactive dye to the vat, then add sodium sulfate, add the material for 15 minutes, react for 10 minutes, then add soda ash, add the soda ash twice, the first time is 1 / 10, add the material for 20 minutes, react for 5 minutes, adjust the pH value to 7.5-8.5, the second time is 9 / 10, add the material for 25 minutes, react for 10 minutes, adjust the pH value to 10.5-11.5, then heat to 60℃, keep warm for 30-40 minutes, and drain; (3) Post-processing After washing, refill the tank with water, add glacial acetic acid, adjust the pH value to 6.0-6.8, heat to 55℃, add polishing enzyme, react for 20-30min, then add soaping agent, run for 5-10min, heat to 90-95℃ for soaping, keep warm for 10-15min, finally cool to 78℃, drain, and rinse the grey cloth with clean water; (4) Antibacterial finishing and shaping Add water, antibacterial finishing agent, penetrant, and sodium laureth sulfate to the trough of the setting machine, and stir evenly to form an antibacterial finishing liquid, wherein the addition amount of penetrant in the antibacterial finishing liquid is 1.0-2.0 g / L, the addition amount of sodium laureth sulfate is 1.5-3.5 g / L, and the addition amount of antibacterial finishing agent is 2.0-3.0% of the mass of the grey fabric; The grey cloth passes through the trough, double dip and double rolling, and the rolling rate is maintained at 80-90%; Finally, the grey fabric is passed through a setting machine oven and dried at 150-170°C to obtain antibacterial children's clothing fabric; The antibacterial finishing agent comprises the following raw materials in parts by weight: 12-25 parts of antibacterial microcapsules, 6-12 parts of modified nano zinc oxide, and 8-15 parts of carboxyl-terminated quaternary ammonium salt. The antibacterial microcapsules are prepared by interfacial polymerization using a composite essential oil as a core material. The composite essential oil comprises the following components in the following mass fractions: 20-28% of mugwort essential oil, 22-30% of Sichuan bergamot essential oil, 30-40% of cypress leaf essential oil, and 10-18% of Sichuan sunflower essential oil. The modified nano zinc oxide is prepared by the following method: adding nano zinc oxide to a reactor filled with water, ultrasonically dispersing for 20-40 minutes, then adding vinyl trimethoxyethoxy silane, heating to 50-60° C., stirring and reacting for 6-10 hours, then adding an initiator to the reactor, heating to 70-80° C., dropwise adding 2-ethyl isocyanate of acrylic acid, reacting for 3-6 hours, and after the reaction is completed, centrifuging, washing, and drying to obtain the modified nano zinc oxide; The antibacterial microcapsules are prepared by the following method: a. The composite essential oil and diphenylmethane diisocyanate were added to the toluene solvent and stirred to mix to obtain an oil phase; b. Add the emulsifier and dispersant to water and stir to mix to obtain an aqueous phase; c. The oil phase obtained in the above step is mixed with the aqueous phase and homogenized to obtain an emulsion, wherein the mass ratio of the oil phase to the aqueous phase is 1:2-4, the mass fraction of the composite essential oil in the oil phase is 35-50%, the mass fraction of diphenylmethane diisocyanate is 25-35%, the mass fraction of the emulsifier in the aqueous phase is 2-4%, and the mass fraction of the dispersant is 1-3%; d. Add a 35-55% aqueous solution of aliphatic polyether diamine to the emulsion, heat to 55-65°C after the addition, stir and react for 2-3h, filter after the reaction, wash with water, and dry to obtain antibacterial microcapsules; The grey cloth is cotton fabric.

2. The method for processing antibacterial children's clothing fabric according to claim 1, characterized in that: step The concentrations of the additives in step (1) are: high-efficiency energy-saving bath agent 2.0-2.5g / L, hydrogen peroxide 1.0-3.0g / L, Degreasing agent 2.0-3.0g / L, dehydrogenase 0.12-0.18g / L.

3. The method for processing antibacterial children's clothing fabric according to claim 1, characterized in that: In step (2), the amount of sodium sulfate added is 25-30 g / L, and the amount of soda ash added is 10-15 g / L.

4. The method for processing antibacterial children's clothing fabric according to claim 1, characterized in that: The reactive dye consists of reactive red BES, reactive yellow 3RE and reactive military blue XL-3G. Based on 100% of the mass of the grey cloth, the added mass of each component in the reactive dye is: reactive red BES 0.5-1.0%, reactive yellow 3RE 0.2-1.5%, and reactive military blue XL-3G 0.18-0.24%.

5. The method for processing antibacterial children's clothing fabric according to claim 1, characterized in that: The concentrations of the auxiliary agents in step (3) are: polishing enzyme 1.0-1.5 g / L, soaping agent 1.0-2.0 g / L.

6. The method for processing antibacterial children's clothing fabric according to claim 1, characterized in that: The nano zinc oxide, vinyl trimethoxyethoxysilane, initiator, 2-ethyl isocyanate The mass ratio is 1-3:1:0.02-0.08:0.5-0.

8.

7. The method for processing antibacterial children's clothing fabric according to claim 1, characterized in that: The mass ratio of the aliphatic polyether diamine to diphenylmethane diisocyanate is 2-4:1.

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