CN119567691A - Multilayer composite nylon fabric and preparation method thereof - Google Patents
Multilayer composite nylon fabric and preparation method thereof Download PDFInfo
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- CN119567691A CN119567691A CN202510137295.5A CN202510137295A CN119567691A CN 119567691 A CN119567691 A CN 119567691A CN 202510137295 A CN202510137295 A CN 202510137295A CN 119567691 A CN119567691 A CN 119567691A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
- B32B5/08—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer the fibres or filaments of a layer being of different substances, e.g. conjugate fibres, mixture of different fibres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/18—Handling of layers or the laminate
- B32B38/1825—Handling of layers or the laminate characterised by the control or constructional features of devices for tensioning, stretching or registration
- B32B38/1833—Positioning, e.g. registration or centering
- B32B38/1841—Positioning, e.g. registration or centering during laying up
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
- B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
- B32B5/26—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B1/00—Preparatory treatment of cellulose for making derivatives thereof, e.g. pre-treatment, pre-soaking, activation
- C08B1/02—Rendering cellulose suitable for esterification
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B3/00—Preparation of cellulose esters of organic acids
- C08B3/14—Preparation of cellulose esters of organic acids in which the organic acid residue contains substituents, e.g. NH2, Cl
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/42—Polyamides containing atoms other than carbon, hydrogen, oxygen, and nitrogen
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/90—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/02—Synthetic macromolecular fibres
- B32B2262/0261—Polyamide fibres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/06—Vegetal fibres
- B32B2262/062—Cellulose fibres, e.g. cotton
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/14—Mixture of at least two fibres made of different materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/70—Other properties
- B32B2307/714—Inert, i.e. inert to chemical degradation, corrosion
- B32B2307/7145—Rot proof, resistant to bacteria, mildew, mould, fungi
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Abstract
The invention relates to the technical field of nylon fabric, and discloses a multilayer composite nylon fabric and a preparation method thereof. The multilayer composite nylon fabric comprises an inner layer, an antibacterial layer and an outer layer, wherein the inner layer is prepared by mixing and weaving nylon fibers and cotton fibers, the antibacterial layer is prepared by weaving antibacterial fibers, the outer layer is prepared by weaving modified nylon fibers, a composite antibacterial agent, sodium alginate and chitin are introduced into the antibacterial fibers, the antibacterial, the moisture absorption and the air permeability of the fabric are improved under the synergistic effect of the antibacterial agent, the sodium alginate and the chitin, and the modified nylon fibers are sulfonic groups with extremely strong hydrophilicity, so that the hydrophilicity of the fibers is improved, and the air permeability and the moisture absorption of the fabric are further improved.
Description
Technical Field
The invention relates to the technical field of nylon fabric, in particular to a multilayer composite nylon fabric and a preparation method thereof.
Background
Nylon fabric, also called polyamide fabric, has the advantages of good wear resistance, elasticity, corrosion resistance and the like, and is made into clothing, textiles and the like. However, with the continuous progress of textile technology and the improvement of living standard of people, the performance requirements of the market on the clothing fabric are increasingly diversified. Although the traditional single-layer nylon fabric has good wear resistance and elasticity, the traditional single-layer nylon fabric has the defects in the aspects of antistatic, quick drying, ventilation and the like, and is difficult to meet the requirements of modern consumers on high-performance and multifunctional fabrics.
For example, the traditional nylon fabric is poor in moisture absorption and sweat release, is easy to cause uncomfortable wearing, does not have antibacterial performance, cannot effectively kill existing bacteria, and inhibits the breeding and reproduction of the bacteria, so that the transmission and infection of viruses and bacteria are reduced. Therefore, the nylon fabric formed by compounding the multi-layer fabrics with different functions can be designed according to different demands of people, so that the requirements of people on the aspects of antibiosis, moisture absorption, ventilation and the like of the fabric are met.
Disclosure of Invention
In order to solve the technical problems, the invention provides a multilayer composite nylon fabric and a preparation method thereof.
The aim of the invention can be achieved by the following technical scheme:
The multi-layer composite nylon fabric comprises an inner layer, an antibacterial layer and an outer layer from top to bottom, wherein the inner layer is formed by mixing and weaving nylon fibers and cotton fibers according to the proportion of 2:1, the antibacterial layer is formed by interweaving antibacterial fibers, and the outer layer is formed by weaving modified nylon fibers;
The antibacterial fiber consists of the following raw materials, by weight, 40-60 parts of polyamide solution, 3-6 parts of sodium alginate, 5-10 parts of a composite antibacterial agent and 1-4 parts of chitin;
The composite antibacterial agent is prepared by the following steps:
step A1, ultrasonically dispersing cellulose in acetic acid solution with the concentration of 1-2wt%, stirring for 3-5 hours at the temperature of 40-50 ℃, filtering, washing and drying to obtain pretreated cellulose;
further, in the step A1, the mass ratio of the cellulose to the acetic acid solution is 1:10;
Step A2, uniformly mixing and stirring pretreated cellulose and 2, 3-dimercaptosuccinic acid in DMF (N, N-dimethylformamide), adding p-toluenesulfonic acid, reacting for 1h at 120-140 ℃ under nitrogen, reacting for 1.5-2.5h under vacuum, adding acetone and N-hexane, uniformly stirring, and distilling under reduced pressure to obtain modified cellulose;
Further, the dosage ratio of the pretreated cellulose, the 2, 3-dimercaptosuccinic acid, the DMF, the p-toluenesulfonic acid, the acetone and the n-hexane in the step A2 is 2-5g to 1-3g to 100mL to 0.005-0.015g to 50mL to 20mL;
step A3, adding modified cellulose into DMF under the condition of nitrogen, mixing and stirring uniformly, slowly dripping 0.15-0.25mol/L copper nitrate solution, regulating the pH value of the solution to 8-9, heating to 40 ℃, reacting for 1-3h, distilling under reduced pressure, and drying to obtain the composite antibacterial agent;
Further, the dosage ratio of the modified cellulose, DMF and copper nitrate solution in the step A3 is 3-5g:50mL:20mL.
The modified nylon fiber is prepared by the following steps:
Step B1, adding 5-amino isophthalic acid into N, N dimethyl acetamide, mixing and stirring uniformly, transferring to ice water bath, standing for 10-20min, adding triethylamine, adding undecylenoyl chloride for three times, stirring for 30min at 0-5 ℃, transferring to an oil bath pot, heating to 55-75 ℃, reacting for 4-8h, separating out, washing, drying, recrystallizing, and drying for the second time to obtain a carboxyl end product;
further, in the step B1, the dosage ratio of the 5-amino isophthalic acid, the N, N dimethylacetamide, the triethylamine and the undecylenoyl chloride is 0.1-0.3mol:100mL:2.3-7mL:0.1-0.3mol;
Step B2, mixing and stirring the carboxyl-terminated product, anhydrous sodium sulfite and sodium nitrate uniformly in a flask containing DMF, heating to reflux, slowly dropwise adding sodium bisulfite solution, dropwise adding for 1h, continuously reacting for 8-10h at 90-105 ℃, and obtaining a sulfonated product through chromatography, washing and drying;
Further, in the step B2, the dosage ratio of the carboxyl end product to the anhydrous sodium sulfite, the sodium nitrate to the DMF to the sodium bisulfite solution is 1.7-5.1g to 0.095-0.284 g to 0.07-0.21g to 100mL to 21.5-24.6g, and the sodium bisulfite solution is formed by mixing and stirring sodium bisulfite and deionized water according to the mass ratio of 1.56-4.68:20;
step B3, dispersing the sulfonated product and hexamethylenediamine in equal amount of ethanol respectively to form a sulfonated product solution and a hexamethylenediamine solution, dropwise adding the sulfonated product solution into the hexamethylenediamine solution, heating to 50-70 ℃, stirring and reacting for 1-3 hours, carrying out suction filtration, drying, and collecting sulfonated product-hexamethylenediamine salt; mixing caprolactam, sulfonated product-hexamethylenediamine salt and deionized water, uniformly stirring, transferring into a reaction kettle, replacing gas in the reaction kettle by nitrogen for three times, heating to 100 ℃, starting stirring, heating to 230-250 ℃, maintaining the pressure at 0.5-0.6MPa for 2-4h, adjusting the pressure in the reaction kettle to normal pressure, introducing nitrogen, continuing to react for 4-6h, vacuumizing, continuing to react for 30-60min, standing for 10min, discharging, casting the belt, granulating to obtain hydrophilic polyamide chips, and performing melt spinning to obtain modified nylon fibers;
Further, the mass ratio of the sulfonated product of the step B3, the hexamethylenediamine and the caprolactam is 1-2:0.26-0.52:47.48-48.74, and the deionized water is 4-5% of the total mass of reactants.
The preparation method of the multilayer composite nylon fabric comprises the following steps:
Step S1, weighing raw materials according to parts by weight, mixing a polyamide solution, sodium alginate, a composite antibacterial agent and chitin, and then melt spinning to obtain antibacterial fibers, and interweaving the antibacterial fibers to form an antibacterial layer;
s2, mixing and weaving nylon fibers and cotton fibers according to a ratio of 2:1 to form an inner layer, and weaving modified nylon fibers to form an outer layer;
And S3, stacking the inner layer, the antibacterial layer and the outer layer in sequence from top to bottom, aligning and compositing to obtain the multi-layer composite nylon fabric.
The invention has the beneficial effects that:
The multilayer composite nylon fabric comprises an inner layer, an antibacterial layer and an outer layer, wherein the inner layer is prepared by mixing and weaving nylon fibers and cotton fibers, the antibacterial layer is prepared by weaving antibacterial fibers, the outer layer is prepared by weaving modified nylon fibers, a composite antibacterial agent, sodium alginate and chitin are introduced into the antibacterial fibers, the antibacterial, the moisture absorption and the air permeability of the fabric are improved under the synergistic effect of the antibacterial agent, the sodium alginate and the chitin, and the modified nylon fibers are sulfonic groups with extremely strong hydrophilicity, so that the hydrophilicity of the fibers is improved, and the air permeability and the moisture absorption of the fabric are further improved.
The preparation method comprises the steps of preparing cellulose, preparing modified cellulose by pre-treating cellulose with dilute acid, introducing active groups (carboxyl and sulfhydryl) into cellulose by esterification reaction, and complexing copper ions with the active groups on the modified cellulose to obtain the composite antibacterial agent. The composite antibacterial agent can cooperate with natural antibacterial components (sodium alginate and chitin) to improve the antibacterial performance of the fiber, wherein the composite antibacterial agent can not only utilize the interaction of hydroxyl groups in cellulose molecules with bacteria, viral proteins and lipids to destroy the structure and function of the bacteria and kill the bacteria, but also utilize the surface metal complex to release metal copper ions, and utilize the reaction of the metal ions with ester bonds and olefin structures in the lipid to cause oxidation, rupture and damage of cell membrane lipids so as to kill the bacteria, thereby enabling the fiber to have lasting antibacterial effect.
In addition, the composite antibacterial agent, sodium alginate and chitin introduced into the antibacterial fiber have good hydrophilicity, so that the hydrophilicity of the polyamide fiber can be effectively improved, and the air permeability and the hygroscopicity of the fabric are improved.
In the modified nylon fiber, 5-amino isophthalic acid and undecylenoyl chloride are firstly utilized to react to prepare a carboxyl end product, double bonds in the carboxyl end product and sodium bisulphite are utilized to carry out sulfonation reaction to prepare a sulfonated product, and then the sulfonated product, hexamethylenediamine and caprolactam are used as raw materials to synthesize the modified nylon fiber. The modified nylon fiber is used as the material of the woven outer layer, so that the air permeability and the moisture absorption performance of the fabric can be remarkably improved, because the modified nylon fiber is introduced with the sulfonic acid group with excellent hydrophilicity, the hydrophilic performance of the nylon fiber is improved on the basis of not reducing the original mechanical performance, and the benzene ring structure is introduced into the main chain of the polyamide molecule, so that the mechanical performance of the fiber can be improved.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1 a composite antimicrobial agent was prepared by the following steps:
Step A1, performing ultrasonic dispersion on 10g of cellulose in 100g of acetic acid solution with the concentration of 1wt%, stirring for 3 hours at the temperature of 40 ℃, filtering, washing and drying to obtain pretreated cellulose;
Step A2, mixing and stirring 2g of pretreated cellulose and 1g of 2, 3-dimercaptosuccinic acid uniformly in 100mL of DMF, adding 0.005g of p-toluenesulfonic acid, reacting for 1h at 120 ℃ under nitrogen, reacting for 1.5h under vacuum, adding 50mL of acetone and 20mL of n-hexane, stirring uniformly, and distilling under reduced pressure to obtain modified cellulose;
And A3, adding 3g of modified cellulose into 50mL of DMF under the condition of nitrogen, uniformly mixing and stirring, slowly dropwise adding 20mL of 0.15mol/L copper nitrate solution, regulating the pH value of the solution to 8, heating to 40 ℃, reacting for 1h, distilling under reduced pressure, and drying to obtain the composite antibacterial agent.
The modified nylon fiber is prepared by the following steps:
Step B1, adding 0.1mol of 5-amino isophthalic acid into 100mL of N, N dimethylacetamide, mixing and stirring uniformly, transferring into ice water bath, standing for 10min, adding 2.3mL of triethylamine, adding 0.1mol of undecylenoyl chloride for three times, stirring for 30min at 0 ℃, transferring into an oil bath pot, heating to 55 ℃, reacting for 4h, separating out, washing, drying, recrystallizing, and drying for the second time to obtain a carboxyl end product;
Step B2, mixing and stirring 1.7g of carboxyl end product, 0.095g of anhydrous sodium sulfite and 0.07g of sodium nitrate uniformly in a flask containing 100mL of DMF, heating to reflux, slowly dropwise adding 21.5g of sodium bisulfite solution, dropwise adding for 1h, maintaining the temperature at 90 ℃ for continuous reaction for 8h, and performing chromatography, washing and drying to obtain a sulfonated product, wherein the sodium bisulfite solution is prepared by mixing and stirring sodium bisulfite and deionized water according to a mass ratio of 1.56:20;
And B3, dispersing 1g of sulfonated product and 0.26g of hexamethylenediamine in 10mL of ethanol respectively to form a sulfonated product solution and a hexamethylenediamine solution, dropwise adding the sulfonated product solution into the hexamethylenediamine solution, heating to 50 ℃ for stirring reaction for 1h, carrying out suction filtration and drying, collecting sulfonated product-hexamethylenediamine salt, mixing 48.74g of caprolactam, sulfonated product-hexamethylenediamine salt and 2g of deionized water, uniformly stirring, transferring into a reaction kettle, replacing gas in the reaction kettle by nitrogen for three times, heating to 100 ℃, starting stirring, heating to 230 ℃, maintaining the pressure at 0.5MPa for 2h, adjusting the pressure in the reaction kettle to normal pressure, introducing nitrogen, continuing to react for 4-6h, vacuumizing, continuing to react for 30-60min, standing for 10min, discharging, casting a belt, granulating to obtain hydrophilic polyamide chips, and carrying out melt spinning to obtain the modified nylon fiber.
Example 2a composite antimicrobial agent was prepared by the following steps:
step A1, performing ultrasonic dispersion on 10g of cellulose in 100g of acetic acid solution with the concentration of 1.5wt%, stirring for 4 hours at the temperature of 45 ℃, filtering, washing and drying to obtain pretreated cellulose;
Step A2, mixing 3.5g of pretreated cellulose and 2g of 2, 3-dimercaptosuccinic acid in 100mL of DMF, stirring uniformly, adding 0.01g of p-toluenesulfonic acid, reacting for 1h at 130 ℃ under nitrogen, reacting for 2h under vacuum, adding 50mL of acetone and 20mL of n-hexane, stirring uniformly, and distilling under reduced pressure to obtain modified cellulose;
And A3, adding 4g of modified cellulose into 50mL of DMF under the condition of nitrogen, mixing and stirring uniformly, slowly dripping 20mL of 0.2mol/L copper nitrate solution, regulating the pH value of the solution to 8.5, heating to 40 ℃, reacting for 2 hours, distilling under reduced pressure, and drying to obtain the composite antibacterial agent.
The modified nylon fiber is prepared by the following steps:
Step B1, adding 0.2mol of 5-amino isophthalic acid into 100mL of N, N dimethylacetamide, mixing and stirring uniformly, transferring into ice water bath, standing for 15min, adding 4.6mL of triethylamine, adding 0.2mol of undecylenoyl chloride for three times, stirring for 30min at 2 ℃, transferring into an oil bath pot, heating to 65 ℃, reacting for 4-8h, separating out, washing, drying, recrystallizing, and drying for the second time to obtain a carboxyl end product;
Step B2, mixing and stirring 3.4g of carboxyl end product, 0.19g of anhydrous sodium sulfite and 0.14g of sodium nitrate uniformly in a flask containing 100mL of DMF, heating to reflux, slowly dropwise adding 23g of sodium bisulfite solution, dropwise adding for 1h, maintaining the temperature at 100 ℃ for continuous reaction for 9h, and performing chromatography, washing and drying to obtain a sulfonated product, wherein the sodium bisulfite solution is prepared by mixing and stirring sodium bisulfite and deionized water according to a mass ratio of 3.12:20;
And B3, dispersing 1.5g of sulfonated product and 0.39g of hexamethylenediamine in 10mL of ethanol respectively to form a sulfonated product solution and a hexamethylenediamine solution, dropwise adding the sulfonated product solution into the hexamethylenediamine solution, heating to 60 ℃, stirring for reacting for 2 hours, carrying out suction filtration, drying, collecting sulfonated product-hexamethylenediamine salt, mixing 48.11g of caprolactam, sulfonated product-hexamethylenediamine salt and 2.3g of deionized water uniformly, transferring into a reaction kettle, replacing gas in the reaction kettle by nitrogen for three times, heating to 100 ℃, starting stirring, heating to 240 ℃ and maintaining the pressure at 0.55MPa for reacting for 3 hours, adjusting the pressure in the reaction kettle to normal pressure, introducing nitrogen, continuing to react for 5 hours, vacuumizing, continuing to react for 45 minutes, standing for 10 minutes, discharging, casting a belt, granulating, obtaining hydrophilic polyamide chips, and carrying out melt spinning to obtain the modified nylon fiber.
Example 3A composite antimicrobial agent was prepared by the following steps:
step A1, performing ultrasonic dispersion on 10g of cellulose in 100g of 2wt% acetic acid solution, stirring for 5 hours at 50 ℃, filtering, washing and drying to obtain pretreated cellulose;
step A2, uniformly mixing and stirring 5g of pretreated cellulose and 3g of 2, 3-dimercaptosuccinic acid in 100mL of DMF, adding 0.015g of p-toluenesulfonic acid, reacting for 1h at 140 ℃ under nitrogen, reacting for 2.5h under vacuum, adding 50mL of acetone and 20mL of n-hexane, uniformly stirring, and distilling under reduced pressure to obtain modified cellulose;
and A3, adding 5g of modified cellulose into 50mL of DMF under the condition of nitrogen, uniformly mixing and stirring, slowly dripping 20mL of 0.25mol/L copper nitrate solution, regulating the pH value of the solution to 9, heating to 40 ℃, reacting for 3h, distilling under reduced pressure, and drying to obtain the composite antibacterial agent.
The modified nylon fiber is prepared by the following steps:
Step B1, adding 0.3mol of 5-amino isophthalic acid into 100mL of N, N dimethylacetamide, mixing and stirring uniformly, transferring into ice water bath, standing for 20min, adding 7mL of triethylamine, adding 0.3mol of undecylenoyl chloride for three times, stirring for 30min at 5 ℃, transferring into an oil bath pot, heating to 75 ℃, reacting for 8h, separating out, washing, drying, recrystallizing, and drying for the second time to obtain a carboxyl end product;
step B2, mixing and stirring 5.1g of carboxyl end product, 0.285g of anhydrous sodium sulfite and 0.21g of sodium nitrate uniformly in a flask containing 100mL of DMF, heating to reflux, slowly dropwise adding 24.6g of sodium bisulfite solution, dropwise adding for 1h, maintaining the temperature at 105 ℃ for continuous reaction for 10h, and performing chromatography, washing and drying to obtain a sulfonated product, wherein the sodium bisulfite solution is prepared by mixing and stirring sodium bisulfite and deionized water according to a mass ratio of 4.68:20;
And B3, dispersing 2g of sulfonated product and 0.52g of hexamethylenediamine in 10mL of ethanol respectively to form a sulfonated product solution and a hexamethylenediamine solution, dropwise adding the sulfonated product solution into the hexamethylenediamine solution, heating to 70 ℃ for stirring reaction for 3 hours, carrying out suction filtration and drying, collecting sulfonated product-hexamethylenediamine salt, mixing 47.48g of caprolactam, sulfonated product-hexamethylenediamine salt and 2.5g of deionized water, uniformly stirring, transferring into a reaction kettle, replacing gas in the reaction kettle by nitrogen for three times, heating to 100 ℃, starting stirring, heating to 250 ℃, maintaining the pressure at 0.6MPa for reaction for 4 hours, adjusting the pressure in the reaction kettle to normal pressure, introducing nitrogen, continuing to react for 6 hours, vacuumizing, continuing to react for 60 minutes, standing for 10 minutes, discharging, casting a belt, cutting into particles, obtaining hydrophilic polyamide chips, and carrying out melt spinning to obtain the modified nylon fiber.
Example 4A preparation method of the multilayer composite nylon fabric comprises the following steps:
Step S1, weighing raw materials according to parts by weight, mixing 40 parts of polyamide solution, 3 parts of sodium alginate, 5 parts of the composite antibacterial agent prepared in the embodiment 1 and 1 part of chitin, and then melt spinning to obtain antibacterial fibers, and interweaving the antibacterial fibers to form an antibacterial layer;
s2, mixing and weaving nylon fibers and cotton fibers according to a ratio of 2:1 to form an inner layer, and weaving the modified nylon fibers prepared in the embodiment 1 to form an outer layer;
And S3, stacking the inner layer, the antibacterial layer and the outer layer in sequence from top to bottom, aligning and compositing to obtain the multi-layer composite nylon fabric.
Example 5A preparation method of the multilayer composite nylon fabric comprises the following steps:
Step S1, weighing raw materials according to parts by weight, mixing 50 parts of polyamide solution, 4.5 parts of sodium alginate, 7.5 parts of the composite antibacterial agent prepared in the example 2 and 2.5 parts of chitin, and then melt spinning to obtain antibacterial fibers, and interweaving the antibacterial fibers to form an antibacterial layer;
S2, mixing and weaving nylon fibers and cotton fibers according to a ratio of 2:1 to form an inner layer, and weaving the modified nylon fibers prepared in the embodiment 2 to form an outer layer;
And S3, stacking the inner layer, the antibacterial layer and the outer layer in sequence from top to bottom, aligning and compositing to obtain the multi-layer composite nylon fabric.
Example 6A preparation method of the multilayer composite nylon fabric comprises the following steps:
Step S1, weighing raw materials according to parts by weight, mixing 60 parts of polyamide solution, 6 parts of sodium alginate, 10 parts of the composite antibacterial agent prepared in the embodiment 3 and 4 parts of chitin, and then melt spinning to obtain antibacterial fibers, and interweaving the antibacterial fibers to form an antibacterial layer;
s2, mixing and weaving nylon fibers and cotton fibers according to a ratio of 2:1 to form an inner layer, and weaving the modified nylon fibers prepared in the embodiment 3 to form an outer layer;
And S3, stacking the inner layer, the antibacterial layer and the outer layer in sequence from top to bottom, aligning and compositing to obtain the multi-layer composite nylon fabric.
Comparative example 1 this comparative example is a nylon fabric, which differs from example 6 in that the commercial quaternary ammonium salt antimicrobial agent was used instead of the composite antimicrobial agent prepared in example 3, and the remainder were identical.
Comparative example 2 this comparative example is a nylon fabric, which differs from example 6 in that the modified nylon fiber prepared in example 3 was replaced with a nylon fiber, and the rest were the same.
Performance testing was performed on the nylon fabrics prepared in examples 4-6 and comparative examples 1-2:
antibacterial performance test, namely testing according to GB/T20944.3-2008 textile antibacterial performance evaluation part 3: vibration method, and analyzing the antibacterial rate of each nylon fabric after washing for 100 times;
Air permeability test, namely detecting the air permeability (mm/s) of the nylon fabric by using GBT5453-1997 'determination of air permeability of textile fabrics';
the hygroscopicity test is carried out according to GB/T21655.1-2008, 1 st part of evaluation of moisture absorption and quick drying Property of textiles, single item combination test method;
the test results are shown in table 1:
TABLE 1 Performance test results
As can be seen from Table 1, the multi-layer composite nylon fabric prepared by the invention has excellent antibacterial property, air permeability and hygroscopicity after being tested.
The foregoing is merely illustrative and explanatory of the principles of the invention, as various modifications and additions may be made to the specific embodiments described, or similar alternatives may be made by those skilled in the art, without departing from the scope of the invention as defined by the principles of the invention.
Claims (10)
1. A multi-layer composite nylon fabric is characterized by sequentially comprising an inner layer, an antibacterial layer and an outer layer from top to bottom, wherein the inner layer is formed by mixing and weaving nylon fibers and cotton fibers according to the proportion of 2:1, the antibacterial layer is formed by interweaving antibacterial fibers, and the outer layer is formed by weaving modified nylon fibers;
the antibacterial fiber consists of, by weight, 40-60 parts of polyamide solution, 3-6 parts of sodium alginate, 5-10 parts of a composite antibacterial agent and 1-4 parts of chitin.
2. The multilayer composite nylon fabric of claim 1, wherein the composite antimicrobial agent is prepared by the steps of:
step A1, ultrasonically dispersing cellulose in acetic acid solution with the concentration of 1-2wt%, stirring for 3-5 hours at the temperature of 40-50 ℃, filtering, washing and drying to obtain pretreated cellulose;
Step A2, uniformly mixing and stirring pretreated cellulose and 2, 3-dimercaptosuccinic acid in DMF, adding p-toluenesulfonic acid, reacting for 1h at 120-140 ℃ under nitrogen, reacting for 1.5-2.5h under vacuum, adding acetone and n-hexane, uniformly stirring, and distilling under reduced pressure to obtain modified cellulose;
And A3, adding the modified cellulose into DMF under the condition of nitrogen, mixing and stirring uniformly, slowly dripping 0.15-0.25mol/L copper nitrate solution, regulating the pH value of the solution to 8-9, heating to 40 ℃, reacting for 1-3h, distilling under reduced pressure, and drying to obtain the composite antibacterial agent.
3. The multilayer composite nylon fabric according to claim 1, wherein the mass ratio of cellulose to acetic acid solution in the step A1 is 1:10.
4. The multilayer composite nylon fabric according to claim 1, wherein the dosage ratio of the pretreated cellulose, the 2, 3-dimercaptosuccinic acid, the DMF, the p-toluenesulfonic acid, the acetone and the n-hexane in the step A2 is 2-5g to 1-3g to 100mL to 0.005-0.015g to 50mL to 20mL.
5. The multilayer composite nylon fabric according to claim 1, wherein the dosage ratio of the modified cellulose, DMF and copper nitrate solution in the step A3 is 3-5 g/50 mL/20 mL.
6. The multilayer composite nylon fabric of claim 1, wherein the modified nylon fiber is prepared by the steps of:
Step B1, adding 5-amino isophthalic acid into N, N dimethyl acetamide, mixing and stirring uniformly, transferring to ice water bath, standing for 10-20min, adding triethylamine, adding undecylenoyl chloride for three times, stirring for 30min at 0-5 ℃, transferring to an oil bath pot, heating to 55-75 ℃, reacting for 4-8h, separating out, washing, drying, recrystallizing, and drying for the second time to obtain a carboxyl end product;
Step B2, mixing and stirring the carboxyl-terminated product, anhydrous sodium sulfite and sodium nitrate uniformly in a flask containing DMF, heating to reflux, slowly dropwise adding sodium bisulfite solution, dropwise adding for 1h, continuously reacting for 8-10h at 90-105 ℃, and obtaining a sulfonated product through chromatography, washing and drying;
And B3, dispersing the sulfonated product and hexamethylenediamine in equal amount of ethanol to form a sulfonated product solution and a hexamethylenediamine solution, dropwise adding the sulfonated product solution into the hexamethylenediamine solution, heating to 50-70 ℃ for stirring reaction for 1-3 hours, carrying out suction filtration and drying, collecting sulfonated product-hexamethylenediamine salt, mixing and stirring caprolactam, sulfonated product-hexamethylenediamine salt and deionized water uniformly, transferring the mixture into a reaction kettle, replacing gas in the reaction kettle by nitrogen for three times, heating to 100 ℃, starting stirring, heating to 230-250 ℃, maintaining the pressure at 0.5-0.6MPa for 2-4 hours, adjusting the pressure in the reaction kettle to normal pressure, introducing nitrogen, continuing to react for 4-6 hours, vacuumizing, continuing to react for 30-60 minutes, standing for 10 minutes, discharging, casting a belt, granulating, obtaining hydrophilic polyamide chips, and carrying out melt spinning to obtain the modified nylon fiber.
7. The multilayer composite nylon fabric according to claim 6, wherein the dosage ratio of 5-amino isophthalic acid, N dimethylacetamide, triethylamine and undecylenoyl chloride in the step B1 is 0.1-0.3mol:100mL:2.3-7mL:0.1-0.3mol.
8. The multilayer composite nylon fabric according to claim 6, wherein in the step B2, the carboxyl end product, anhydrous sodium sulfite, sodium nitrate, DMF and sodium bisulphite solution are mixed and stirred according to the mass ratio of 1.7-5.1 g:0.095-0.284 g:0.07-0.21g:100mL:21.5-24.6g, and the sodium bisulphite solution is formed by mixing sodium bisulphite and deionized water according to the mass ratio of 1.56-4.68:20.
9. The multilayer composite nylon fabric according to claim 6, wherein the mass ratio of sulfonated product, hexamethylenediamine and caprolactam in the step B3 is 1-2:0.26-0.52:47.48-48.74%, and deionized water is 4-5% of the total mass of the reactants.
10. A method for preparing the multilayer composite nylon fabric as claimed in any one of claims 1 to 9, comprising the following steps:
Step S1, weighing raw materials according to parts by weight, mixing a polyamide solution, sodium alginate, a composite antibacterial agent and chitin, and then melt spinning to obtain antibacterial fibers, and interweaving the antibacterial fibers to form an antibacterial layer;
s2, mixing and weaving nylon fibers and cotton fibers according to a ratio of 2:1 to form an inner layer, and weaving modified nylon fibers to form an outer layer;
And S3, stacking the inner layer, the antibacterial layer and the outer layer in sequence from top to bottom, aligning and compositing to obtain the multi-layer composite nylon fabric.
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| US20220333278A1 (en) * | 2021-04-07 | 2022-10-20 | LUOLAI LIFESTYLE TECHNOLOGY Co.,Ltd. | Antibacterial textile and preparation method thereof |
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| KR20110032236A (en) * | 2009-09-22 | 2011-03-30 | 주식회사 효성 | Polyamide-based Release Section Fibers and Manufacturing Method Thereof |
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| US20220333278A1 (en) * | 2021-04-07 | 2022-10-20 | LUOLAI LIFESTYLE TECHNOLOGY Co.,Ltd. | Antibacterial textile and preparation method thereof |
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