Preparation method of polyester-nylon composite yarn with silver-plated surface
By modifying the coextrusion spinning technology of chitosan with polyester and polyamide 6, and using glucose as a reducing agent, a polyester and brocade composite wire with silver plated surface was prepared, which solved the problems of environmental pollution in the existing silver plated fiber process and uneven adhesion of silver particles, and achieved excellent mechanical, antibacterial and conductive properties of the composite wire.
Patent Information
- Application Number
- CN202510450212.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-11
- Publication Date
- 2025-06-06
AI Technical Summary
The existing silver plating fiber process has environmental pollution problems, and the surface of the polyester composite silk is highly hydrophobic, making it difficult to evenly adhere silver particles.
Using glucose as a reducing agent, polyester and polyamide 6 is prepared by coextrusion spinning technology of modified chitosan, polyester and polyamide 6. The method includes steps such as drying, mixing, spinning, side-blowing cooling, oiling, winding, oil removal, coarsing, activation and reduction of silver plating.
The excellent mechanical properties and antibacterial properties of the composite wire are achieved. At the same time, due to the use of glucose as a reducing agent, the process is more environmentally friendly and the adhesion effect of the silver ions is good, ensuring the efficient conductive and electromagnetic shielding performance of the composite wire.
Smart Images

Figure BDA0005353783380000031 
Figure BDA0005353783380000041 
Figure BDA0005353783380000051
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of polyester-nylon composite yarns, and in particular relates to a method for preparing polyester-nylon composite yarns with silver-plated surfaces. Background Art
[0002] With the rapid development of the modern textile industry, the research and application of functional fiber materials has gradually become an important direction of the industry. Among the many functional fibers, composite fibers with silver coating on the surface have attracted much attention due to their unique conductivity, antibacterial and electromagnetic shielding properties. These properties make them show broad application prospects in high-end clothing, medical protection, smart wearable devices and electronic textiles.
[0003] At present, the application demand of surface silver-plated fibers is growing, especially in the medical and electronic fields. For example, in the medical field, silver-plated fibers can be used to make antibacterial dressings or surgical gowns. Its excellent antibacterial properties can effectively inhibit bacterial reproduction and reduce the risk of infection. In smart wearable devices, it can be used as a flexible circuit substrate to provide lightweight and flexible solutions for wearable electronic devices. In addition, in the aerospace and military fields, silver-plated fibers can also be used as electromagnetic shielding materials to protect sensitive electronic components from external electromagnetic interference. However, the existing silver plating process still mostly uses the traditional cyanide-containing reduction system, which has certain pollution to the environment.
[0004] Polyester-nylon composite yarn is a special-section fiber made of polyester (PET) and polyamide (PA) through co-extrusion spinning technology. This composite structure gives the fiber a variety of excellent properties, such as high strength, high elastic modulus, good hygroscopicity and softness. However, the surface of polyester-nylon composite yarn is usually hydrophobic, which makes it difficult for silver particles to adhere evenly. In summary, the above problems need to be solved urgently to meet the higher requirements in the field of polyester-nylon composite yarn technology. Summary of the invention
[0005] The purpose of the present invention is to overcome the defects of the prior art and provide a method for preparing a polyester-nylon composite yarn with a silver-plated surface.
[0006] The purpose of the present invention can be achieved through the following technical solutions:
[0007] A method for preparing a polyester-nylon composite yarn with a silver-plated surface comprises the following steps:
[0008] A1, drying the polyester slices in an oven, mixing with modified chitosan after drying, adding them into a twin-screw extruder, and melt blending to obtain modified polyester;
[0009] A2. The modified polyester and polyamide 6 slices obtained in step A1 are melted separately to obtain polyester spinning melt and nylon spinning melt, and the two are mixed and then spun, side-blown cooled, oiled, and wound to obtain polyester-nylon composite yarn, and finally the surface is silver-plated to obtain polyester-nylon composite yarn with silver surface.
[0010] Nylon is expensive to use alone, so we use polyester to form a composite yarn structure to reduce the cost of the silver-plated substrate. The combination of the two fibers gives the composite yarn excellent mechanical properties.
[0011] Furthermore, the raw materials are calculated in parts by weight as follows: 47-59 parts of polyester chips, 5-15 parts of modified chitosan, and 33-41 parts of polyamide 6 chips.
[0012] Furthermore, the surface silver plating comprises the following steps:
[0013] B1. Degreasing treatment: the polyester-nylon composite yarn is completely immersed in an acetone / sodium hydroxide solution (the mass fraction of sodium hydroxide is 10%) for immersion washing, and then degreasing is performed by ultrasonic vibration for 2-10 minutes to obtain the degreasing polyester-nylon composite yarn;
[0014] B2. Roughening treatment: the degreased polyester-nylon composite yarn is placed in a sodium hydroxide solution (mass fraction is 10%), and subjected to low-frequency oscillation treatment for 3-10 minutes in a water bath at 60-80° C. to obtain a roughened polyester-nylon composite yarn;
[0015] B3, activation treatment: in a stannous chloride solution with a concentration of 10-20g / L, hydrochloric acid (mass fraction of 12%) is added dropwise to adjust the pH to 1.5-3.0, and then the roughened polyester-nylon composite yarn is added to the solution, soaked for 0.5-10min, and then a thiourea solution with a concentration of 0.1-1mg / L is added to obtain the activated polyester-nylon composite yarn;
[0016] B4. Reduction silver plating: Mix a glucose solution with a concentration of 5-10g / L and a silver ammonia solution in a volume ratio of 1:5-10, add the activated polyester-nylon composite yarn, and soak it in an environment of 30-70℃ for 4-6h to obtain a polyester-nylon composite yarn with a silver-plated surface.
[0017] In this process, glucose acts as a reducing agent to reduce the silver ions (Ag + ) is reduced to metallic silver and evenly deposited on the fiber surface. Compared with other reducing agents, it is more environmentally friendly.
[0018] Further, the silver ammonia solution in step B4 is prepared by the following steps:
[0019] At room temperature, add ammonia water (mass fraction 25%) dropwise into a 5-20 g / L silver nitrate solution, stirring while adding, until the generated precipitate is just completely dissolved to form a clear and transparent solution, and adjust the pH to 8-11 to obtain a silver ammonia solution.
[0020] The solution can form an activation layer on the fiber surface, enhancing the adsorption and deposition effect of silver ions in the subsequent silver plating process.
[0021] Furthermore, the modified chitosan is prepared by the following steps:
[0022] S1, acetic anhydride and dimethyl sulfoxide were added to a three-necked flask equipped with a magnetic stirrer, a condenser and a thermometer, and the air was excluded and the reaction was carried out for 30 minutes to fully activate the dimethyl sulfoxide. Polyethylene glycol (PEG, molecular weight 400) was then vacuum dried at 80°C for 4 hours and then added to the three-necked flask. The reaction temperature was controlled to be 60°C and the reaction was kept warm for 6 hours. After the reaction was completed, the solution was added to ice ether, and the solution was layered. The lower layer was repeatedly added to the ice ether until a powdery solid precipitate appeared. The solid precipitate was placed in a fume hood to remove the residual ether to obtain an intermediate product 1; the ratio of acetic anhydride, dimethyl sulfoxide and polyethylene glycol was 21.3 g:100 mL:39.8 g;
[0023] Using the oxidation method, the terminal hydroxyl group of PEG is oxidized to obtain the intermediate product 1. The specific reaction process is as follows:
[0024]
[0025] S2. Add ethylenediamine, 5-chloro-2-methyl-4-isothiazoline-3-one (CMIT), potassium carbonate and N,N-dimethylformamide into a three-necked flask equipped with a magnetic stirrer, a condenser and a thermometer, slowly heat to 70°C, and keep warm for 5 hours. After the reaction is completed, add deionized water, stir evenly and filter, take the filter residue, wash it with anhydrous ethanol for several times, and vacuum dry to obtain intermediate 2; the ratio of ethylenediamine, 5-chloro-2-methyl-4-isothiazoline-3-one, potassium carbonate and N,N-dimethylformamide is 6.2g:14.8g:13.8g:100mL;
[0026] Under the catalysis of potassium carbonate, 5-chloro-2-methyl-4-isothiazolin-3-one and ethylenediamine undergo nucleophilic substitution. By controlling the molar ratio of the two to be close to 1:1 and a slight excess of ethylenediamine, only one amino group on ethylenediamine participates in the reaction to obtain intermediate 2. The specific reaction is shown below:
[0027]
[0028] S3, intermediate product 1, intermediate product 2, piperidine and N, N-dimethylformamide are added to a three-necked flask equipped with a magnetic stirrer, a condenser and a thermometer, the reaction temperature is controlled to 75 ° C, stirring continuously during the reaction, and the reaction is completed after 6 hours of reaction. Part of the solvent is removed by distillation under reduced pressure, and then purified by column chromatography (eluent is a mixed solvent of petroleum ether / ethyl acetate, and the volume ratio of the two is 2:1), and the eluent is removed by rotary evaporation to obtain intermediate product 3; the ratio of the amount of intermediate product 1, intermediate product 2, piperidine and N, N-dimethylformamide is 53.3g:17.3g:15mL:200mL;
[0029] The aldehyde group on the intermediate product 1 condenses with the amino group on the intermediate product 2 to form an imine group (C=N Schiff base structure), and the intermediate product 1 is in excess to obtain the intermediate product 3; the specific reaction process is as follows:
[0030]
[0031] S4, chitosan was added to a three-necked flask equipped with a magnetic stirrer, a condenser and a thermometer, and hydrochloric acid solution was added thereto, and the mixture was stirred continuously until the chitosan was completely dissolved, and the intermediate product 3, piperidine and N,N-dimethylformamide were mixed and added to the flask, and the temperature was controlled to 70°C. After stirring for 6 hours, sodium hydroxide solution was added to adjust the pH to 11, and the reaction was continued for 2 hours. After the reaction was completed, the mixture was allowed to stand for precipitation, filtered, washed with ethanol and water in turn, and dried in an oven to obtain modified chitosan; the ratio of chitosan, hydrochloric acid solution, intermediate product 3, piperidine and N,N-dimethylformamide was 1g:10mL:16.7g:7.3mL:100mL;
[0032] Under the action of the condensation agent, the aldehyde group on the intermediate product 3 condenses with the amino group on the chitosan to form an imine group (C=N Schiff base structure) to obtain modified chitosan;
[0033] Chitosan is a natural degradable material with good stability and antibacterial properties. Chitosan has good hydrophilicity and can improve the hydrophilicity of the substrate, so that the silver-plated particles can be better attached to the substrate. In addition, by modifying chitosan and connecting it with the organic molecular chain through C=N, the hydrogen bonding effect of the chitosan amino group is weakened, and the biological activity and antibacterial properties of chitosan are improved. Moreover, the modified chitosan molecule also contains a polyethylene glycol molecular chain, which can further improve the hydrophilicity of the substrate. Finally, the introduced isothiazolinone has excellent properties such as strong antibacterial ability, environmental safety and a broad antibacterial spectrum. It forms a disulfide bond with the thiol group on the cysteine in the pathogen protein through the bond active site on the heterocycle, thereby inactivating the protein to achieve the purpose of sterilization. It can synergize with Schiff base and chitosan to greatly improve the antibacterial properties of the substrate.
[0034] Beneficial effects of the present invention:
[0035] 1. The composite yarn prepared by the present invention combines polyester and nylon fibers, giving the composite yarn excellent mechanical properties;
[0036] 2. Silver plating uses glucose as a reducing agent, which is more environmentally friendly than other reducing agents;
[0037] 3. The prepared modified chitosan has good hydrophilicity, which can improve the hydrophilicity of the composite silk, enhance the adhesion effect of silver ions on the surface of the composite silk, ensure the firm and uniform adhesion of silver ions, and further improve the antibacterial property of the composite silk;
[0038] In summary, the composite yarn prepared by the present invention has good adhesion effect on silver ions, excellent mechanical properties and antibacterial properties, and is environmentally friendly, and has important application value in the field of polyester-nylon composite yarn technology. DETAILED DESCRIPTION
[0039] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0040] Embodiment 1
[0041] Preparation of modified chitosan:
[0042] S1, 21.3g of acetic anhydride and 100mL of dimethyl sulfoxide were added to a three-necked flask equipped with a magnetic stirrer, a condenser and a thermometer, and the air was excluded and the reaction was carried out for 30min to fully activate the dimethyl sulfoxide. Then, 39.8g of polyethylene glycol (PEG, molecular weight 400) was vacuum dried at 80°C for 4h, and then added to the three-necked flask. The reaction temperature was controlled to 60°C and the reaction was kept warm for 6h. After the reaction was completed, the solution was added to ice ether, and the solution was layered. The lower layer liquid was repeatedly added to the ice ether until a powdery solid precipitate appeared. The solid precipitate was placed in a fume hood to remove the residual ether to obtain an intermediate product 1;
[0043] S2, add 6.2g ethylenediamine, 14.8g 5-chloro-2-methyl-4-isothiazoline-3-one, 13.8g potassium carbonate and 100mL N,N-dimethylformamide into a three-necked flask equipped with a magnetic stirrer, a condenser and a thermometer, slowly heat to 70°C, keep warm for 5h, and after the reaction is complete, add deionized water, stir evenly and filter, take the filter residue, wash it with anhydrous ethanol for several times, and vacuum dry it to obtain intermediate 2;
[0044] S3, 53.3g of intermediate product 1, 17.3g of intermediate product 2, 15mL of piperidine and 200mL of N,N-dimethylformamide were added to a three-necked flask equipped with a magnetic stirrer, a condenser and a thermometer, the reaction temperature was controlled to 75°C, stirring was continued during the reaction, and after 6h of reaction, the reaction was completed, part of the solvent was distilled off under reduced pressure, and then purified by column chromatography (the eluent was a mixed solvent of petroleum ether / ethyl acetate, and the volume ratio of the two was 2:1), and the eluent was removed by rotary evaporation to obtain intermediate product 3;
[0045] S4. Add 1 g of chitosan into a three-necked flask equipped with a magnetic stirrer, a condenser and a thermometer, then drop 10 mL of hydrochloric acid solution into it, and keep stirring until the chitosan is completely dissolved. Then mix 16.7 g of intermediate product 3, 7.3 mL of piperidine and 100 mL of N,N-dimethylformamide, add to the flask, control the temperature to 70 ° C, stir for 6 hours, then drop sodium hydroxide solution to adjust the pH to 11, continue the reaction for 2 hours, and after the reaction is completed, let it stand and precipitate, filter, wash with ethanol and water in turn, and dry in an oven to obtain modified chitosan.
[0046] Embodiment 2
[0047] Preparation of modified chitosan:
[0048] S1, 42.6g of acetic anhydride and 200mL of dimethyl sulfoxide were added to a three-necked flask equipped with a magnetic stirrer, a condenser and a thermometer, and the air was excluded and the reaction was carried out for 30min to fully activate the dimethyl sulfoxide. Then, 79.6g of polyethylene glycol (PEG, molecular weight 400) was vacuum dried at 80°C for 4h, and then added to the three-necked flask. The reaction temperature was controlled to 60°C and the reaction was kept warm for 6h. After the reaction was completed, the solution was added to ice ether, and the solution was layered. The lower layer liquid was repeatedly added to the ice ether until a powdery solid precipitate appeared. The solid precipitate was placed in a fume hood to remove the residual ether to obtain an intermediate product 1;
[0049] S2, add 12.4g ethylenediamine, 29.6g 5-chloro-2-methyl-4-isothiazoline-3-one, 27.6g potassium carbonate and 200mL N,N-dimethylformamide into a three-necked flask equipped with a magnetic stirrer, a condenser and a thermometer, slowly heat to 70°C, keep warm for 5h, and after the reaction is complete, add deionized water, stir evenly and filter, take the filter residue, wash it with anhydrous ethanol for several times, and vacuum dry it to obtain intermediate 2;
[0050] S3, 106.6g of intermediate product 1, 34.6g of intermediate product 2, 30mL of piperidine and 400mL of N,N-dimethylformamide were added to a three-necked flask equipped with a magnetic stirrer, a condenser and a thermometer, the reaction temperature was controlled to 75°C, stirring was continued during the reaction, the reaction was completed after 6h, part of the solvent was distilled off under reduced pressure, and then purified by column chromatography (the eluent was a mixed solvent of petroleum ether / ethyl acetate, the volume ratio of the two was 2:1), and the eluent was removed by rotary evaporation to obtain intermediate product 3;
[0051] S4. Add 2 g of chitosan into a three-necked flask equipped with a magnetic stirrer, a condenser and a thermometer, then drop 20 mL of hydrochloric acid solution into it, and keep stirring until the chitosan is completely dissolved. Then mix 33.4 g of intermediate product 3, 14.6 mL of piperidine and 200 mL of N,N-dimethylformamide, add to the flask, control the temperature to 70 ° C, stir for 6 hours, then drop sodium hydroxide solution to adjust the pH to 11, continue the reaction for 2 hours, and after the reaction is completed, let it stand and precipitate, filter, wash with ethanol and water in turn, and dry in an oven to obtain modified chitosan.
[0052] Embodiment 3
[0053] A1, 47g of polyester chips were dried in an oven, mixed with 5g of modified chitosan prepared in Example 1 after drying, and then added into a twin-screw extruder, and melt-blended to obtain modified polyester;
[0054] A2, melting the modified polyester obtained in step A1 and 33g of polyamide 6 slices respectively to obtain polyester spinning melt and nylon spinning melt, mixing the two, spinning, side-blowing cooling, oiling, winding, to obtain polyester-nylon composite yarn, and finally silver-plating the surface to obtain polyester-nylon composite yarn with silver surface;
[0055] The surface silver plating comprises the following steps:
[0056] B1. Degreasing treatment: the polyester-nylon composite yarn is completely immersed in an acetone / sodium hydroxide solution (the mass fraction of sodium hydroxide is 10%) for immersion washing, and then degreasing is performed by ultrasonic vibration for 2 minutes to obtain the degreasing polyester-nylon composite yarn;
[0057] B2. Roughening treatment: the degreased polyester-nylon composite yarn is placed in a sodium hydroxide solution (mass fraction is 10%), and subjected to low-frequency oscillation treatment for 3 minutes in a water bath at 60° C. to obtain a roughened polyester-nylon composite yarn;
[0058] B3, activation treatment: hydrochloric acid (mass fraction of 12%) was added dropwise to a 10 g / L stannous chloride solution to adjust the pH to 1.5, and then the roughened polyester-nylon composite yarn was added to the solution, soaked for 0.5 min, and then a 0.1 mg / L thiourea solution was added to obtain the activated polyester-nylon composite yarn;
[0059] B4, reduction silver plating: a 5 g / L glucose solution and a silver ammonia solution were mixed in a volume ratio of 1:5, and then the activated polyester-nylon composite yarn was added and immersed in an environment of 30°C for 4 hours to obtain a polyester-nylon composite yarn with a silver-plated surface;
[0060] The silver ammonia solution is prepared by the following steps:
[0061] At room temperature, add ammonia water (mass fraction 25%) dropwise into a 5 g / L silver nitrate solution while stirring until the precipitate is completely dissolved to form a clear and transparent solution, and adjust the pH to 8 to obtain a silver ammonia solution.
[0062] Embodiment 4
[0063] A1, 53g of polyester chips were dried in an oven, mixed with 10g of modified chitosan prepared in Example 2 after drying, and then added into a twin-screw extruder, and melt-blended to obtain modified polyester;
[0064] A2, melting the modified polyester obtained in step A1 and 37g of polyamide 6 slices respectively to obtain polyester spinning melt and nylon spinning melt, mixing the two, spinning, side-blowing cooling, oiling, winding, to obtain polyester-nylon composite yarn, and finally silver-plating the surface to obtain polyester-nylon composite yarn with silver surface;
[0065] The surface silver plating comprises the following steps:
[0066] B1. Degreasing treatment: the polyester-nylon composite yarn is completely immersed in an acetone / sodium hydroxide solution (the mass fraction of sodium hydroxide is 10%) for immersion washing, and then degreasing is performed by ultrasonic vibration for 6 minutes to obtain the degreasing polyester-nylon composite yarn;
[0067] B2. Roughening treatment: the degreased polyester-nylon composite yarn is placed in a sodium hydroxide solution (mass fraction is 10%), and subjected to low-frequency oscillation treatment for 6 minutes in a water bath at 70° C. to obtain a roughened polyester-nylon composite yarn;
[0068] B3, activation treatment: hydrochloric acid (mass fraction of 12%) was added dropwise to a 15g / L stannous chloride solution to adjust the pH to 2.0, and then the roughened polyester-nylon composite yarn was added to the solution, soaked for 5 minutes, and then a 0.5mg / L thiourea solution was added to obtain the activated polyester-nylon composite yarn;
[0069] B4, reduction silver plating: a 7g / L glucose solution and a silver ammonia solution were mixed in a volume ratio of 1:7, and then the activated polyester-nylon composite yarn was added and immersed in an environment of 50°C for 5h to obtain a polyester-nylon composite yarn with a silver-plated surface;
[0070] The silver ammonia solution is prepared by the following steps:
[0071] At room temperature, add ammonia water (mass fraction 25%) dropwise into a 12 g / L silver nitrate solution while stirring until the precipitate is completely dissolved to form a clear and transparent solution, and adjust the pH to 9 to obtain a silver ammonia solution.
[0072] Embodiment 5
[0073] A1, 59g of polyester chips were dried in an oven, mixed with 15g of modified chitosan prepared in Example 2 after drying, and then added into a twin-screw extruder, and melt-blended to obtain modified polyester;
[0074] A2, melting the modified polyester obtained in step A1 and 41g of polyamide 6 slices respectively to obtain polyester spinning melt and nylon spinning melt, mixing the two, spinning, side-blowing cooling, oiling, winding, to obtain polyester-nylon composite yarn, and finally silver-plating the surface to obtain polyester-nylon composite yarn with silver surface;
[0075] The surface silver plating comprises the following steps:
[0076] B1. Degreasing treatment: the polyester-nylon composite yarn is completely immersed in an acetone / sodium hydroxide solution (the mass fraction of sodium hydroxide is 10%) for immersion washing, and then degreasing is performed by ultrasonic vibration for 10 minutes to obtain the degreasing polyester-nylon composite yarn;
[0077] B2. Roughening treatment: the degreased polyester-nylon composite yarn is placed in a sodium hydroxide solution (mass fraction is 10%), and subjected to low-frequency oscillation treatment for 10 minutes in a water bath at 80° C. to obtain a roughened polyester-nylon composite yarn;
[0078] B3, activation treatment: hydrochloric acid (mass fraction of 12%) was added dropwise to a 20 g / L stannous chloride solution to adjust the pH to 3.0, and then the roughened polyester-nylon composite yarn was added to the solution, soaked for 10 min, and then a 1 mg / L thiourea solution was added to obtain the activated polyester-nylon composite yarn;
[0079] B4, reduction silver plating: a 10 g / L glucose solution and a silver ammonia solution were mixed in a volume ratio of 1:10, and then the activated polyester-nylon composite yarn was added and immersed in an environment of 70°C for 6 hours to obtain a polyester-nylon composite yarn with a silver-plated surface;
[0080] The silver ammonia solution is prepared by the following steps:
[0081] At room temperature, add ammonia water (mass fraction 25%) dropwise into a 20 g / L silver nitrate solution while stirring until the precipitate is completely dissolved to form a clear and transparent solution, and adjust the pH to 11 to obtain a silver ammonia solution.
[0082] Comparative Example 1
[0083] Ordinary chitosan of the same mass was used to replace the modified chitosan in Example 5, and the remaining steps were the same as those in Example 5.
[0084] Comparative Example 2
[0085] Commercially available silver-coated fibers were used.
[0086] The following performance tests were performed on Examples 3, 4, 5 and Comparative Examples 1 and 2 according to different test standards:
[0087] The elongation at break was determined using the national standard GB / T 3923.1-2013 “Tensile properties of textile fabrics Part 1: Determination of breaking strength and elongation at break (strip method)”;
[0088] The national standard GB / T 20944.2-2007 "Evaluation of antibacterial properties of textiles - Part 2: Absorption method" was used to determine the antibacterial rates of Escherichia coli and Staphylococcus aureus in Examples 3, 4, and 5 before and after 40 washes;
[0089] The measured results are shown in the following table:
[0090]
[0091] It can be seen from the above table that the mechanical properties and antibacterial properties of the composite yarn prepared in the embodiment of the present invention are higher than those of the control example, and after multiple water treatments, the excellent antibacterial properties can still be guaranteed. Therefore, the present invention has important application value in the field of polyester-nylon composite yarn technology.
[0092] In the description of the specification, the description with reference to the terms "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.
[0093] The above contents are merely examples and explanations of the present invention. Those skilled in the art may make various modifications or additions to the specific embodiments described or replace them in a similar manner. As long as they do not deviate from the invention or exceed the scope defined by the claims, they shall all fall within the protection scope of the present invention.
Claims
1. A method for preparing a polyester-nylon composite yarn with a silver-plated surface, characterized in that: The following steps are involved: A1, drying the polyester slices in an oven, mixing with modified chitosan after drying, adding them into a twin-screw extruder, and melt blending to obtain modified polyester; A2. The modified polyester and polyamide 6 slices obtained in step A1 are melted separately to obtain polyester spinning melt and nylon spinning melt, and the two are mixed and then spun, side-blown cooled, oiled, and wound to obtain polyester-nylon composite yarn, and finally the surface is silver-plated to obtain polyester-nylon composite yarn with silver surface.
2. The method for preparing a polyester-nylon composite yarn with a silver-plated surface according to claim 1, characterized in that: The raw materials are calculated in parts by weight as follows: 47-59 parts of polyester chips, 5-15 parts of modified chitosan, and 33-41 parts of polyamide 6 chips.
3. The method for preparing a polyester-nylon composite yarn with a silver-plated surface according to claim 1, characterized in that: The modified chitosan is prepared by the following steps: S1, acetic anhydride and dimethyl sulfoxide were added to a flask, and the air was excluded and the reaction was carried out for 30 minutes. Then, the polyethylene glycol was dried and added to a three-necked flask, and the reaction was carried out at 60°C for 6 hours. After the reaction was completed, the solution was added to ice ether, and the solution was separated into layers. The lower layer was added to ice ether until precipitation occurred. The precipitation was placed in a fume hood to remove the residual ether to obtain an intermediate product 1; S2, add ethylenediamine, 5-chloro-2-methyl-4-isothiazoline-3-one, potassium carbonate and N,N-dimethylformamide into a flask, keep warm at 70°C for 5 hours, and after the reaction is complete, add deionized water, stir evenly and filter, take the filter residue, wash and vacuum dry to obtain intermediate 2; S3, adding intermediate product 1, intermediate product 2, piperidine and N,N-dimethylformamide into a flask, stirring and reacting at 75°C for 6 hours, the reaction is completed, and vacuum distillation, column chromatography purification, and rotary evaporation are performed to obtain intermediate product 3; S4. Add chitosan into a flask, and then add hydrochloric acid solution until the chitosan is completely dissolved. Then mix the intermediate product 3, piperidine and N,N-dimethylformamide, add them to the flask, stir at 70°C for 6 hours, adjust the pH to 11, and continue the reaction for 2 hours. After the reaction is completed, let it stand and precipitate, filter, wash, and dry to obtain modified chitosan.
4. The method for preparing a polyester-nylon composite yarn with a silver-plated surface according to claim 3, characterized in that: In step S1, the ratio of acetic anhydride, dimethyl sulfoxide and polyethylene glycol is 21.3 g:100 mL:39.8 g.
5. The method for preparing a polyester-nylon composite yarn with a silver-plated surface according to claim 3, characterized in that: In step S2, the ratio of ethylenediamine, 5-chloro-2-methyl-4-isothiazoline-3-one, potassium carbonate and N,N-dimethylformamide is 6.2 g:14.8 g:13.8 g:100 mL.
6. The method for preparing a polyester-nylon composite yarn with a silver-plated surface according to claim 3, characterized in that: In step S3, the ratio of the amount of intermediate product 1, intermediate product 2, piperidine and N,N-dimethylformamide is 53.3 g:17.3 g:15 mL:200 mL.
7. The method for preparing a polyester-nylon composite yarn with a silver-plated surface according to claim 3, characterized in that: In step S4, the ratio of chitosan, hydrochloric acid solution, intermediate product 3, piperidine and N,N-dimethylformamide is 1 g:10 mL:16.7 g:7.3 mL:100 mL.
8. The method for preparing a polyester-nylon composite yarn with a silver-plated surface according to claim 1, characterized in that: The surface silver plating comprises the following steps: B1. Degreasing treatment: the polyester-nylon composite yarn is completely immersed in an acetone / sodium hydroxide solution for immersion washing, and then degreasing is performed by ultrasonic vibration for 2-10 minutes to obtain the degreasing polyester-nylon composite yarn; B2. Roughening treatment: put the degreased polyester-nylon composite yarn into a sodium hydroxide solution, and perform low-frequency oscillation treatment for 3-10 minutes in a water bath at 60-80°C to obtain a roughened polyester-nylon composite yarn; B3. Activation treatment: add hydrochloric acid to the stannous chloride solution to adjust the pH to 1.5-3.0, then add the roughened polyester-nylon composite yarn to the solution, soak for 0.5-10 minutes, and then add thiourea solution to obtain the activated polyester-nylon composite yarn; B4. Reduction silver plating: Mix the glucose solution with the silver ammonia solution, add the activated polyester-nylon composite yarn, and soak it in an environment of 30-70°C for 4-6 hours to obtain the polyester-nylon composite yarn with silver plated surface.
9. The method for preparing a polyester-nylon composite yarn with a silver-plated surface according to claim 8, characterized in that: In step B4, the silver ammonia solution is prepared by the following steps: Add ammonia water dropwise into the silver nitrate solution while stirring until the precipitate is completely dissolved to form a clear and transparent solution. Adjust the pH to 8-11 to obtain a silver ammonia solution.