Long-acting antibacterial and bacteriostatic fiber and preparation method thereof

Abstract

The invention belongs to the field of polyester fiber preparation, and particularly relates to a long-acting antibacterial fiber and a preparation method thereof. The long-acting antibacterial and bacteriostatic fiber is prepared from the following raw materials in parts by mass: 85 to 100 parts of PET (Polyethylene Terephthalate) slices / master batches, 8 to 15 parts of graphene modified PET slices / master batches and 1.5 to 3 parts of a composite antibacterial agent. The antibacterial and bacteriostatic fiber prepared by the invention has excellent comprehensive performance and higher antibacterial performance, and still has better antistatic performance after being washed with water for 30 times.

Description

Technical Field

[0001] The invention belongs to the field of polyester fiber preparation, and specifically relates to a long-acting antibacterial and bacteriostatic fiber and a preparation method thereof. Background Art

[0002] Polyester fiber (PET fiber) is a synthetic fiber composed of macromolecular chains connected by ester groups. It is called polyester in China. This fiber has been widely used in the textile industry for its excellent properties, such as high breaking strength, high elastic modulus, moderate resilience, excellent heat setting effect, good heat resistance and light resistance, etc., such as for making various clothing and household items. In addition to the textile industry, polyester fiber can also be used in technical textiles (such as greenhouses, shade nets, filter materials, insulation materials, surgical gowns, masks, building reinforcement materials, automobile tire cords, seat belts), asphalt concrete improvement, non-woven fabrics, packaging materials, industrial and agricultural products and other fields.

[0003] The advantages of polyester fiber fabrics include sunshade, light transmission, ventilation, heat insulation, UV protection, fire prevention, moisture resistance, etc., but with the expansion of the application field of polyester fiber, the requirements for its performance are also increasing. The patent with publication number CN 108315835A discloses a polyester fiber with good antibacterial properties. The invention mixes TiO2 / zeolite antibacterial agent and Cu2O / zeolite antibacterial agent to form an antibacterial agent mixture, and then blends pure PET slices with the antibacterial agent mixture to prepare antibacterial modified PET slices, and then obtains polyester fibers with good antibacterial properties by melt spinning. However, the antibacterial property of the polyester fiber in this patent still needs to be improved. In addition, due to the poor hygroscopicity of polyester fiber, it is easy to generate static electricity, which will absorb dust and dirt, interfere with electronic equipment, and cause safety hazards in some special scenarios, such as coal mines, chemicals, petroleum processing and other industries. Static electricity may cause fires or explosions.

[0004] Polyester fiber has a bright future in the market. With the development of science and technology and the increasing demand for comfort and versatility of clothing, the development of new multifunctional and composite fibers is the future development direction. It is of great significance to expand the application scope of polyester fiber by improving the antibacterial and antimicrobial properties of polyester fiber through physical or chemical means while reducing its proneness to static electricity. Summary of the invention

[0005] The invention discloses a long-acting antibacterial and antimicrobial fiber and a preparation method thereof. The prepared composite antibacterial agent is used together with graphene-modified PET chips / masterbatches. The prepared antibacterial and antimicrobial fiber has excellent comprehensive performance, good antibacterial performance, and still has good antistatic performance after being washed 30 times.

[0006] To achieve the above purpose, the technical solution adopted by the present invention is as follows:

[0007] The first aspect of the present invention provides a long-acting antibacterial and bacteriostatic fiber, which comprises the following raw materials in terms of weight:

[0008] PET chips / masterbatch 85-100 parts, graphene modified PET chips / masterbatch 8-15 parts, composite antibacterial agent 1.5-3 parts.

[0009] In some embodiments, the preparation steps of the composite antibacterial agent are:

[0010] (1) dissolving zinc sulfate and copper sulfate in deionized water, adding citric acid thereto, stirring evenly, adjusting the pH, evaporating to dryness at 75-80° C. to form a wet gel, drying to constant weight to obtain a dry gel, calcining at 600-650° C. for 2-3 h, and cooling naturally to obtain antibacterial nanoparticles;

[0011] (2) dispersing silver powder in deionized water, adding the antibacterial nanoparticles and zeolite powder of step (1), stirring at 70-80° C. for 1-2 h, keeping the temperature constant, adding α-lipoic acid solution dropwise thereto, adjusting the pH to 5-6, adding water-soluble chitosan and sodium alginate, stirring for 1-2 h, adding α-lipoic acid solution dropwise again, adjusting the pH to 5-6, stirring at 60-70° C. until a viscous state is formed, drying, and grinding to obtain a composite antibacterial agent.

[0012] In some embodiments, the molar ratio of zinc sulfate, copper sulfate, and citric acid is 1:(0.04-0.06):(1.3-1.5).

[0013] Preferably, the molar ratio of zinc sulfate, copper sulfate and citric acid is 1:0.05:1.4.

[0014] In some embodiments, the mass ratio of silver powder, antibacterial nanoparticles and nano zeolite powder in step (2) is (1-3):(98-103):(260-280); the silver powder is flaky silver powder with an average particle size of 1-5 μm, and the zeolite powder has an average particle size of 2.5-10 μm.

[0015] Preferably, the mass ratio of the silver powder, the antibacterial nanoparticles and the zeolite powder is 2:100:270.

[0016] In some embodiments, the usage amounts of the water-soluble chitosan and sodium alginate are 6-7wt% and 3-3.5wt% of the total mass of the silver powder, antibacterial nanoparticles and nano-zeolite powder respectively; and the deacetylation degree of the water-soluble chitosan is ≥90%.

[0017] Preferably, the usage amounts of the water-soluble chitosan and sodium alginate are 6.5wt% and 3.25wt% of the total mass of the silver powder, the antibacterial nanoparticles and the nano-zeolite powder respectively.

[0018] In some embodiments, the preparation steps of the graphene-modified PET chips / masterbatch are:

[0019] S1: dispersing graphene oxide in an organic solvent, adding a condensing agent, ultrasonicating, then adding ethyl 3-aminobenzoate, stirring for 1-4 hours, separating, drying, dispersing the obtained solid in deionized water, adding a carboxyl activator, stirring, then adding hydroxymethyl chitosan, adjusting the pH, reacting at 20-30°C for 10-12 hours, separating, washing, and drying to obtain modified graphene;

[0020] S2: The modified graphene of step S1 is evenly mixed with the dried PET chips / masterbatch, and the mixture is co-extruded to prepare graphene-modified PET chips / masterbatch.

[0021] In some embodiments, the mass ratio of graphene oxide to ethyl 3-aminobenzoate is 1:(0.22-0.235).

[0022] Preferably, the mass ratio of the graphene oxide to ethyl 3-aminobenzoate is 1:0.23.

[0023] In some embodiments, the condensing agent is at least one of COFU, HATU, and DIPEA.

[0024] Preferably, the condensing agent is COFU.

[0025] In some embodiments, the solid is used in an amount of 0.01-0.03 wt % of the hydroxymethyl chitosan.

[0026] Preferably, the solid is used in an amount of 0.02 wt % of the hydroxymethyl chitosan.

[0027] In some embodiments, the carboxyl activating agent includes but is not limited to at least one of NHS and EDC.

[0028] In some embodiments, the amount of modified graphene used in step S2 is 0.005-0.015wt% of the PET chips / masterbatch.

[0029] Preferably, the amount of modified graphene used in step S2 is 0.01wt% of the PET chips / masterbatch.

[0030] The second aspect of the present invention provides a method for preparing the antibacterial and antibacterial fiber of the above scheme, comprising the following preparation steps:

[0031] The dried PET chips / masterbatch are evenly mixed with the composite antibacterial agent and graphene-modified PET chips / masterbatch, dried in a vacuum environment at 140-150° C. for 40-48 hours, put into a screw extruder for processing, spun, and then subjected to a drawing and oiling process to obtain antibacterial and antimicrobial fibers.

[0032] In some embodiments, the specific operation of feeding into the screw extruder for treatment is: feeding into the feeding port of the screw extruder, adjusting the temperature of each zone of the screw, and then extruding through the screw.

[0033] In some embodiments, the specific operation of spinning is:

[0034] Graphene oxide is a graphene derivative prepared by a chemical oxidation method, and its surface contains a large number of oxygen-containing functional groups such as hydroxyl, epoxy, and carboxyl. The present invention uses the functional groups of graphene oxide to perform functional modification through chemical reactions. First, in a specific condensing agent and solvent, the amino functional group of 3-aminobenzoic acid ethyl ester undergoes an amide condensation reaction with the carboxyl group on the surface of graphene oxide to form an amide bond, and 3-aminobenzoic acid ethyl ester is covalently bonded to the surface of graphene oxide; secondly, the hydroxymethyl functional group in hydroxymethyl chitosan reacts with the carboxyl group on the surface of graphene oxide to form a stable chemical bond to obtain functionalized modified graphene. The modified graphene has enhanced compatibility and antibacterial properties with PET due to the introduction of new functional groups, and can improve the antistatic properties of polyester fibers. This may be because the modified graphene has good electrical conductivity, and the modified graphene is evenly dispersed in the polyester fiber to form a conductive network, thereby improving the electrical conductivity and antistatic properties of the fiber. In addition, the high strength and rigidity of modified graphene can also enhance the mechanical properties of polyester fibers.

[0035] The present invention also synthesizes a composite antibacterial agent, which is applied to the preparation process of PET fiber, and can significantly improve the antibacterial and antibacterial properties of PET fiber. First, the present invention obtains antibacterial nanoparticles through zinc sulfate, copper sulfate and citric acid under a certain preparation process, and the copper ions in copper sulfate are reduced to copper nanoparticles through the reduction effect of citric acid, and the zinc ions in zinc sulfate can form a zinc nanostructure, which has excellent antibacterial effect. However, the antibacterial nanoparticles also have certain surface activity and catalytic activity, which will cause the aging speed of PET fiber to accelerate, which is not conducive to the long-term use of PET fiber. Therefore, the present invention mixes the synthesized antibacterial nanoparticles with silver powder and zeolite powder of a certain particle size, and the silver powder is an excellent antibacterial and conductive material, which can enhance the antibacterial property of the fiber while enhancing its antistatic performance; the zeolite powder can be used as a carrier to adsorb the antibacterial nanoparticles and the silver powder, reduce the catalytic performance of the antibacterial nanoparticles to a certain extent, slowly release the antibacterial active ingredients, and improve the antibacterial and antibacterial duration of the PET fiber. In addition, a composite antibacterial agent with good dispersibility, stability and sustained-release effect is prepared by reacting water-soluble chitosan, sodium alginate and α-lipoic acid. The water-soluble chitosan and sodium alginate with good biocompatibility and biodegradability form a stable gel network structure as a carrier of the antibacterial agent, and the antibacterial effect is enhanced and the catalytic activity is reduced through the antioxidant mechanism of α-lipoic acid. The composite antibacterial agent is applied to PET fiber to improve its antibacterial and antimicrobial properties and aging resistance.

[0036] Compared with the prior art, the present invention has the following beneficial effects:

[0037] 1. The present invention uses the prepared composite antibacterial agent together with graphene-modified PET chips / masterbatches to prepare antibacterial and antibacterial fibers with excellent comprehensive performance, good antibacterial performance, and good antistatic performance after washing 30 times.

[0038] 2. The present invention modifies graphene oxide and applies it to polyester fibers to form a conductive network, thereby improving the conductivity and antistatic properties of the polyester fibers. In addition, the high strength and rigidity of the modified graphene can also enhance the mechanical properties of the polyester fibers.

[0039] 3. The present invention also synthesizes a composite antibacterial agent, which is used in the preparation process of PET fiber, and can significantly improve the antibacterial and anti-aging properties of PET fiber. DETAILED DESCRIPTION

[0040] Now describe in detail various exemplary embodiments of the present invention, this detailed description should not be considered as limitation of the present invention, but should be understood as a more detailed description of certain aspects, characteristics and embodiments of the present invention. It should be understood that the terms described in the present invention are only for describing a particular embodiment, and are not used to limit the present invention. In addition, for the numerical range in the present invention, it should be understood that each intermediate value between the upper limit and the lower limit of the range is also specifically disclosed. Each smaller range between the intermediate value in any stated value or stated range and any other stated value or intermediate value in the range is also included in the present invention. The upper and lower limits of these smaller ranges can be independently included or excluded in the range.

[0041] Unless otherwise indicated, all technical and scientific terms used herein have the same meanings as commonly understood by those skilled in the art. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein may also be used in the practice or testing of the present invention. Various modifications and variations may be made to the specific embodiments of the present invention specification without departing from the scope or spirit of the present invention, which will be apparent to those skilled in the art. Other embodiments obtained from the present invention specification will be apparent to the technician. The present application specification and examples are exemplary only.

[0042] The words “include,” “including,” “have,” or “contain,” etc. used in this document are open-ended terms, meaning including but not limited to.

[0043] It should be noted that the drying method and spinning conditions of the PET chips / masterbatch described in the present invention are conventional operations of those skilled in the art and can be selected according to actual operations.

[0044] The mass fractions described in the following embodiments may be grams, kilograms, tons or other mass units.

[0045] The flaky silver powder used in the present invention was purchased from Jinlei Technology with the item number JL-Ag-P03; the zeolite powder used was 1500 mesh and was purchased from Chaoyang Xinhe Zeolite Technology Co., Ltd.; the water-soluble chitosan (deacetylation degree ≥ 90%) and hydroxymethyl chitosan used were purchased from Qingdao Hehai Biotechnology Co., Ltd.; the graphene oxide used was purchased from Hangzhou Gaoxun Technology Co., Ltd. with the item number GX-pGO-1; the PET slices used were purchased from Kanghui New Material Technology Co., Ltd.

[0046] Preparation Example 1

[0047] The preparation steps of the composite antibacterial agent are:

[0048] (1) 1 mol of zinc sulfate and 0.05 mol of copper sulfate were dissolved in 200 mL of deionized water, 1.4 mol of citric acid was added thereto, and the mixture was stirred evenly. The pH value was adjusted to 9 with a 1 mol / L sodium hydroxide aqueous solution, and the mixture was evaporated to dryness at 80° C. to form a wet gel, and then dried at 105° C. to constant weight to obtain a dry gel, which was calcined at 625° C. for 2.5 h and then naturally cooled to obtain antibacterial nanoparticles;

[0049] (2) 0.2 g of silver powder was dispersed in 200 mL of deionized water, and 10 g of the antibacterial nanoparticles of step (1) and 27 g of zeolite powder were added thereto, and the mixture was stirred at 75° C. and 100 r / min for 1.5 h, while keeping the temperature constant. 20 mL of 0.25 wt% α-lipoic acid solution was added dropwise to adjust the pH to 5.5, and 2.42 g of water-soluble chitosan and 1.2 g of sodium alginate were added thereto, and the mixture was stirred for 1.5 h. 20 mL of 0.25 wt% α-lipoic acid solution was added dropwise to adjust the pH to 5.5, and the mixture was stirred at 65° C. until a viscous state was formed, and the mixture was dried at 100° C. to constant weight and ground to pass through a 600-mesh sieve to obtain a composite antibacterial agent.

[0050] Preparation Example 2

[0051] The preparation steps of the composite antibacterial agent are the same as those in Preparation Example 1, except that 0.03 mol of copper sulfate is used.

[0052] Preparation Example 3

[0053] The preparation steps of the composite antibacterial agent are the same as those in Preparation Example 1, except that 0.4 g of silver powder is used.

[0054] Preparation Example 4

[0055] The preparation steps of the composite antibacterial agent are the same as those in Preparation Example 1, except that 2.05 g of water-soluble chitosan is used.

[0056] Preparation Example 5

[0057] The preparation steps of graphene modified PET chips / masterbatch are as follows:

[0058] S1: 1 g of graphene oxide was dispersed in 5 mL of 2-methyltetrahydrofuran, 1.28 g of COFU condensation agent was added, ultrasonication was performed for 15 min, 0.23 g of ethyl 3-aminobenzoate was added, the mixture was stirred for reaction for 2 h, centrifuged, washed with anhydrous ethanol for 3 times, and dried at 60 ° C to constant weight, 0.1 g of the obtained solid was dispersed in 100 mL of deionized water, 0.1 g of NHS and 0.1 g of EDC were added, stirred, and 500 g of hydroxymethyl chitosan was added, the pH was adjusted to 5, the mixture was reacted at 25 ° C for 12 h, filtered, washed with deionized water for 3 times, and dried at 60 ° C to constant weight to obtain modified graphene;

[0059] S2: 0.01 g of the modified graphene prepared in step S1 is uniformly mixed with 100 g of the dried PET chips / masterbatches, and the mixture is co-extruded to prepare graphene-modified PET chips / masterbatches.

[0060] Preparation Example 6

[0061] The preparation steps of graphene-modified PET chips / masterbatch are the same as those in Preparation Example 5, except that 0.2 g of ethyl 3-aminobenzoate is used.

[0062] Preparation Example 7

[0063] The preparation steps of graphene-modified PET chips / masterbatch are the same as those in Preparation Example 5, except that 0.05 g of solid is used.

[0064] Preparation Example 8

[0065] The preparation steps of graphene-modified PET chips / masterbatch are the same as those in Preparation Example 5, except that the modified graphene used in step (2) is 0.003 g.

[0066] Preparation Example 9

[0067] The preparation steps of graphene-modified PET chips / masterbatch are the same as those in Preparation Example 5, except that 0.02 g of modified graphene is used in step (2).

[0068] Example 1

[0069] A method for preparing a long-lasting antibacterial and antimicrobial fiber comprises the following steps:

[0070] According to the weight proportion, 85 parts of dried PET chips were mixed evenly with 1.5 parts of composite antibacterial agent and 8 parts of graphene modified PET chips / masterbatch, dried for 48 hours in a vacuum environment at 140°C, and put into the feeding port of the screw extruder. The temperatures of each zone of the screw were adjusted to be 300°C for zone 1, 320°C for zone 2, 350°C for zone 3, 350°C for zone 4, 350°C for zone 5, 320°C for flange zone, and 295°C for spinning box. The raw material reached the spinning box through screw extrusion. The speed of the metering pump was 33r / min, the specification was 12mL / r, the pump supply was 900g / min, and the spinning speed was 650m / min. The polyester pre-oriented yarn was prepared and allowed to stand for 6 hours. Then, the yarn was stretched and oiled with a stretching multiple of 2.1 times. After the fiber passed through a seven-roller stretching machine, a crimping machine, a drying oven, and a cutting machine, the antibacterial and antibacterial fiber was obtained.

[0071] The composite antibacterial agent used is obtained from Preparation Example 1; the graphene-modified PET chips / masterbatch used is obtained from Preparation Example 5.

[0072] Example 2

[0073] A method for preparing a long-lasting antibacterial and antimicrobial fiber comprises the following steps:

[0074] According to the weight proportion, 100 parts of dried PET chips were mixed evenly with 3 parts of composite antibacterial agent and 15 parts of graphene modified PET chips / masterbatch, dried for 40 hours in a vacuum environment at 150°C, and put into the feeding port of the screw extruder. The temperature of each zone of the screw was adjusted to be 300°C for zone 1, 320°C for zone 2, 350°C for zone 3, 350°C for zone 4, 350°C for zone 5, 350°C for flange zone, 320°C for spinning box, 295°C for spinning box, the raw material was extruded by the screw to reach the spinning box, the metering pump speed was 33r / min, the specification was 12mL / r, the pump supply was 900g / min, the spinning speed was 650m / min, the polyester pre-oriented yarn was prepared, and it was allowed to stand for 6 hours, and then subjected to the drawing and oiling process, with a drawing multiple of 2.1 times. After the fiber passed through a seven-roller drawing machine, a crimping machine, a drying oven, and a cutting machine, the antibacterial and antibacterial fiber was obtained.

[0075] The composite antibacterial agent used is obtained from Preparation Example 1; the graphene-modified PET chips / masterbatch used is obtained from Preparation Example 5.

[0076] Example 3

[0077] A method for preparing a long-lasting antibacterial and antimicrobial fiber comprises the following steps:

[0078] According to the weight proportion, 95 parts of dried PET chips were mixed evenly with 2 parts of composite antibacterial agent and 10 parts of graphene modified PET chips / masterbatch, dried for 44 hours in a vacuum environment at 145°C, and put into the feeding port of the screw extruder. The temperatures of each zone of the screw were adjusted to be 300°C for zone 1, 320°C for zone 2, 350°C for zone 3, 350°C for zone 4, 350°C for zone 5, 320°C for flange zone, and 295°C for spinning box. The raw material reached the spinning box through screw extrusion. The speed of the metering pump was 33r / min, the specification was 12mL / r, the pump supply was 900g / min, and the spinning speed was 650m / min. The polyester pre-oriented yarn was prepared and allowed to stand for 6 hours. Then, it was stretched and oiled with a stretching multiple of 2.1 times. After the fiber passed through a seven-roller stretching machine, a crimping machine, a drying oven, and a cutting machine, the antibacterial and antibacterial fiber was obtained.

[0079] The composite antibacterial agent used is obtained from Preparation Example 1; the graphene-modified PET chips / masterbatch used is obtained from Preparation Example 5.

[0080] Example 4

[0081] A method for preparing a long-acting antibacterial and antimicrobial fiber, the specific implementation method is the same as Example 3, the difference is that the composite antibacterial agent used is obtained from Preparation Example 2.

[0082] Example 5

[0083] A method for preparing a long-acting antibacterial and antimicrobial fiber, the specific implementation method is the same as Example 3, the difference is that the composite antibacterial agent used is obtained from Preparation Example 3.

[0084] Example 6

[0085] A method for preparing a long-acting antibacterial and antimicrobial fiber, the specific implementation method is the same as that of Example 3, except that the composite antibacterial agent used is obtained from Preparation Example 4.

[0086] Example 7

[0087] A method for preparing a long-lasting antibacterial and antimicrobial fiber, the specific implementation method is the same as that of Example 3, except that the graphene-modified PET chips / masterbatch used is obtained from Preparation Example 6.

[0088] Example 8

[0089] A method for preparing a long-lasting antibacterial and antimicrobial fiber, the specific implementation method is the same as Example 3, except that the graphene-modified PET chips / masterbatch used is obtained from Preparation Example 7.

[0090] Example 9

[0091] A method for preparing a long-lasting antibacterial and antimicrobial fiber, the specific implementation method is the same as Example 3, except that the graphene-modified PET chips / masterbatch used is obtained from Preparation Example 8.

[0092] Example 10

[0093] A method for preparing a long-lasting antibacterial and antimicrobial fiber, the specific implementation method is the same as that of Example 3, except that the graphene-modified PET chips / masterbatch used is obtained from Preparation Example 9.

[0094] Comparative Example 1

[0095] A method for preparing a long-lasting antibacterial and antimicrobial fiber comprises the following steps:

[0096] According to the weight proportion, 95 parts of dried PET chips were evenly mixed with 2 parts of composite antibacterial agent, dried at 145°C in a vacuum environment for 44 hours, and put into the feeding port of the screw extruder. The temperature of each zone of the screw was adjusted to be 300°C for zone 1, 320°C for zone 2, 350°C for zone 3, 350°C for zone 4, 350°C for zone 5, 320°C for flange zone, and 295°C for spinning box. The raw material reached the spinning box through screw extrusion. The speed of the metering pump was 33r / min, the specification was 12mL / r, the pump supply was 900g / min, and the spinning speed was 650m / min. The polyester pre-oriented yarn was prepared and allowed to stand for 6 hours. Then, it was stretched and oiled with a stretching multiple of 2.1 times. After the fiber passed through a seven-roller stretching machine, a crimping machine, a drying oven, and a cutting machine, the antibacterial and antibacterial fiber was obtained.

[0097] The composite antibacterial agent used is obtained from Preparation Example 1.

[0098] Comparative Example 2

[0099] A method for preparing polyester fiber comprises the following steps:

[0100] According to the weight proportion, 95 parts of dried PET chips and 10 parts of graphene-modified PET chips / masterbatch were mixed evenly, dried at 145°C in a vacuum environment for 44 hours, and put into the feeding port of the screw extruder, and the temperatures of each zone of the screw were adjusted to be 300°C for zone 1, 320°C for zone 2, 350°C for zone 3, 350°C for zone 4, 350°C for zone 5, 320°C for flange zone, and 295°C for spinning box. The raw material reached the spinning box through screw extrusion. The speed of the metering pump was 33r / min, the specification was 12mL / r, the pump supply was 900g / min, and the spinning speed was 650m / min. The polyester pre-oriented yarn was prepared and allowed to stand for 6 hours. Then, the yarn was stretched and oiled with a stretching multiple of 2.1 times. After the fiber passed through a seven-roller stretching machine, a crimping machine, a drying box, and a cutting machine, the polyester fiber was obtained.

[0101] The graphene-modified PET chips / masterbatch used are obtained from Preparation Example 5.

[0102] Performance Testing

[0103] The fibers obtained in the embodiments and comparative examples were subjected to the following performance tests:

[0104] 1. Antibacterial performance: Referring to GB / T 20944.3-2008 "Evaluation of antibacterial properties of textiles Part 3: Oscillation method", the antibacterial rates (%) of the fibers prepared in each embodiment and comparative example against Staphylococcus aureus, Escherichia coli and Candida albicans were tested respectively;

[0105] 2. Antistatic performance: The fibers of the embodiment and the comparative example were made into fabrics of the same size as test samples. The surface resistivity of the samples was tested by a YG(B)406 fabric resistivity tester with reference to GB / T 12703.4-2010 “Evaluation of electrostatic properties of textiles - Part 4: Resistivity”. The washing fastness of the antistatic performance of the fabric was evaluated by the change in resistivity before and after 30 washes.

[0106] Specific test data are shown in Table 1.

[0107] Table 1

[0108]

[0109] As shown in Table 1, the antibacterial and antibacterial fibers prepared in Examples 1-3 have excellent comprehensive performance, good antibacterial performance, and good antistatic performance after washing 30 times. Compared with Example 3, the proportion of raw materials in the preparation process of the composite antibacterial agent used in Examples 4-6 changes, which reduces the antibacterial and antibacterial performance of the composite antibacterial agent, thereby reducing the antibacterial rate of the prepared fiber to varying degrees; the proportion of raw materials in the preparation process of the graphene-modified PET chips / masterbatch used in Examples 7 and 8 changes, the degree of amidation of the carboxyl groups on the surface of graphene oxide changes, and the properties of the modified graphene change, while the ratio of modified graphene to PET chips / masterbatch is changed in Examples 9 and 10, which will reduce the antistatic performance of the fiber; in Comparative Example 1, graphene-modified PET chips / masterbatch are not added, and the fiber antistatic performance prepared is the worst; in Comparative Example 2, no composite antibacterial agent is added, and the fiber antibacterial rate prepared is the worst.

[0110] The above is only a preferred embodiment of the present invention and does not constitute any form of limitation to the present application. Although the present application is disclosed as above in the preferred embodiment, it is not intended to limit the present application. Any technician familiar with the profession, without departing from the scope of the technical solution of the present application, using the technical content disclosed above to make slight changes or modifications are equivalent to equivalent implementation cases. However, any simple modifications, equivalent changes and modifications made to the above embodiments based on the technical essence of the present invention without departing from the content of the technical solution of the present invention are still within the scope of the technical solution.

Claims

1. A long-lasting antibacterial and bacteriostatic fiber, characterized in that: According to the weight percentage, it includes the following raw materials: PET chips / masterbatch 85-100 parts, graphene modified PET chips / masterbatch 8-15 parts, composite antibacterial agent 1.5-3 parts.

2. The antibacterial and antimicrobial fiber according to claim 1, characterized in that: The preparation steps of the composite antibacterial agent are: (1) dissolving zinc sulfate and copper sulfate in deionized water, adding citric acid thereto, stirring evenly, adjusting the pH, evaporating to dryness at 75-80° C. to form a wet gel, drying to constant weight to obtain a dry gel, calcining at 600-650° C. for 2-3 h, and cooling naturally to obtain antibacterial nanoparticles; (2) dispersing silver powder in deionized water, adding the antibacterial nanoparticles and zeolite powder of step (1), stirring at 70-80° C. for 1-2 h, keeping the temperature constant, adding α-lipoic acid solution dropwise thereto, adjusting the pH to 5-6, adding water-soluble chitosan and sodium alginate, stirring for 1-2 h, adding α-lipoic acid solution dropwise again, adjusting the pH to 5-6, stirring at 60-70° C. until a viscous state is formed, drying, and grinding to obtain a composite antibacterial agent.

3. The antibacterial and antimicrobial fiber according to claim 2, characterized in that: The molar ratio of the zinc sulfate, copper sulfate and citric acid is 1:(0.04-0.06):(1.3-1.5).

4. The antibacterial and antimicrobial fiber according to claim 2, characterized in that: In the step (2), the mass ratio of the silver powder, antibacterial nanoparticles and nano zeolite powder is (1-3):(98-103):(260-280); the silver powder is a flaky silver powder with an average particle size of 1-5 μm, and the average particle size of the zeolite powder is 2.5-10 μm.

5. The antibacterial and bacteriostatic fiber according to claim 2, characterized in that: The usage amounts of the water-soluble chitosan and sodium alginate are 6-7wt% and 3-3.5wt% of the total weight of the silver powder, antibacterial nanoparticles and nano zeolite powder respectively; the deacetylation degree of the water-soluble chitosan is ≥90%.

6. The antibacterial and bacteriostatic fiber according to claim 1, characterized in that: The preparation steps of the graphene-modified PET chips / masterbatch are as follows: S1: dispersing graphene oxide in an organic solvent, adding a condensing agent, ultrasonicating, then adding ethyl 3-aminobenzoate, stirring for 1-4 hours, separating, drying, dispersing the obtained solid in deionized water, adding a carboxyl activator, stirring, then adding hydroxymethyl chitosan, adjusting the pH, reacting at 20-30°C for 10-12 hours, separating, washing, and drying to obtain modified graphene; S2: The modified graphene of step S1 is evenly mixed with the dried PET chips / masterbatch, and the mixture is co-extruded to prepare graphene-modified PET chips / masterbatch.

7. The antibacterial and antimicrobial fiber according to claim 6, characterized in that: The mass ratio of the graphene oxide to ethyl 3-aminobenzoate is 1:(0.22-0.235).

8. The antibacterial and bacteriostatic fiber according to claim 6, characterized in that: The solid is used in an amount of 0.01-0.03 wt % of the hydroxymethyl chitosan.

9. The antibacterial and bacteriostatic fiber according to claim 6, characterized in that: The amount of modified graphene used in step S2 is 0.005-0.015wt% of the PET chips / masterbatch.

10. A method for preparing the antibacterial and antimicrobial fiber according to any one of claims 1 to 9, characterized in that: The method comprises the following preparation steps: The dried PET chips / masterbatch are evenly mixed with the composite antibacterial agent and graphene-modified PET chips / masterbatch, dried in a vacuum environment at 140-150° C. for 40-48 hours, put into a screw extruder for processing, spun, and then subjected to a drawing and oiling process to obtain antibacterial and antimicrobial fibers.

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