High moisture regain antibacterial viscose fiber and preparation method thereof

Abstract

The present disclosure provides a high moisture regain antibacterial viscose fiber and a preparation method thereof, wherein the bonding fiber comprises: fiber, silver antibacterial agent, coagulation bath; wherein the silver antibacterial agent is a complex of sodium alginate macromolecule and silver ions, and the silver ion content in the bonding fiber is 20-60 mg / kg; wherein the silver antibacterial agent is uniformly dispersed in the spinning solution of the bonding fiber in the form of a solution through pre-spinning injection and dynamic mixing processes, and a wet spinning process is used to prepare the high moisture regain antibacterial bonding fiber. The standard moisture regain of the viscose fiber prepared by the present disclosure is ≥15%, the whiteness is ≥80%, and the dry breaking strength is ≥2.2 cN / dtex; after 20 times of washing, the antibacterial rate of the bonding fiber against Staphylococcus aureus, Escherichia coli and Candida albicans is ≥90%.

Description

Technical Field

[0001] The invention belongs to the technical field of textile materials, and particularly relates to a high moisture regain antibacterial viscose fiber and a preparation method thereof. Background Art

[0002] Viscose fiber is a regenerated cellulose fiber obtained from cellulose pulp through wet spinning process and a series of post-processing procedures. Viscose fiber can not only make up for the shortage of natural fiber in quantity, but also outperform natural fiber and synthetic fiber in some aspects. It is derived from nature and is better than nature, with "the essence of cotton" and "the quality of silk". The hygroscopicity of viscose fiber meets the physiological needs of human skin, and it is smooth, cool, breathable, soft, antistatic, colorful, and has good color fastness. It is the cellulose regenerated fiber with the longest development history and the largest output. Viscose fiber has excellent wearing comfort and is an ideal underwear fabric. However, viscose fiber products are prone to breed bacteria, which leads to the loss of mechanical properties of the fabric and affects its wearing performance; on the other hand, bacteria, fungi, and viruses adsorbed on the fiber surface will pose a potential threat to human health. With the improvement of social living standards and the enhancement of people's safety and health awareness, it is necessary to develop viscose fibers with excellent antibacterial effects and wearing comfort to meet the consumer demand of the market.

[0003] In the prior art, patent publication number CN1544725A discloses an antibacterial viscose fiber and a production process thereof, in which an antibacterial agent is diluted and added to viscose for mixing, and then spinning and post-treatment are performed to obtain viscose fiber with durable broad-spectrum antibacterial effect; patent publication number CN101525777A discloses a viscose fiber with mint antibacterial function and a preparation method thereof, in which natural mint extract is added to viscose spinning stock solution, and viscose fiber with mint antibacterial function is obtained according to a conventional wet spinning process; patent publication number CN113564742A discloses an antibacterial viscose fiber containing epimedium extract and a preparation method thereof, in which an epimedium extract dispersion and a viscose spinning solution are fully mixed, and then the antibacterial viscose fiber is obtained through a wet spinning process and post-treatment. In the above disclosed process, the amount of antimicrobial agent used is relatively high, and the antimicrobial agent can only be added in the viscose spinning solution preparation system, so it is easy to contaminate the spinning pipeline. It will also lead to high maintenance costs due to cleaning the pipeline when changing fiber varieties. In addition, the addition of antimicrobial agents leads to a decrease in the strength and moisture regain properties of viscose fibers.

[0004] Silver-based antimicrobial agents have excellent properties such as high temperature resistance, safety, high efficiency, broad-spectrum antibacterial and good drug resistance. They are one of the important types of textile antimicrobial agents. Using silver-based antimicrobial agents to prepare antibacterial viscose fibers can help reduce the amount of antimicrobial agents used and improve the performance of the fibers. Patent publication number CN1779004A discloses an antibacterial viscose fiber and a production method thereof. The application adopts a pre-spinning injection method to add a silver zeolite antibacterial agent aqueous emulsion to a cellulose sulfonate solution and mix them evenly to prepare the antibacterial viscose fiber; Patent publication number CN105177747A discloses an antibacterial viscose fiber and a preparation method thereof. The application adds a nano-silver colloidal solution during the colloid preparation process, and then obtains the antibacterial viscose fiber through spinning, bundling, cutting, refining, drying, packaging and other steps; Patent publication number CN105887227A discloses a preparation method for antibacterial and deodorizing viscose fiber. The application deposits nano-silver on the surface of waste hair activated carbon particles, and then puts them into the viscose spinning stock solution to obtain the antibacterial and deodorizing viscose fiber through wet spinning; Patent publication number CN110373895 A discloses a method for preparing silver-loaded antibacterial viscose fiber, which first soaks the viscose fiber in a silver nitrate aqueous solution, and then soaks the treated fiber in a silane coupling agent solution to obtain the silver-loaded antibacterial viscose fiber. In the above technology, the antibacterial agent is distributed in the viscose fiber in the form of silver nanoparticles, which poses a great risk to the environment and human health, and the strength and moisture regain properties of the antibacterial viscose fiber prepared by the above method are also unsatisfactory. Summary of the invention

[0005] In view of the deficiencies in the prior art, the present invention aims to provide a high moisture regain antibacterial viscose fiber and a preparation method thereof. The viscose fiber prepared by the present invention has high moisture regain, antibacterial properties and comprehensive mechanical properties. The method for preparing the viscose fiber is simple, has high production efficiency and appropriate cost in actual production.

[0006] In order to achieve the above-mentioned object, the present disclosure provides a high moisture regain antibacterial viscose fiber and a preparation method thereof.

[0007] In a first aspect of the present disclosure, a high moisture regain antibacterial viscose fiber is provided, comprising: fiber, a silver-based antibacterial agent, and a coagulation bath; wherein the silver-based antibacterial agent is a complex of sodium alginate macromolecules and silver ions, and the silver ion content in the bonding fiber is 20-60 mg / kg; wherein the silver-based antibacterial agent is uniformly dispersed in the spinning solution of the bonding fiber in the form of a solution through pre-spinning injection and dynamic mixing processes, and a wet spinning process is adopted to prepare the high moisture regain antibacterial bonding fiber.

[0008] In the present disclosure, a highly efficient hydrophilic silver ion complex is used as an antibacterial agent for viscose fiber. The antibacterial agent is dispersed into the viscose fiber spinning solution by pre-spinning injection and dynamic mixing. Then, the antibacterial agent is uniformly fixed in the fiber matrix by optimizing the spinning coagulation system. Finally, the above-mentioned high moisture regain and antibacterial viscose fiber is obtained through post-processing.

[0009] The silver nitrate aqueous solution is added dropwise to the sodium alginate aqueous solution, and part of the carboxyl groups in the sodium alginate macromolecule react with the silver ions to obtain a sol-type silver antibacterial agent. Since the silver ion complex has high antibacterial properties, only a small amount of addition is needed to achieve the antibacterial function of viscose fiber. Therefore, the silver antibacterial agent can be evenly dispersed in the viscose fiber spinning solution by pre-spinning injection and dynamic mixing.

[0010] In some embodiments, the silver-based antibacterial agent is prepared by mixing the sodium alginate macromolecule aqueous solution with a silver nitrate aqueous solution, wherein the viscosity of the sodium alginate macromolecule is 20-50 mPa.s.

[0011] In this embodiment, the mass percentage concentration of the sodium alginate macromolecular aqueous solution is 0.5%-1%, and the concentration of the silver nitrate aqueous solution is 0.5-1 mol / L; wherein the volume ratio of the silver nitrate aqueous solution to the sodium alginate macromolecular aqueous solution is between 1:100-5:100.

[0012] In the present disclosure, sodium alginate macromolecules can react with silver ions to form a complex reaction, but the viscosity of sodium alginate macromolecules has a great influence on the state of the complex reaction product. When the viscosity is too low, the sodium alginate solution reacts with silver nitrate to form a precipitate, which cannot meet the use requirements; when the viscosity is too high, the sodium alginate aqueous solution reacts with silver nitrate to form a gel, which is easy to clog the spinneret. The present disclosure regulates the reaction of sodium alginate aqueous solution and silver nitrate to form a sol-like complex. Under this idea, after repeated experiments, it is determined that the viscosity of the sodium alginate raw material preferably ranges from 20 to 50 mPa.s. In addition, the concentrations of sodium alginate and silver nitrate aqueous solutions have an effect on the state of the complex product and the content of the active ingredients in the preparation of the antibacterial solution, thereby affecting the subsequent addition amount of the antibacterial solution. In order to ensure that the antibacterial solution can be dispersed into the viscose fiber spinning solution by pre-spinning injection, the preferred concentration of the sodium alginate aqueous solution in the scheme provided by the present invention is 0.5%-1%, and the preferred concentration of the silver nitrate aqueous solution is 0.5-1 mol / L.

[0013] In the present disclosure, the mixing method of the silver nitrate aqueous solution and the sodium alginate aqueous solution directly affects the state of the reaction product; the mixing volume ratio of the silver nitrate aqueous solution and the sodium alginate aqueous solution directly affects the state of the reaction product and the content of the active ingredient in the antibacterial agent solution. In order to achieve the purpose of the present invention, to ensure the generation of a sol-like antibacterial agent, and to disperse the antibacterial agent solution into the viscose fiber spinning solution by pre-spinning injection, the mixing volume ratio of the silver nitrate aqueous solution and the sodium alginate aqueous solution in the solution provided by the present invention is preferably 1:100-5:100.

[0014] In some embodiments, the coagulation bath is obtained by preparing a mixed aqueous solution of sulfuric acid, sodium sulfate, and zinc sulfate.

[0015] In this embodiment, the concentration of the sulfuric acid is 150-160 g / L, the concentration of the sodium sulfate is 380-410 g / L, and the concentration of the zinc sulfate is 10-20 g / L.

[0016] In the present disclosure, when a conventional viscose fiber spinning coagulation bath is used, after the spinning solution of the antibacterial viscose fiber enters the coagulation bath, the sol-like antibacterial agent in the filaments reacts with sulfuric acid, which slows down the forming speed of the nascent fiber, affects the drafting performance of the nascent fiber, and causes the mechanical properties of the formed fiber to decrease. Therefore, the present disclosure adopts the idea of ​​accelerating the gelation speed of the antibacterial agent in the fiber filaments and the dehydration speed of the nascent fiber, while reducing the decomposition speed of sodium cellulose xanthate in the spinning solution, and regulating the three-dimensional gel structure of the nascent fiber so that it can withstand high-fold drafting, thereby improving the mechanical properties of the fiber. Under the guidance of this idea, after repeated debugging, it is preferred that the concentration of sulfuric acid in the coagulation bath is 150-160g / L, the concentration of sodium sulfate is 380-410g / L, and the concentration of zinc sulfate is 10-20g / L. At this time, the dry breaking strength of the prepared antibacterial viscose fiber is ≥2.2cN / dtex.

[0017] When the viscose spinning solution mixed with the above antibacterial agent enters the coagulation bath, the carboxyl groups in the sodium alginate macromolecule that are not involved in the silver ion complexation react with the hydrogen ions in the coagulation bath, and the sol-type silver antibacterial agent in the fiber matrix is ​​converted into a water-insoluble gel and fixed in the fiber matrix. The antibacterial viscose fiber thus prepared has good washing resistance. After 20 washes, the antibacterial rate against Staphylococcus aureus, Escherichia coli and Candida albicans is still ≥90%.

[0018] In any of the above embodiments, the standard moisture regain of the prepared bonding fiber is ≥15%, the whiteness is ≥80%, and the dry breaking strength is ≥2.2 cN / dtex; after 20 times of washing, the antibacterial rate of the bonding fiber against Staphylococcus aureus, Escherichia coli and Candida albicans is ≥90%.

[0019] In a second aspect of the present disclosure, there is provided a method for preparing high moisture regain antibacterial viscose fiber, which is applied to any of the bonding fibers described in the first aspect, and the method comprises:

[0020] S1: uniformly mixing a sodium alginate macromolecular aqueous solution with a silver nitrate aqueous solution to obtain a silver-based antibacterial agent solution; preparing a mixed aqueous solution of sulfuric acid, sodium sulfate and zinc sulfate as a coagulation bath for fiber spinning;

[0021] S2: using a pre-spinning injection process, the silver-based antibacterial agent solution and the viscose spinning solution are synchronously transported to a dynamic mixer to obtain a spinning solution containing the silver-based antibacterial agent;

[0022] S3: Extruding the spinning solution containing the silver antibacterial agent from a spinneret with a pore size of 0.05-0.1 mm through a metering pump, and passing through the coagulation bath to obtain a primary fiber;

[0023] S4: The primary fibers are post-processed to obtain the bonding fibers.

[0024] Sodium alginate is a natural polysaccharide extracted from marine algae such as kelp and giant kelp, with good biocompatibility and excellent water solubility. The macromolecular structure of sodium alginate contains a large number of hydrophilic hydroxyl and carboxyl groups, among which the carboxyl groups can react with silver ions to form a sol-like silver alginate compound by controlling the reaction conditions. The compound has high antibacterial properties, good alkali resistance and stability, excellent compatibility with viscose spinning solution, and will not block the spinning nozzle of viscose fiber. Moreover, a small amount of the antibacterial agent is evenly distributed in the viscose spinning solution in a sol state, which has little effect on the spinnability of the viscose spinning solution and does not affect the spinning process of the fiber.

[0025] There are many processes and procedures for preparing viscose fiber spinning solution. In the existing technology, antibacterial agents are usually added in the preparation stage of the spinning solution to prepare antibacterial viscose fiber. However, this method will pollute the pipeline of the viscose fiber. When producing different varieties of viscose fibers, the pipeline needs to be cleaned, which not only wastes raw materials and increases costs, but also makes cleaning difficult. The present disclosure adopts a pre-spinning injection and dynamic mixing device to evenly disperse the antibacterial agent into the viscose fiber spinning solution before spinning, which can solve the above problems.

[0026] Furthermore, the preparation method of the antibacterial viscose fiber provided by the present invention has little impact on the existing production equipment and processes of ordinary viscose fibers. By adding a pre-spinning injection device and a dynamic mixing device, the production of antibacterial viscose fibers can be achieved in the production of ordinary viscose fibers. The operation is simple and the production of different types of viscose fibers can be taken into account, thereby reducing costs.

[0027] The coagulation bath is an important factor affecting the mechanical properties of viscose fiber. The synergistic effect of sulfuric acid, sodium sulfate and zinc sulfate in the coagulation bath can adjust the coagulation speed and dehydration speed of the primary filaments of viscose fiber, ensuring that the primary fibers can withstand high-multiple stretching and making the fibers have good physical and mechanical properties.

[0028] Preferably, in some embodiments, a method for preparing high moisture regain antibacterial viscose fiber is provided:

[0029] 1) Prepare a sodium alginate aqueous solution with a mass percentage concentration of 0.5%-1% and a silver nitrate aqueous solution with a concentration of 0.5-1 mol / L respectively. The viscosity of the raw material of the sodium alginate macromolecule is 20-50 mpa.s.

[0030] 2) In a light-proof environment, the prepared silver nitrate aqueous solution is added dropwise while the sodium alginate aqueous solution is mechanically stirred until the volume ratio of the silver nitrate aqueous solution to the sodium alginate aqueous solution is 1:100-5:100, thereby obtaining a mixed solution.

[0031] 3) In a light-proof environment, the mixed solution is stirred and reacted at 10-40° C. for 30-60 min to obtain an antibacterial solution.

[0032] 4) Using the pre-spinning injection process, the antibacterial agent solution and the viscose spinning solution are synchronously transported to the dynamic mixer, and then output to obtain the spinning solution containing the silver-based antibacterial agent, wherein the injection amount of the antibacterial agent solution is 0.1%-0.5% of the viscose spinning solution.

[0033] 5) preparing a mixed aqueous solution of sulfuric acid, sodium sulfate and zinc sulfate as a coagulation bath for the fiber, wherein the concentration of sulfuric acid in the coagulation bath is 150-160 g / L, the concentration of sodium sulfate is 380-410 g / L, and the concentration of zinc sulfate is 10-20 g / L.

[0034] 6) The spinning solution containing the silver antibacterial agent is extruded from a spinneret hole with an aperture of 0.05-0.1 mm through a metering pump and enters a spinning coagulation bath to obtain primary fibers. The primary fibers are post-treated to obtain high moisture regain antibacterial viscose fibers.

[0035] In some embodiments, the step S1 includes:

[0036] In a light-proof environment, the sodium alginate macromolecular aqueous solution is mechanically stirred while the prepared silver nitrate aqueous solution is added dropwise until the volume ratio of the silver nitrate aqueous solution to the sodium alginate macromolecular aqueous solution is 1:100-5:100, thereby preparing a mixed solution; the mixed solution is continuously stirred at 10-40° C. for 30-60 minutes to obtain the silver-based antibacterial agent solution.

[0037] In the present disclosure, a certain temperature is required for the complexation reaction between the sodium alginate aqueous solution and the silver nitrate aqueous solution. When the temperature is too high, the silver nitrate will be reduced to granular elemental silver by the sodium alginate; when the temperature is too low, the complexation reaction time is too long and the cost is too high. After repeated experiments, it is determined that the preferred conditions for the reaction of the sodium alginate and silver nitrate mixed solution are: temperature of 10-40°C and reaction time of 30-60min.

[0038] In some embodiments, in the step S2, the injection amount of the silver-based antibacterial agent solution is 0.1%-0.5% of the viscose spinning solution.

[0039] In the present disclosure, the antibacterial agent is added to the viscose spinning solution by pre-spinning injection, which has the advantages of simple operation, good compatibility in the production of multiple varieties of viscose fibers, and low cost. However, when this method is used, the injection volume has an appropriate range. When the injection volume is too small, the error is large, resulting in poor stability of the finished product; when the injection volume is too large, it is not easy to mix evenly. The silver-based antibacterial agent prepared by the present disclosure has a high-efficiency antibacterial function, and the effective ingredients in the antibacterial agent solution are regulated by the technical solution provided by the present disclosure. When the injection volume of the antibacterial agent solution is preferably 0.1%-0.5% of the viscose spinning solution, the prepared fiber has excellent antibacterial properties, and the injection volume can meet the requirements of the pre-spinning injection process.

[0040] In some embodiments, the post-treatment of the spun fibers includes: cutting, desulfurization, bleaching, washing, oiling, opening, drying and the like.

[0041] According to the different uses and properties of the fibers, there are two ways to post-process viscose fibers: filament post-processing and staple fiber post-processing. The present disclosure provides a method for preparing high moisture regain and antibacterial viscose fibers, preferably using the post-processing process of ordinary viscose staple fibers, including cutting, desulfurization, bleaching, washing, oiling, opening, drying and other processes.

[0042] Therefore, the preparation method of high moisture regain and antibacterial viscose fiber provided by the present invention can take into account the production of ordinary viscose fiber and antibacterial viscose fiber, which is convenient for production enterprises to switch to produce different varieties of viscose fiber according to orders and reduce production costs.

[0043] Beneficial effects of the present disclosure:

[0044] The present invention adopts silver alginate complex as a highly effective antibacterial agent for viscose fiber, and through the regulation of the preparation process, the antibacterial agent exists in the form of sol in the spinning solution, and is transformed into a non-water-soluble gel in the coagulation bath and distributed in the viscose fiber matrix. Therefore, the addition of the antibacterial agent has little effect on the rheology and spinnability of the spinning solution, does not clog the nozzle, and is easy to process; and the prepared antibacterial viscose fiber has excellent washing resistance, and the antibacterial rates of Staphylococcus aureus, Escherichia coli and Candida albicans after 20 washings are all ≥90%.

[0045] The present invention solves the problem of mutual restriction between the antibacterial property, hygroscopicity and physical and mechanical properties of viscose fiber by optimizing the high-efficiency antibacterial agent added to the viscose fiber matrix and regulating the preparation process, as well as the design and regulation of the coagulation bath system and other comprehensive means. Therefore, the standard moisture regain of the antibacterial viscose fiber prepared by the present invention is ≥15%, the dry breaking strength is ≥2.2cN / dtex, and the antibacterial property is excellent. After 20 times of washing, the antibacterial rate of Staphylococcus aureus, Escherichia coli and Candida albicans is ≥90%.

[0046] The present invention solves the contradiction between the precise control of the amount of antibacterial agent added and the uniformity of dispersion in the fiber matrix through the structural design and optimization of the antibacterial agent, and through the comprehensive regulation of the preparation process and the addition amount of the antibacterial agent, and realizes the preparation of antibacterial viscose fiber by the pre-spinning injection process. Therefore, the preparation method of the antibacterial viscose fiber provided by the present invention has a simple process, can take into account the production of antibacterial viscose fiber and ordinary viscose fiber, reduce the production cost of the fiber, and the fiber has excellent properties.

[0047] The antibacterial viscose fiber provided by the present disclosure has excellent antibacterial properties, hygroscopicity and physical and mechanical properties, taking into account the comfort, functionality and processability of textile fibers, and is very suitable for pure spinning or blending with cotton fiber, ordinary viscose fiber, Tencel fiber, modal fiber, bamboo fiber, etc. to make high value-added textile fabrics. In addition, the antibacterial viscose fiber provided by the invention solves the problems of environmental pollution and potential harm to the human body caused by nano antibacterial agents and organic antibacterial agents. BRIEF DESCRIPTION OF THE DRAWINGS

[0048] The present disclosure will be further described in detail below in conjunction with the accompanying drawings and preferred embodiments, but those skilled in the art will appreciate that these drawings are only drawn for the purpose of explaining the preferred embodiments and therefore should not be taken as limiting the scope of the present disclosure.

[0049] Figure 1 : Schematic diagram of the preparation process of antibacterial viscose fiber. DETAILED DESCRIPTION

[0050] The following will be combined with the drawings in 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.

[0051] In the present disclosure, a method for preparing a high moisture regain antibacterial viscose fiber provided in the second aspect can be applied to prepare any bonding fiber described in the first aspect. In conjunction with the method for preparing a high moisture regain antibacterial viscose fiber in the present disclosure, the following related embodiments are provided:

[0052] Embodiment 1:

[0053] Using sodium alginate raw material with a viscosity of 20mpa.s, a sodium alginate macromolecular aqueous solution with a mass percentage concentration of 1% is prepared; a silver nitrate aqueous solution with a concentration of 1mol / L is prepared;

[0054] Under a light-proof environment, the sodium alginate macromolecular aqueous solution was mechanically stirred while the silver nitrate aqueous solution was added dropwise until the volume ratio of the silver nitrate aqueous solution to the sodium alginate aqueous solution was 1:100, thereby obtaining a mixed solution.

[0055] In a light-proof environment, the mixed solution was stirred and reacted at 40° C. for 30 min to obtain an antibacterial agent solution.

[0056] Use Figure 1 In the pre-spinning injection process shown, the injection amount of the antibacterial agent solution is 0.5% of the viscose spinning solution, the prepared antibacterial agent solution and the viscose spinning solution are synchronously transported to the dynamic mixer to obtain a spinning solution containing a silver-based antibacterial agent.

[0057] A mixed aqueous solution of sulfuric acid, sodium sulfate and zinc sulfate was prepared as a coagulation bath for the fiber, wherein the concentration of sulfuric acid was 150 g / L, the concentration of sodium sulfate was 380 g / L, and the concentration of zinc sulfate was 10 g / L.

[0058] The spinning solution containing silver antibacterial agent is extruded from a spinneret with an aperture of 0.05 mm through a metering pump and enters a prepared spinning coagulation bath to obtain primary fiber, which is then subjected to post-treatment steps such as cutting, desulfurization, bleaching, washing, oiling, opening, and drying to obtain high moisture regain and antibacterial viscose fiber.

[0059] Embodiment 2:

[0060] A sodium alginate raw material with a viscosity of 50 mPa.s is used to prepare a sodium alginate macromolecular aqueous solution with a mass percentage concentration of 0.5%; and a silver nitrate aqueous solution with a concentration of 0.5 mol / L is prepared.

[0061] Under a light-proof environment, the sodium alginate aqueous solution was mechanically stirred while the silver nitrate aqueous solution was added dropwise until the volume ratio of the silver nitrate aqueous solution to the sodium alginate aqueous solution was 5:100, thereby obtaining a mixed solution.

[0062] The mixed solution was stirred and reacted at 10° C. for 60 min in a light-proof environment to obtain an antibacterial agent solution.

[0063] Use Figure 1 In the pre-spinning injection process shown, the injection amount of the antibacterial agent solution is 0.1% of the viscose spinning solution, and the prepared antibacterial agent solution and the viscose spinning solution are synchronously transported to the dynamic mixer to obtain a spinning solution containing a silver-based antibacterial agent.

[0064] A mixed aqueous solution of sulfuric acid, sodium sulfate and zinc sulfate was prepared as a coagulation bath for the fiber, wherein the concentration of sulfuric acid was 160 g / L, the concentration of sodium sulfate was 410 g / L, and the concentration of zinc sulfate was 20 g / L.

[0065] The spinning solution containing silver antibacterial agent is extruded from a spinneret with an aperture of 0.1 mm through a metering pump and enters a prepared spinning coagulation bath to obtain primary fibers, which are then subjected to post-treatment steps such as cutting, desulfurization, bleaching, washing, oiling, opening, and drying to obtain high moisture regain and antibacterial viscose fibers.

[0066] Embodiment 3:

[0067] A sodium alginate raw material with a viscosity of 28 mpa.s was used to prepare a sodium alginate macromolecular aqueous solution with a mass percentage concentration of 0.9%; and a silver nitrate aqueous solution with a concentration of 0.7 mol / L was prepared.

[0068] Under a light-proof environment, the sodium alginate aqueous solution was mechanically stirred while the silver nitrate aqueous solution was added dropwise until the volume ratio of the silver nitrate aqueous solution to the sodium alginate aqueous solution was 4:100, thereby obtaining a mixed solution.

[0069] The mixed solution was stirred and reacted at 20° C. for 50 min in a light-proof environment to obtain an antibacterial agent solution.

[0070] Use Figure 1 In the pre-spinning injection process shown, the injection amount of the antibacterial agent solution is 0.2% of the viscose spinning solution, and the prepared antibacterial agent solution and the viscose spinning solution are synchronously transported to the dynamic mixer to obtain a spinning solution containing a silver-based antibacterial agent.

[0071] A mixed aqueous solution of sulfuric acid, sodium sulfate and zinc sulfate was prepared as a coagulation bath for the fiber, wherein the concentration of sulfuric acid was 155 g / L, the concentration of sodium sulfate was 400 g / L, and the concentration of zinc sulfate was 15 g / L.

[0072] The spinning solution containing silver antibacterial agent is extruded from a spinneret with an aperture of 0.07 mm through a metering pump and enters a prepared spinning coagulation bath to obtain primary fiber, which is then subjected to post-treatment steps such as cutting, desulfurization, bleaching, washing, oiling, opening, and drying to obtain high moisture regain and antibacterial viscose fiber.

[0073] Embodiment 4:

[0074] A sodium alginate raw material with a viscosity of 35 mpa.s is used to prepare a sodium alginate macromolecular aqueous solution with a mass percentage concentration of 0.8%; and a silver nitrate aqueous solution with a concentration of 0.8 mol / L is prepared.

[0075] Under a light-proof environment, the sodium alginate aqueous solution was mechanically stirred while the silver nitrate aqueous solution was added dropwise until the volume ratio of the silver nitrate aqueous solution to the sodium alginate aqueous solution was 3:100, thereby obtaining a mixed solution.

[0076] The mixed solution was stirred and reacted at 25° C. for 45 min in a light-proof environment to obtain an antibacterial agent solution.

[0077] Use Figure 1 In the pre-spinning injection process shown, the injection amount of the antibacterial agent solution is 0.3% of the viscose spinning solution, and the prepared antibacterial agent solution and the viscose spinning solution are synchronously transported to the dynamic mixer to obtain a spinning solution containing a silver-based antibacterial agent.

[0078] A mixed aqueous solution of sulfuric acid, sodium sulfate and zinc sulfate was prepared as a coagulation bath for the fiber, wherein the concentration of sulfuric acid was 158 g / L, the concentration of sodium sulfate was 390 g / L, and the concentration of zinc sulfate was 18 g / L.

[0079] The spinning solution containing silver antibacterial agent is extruded from a spinneret with an aperture of 0.09 mm through a metering pump and enters a prepared spinning coagulation bath to obtain primary fiber, which is then subjected to post-treatment steps such as cutting, desulfurization, bleaching, washing, oiling, opening, and drying to obtain high moisture regain and antibacterial viscose fiber.

[0080] Embodiment 5:

[0081] A sodium alginate raw material with a viscosity of 40 mpa.s is used to prepare a sodium alginate aqueous solution with a mass percentage concentration of 0.6%; and a silver nitrate aqueous solution with a concentration of 0.9 mol / L is prepared.

[0082] Under a light-proof environment, the sodium alginate aqueous solution was mechanically stirred while the silver nitrate aqueous solution was added dropwise until the volume ratio of the silver nitrate aqueous solution to the sodium alginate aqueous solution was 2:100, thereby obtaining a mixed solution.

[0083] The mixed solution was stirred and reacted at 30° C. for 40 min in a light-proof environment to obtain an antibacterial agent solution.

[0084] Use Figure 1 In the pre-spinning injection process shown, the injection amount of the antibacterial agent solution is 0.4% of the viscose spinning solution, and the prepared antibacterial agent solution and the viscose spinning solution are synchronously transported to the dynamic mixer to obtain a spinning solution containing a silver-based antibacterial agent.

[0085] A mixed aqueous solution of sulfuric acid, sodium sulfate and zinc sulfate was prepared as a coagulation bath for the fiber, wherein the concentration of sulfuric acid was 152 g / L, the concentration of sodium sulfate was 410 g / L, and the concentration of zinc sulfate was 12 g / L.

[0086] The spinning solution containing silver antibacterial agent is extruded from a spinneret with an aperture of 0.08mm through a metering pump and enters a prepared spinning coagulation bath to obtain primary fiber, which is then subjected to post-treatment steps such as cutting, desulfurization, bleaching, washing, oiling, opening, and drying to obtain high moisture regain and antibacterial viscose fiber.

[0087] The viscose fibers prepared in the above examples were taken at about 100 g each and dried to a constant weight, weighed, and recorded as M (kg); the fibers were then digested and then fixed to 100 mL, and the concentration of silver ions C (mg / L) in the digestion solution was tested by atomic absorption spectrometry; the silver content N in the fiber was calculated according to the following formula (1).

[0088]

[0089] The dry breaking strength of the prepared fiber was tested with reference to GB / T 14337-2008 Test method for tensile properties of chemical staple fibers; the standard moisture regain of the prepared fiber was tested with reference to GB / T 6503-2017 Test method for moisture regain of chemical fibers; the whiteness of the prepared fiber was tested with reference to GB / T 17644-2008 Test method for whiteness and chromaticity of textile fibers; the prepared fiber was washed with reference to the antibacterial fabric sample washing test method provided in FZ / T73023-2006 Antibacterial knitwear, and then the antibacterial rate of the fiber after washing was tested with reference to GB / T 20944.3-2008 Evaluation of antibacterial properties of textiles Part 3: Oscillation method.

[0090] According to the above method, the various properties of the high moisture regain and antibacterial viscose fibers prepared in Examples 1, 2, 3, 4, and 5 are measured and shown in Table 1.

[0091] Table 1 Various properties of high moisture regain antibacterial viscose fiber

[0092]

[0093]

[0094] Note: strain A is Staphylococcus aureus, strain B is Escherichia coli, and strain C is Candida albicans.

[0095] The standard moisture regain of the viscose fiber prepared by the present invention is ≥15%, the whiteness is ≥80%, and the dry breaking strength is ≥2.2 cN / dtex; and the antibacterial rates of the bonding fiber against Staphylococcus aureus, Escherichia coli and Candida albicans are all ≥90% after being washed 20 times.

[0096] The above is only a specific implementation of the present application, but the protection scope of the present application is not limited thereto. Any person skilled in the art who is familiar with the present technical field can easily think of changes or substitutions within the technical scope disclosed in the present application, which should be included in the protection scope of the present application. Therefore, the protection scope of the present application should be based on the protection scope of the claims.

Claims

1. A method for preparing high moisture regain antibacterial viscose fiber, characterized in that: The method comprises: S1: uniformly mixing a sodium alginate macromolecular aqueous solution with a silver nitrate aqueous solution to obtain a silver-based antibacterial agent solution; preparing a mixed aqueous solution of sulfuric acid, sodium sulfate and zinc sulfate as a coagulation bath for fiber spinning; S2: using a pre-spinning injection process, the silver antibacterial agent solution and the viscose spinning solution are synchronously transported to a dynamic mixer to output a spinning solution containing the silver antibacterial agent; the injection amount of the silver antibacterial agent solution is 0.1%-0.5% by mass of the viscose spinning solution; S3: Extruding the spinning solution containing the silver antibacterial agent from a spinneret with a pore size of 0.05-0.1 mm through a metering pump, and passing through the coagulation bath to obtain a primary fiber; S4: The primary fibers are post-processed to obtain bonding fibers; The silver antibacterial agent is prepared by mixing the sodium alginate macromolecule aqueous solution with the silver nitrate aqueous solution, wherein the viscosity of the sodium alginate macromolecule is 20-50 mPa·s; The mass percentage concentration of the sodium alginate macromolecular aqueous solution is 0.5%-1%, and the concentration of the silver nitrate aqueous solution is 0.5-1 mol / L; wherein the volume ratio of the silver nitrate aqueous solution to the sodium alginate macromolecular aqueous solution is between 1:100-5:100; The coagulation bath is obtained by preparing a mixed aqueous solution of sulfuric acid, sodium sulfate and zinc sulfate; The concentration of the sulfuric acid is 150-160 g / L, the concentration of the sodium sulfate is 380-410 g / L, and the concentration of the zinc sulfate is 10-20 g / L.

2. The method for preparing a high moisture regain antibacterial viscose fiber according to claim 1, characterized in that: In the step S1, it includes: In a light-proof environment, mechanically stirring the sodium alginate macromolecular aqueous solution, while dropwise adding the prepared silver nitrate aqueous solution, until the volume ratio of the silver nitrate aqueous solution to the sodium alginate macromolecular aqueous solution is 1:100-5:100, to prepare a mixed solution; The mixed solution is stirred at 10-40° C. for 30-60 min to obtain the silver-based antibacterial agent solution.

3. The method for preparing a high moisture regain antibacterial viscose fiber according to claim 2, characterized in that: The post-treatment of the nascent fiber includes the following steps: cutting, desulfurization, bleaching, washing, oiling, opening and drying.

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