Multifunctional health-care regenerated cellulose fiber as well as preparation method and application thereof

Abstract

The invention provides a multifunctional health-care regenerated cellulose fiber, and a preparation method and application thereof, and relates to the field of regenerated cellulose fibers. The preparation method of the multifunctional health-care regenerated cellulose fiber comprises the following steps: preparation of a plant essential oil dispersion system, preparation of an iron oxide red dispersion system, preparation of a blended spinning stock solution and spinning. According to the multifunctional health-care regenerated cellulose fiber as well as the preparation method and the application thereof, the problems that plant essential oil is poor in stability and is easily influenced by external environment factors such as temperature and the like, and the plant essential oil is volatilized at high temperature and loses efficacy when being used for preparing the cellulose fiber can be effectively solved; and the problems of poor compatibility with a cellulose fiber matrix, poor stability and poor combination firmness when iron oxide red is used as a sun-screening agent in the cellulose fiber are solved.

Description

Technical Field

[0001] The present invention relates to the field of regenerated cellulose fibers, in particular to a multifunctional health-care regenerated cellulose fiber, a preparation method and an application thereof. Background Art

[0002] Viscose, a type of regenerated cellulose fiber, is obtained by extracting cellulose from abundant natural cellulose and reshaping the fiber molecules using the viscose process. Viscose fiber has high hygroscopicity, which meets the physiological requirements of human skin. It is also smooth, cool, breathable, and anti-static. It is suitable for a wide variety of dyes, boasts vibrant colors, and exhibits excellent color fastness. It is comfortable to wear and is currently widely used in various clothing, nonwovens, and other fields.

[0003] In recent years, the textile industry has introduced a number of fibers and textiles with health-promoting properties that benefit human health and the environment, demonstrating significant market potential. Cellulose fiber products, due to their moisture absorption, breathability, and comfort, are a key textile fiber type. In recent years, they have seen significant development in health-promoting properties, with antibacterial and skin-care benefits becoming increasingly sought-after.

[0004] Essential oils are a general term for aromatic, oily liquids obtained from natural plants. Found in the leaves, stems, flowers, fruits, bark, and roots of plants, they are primarily composed of terpenes, terpenes, and phenylpropanoids. As the essence of natural plants and spices, essential oils are widely available, fast-acting, and non-resistant natural antimicrobial agents. Currently, over 17,000 plant species produce essential oils, but only around 300 are commercially available. Studies have shown that essential oils can inhibit the growth and reproduction of harmful bacteria, and even directly kill them, exerting broad-spectrum antibacterial and antimicrobial effects. Furthermore, essential oils exhibit physiological effects such as anti-inflammatory, antiviral, and antioxidant properties, and promote growth in livestock and poultry. They are considered one of the most promising natural alternatives to antibiotics and have been extensively studied in biomedicine and pharmaceutical fields, with promising prospects for development and utilization. However, plant essential oils have poor stability and are easily affected by external environmental factors such as temperature. When using plant essential oils in the preparation of cellulose fibers, there are problems such as high-temperature volatilization and failure, and they cannot resist the destruction of the effective ingredients in plant essential oils by high-temperature and other process environments.

[0005] Red iron oxide is a red powder with high hiding power, good light resistance, weather resistance, alkali resistance and dilute acid resistance, and it only dissolves when heated with concentrated acid. Red iron oxide has many important functions. It can absorb ultraviolet rays and convert them into heat energy. It can be used as an important raw material for many sunscreens, thereby protecting the skin from ultraviolet damage; red iron oxide can accelerate skin healing and protect the skin. The inventors found that when using red iron oxide in the preparation of cellulose fibers, due to the different structures and polarities of red iron oxide and cellulose fibers, red iron oxide has poor compatibility, poor stability and poor bonding strength in the cellulose fiber matrix. Red iron oxide is uneven in the cellulose fiber matrix, which directly leads to uneven functionality of the cellulose fibers. Summary of the Invention

[0006] In order to solve the technical problems existing in the prior art, the present invention provides a multifunctional health-care regenerated cellulose fiber, a preparation method and an application, which can effectively solve the problems of poor stability of plant essential oils and susceptibility to external environmental factors such as temperature, high-temperature volatilization and ineffectiveness in the preparation of cellulose fibers; and overcome the problems of poor compatibility, poor stability and poor bonding strength of red iron oxide used as a sunscreen in cellulose fibers.

[0007] In order to solve the above technical problems, the technical solutions adopted by the present invention are as follows: A method for preparing multifunctional health-care regenerated cellulose fiber comprises the following steps: preparing a plant essential oil dispersion system, preparing an iron oxide red dispersion system, preparing a blended spinning solution, and spinning; The preparation of the plant essential oil dispersion system includes the following steps: preparation and modification of an oily blend powder containing the plant essential oil; The preparation of the oily blend powder containing plant essential oil comprises the following steps: uniformly mixing molten n-alkane and plant essential oil to obtain the plant essential oil oily blend; then mixing low thermal conductivity porous silicate mineral powder and the plant essential oil oily blend, and ultrasonically treating the mixture to obtain the plant essential oil oily blend powder; In the modification treatment, the dispersant, the coupling agent, the oily blend powder containing the plant essential oil and deionized water are ground and dispersed to obtain a plant essential oil dispersion system.

[0008] Preferably, the plant essential oil is at least one of the following: lavender essential oil, peppermint essential oil, sarcandra essential oil, isatis root essential oil, thyme essential oil, melaleuca oil, cinnamon essential oil, clove essential oil, eucalyptus essential oil, tea tree essential oil, camellia seed oil, oregano essential oil; more preferably, it is at least one of the following: lavender essential oil, thyme essential oil, camellia seed oil, cinnamon essential oil, clove essential oil, eucalyptus essential oil, oregano essential oil.

[0009] Preferably, the n-alkane is a mixture of n-eicosane, n-heneicosane and n-tricosane; The low thermal conductivity porous silicate mineral powder is one of the following: mica powder, diatomaceous earth, kaolin, sepiolite, and zeolite.

[0010] Preferably, the mass ratio of the plant essential oil to the normal alkane is 1-2:1; The mass ratio of n-eicosane, n-heneicosane and n-tricosane is 1:1-2:2-3; The mass ratio of the low thermal conductivity porous silicate mineral powder to the plant essential oil oily blend is 1:1-2.

[0011] Preferably, the mixing temperature of the n-alkane and the plant essential oil is 45-50° C., the mixing speed is 300-500 rpm, and the mixing time is 1.5-2 h.

[0012] Preferably, the ultrasonic treatment temperature of the low thermal conductivity porous silicate mineral powder and the plant essential oil oily mixture after mixing is 25-30° C., the ultrasonic treatment frequency is 3.5-5.5 MHz, and the ultrasonic treatment time is 20-30 min.

[0013] Preferably, in the modification treatment, the dispersant is one of the following: sodium dodecylbenzenesulfonate, sodium methylene bisnaphthalenesulfonate; the coupling agent is one of the following: silane coupling agent kh-570, silane coupling agent kh-560, coupling agent A-151, coupling agent A-171; The mass ratio of the dispersant, the coupling agent and the oily blend powder containing plant essential oil is 8-12:2-5:100.

[0014] Preferably, during the grinding and dispersion, the mass fraction of the oily blend powder containing plant essential oil is maintained at 35-45% by controlling the amount of deionized water added; the grinding and dispersion speed is 2500-3500 r / min, the grinding and dispersion vacuum is 0.080-0.092 MPa, and the grinding and dispersion temperature is maintained in the range of 15-25°C, and the grinding and dispersion is stopped when the particle size of the dispersed system reaches D90≤2.150 μm.

[0015] Preferably, the preparation of the iron oxide red dispersion system comprises grinding and dispersing a dispersant, a defoaming agent, a coupling agent, nano iron oxide red, and deionized water to obtain a nano iron oxide red aqueous dispersion system; then, gelatin and gum arabic are added to the nano iron oxide red aqueous dispersion system, and the mixture is stirred evenly at a speed of 2000-2200 r / min and a temperature of 20-30°C, and the pH is adjusted to acidic, and the mixture is stirred for reaction; transglutaminase is added, and the pH is adjusted to alkaline, and the mixture is stirred for reaction; a thickener is used to adjust the viscosity to 25-35s to obtain an iron oxide red dispersion system.

[0016] Preferably, in the preparation of the iron oxide red dispersion system, the dispersant is sodium dodecylbenzenesulfonate or sodium methylene bisnaphthalenesulfonate; the defoaming agent is polyoxypropylene glycerol ether or polyoxypropylene polyoxyethylene glycerol ether; the coupling agent is one of the following: silane coupling agent KH-570, silane coupling agent KH-560, coupling agent A-151, coupling agent A-171; The mass ratio of dispersant, defoaming agent, coupling agent and nano iron oxide red is 10-15:3-5:2-5:100; 7-8% by mass of gelatin and 7-8% by mass of gum arabic were added to the nano-iron oxide red aqueous dispersion system.

[0017] Preferably, in the preparation of the iron oxide red dispersion system, the mass fraction of the nano iron oxide red powder is maintained at 20-35% by controlling the amount of deionized water added during grinding and dispersion; and the dispersion system is ground and dispersed until the particle size D90 is 0.551-0.895 μm.

[0018] Preferably, in the preparation of the iron oxide red dispersion system, the pH is adjusted to an acidic pH value of preferably 4.5-6.5, and the stirring reaction time under acidic conditions is 30-50 minutes; the pH is adjusted to an alkaline pH value of preferably 7.5-9.5, and the stirring reaction time under alkaline conditions is 40-50 minutes; then the stirring speed is reduced to 850-900 r / min, and the reaction is continued for 1.0-2.0 hours to obtain the iron oxide red primary dispersion system.

[0019] Preferably, in the preparation of the red iron oxide dispersion system, the thickener is one of sodium carboxymethyl cellulose, polyvinyl pyrrolidone, and sodium alginate, and the added amount is 5-8% of the mass of the nano red iron oxide.

[0020] Preferably, the blended spinning solution is prepared by uniformly mixing the plant essential oil dispersion system, the iron oxide red dispersion system and the spinning solution to obtain the blended spinning solution; The cellulose A content in the spinning solution is 8.90-9.25 wt%; The amount of the plant essential oil dispersion system added is 5-9% of the mass of the cellulose amine in the spinning solution; The added amount of the iron oxide red dispersion system is 3-6% of the mass of the type A cellulose in the spinning solution.

[0021] Preferably, the specifications of the spinning solution are: cellulose methyl content 8.90-9.25wt%, sodium hydroxide content 4.55-4.85wt%, falling ball viscosity at 20°C of 40-55s, maturity (10% NH4Cl value) of 15-20mL, denaturant polyethylene glycol (molecular weight 1500) content of 0.8-1.2%, and denaturant EBT content of 1.0-1.5%.

[0022] Preferably, the spinning is carried out by spinning the blended spinning solution into a coagulation bath at 45-50°C, and the obtained spun filaments are drawn to obtain a formed filament, and the formed filaments are post-treated to obtain multifunctional health-care regenerated cellulose fibers; The coagulation bath includes: 95-105 g / L of sulfuric acid, 310-330 g / L of sodium sulfate, 9.5-11.0 g / L of zinc sulfate, 5-8 g / L of acid bath auxiliary agent, 3-5 g / L of denaturant EBT, and the solvent is deionized water.

[0023] The post-treatment includes: first water washing, desulfurization, second water washing, pickling, third water washing, fourth water washing, oiling, vacuum drying and opening.

[0024] The temperatures of the first, second, third and fourth water washes are 65-75° C. After the fourth water wash is used up, the second water wash is added, and after the third water wash, the first water wash is added, thereby improving the recycling rate of water.

[0025] In the desulfurization, the desulfurization bath adopts Na2SO3 solution with a concentration of 6.0-10.0 g / L and a desulfurization bath temperature of 75-85°C.

[0026] In the pickling, the pickling bath uses lactic acid or acetic acid solution with a concentration of 3-6 g / L and a pickling bath temperature of 45-55°C.

[0027] After the first water washing, desulfurization, second water washing, acid washing, third water washing and fourth water washing are completed, a pressing process is performed, and the pressing pressure is controlled to be 0.10-0.15MPa.

[0028] Before the vacuum drying, a high-pressure roller is used for squeezing and dehydration. The pressure of the high-pressure roller is 0.35-0.4 MPa. The moisture regain of the fiber after squeezing and dehydration is 120-135%. During the vacuum drying, the vacuum degree is controlled to be 0.03-0.09 MPa, and the vacuum drying temperature is 45-48° C., and the vacuum drying is stopped until the moisture regain of the fiber reaches 11.6-13.8%.

[0029] A multifunctional health-care regenerated cellulose fiber is prepared by the above-mentioned preparation method.

[0030] A use of the multifunctional health-care regenerated cellulose fiber in textile fabrics and / or non-woven fabrics.

[0031] Compared with the prior art, the present invention has the following beneficial effects: (1) The method for preparing the multifunctional health-care regenerated cellulose fiber of the present invention can effectively solve the problems of poor stability of plant essential oils and susceptibility to external environmental factors such as temperature, which lead to high-temperature volatilization and failure of plant essential oils in the preparation of cellulose fibers by using the plant essential oil dispersion system and the iron oxide red dispersion system in the preparation of regenerated cellulose fibers; and overcome the problems of poor compatibility, poor stability and poor bonding strength of iron oxide red as a sunscreen in cellulose fibers.

[0032] (2) In the preparation of the multifunctional health-care regenerated cellulose fiber of the present invention, the plant essential oil has poor stability and is easily affected by external environmental factors such as temperature. In the preparation of cellulose fiber, the plant essential oil is used in combination with n-alkanes with multi-layer melting points. The phase change process of n-alkanes during temperature changes is used to buffer the plant essential oil, so that the plant essential oil is not affected by large temperature fluctuations, thereby avoiding damage to the plant essential oil and providing a first layer of protection for the stability of the plant essential oil in the fiber preparation process. The low thermal conductivity porous silicate mineral powder fully adsorbs the plant essential oil oily blend and exists in the porous structure. The low thermal conductivity of the silicate mineral powder is used to reduce heat transfer, thereby achieving a second layer of protection for the plant essential oil.

[0033] (3) In the preparation of the multifunctional health-care regenerated cellulose fiber of the present invention, in the preparation of the iron oxide red dispersion system, the stability of the nano iron oxide red is further increased and its compatibility with the regenerated cellulose fiber matrix is improved through complex coagulation reaction and cross-linking reaction; the stability of the iron oxide red dispersion system is increased by using a thickener, thereby ensuring its effect in the preparation of the regenerated cellulose fiber.

[0034] (4) The multifunctional health-care regenerated cellulose fiber of the present invention is made of plant essential oil, red iron oxide and cellulose pulp as main raw materials. By protecting and modifying the plant essential oil and red iron oxide, the regenerated cellulose fiber is endowed with good health-care functions such as antibacterial, antiviral, skin care and UV protection. The multifunctional health-care regenerated cellulose fiber has an antibacterial rate of ≥88.5% against Staphylococcus aureus, an antibacterial rate of ≥86.7% against Escherichia coli and an antibacterial rate of ≥89.2% against Candida albicans; the antiviral activity value against influenza A virus is ≥2.5, and the antiviral activity value against influenza B virus is ≥2.3; the ultraviolet protection factor (UPF) is ≥45, the ultraviolet transmittance T (UVA) is ≤4.5%, and the regenerated cellulose fiber contains red iron oxide, which has good skin protection and skin care effects.

[0035] (5) After washing 30 times, the multifunctional health-care regenerated cellulose fiber of the present invention still has an antibacterial rate against Staphylococcus aureus of ≥87.0%, an antibacterial rate against Escherichia coli of ≥85.8%, and an antibacterial rate against Candida albicans of ≥87.9%; the antiviral activity value against influenza A virus is still ≥2.5, and the antiviral activity value against influenza B virus is still ≥2.3; the ultraviolet protection factor (UPF) is still ≥43, and the ultraviolet transmittance T (UVA) is still ≥4.56%.

[0036] (6) The preparation method of the multifunctional health-care regenerated cellulose fiber of the present invention is reliable and can be prepared on the basis of the existing viscose fiber production process and production line, which is conducive to large-scale industrial production.

[0037] (7) The multifunctional health-care regenerated cellulose fiber of the present invention can be effectively used in protective fabrics and / or non-woven fabrics such as clothing and home textiles, and has broad application prospects. DETAILED DESCRIPTION

[0038] In order to provide a clearer understanding of the technical features, objectives, and effects of the present invention, specific embodiments of the present invention are now described. It should be noted that the following detailed description is illustrative and is intended to further illustrate the present invention. Unless otherwise specified, all technical and scientific terms used in the present invention have the same meanings as those commonly understood by those skilled in the art to which the present invention belongs.

[0039] It should be noted that the terms used herein are intended only to describe specific embodiments and are not intended to limit the exemplary embodiments of the present invention. As used herein, "first," "second," and the like are used to distinguish similar objects and are not used to describe a specific order or precedence. In addition, it should be understood that when the terms "comprise" and / or "include" are used in this specification, they indicate the presence of features, steps, operations, devices, components, and / or combinations thereof.

[0040] The embodiment of the present invention provides a preparation method of multifunctional health-care regenerated cellulose fiber, comprising the following steps: preparing a plant essential oil dispersion system, preparing a red iron oxide dispersion system, preparing a blended spinning solution, and spinning.

[0041] The preparation of the plant essential oil dispersion system comprises the following steps: preparation of an oily blend powder containing the plant essential oil and modification treatment.

[0042] The preparation method of the oily blend powder containing plant essential oil comprises the following steps: stirring and mixing the plant essential oil and molten n-alkane at a mass ratio of 1-2:1 at a temperature of 47-52° C., a stirring speed of 300-500 r / min, and a stirring time of 1.5-2 hours to obtain the plant essential oil oily blend; then adding low thermal conductivity porous silicate mineral powder to the plant essential oil oily blend, and ultrasonically treating the mixture at a temperature of 25-30° C. and an ultrasonic wave condition of a frequency of 3.5-5.5 MHz for 20-30 minutes to obtain the plant essential oil oily blend powder.

[0043] In the preparation of the oily blend powder containing plant essential oil, the plant essential oil is an oily liquid obtained by extraction from plants and containing at least one of terpenes, terpenes, and phenylpropanoid components; the plant essential oil is preferably at least one of the following: lavender essential oil, peppermint essential oil, sargassum essential oil, isatis root essential oil, thyme essential oil, melaleuca oil, cinnamon essential oil, clove essential oil, eucalyptus essential oil, tea tree essential oil, camellia seed oil, oregano essential oil; the plant essential oil is more preferably one of the following: lavender essential oil, thyme essential oil, camellia seed oil, cinnamon essential oil, clove essential oil, eucalyptus essential oil, oregano essential oil.

[0044] The n-alkane is a mixture of n-eicosane, n-heneicosane, and n-tricosane in a mass ratio of 1:1-2:2-3; it utilizes the phase change effect of n-alkanes with different melting points to have a continuous heat absorption function during the temperature increase process, providing the first layer of protection for the stability of plant essential oils during the fiber preparation process.

[0045] The low-thermal-conductivity porous silicate mineral powder is one of the following: mica powder, diatomaceous earth, kaolin, sepiolite, and zeolite. The mass ratio of the low-thermal-conductivity porous silicate mineral powder to the plant essential oil blend is 1:1-2. During the mixing process, ultrasonic treatment is used to promote the low-thermal-conductivity porous silicate mineral powder to fully adsorb the plant essential oil blend, allowing it to reside in its porous structure. The low thermal conductivity of the silicate mineral powder is utilized to reduce heat transfer, providing a secondary layer of protection for the stability of the plant essential oil during the fiber preparation process.

[0046] The modification treatment comprises uniformly mixing a dispersant, a coupling agent, an oily blend powder containing plant essential oils, and deionized water, grinding and dispersing the mixture in a vacuum and wet state using a sand mill disperser, controlling the mass fraction of the oily blend powder containing plant essential oils to be 35-45%, and grinding at a speed of 2500-3500 r / min until the particle size of the dispersed system reaches D90 ≤ 2.150 μm, thereby stopping the grinding and dispersing to obtain a modified oily blend powder dispersion system containing plant essential oils, i.e., a plant essential oil dispersion system; and controlling the temperature of the grinding dispersion system to be 15-25° C. by jacket condensation during the grinding process, wherein the jacket medium is deionized water.

[0047] In the modification treatment, the dispersant is one of sodium dodecylbenzenesulfonate and sodium methylenebisnaphthalenesulfonate; the coupling agent is one of silane coupling agent KH-570, silane coupling agent KH-560, coupling agent A-151, and coupling agent A-171, purchased from Nanjing Xiangqian Chemical Co., Ltd., and the coupling agent is used for modification to improve the compatibility of the powder with the oily substance and the final fiber matrix; the dispersant, coupling agent, and oily blend powder containing plant essential oil are mixed in a mass ratio of 8-12:2-5:100; the vacuum degree of grinding and dispersion is 0.080-0.092 MPa, and grinding and dispersion are carried out under vacuum conditions to reduce the occurrence of bubbles during the grinding and dispersion process.

[0048] The preparation of the iron oxide red dispersion system comprises adding a dispersant, a defoaming agent, a coupling agent, nano iron oxide red, and deionized water into a dispersing sand mill, grinding and dispersing the mixture at a rotation speed of 2500-3500 r / min to obtain a nano iron oxide red aqueous dispersion system; wherein the mass fraction of the nano iron oxide red powder is 20-25%, and the particle size D90 of the dispersion system is 0.551-0.895 μm.

[0049] In the preparation of the red iron oxide dispersion system, the dispersant is one of sodium dodecylbenzene sulfonate and sodium methylene bisnaphthalene sulfonate; the defoamer is one of polyoxypropylene glycerol ether and polyoxypropylene polyoxyethylene glycerol ether; and the coupling agent is one of silane coupling agent KH-570, silane coupling agent KH-560, coupling agent A-151, and coupling agent A-171, all purchased from Nanjing Xiangqian Chemical Co., Ltd. The mass ratio of the dispersant, defoamer, coupling agent, and nano red iron oxide is 10-15:3-5:2-5:100.

[0050] Then, gelatin (mass fraction of 7.0-8.0%) and gum arabic (mass fraction of 7.0-8.0%) are added to the above-mentioned nano-iron oxide red aqueous dispersion system, and the mixture is stirred at a speed of 2000-2200 r / min and a temperature of 20-30°C to dissolve the mixture, and the mixture is kept warm. The pH value is adjusted to 4.5-6.5, and a complex coagulation reaction is carried out at the aforementioned temperature and stirring speed conditions for 30-50 minutes. After that, a curing agent, transglutaminase, is added, and the pH value is adjusted to 7.5-9.5. A cross-linking reaction is carried out at the aforementioned temperature and stirring speed conditions for 40-50 minutes. The stirring speed is then reduced to 850-900 r / min and the reaction is continued for 1.0-2.0 hours to obtain a primary dispersion system of iron oxide red. In this process, the stability of the nano-iron oxide red is further increased by utilizing the complex coagulation reaction and cross-linking reaction, and its compatibility with the fiber matrix is improved.

[0051] A thickener is then added to the primary iron oxide red dispersion to adjust its viscosity to 25-35 seconds (falling ball viscosity) to prepare an iron oxide red dispersion. This increases the stability of the final iron oxide red dispersion and prevents precipitation. The thickener is selected from sodium carboxymethyl cellulose, polyvinyl pyrrolidone, or sodium alginate, and is added in an amount of 5-8% by weight of the nano-iron oxide red.

[0052] The blended spinning solution is prepared using cellulose pulp as the raw material and undergoing a viscose preparation process to produce a cellulose spinning solution with the following specifications: 8.90-9.25% cellulose amine, 4.55-4.85% sodium hydroxide, a falling ball viscosity of 40-55 seconds at 20°C, and a degree of maturity (10% NH₄Cl value) of 15-20 mL. 0.8-1.2% of polyethylene glycol (molecular weight, 1500) and 1.0-1.5% of EBT (Klein, Germany) are also added as denaturants. Using a pre-spinning injection device, the prepared plant essential oil dispersion and red iron oxide dispersion are added to the regenerated cellulose fiber spinning solution at a mass ratio of 5.0-9.0% of plant essential oil to cellulose amine and 3.0-6.0% of nano red iron oxide to cellulose amine in the spinning solution, to produce the blended spinning solution.

[0053] The pre-spinning injection device comprises a functional additive filtration device, a pre-spinning injection buffer tank, a metering device, a dynamic mixer, and a static mixer. The additive filtration device uses a plate-and-frame filter, made of one layer of polypropylene felt and two layers of silk cloth, with a pore size of 15-20 μm. This filtration prevents impurities introduced during the production process, improving the additive's usability and the fiber's spinnability. The pre-spinning injection buffer tank ensures better liquid level stability for the blended additives, preventing instability in the added additive content. The metering device uses a mechanical diaphragm pump (Q = 1500 L / h) with an outlet pressure of 0.7-0.9 MPa. The dynamic mixer and static mixer are used in series to improve the uniformity of the blended spinning solution.

[0054] The spinning comprises filtering the blended spinning solution through a candle filter and then passing the solution through a spinneret into a coagulation bath for spinning. The obtained nascent filament bundle is drawn to obtain a formed filament bundle, and the formed filament bundle is cut and post-processed to obtain multifunctional health-care regenerated cellulose fiber.

[0055] The candle filter is made of polypropylene and adopts an inside-out filtering method. The filtering material is two layers of silk cloth.

[0056] The coagulation bath includes 95-105 g / L of sulfuric acid, 310-330 g / L of sodium sulfate, 9.5-11.0 g / L of zinc sulfate, 5-8 g / L of acid bath additive (Berol Spin 653 from Swedish company Berol Kemi), and 3-5 g / L of denaturant EBT. The solvent is deionized water, and the coagulation bath temperature is 45-50°C.

[0057] The post-treatment includes the following steps: first water washing, desulfurization, second water washing, pickling, third water washing, fourth water washing, oiling, vacuum drying, and opening treatment. After each bath treatment, the product is pressed, and before entering the vacuum drying step, a high-pressure rolling mill is used for pressing and dehydration.

[0058] The desulfurization bath uses Na2SO3 solution with a concentration of 6.0-10.0 g / L and a desulfurization bath temperature of 75-85°C.

[0059] The pickling bath uses lactic acid or acetic acid solution with a concentration of 3-6 g / L and a temperature of 45-55° C. A weak acid is used for pickling. Pickling can not only remove some impurities on the fiber, but also make the fiber brighter.

[0060] The temperatures of the first, second, third and fourth water washes are 65-75° C. After the fourth water wash is used up, the second water wash is added, and after the third water wash, the first water wash is added, thereby improving the recycling rate of water.

[0061] The squeezing pressure after each bath treatment is 0.10-0.15MPa; The fiber is squeezed and dehydrated by a high-pressure roller before entering the vacuum drying process. The pressure of the high-pressure roller is 0.35-0.4 MPa. The moisture regain of the fiber after dehydration is 120-135%.

[0062] The vacuum drying adopts a vacuum decompression drying method, controls the vacuum degree to 0.03-0.09 MPa, and the vacuum drying temperature to 45-48° C., until the fiber regain reaches 11.6-13.8%. By using the vacuum decompression drying method to dry the prepared fiber, the damage to the plant essential oil caused by temperature is further avoided, providing a third layer of protection for the plant essential oil.

[0063] The embodiment of the present invention also provides multifunctional health-care regenerated cellulose fiber prepared by the above method.

[0064] The embodiments of the present invention also provide applications of the multifunctional health-care regenerated cellulose fiber, in particular, applications of the multifunctional health-care regenerated cellulose fiber in textile fabrics and / or non-woven fabrics.

[0065] The present invention will be further described below with reference to some specific embodiments.

[0066] Example 1 This embodiment provides a method for preparing multifunctional health-care regenerated cellulose fiber with a specification of 1.33 dtex×38 mm, and the specific steps are as follows: 1. Preparation of plant essential oil dispersion system 1) Preparation of oily blend powder containing plant essential oils The plant essential oil and molten n-alkane were stirred uniformly at a mass ratio of 1:1 at 47°C, at a speed of 300 r / min, and for 2 hours to obtain a plant essential oil blend. The plant essential oil was lavender essential oil, and the n-alkane was a mixture of n-eicosane, n-heneicosane, and n-tricosane in a mass ratio of 1:1:2.

[0067] Low thermal conductivity porous silicate mineral powder is then added to the plant essential oil blend and ultrasonically treated at 25°C and 3.5 MHz for 30 minutes to obtain a plant essential oil-containing oil blend powder. The low thermal conductivity porous silicate mineral powder is mica powder, and the mass ratio of the low thermal conductivity porous silicate mineral powder to the plant essential oil blend is 1:1.

[0068] 2) Modification treatment A dispersant, a coupling agent, an oily blend powder containing plant essential oils, and deionized water were uniformly mixed and then ground and dispersed using a sand mill under vacuum and wet conditions. The mass fraction of the oily blend powder containing plant essential oils was 35%, and the grinding speed was 2500 r / min. Grinding and dispersion was stopped when the particle size of the dispersed system reached D90 = 2.150 μm, thereby obtaining a modified oily blend powder dispersion containing plant essential oils, i.e., a plant essential oil dispersion system. During the grinding process, jacket condensation was performed using deionized water as the jacket medium to prevent the temperature of the grinding dispersion system from rising, maintaining it at 15°C.

[0069] Among them, the dispersant is sodium dodecylbenzenesulfonate; the coupling agent is silane coupling agent KH-570, purchased from Nanjing Xiangqian Chemical Co., Ltd.; the dispersant, coupling agent, and oily blend powder containing plant essential oil are mixed in a mass ratio of 8:2:100; the vacuum degree of the grinding and dispersion is -0.080 MPa, and the grinding and dispersion is carried out under vacuum conditions to reduce the occurrence of bubbles during the grinding and dispersion process.

[0070] 2. Preparation of Iron Oxide Red Dispersion System A dispersant, defoamer, coupling agent, nano-iron oxide red, and deionized water were added to a dispersing sand mill and ground and dispersed at 2500 r / min to prepare a nano-iron oxide red aqueous dispersion. The mass fraction of the nano-iron oxide red powder was 20%, and the particle size D90 of the dispersion was 0.551 μm. The dispersant was sodium dodecylbenzene sulfonate; the defoamer was polyoxypropylene glycerol ether; and the coupling agent was silane coupling agent KH-570, purchased from Nanjing Xiangqian Chemical Co., Ltd. The mass ratio of the dispersant, defoamer, coupling agent, and iron oxide red was 10:3:2:100.

[0071] Gelatin (7.0% by mass) and gum arabic (7.0% by mass) were added to the nano-iron oxide red aqueous dispersion, stirred at 2000 r / min and 30°C to dissolve, and kept warm. The pH was adjusted to 4.5, and a complex coacervation reaction was carried out at the aforementioned temperature and stirring speed for 30 minutes. Transglutaminase, a curing agent, was then added, and the pH was adjusted to 7.5. A cross-linking reaction was carried out at the aforementioned temperature and stirring speed for 40 minutes. The stirring speed was then reduced to 850 r / min, and the reaction was continued for 1.0 hour to obtain a primary iron oxide red dispersion. A thickener was then added to a viscosity of 25 seconds (falling ball viscosity) to obtain an iron oxide red dispersion. The thickener was sodium carboxymethyl cellulose, added in an amount of 5% by mass of the nano-iron oxide red.

[0072] 3. Preparation of blended spinning solution A cellulose spinning dope was prepared using cellulose pulp as raw material through a viscose preparation process. Its specifications included 8.90% cellulose α-cellulose, 4.55% sodium hydroxide, a ball-falling viscosity of 40 seconds at 20°C, and a maturity (10% NH₄Cl value) of 15 mL. 0.8% polyethylene glycol (molecular weight, 1500) and 1.5% EBT (Kline, Germany) were added as denaturants. A plant essential oil dispersion and a red iron oxide dispersion were added to the regenerated cellulose fiber spinning dope using a pre-spinning injection device, with the plant essential oil accounting for 5.0% of the cellulose α-cellulose weight and the nano-red iron oxide accounting for 3.0% of the cellulose α-cellulose weight in the spinning dope, to produce a blended spinning dope.

[0073] The pre-spinning injection device includes a functional additive filter, a pre-spinning injection buffer tank, a metering device, a dynamic mixer, and a static mixer. The additive filter utilizes a plate-and-frame filter, made of one layer of polypropylene felt and two layers of silk cloth, with a pore size of 15-20 μm. This filtration prevents impurities introduced during the production process, improving the additive's usability and the fiber's spinnability. The pre-spinning injection buffer tank ensures better liquid level stability for the blended additive, preventing instability in the added additive content. The metering device utilizes a mechanical diaphragm pump (Q = 1500 L / h) with an outlet pressure of 0.7 MPa. The dynamic mixer and static mixer are used in series to improve the uniformity of the blended spinning solution.

[0074] 4. Spinning The blended spinning solution is filtered through a candle filter and then passed through a spinneret into a coagulation bath for spinning. The obtained nascent filament bundle is drawn to obtain a formed filament bundle, which is cut and post-processed to obtain multifunctional health-care regenerated cellulose fiber.

[0075] The candle filter is made of polypropylene and adopts an inside-out filtering method. The filtering material is two layers of silk cloth.

[0076] The coagulation bath includes 95 g / L sulfuric acid, 310 g / L sodium sulfate, 9.5 g / L zinc sulfate, 5 g / L acid bath additive (Berol Spin 653 from Berol Kemi, Sweden), and 3 g / L denaturant EBT. The solvent is deionized water, and the coagulation bath temperature is 45°C.

[0077] The post-treatment includes the following steps: first water washing, desulfurization, second water washing, pickling, third water washing, fourth water washing, oiling, vacuum drying, and opening treatment. After each bath treatment, the product is pressed, and before entering the vacuum drying step, a high-pressure rolling mill is used for pressing and dehydration.

[0078] The desulfurization bath uses Na2SO3 solution with a concentration of 6.0g / L and a desulfurization bath temperature of 85°C; The pickling bath uses a lactic acid solution with a concentration of 3 g / L, a pickling bath temperature of 55° C., and a weak acid is used for pickling.

[0079] The temperature of the first, second, third and fourth water washes is 65° C. After the fourth water wash is used up, the second water wash is added, and after the third water wash, the first water wash is added, thereby improving the recycling rate of water.

[0080] The squeezing pressure after each bath treatment is 0.10 MPa; the high-pressure roller is used for squeezing and dehydration before entering the vacuum drying, and the pressure of the high-pressure roller is 0.35 MPa. The moisture regain of the fiber after dehydration is 135%.

[0081] The vacuum drying adopts a vacuum decompression drying method, controls the vacuum degree to 0.03MP, and the vacuum drying temperature to 45°C, until the fiber moisture regain reaches 13.8%.

[0082] This embodiment also provides multifunctional health-care regenerated cellulose fiber prepared by the above method.

[0083] This embodiment also provides the use of the multifunctional health-care regenerated cellulose fiber in textile fabrics and / or non-woven fabrics.

[0084] Testing showed that the multifunctional health-care regenerated cellulose fiber prepared in this embodiment had an antibacterial rate of 88.5% against Staphylococcus aureus, 86.7% against Escherichia coli, and 89.2% against Candida albicans; its antiviral activity against influenza A virus was 2.5, and its antiviral activity against influenza B virus was 2.3; its ultraviolet protection factor (UPF) was 45, and its ultraviolet transmittance T (UVA) was 4.5%; and the cellulose fiber contained red iron oxide, which has excellent skin protection and skin care effects.

[0085] Meanwhile, after the multifunctional health-care regenerated cellulose fiber prepared in this embodiment was washed 30 times according to the washing method in Appendix C 4. Simplified Washing Conditions and Procedures of Standard FZ / T 73023-2006, the antibacterial rates against Staphylococcus aureus, Escherichia coli, and Candida albicans still reached 87.0%, 85.8%, and 87.9%, respectively; the antiviral activity values against influenza A virus and influenza B virus still reached 2.5 and 2.3, respectively; the ultraviolet protection factor (UPF) still reached 43, and the ultraviolet transmittance T (UVA) still reached 4.56%.

[0086] Example 2 This embodiment provides a method for preparing multifunctional health-care regenerated cellulose fiber with a specification of 1.56 dtex×38 mm, and the specific steps are as follows: 1. Preparation of plant essential oil dispersion system 1) Preparation of oily blend powder containing plant essential oils The plant essential oil and molten n-alkane were stirred uniformly at 49.5° C. in a mass ratio of 1.5:1 at a stirring speed of 410 r / min for 1.8 hours to obtain a plant essential oil blend. The plant essential oil was lavender essential oil, and the n-alkane was a mixture of n-eicosane, n-heneicosane, and n-tricosane in a mass ratio of 1:2:2.

[0087] A low-thermal-conductivity porous silicate mineral powder was then added to the essential oil blend and ultrasonically treated at 28°C and a frequency of 4.4 MHz for 26 minutes to obtain a powder containing the essential oil. The low-thermal-conductivity porous silicate mineral powder was diatomaceous earth, and the mass ratio of the low-thermal-conductivity porous silicate mineral powder to the essential oil blend was 1:1.5.

[0088] 2) Modification treatment A dispersant, a coupling agent, an oily blend powder containing plant essential oils, and deionized water were uniformly mixed and then ground and dispersed using a sand mill under vacuum and wet conditions. The mass fraction of the oily blend powder containing plant essential oils was 40%, and the grinding speed was 3000 r / min. Grinding and dispersion was stopped when the particle size of the dispersed system reached D90 = 1.975 μm, thereby obtaining a modified oily blend powder dispersion containing plant essential oils, i.e., a plant essential oil dispersion system. During the grinding process, jacket condensation was performed using deionized water as the jacket medium to prevent the temperature of the grinding dispersion system from rising, maintaining it at 20°C.

[0089] Among them, the dispersant is sodium dodecylbenzenesulfonate; the coupling agent is silane coupling agent KH-560, purchased from Nanjing Xiangqian Chemical Co., Ltd.; the dispersant, coupling agent, and oily blend powder containing plant essential oil are mixed in a mass ratio of 10:3.8:100; the vacuum degree of the grinding and dispersion is -0.086 MPa, and the grinding and dispersion is carried out under vacuum conditions to reduce the occurrence of bubbles during the grinding and dispersion process.

[0090] 2. Preparation of Iron Oxide Red Dispersion System A dispersant, defoamer, coupling agent, nano-iron oxide red, and deionized water were added to a dispersing sand mill and ground and dispersed at 3000 r / min to prepare a nano-iron oxide red aqueous dispersion. The mass fraction of the nano-iron oxide red powder was 23.2%, and the particle size D90 of the dispersion was 0.726 μm. The dispersant was sodium dodecylbenzene sulfonate; the defoamer was polyoxypropylene glycerol ether; and the coupling agent was silane coupling agent KH-560, purchased from Nanjing Xiangqian Chemical Co., Ltd. The mass ratio of the dispersant, defoamer, coupling agent, and iron oxide red was 12.6:4:4:100.

[0091] Gelatin (7.5% by mass) and gum arabic (7.5% by mass) were added to the nano-iron oxide red aqueous dispersion, stirred at 2110 r / min and 25.6°C to dissolve, and then kept warm. The pH was adjusted to 5.6, and a complex coacervation reaction was carried out at the aforementioned temperature and stirring speed for 41 minutes. Transglutaminase, a curing agent, was then added, and the pH was adjusted to 8.6. A cross-linking reaction was carried out at the aforementioned temperature and stirring speed for 45 minutes. The stirring speed was then reduced to 875 r / min and the reaction was continued for 1.5 hours to obtain a primary iron oxide red dispersion. A thickener was then added to a viscosity of 31 seconds (falling ball viscosity) to obtain an iron oxide red dispersion. The thickener was sodium carboxymethyl cellulose, added in an amount of 6.8% of the mass of the nano-iron oxide red.

[0092] 3. Preparation of blended spinning solution A cellulose spinning dope was prepared using cellulose pulp as raw material through a viscose preparation process. Its specifications included 9.03% cellulose α-cellulose, 4.72% sodium hydroxide, a ball-falling viscosity of 48 seconds at 20°C, and a degree of maturity (10% NH₄Cl value) of 17.5 mL. Polyethylene glycol (molecular weight, 1500) was added as a denaturant at 1.0%, and EBT (Kline, Germany) was added at 1.2%. A plant essential oil dispersion and a red iron oxide dispersion were added to the regenerated cellulose fiber spinning dope using a pre-spinning injection device, with the plant essential oil accounting for 7.5% of the cellulose α-cellulose weight and the nano-red iron oxide accounting for 4.9% of the cellulose α-cellulose weight in the spinning dope to produce a blended spinning dope.

[0093] The pre-spinning injection device includes a functional additive filter, a pre-spinning injection buffer tank, a metering device, a dynamic mixer, and a static mixer. The additive filter utilizes a plate-and-frame filter, made of one layer of polypropylene felt and two layers of silk cloth, with a pore size of 15-20 μm. This filtration prevents impurities introduced during the production process, improving the additive's usability and the fiber's spinnability. The pre-spinning injection buffer tank ensures better liquid level stability for the blended additive, preventing instability in the added additive content. The metering device utilizes a mechanical diaphragm pump (Q = 1500 L / h) with an outlet pressure of 0.8 MPa. The dynamic mixer and static mixer are used in series to improve the uniformity of the blended spinning solution.

[0094] 4. Spinning The blended spinning solution is filtered through a candle filter and then passed through a spinneret into a coagulation bath for spinning. The obtained nascent filament bundle is drawn to obtain a formed filament bundle, which is cut and post-processed to obtain multifunctional health-care regenerated cellulose fiber.

[0095] The candle filter is made of polypropylene and adopts an inside-out filtering method. The filtering material is two layers of silk cloth.

[0096] The coagulation bath includes 101 g / L sulfuric acid, 318 g / L sodium sulfate, 10.3 g / L zinc sulfate, 6.5 g / L acid bath additive (Berol Spin 653 from Berol Kemi, Sweden), and 4.4 g / L denaturant EBT. The solvent is deionized water, and the coagulation bath temperature is 47.3°C.

[0097] The post-treatment includes the following steps: first water washing, desulfurization, second water washing, pickling, third water washing, fourth water washing, oiling, vacuum drying, and opening treatment. After each bath treatment, the product is pressed, and before entering the vacuum drying step, a high-pressure rolling mill is used for pressing and dehydration.

[0098] The desulfurization bath uses Na2SO3 solution with a concentration of 8.6g / L and a desulfurization bath temperature of 79°C; The pickling bath uses a lactic acid solution with a concentration of 5.1 g / L, a pickling bath temperature of 49° C., and a weak acid is used for pickling.

[0099] The temperature of the first, second, third and fourth water washes is 70° C. After the fourth water wash is used up, the second water wash is added, and after the third water wash, the first water wash is added, thereby improving the recycling rate of water.

[0100] The squeezing pressure after each bath treatment is 0.12MPa; the high-pressure roller is used for squeezing and dehydration before entering the vacuum drying, and the pressure of the high-pressure roller is 0.38MPa. The moisture regain of the fiber after dehydration is 129%.

[0101] The vacuum drying adopts a vacuum decompression drying method, controls the vacuum degree to 0.05MP, and the vacuum drying temperature to 47°C, until the fiber moisture regain reaches 12.5%.

[0102] This embodiment also provides multifunctional health-care regenerated cellulose fiber prepared by the above method.

[0103] This embodiment also provides the use of the multifunctional health-care regenerated cellulose fiber in textile fabrics and / or non-woven fabrics.

[0104] Testing showed that the multifunctional health-care regenerated cellulose fiber prepared in this embodiment had an antibacterial rate of 90.2% against Staphylococcus aureus, an antibacterial rate of 89.0% against Escherichia coli, and an antibacterial rate of 91.1% against Candida albicans; the antiviral activity value against influenza A virus was 2.6, and the antiviral activity value against influenza B virus was 2.5; the ultraviolet protection factor (UPF) was 52, and the ultraviolet transmittance T (UVA) was 4.3%; the cellulose fiber contained red iron oxide, which has excellent skin protection and skin care effects.

[0105] Meanwhile, after the multifunctional health-care regenerated cellulose fiber prepared in this embodiment was washed 30 times according to the washing method in Appendix C 4. Simplified Washing Conditions and Procedures of Standard FZ / T 73023-2006, the antibacterial rates against Staphylococcus aureus, Escherichia coli, and Candida albicans were still up to 89.1%, 88.2%, and 90.3%, respectively. The antiviral activity values against influenza A virus and influenza B virus were still up to 2.6 and 2.5, respectively. The ultraviolet protection factor (UPF) was still up to 50, and the ultraviolet transmittance T (UVA) was still up to 4.35%.

[0106] Example 3 This embodiment provides a method for preparing multifunctional health-care regenerated cellulose fiber with a specification of 2.22 dtex×51 mm, and the specific steps are as follows: 1. Preparation of plant essential oil dispersion system 1) Preparation of oily blend powder containing plant essential oils The plant essential oil and molten n-alkane were stirred uniformly at 50° C. in a mass ratio of 2:1, at a stirring speed of 500 r / min, and for 1.5 hours to obtain a plant essential oil blend. The plant essential oil was lavender essential oil, and the n-alkane was a mixture of n-eicosane, n-heneicosane, and n-tricosane in a mass ratio of 1:2:3.

[0107] A low-thermal-conductivity porous silicate mineral powder is then added to the essential oil blend and ultrasonically treated at 30°C and 5.5 MHz for 20 minutes to obtain a powder containing the essential oil. The low-thermal-conductivity porous silicate mineral powder is kaolin, and the mass ratio of the low-thermal-conductivity porous silicate mineral powder to the essential oil blend is 1:2.

[0108] 2) Modification treatment A dispersant, a coupling agent, an oily blend powder containing plant essential oils, and deionized water were uniformly mixed and then ground and dispersed using a sand mill under vacuum and wet conditions. The mass fraction of the oily blend powder containing plant essential oils was 45%, and the grinding speed was 3500 r / min. Grinding and dispersion was stopped when the particle size of the dispersed system reached D90 = 1.516 μm, thereby obtaining a modified oily blend powder dispersion containing plant essential oils, i.e., a plant essential oil dispersion system. During the grinding process, jacket condensation was performed using deionized water as the jacket medium to prevent the temperature of the grinding dispersion system from rising, maintaining it at 25°C.

[0109] The dispersant is sodium methylenebisnaphthalene sulfonate; the coupling agent is silane coupling agent A-17, purchased from Nanjing Xiangqian Chemical Co., Ltd.; the dispersant, coupling agent, and oily blend powder containing plant essential oil are mixed in a mass ratio of 12:5:100; the vacuum degree of the grinding and dispersion is -0.092 MPa, and the grinding and dispersion is carried out under vacuum conditions to reduce the occurrence of bubbles during the grinding and dispersion process.

[0110] 2. Preparation of Iron Oxide Red Dispersion System A dispersant, defoamer, coupling agent, nano-iron oxide red, and deionized water were added to a dispersing sand mill and ground and dispersed at 3500 r / min to prepare a nano-iron oxide red aqueous dispersion. The mass fraction of the nano-iron oxide red powder was 25%, and the particle size D90 of the dispersion was 0.895 μm. The dispersant was sodium methylene bis-naphthalene sulfonate; the defoamer was polyoxypropylene polyoxyethylene glycerol ether; and the coupling agent was silane coupling agent A-171, purchased from Nanjing Xiangqian Chemical Co., Ltd. The mass ratio of the dispersant, defoamer, coupling agent, and iron oxide red was 15:5:5:100.

[0111] Gelatin (8.0% by mass) and gum arabic (8.0% by mass) were added to the nano-iron oxide red aqueous dispersion, stirred at 2200 r / min and 20°C to dissolve, and kept warm. The pH was adjusted to 6.5, and a complex coacervation reaction was carried out at the aforementioned temperature and stirring speed for 50 minutes. Transglutaminase, a curing agent, was then added, and the pH was adjusted to 9.5. A cross-linking reaction was carried out at the aforementioned temperature and stirring speed for 50 minutes. The stirring speed was then reduced to 900 r / min, and the reaction was continued for 2.0 hours to obtain a primary iron oxide red dispersion. A thickener was then added to a viscosity of 35 seconds (falling ball viscosity) to obtain an iron oxide red dispersion. The thickener was sodium carboxymethyl cellulose, added in an amount of 8% by mass of the nano-iron oxide red.

[0112] 3. Preparation of blended spinning solution A cellulose spinning dope was prepared using cellulose pulp as raw material through a viscose preparation process. Its specifications included: 9.25% cellulose α-cellulose, 4.85% sodium hydroxide, a ball-falling viscosity of 55 seconds at 20°C, and a degree of maturity (10% NH₄Cl value) of 20 mL. A denaturant, polyethylene glycol (molecular weight, 1500), was added at 1.2%, and a denaturant, EBT (Klein, Germany), was added at 1.0%. A plant essential oil dispersion and a red iron oxide dispersion were added to the regenerated cellulose fiber spinning dope using a pre-spinning injection device, with the plant essential oil accounting for 9.0% of the cellulose α-cellulose weight and the nano-red iron oxide accounting for 6.0% of the cellulose α-cellulose weight in the spinning dope, to produce a blended spinning dope.

[0113] The pre-spinning injection device includes a functional additive filter, a pre-spinning injection buffer tank, a metering device, a dynamic mixer, and a static mixer. The additive filter utilizes a plate-and-frame filter, made of one layer of polypropylene felt and two layers of silk cloth, with a pore size of 15-20 μm. This filtration prevents impurities introduced during the production process, improving the additive's usability and the fiber's spinnability. The pre-spinning injection buffer tank ensures better liquid level stability for the blended additive, preventing instability in the added additive content. The metering device utilizes a mechanical diaphragm pump (Q = 1500 L / h) with an outlet pressure of 0.9 MPa. The dynamic mixer and static mixer are used in series to improve the uniformity of the blended spinning solution.

[0114] 4. Spinning The blended spinning solution is filtered through a candle filter and then passed through a spinneret into a coagulation bath for spinning. The obtained nascent filament bundle is drawn to obtain a formed filament bundle, which is cut and post-processed to obtain multifunctional health-care regenerated cellulose fiber.

[0115] The candle filter is made of polypropylene and adopts an inside-out filtering method. The filtering material is two layers of silk cloth.

[0116] The coagulation bath includes 105 g / L sulfuric acid, 330 g / L sodium sulfate, 11.0 g / L zinc sulfate, 8 g / L acid bath additive (Berol Spin 653 from Berol Kemi, Sweden), 5 g / L denaturant EBT, the solvent is deionized water, and the coagulation bath temperature is 50°C.

[0117] The post-treatment includes the following steps: first water washing, desulfurization, second water washing, pickling, third water washing, fourth water washing, oiling, vacuum drying, and opening treatment. After each bath treatment, the product is pressed, and before entering the vacuum drying step, a high-pressure rolling mill is used for pressing and dehydration.

[0118] The desulfurization bath uses Na2SO3 solution with a concentration of 10.0 g / L and a desulfurization bath temperature of 70°C; The pickling bath uses an acetic acid solution with a concentration of 6 g / L, a pickling bath temperature of 45° C., and a weak acid is used for pickling.

[0119] The temperature of the first, second, third and fourth water washes is 75° C. After the fourth water wash is used up, the second water wash is added, and after the third water wash, the first water wash is added, thereby improving the recycling rate of water.

[0120] The squeezing pressure after each bath treatment is 0.15MPa; the fiber is squeezed and dehydrated by a high-pressure roller before entering the vacuum drying, and the pressure of the high-pressure roller is 0.4MPa. The moisture regain of the fiber after dehydration is 120%.

[0121] The vacuum drying adopts a vacuum decompression drying method, controls the vacuum degree to 0.09 MPa, and the vacuum drying temperature to 48° C., until the fiber moisture regain reaches 11.6%.

[0122] This embodiment also provides multifunctional health-care regenerated cellulose fiber prepared by the above method.

[0123] This embodiment also provides the use of the multifunctional health-care regenerated cellulose fiber in textile fabrics and / or non-woven fabrics.

[0124] Testing showed that the multifunctional health-care regenerated cellulose fiber prepared in this embodiment had an antibacterial rate of 91.8% against Staphylococcus aureus, 90.9% against Escherichia coli, and 92.5% against Candida albicans; its antiviral activity against influenza A virus was 2.7, and its antiviral activity against influenza B virus was 2.6; its ultraviolet protection factor (UPF) was 60, and its ultraviolet transmittance T (UVA) was 3.9%; and the cellulose fiber contained red iron oxide, which had excellent skin protection and skin care effects.

[0125] Meanwhile, after the multifunctional health-care regenerated cellulose fiber prepared in this embodiment was washed 30 times according to the washing method in Appendix C 4. Simplified Washing Conditions and Procedures of Standard FZ / T 73023-2006, the antibacterial rates against Staphylococcus aureus, Escherichia coli, and Candida albicans still reached 90.5%, 90.1%, and 91.3%, respectively; the antiviral activity values against influenza A virus and influenza B virus still reached 2.6, and the ultraviolet protection factor (UPF) still reached 59, and the ultraviolet transmittance T (UVA) still reached 4.0%.

[0126] Example 4 This embodiment provides a method for preparing a multifunctional health-care regenerated cellulose fiber, which specifically adopts the technical solution of Example 2, with the difference that the plant essential oil used is a mixture of cinnamon essential oil and clove essential oil in a mass ratio of 1:1.

[0127] This embodiment also provides multifunctional health-care regenerated cellulose fiber prepared by the above method.

[0128] This embodiment also provides the use of the multifunctional health-care regenerated cellulose fiber in textile fabrics and / or non-woven fabrics.

[0129] Testing showed that the multifunctional health-care regenerated cellulose fiber prepared in this embodiment had an antibacterial rate of 91.0% against Staphylococcus aureus, 89.5% against Escherichia coli, and 91.3% against Candida albicans; the antiviral activity value against influenza A virus was 2.6, and the antiviral activity value against influenza B virus was 2.6; the ultraviolet protection factor (UPF) was 53, and the ultraviolet transmittance T (UVA) was 4.4%; the cellulose fiber contained red iron oxide, which has excellent skin protection and skin care effects.

[0130] Meanwhile, after the multifunctional health-care regenerated cellulose fiber prepared in this embodiment was washed 30 times according to the washing method in Appendix C 4. Simplified Washing Conditions and Procedures of Standard FZ / T 73023-2006, the antibacterial rates against Staphylococcus aureus, Escherichia coli, and Candida albicans still reached 89.3%, 88.3%, and 90.5%, respectively; the antiviral activity values against influenza A virus and influenza B virus still reached 2.6 and 2.5, respectively; the ultraviolet protection factor (UPF) still reached 51, and the ultraviolet transmittance T (UVA) still reached 4.44%.

[0131] Example 5 This embodiment provides a method for preparing a multifunctional health-care regenerated cellulose fiber, which specifically adopts the technical solution of Example 2, with the difference that the plant essential oil used is a mixture of eucalyptus essential oil and oregano essential oil in a mass ratio of 2:3.

[0132] This embodiment also provides multifunctional health-care regenerated cellulose fiber prepared by the above method.

[0133] This embodiment also provides the use of the multifunctional health-care regenerated cellulose fiber in textile fabrics and / or non-woven fabrics.

[0134] Testing showed that the multifunctional health-care regenerated cellulose fiber prepared in this embodiment had an antibacterial rate of 91.2% against Staphylococcus aureus, an antibacterial rate of 89.3% against Escherichia coli, and an antibacterial rate of 91.0% against Candida albicans; the antiviral activity value against influenza A virus was 2.6, and the antiviral activity value against influenza B virus was 2.5; the ultraviolet protection factor (UPF) was 54, and the ultraviolet transmittance T (UVA) was 4.4%; the cellulose fiber contained red iron oxide, which has excellent skin protection and skin care effects.

[0135] Meanwhile, after the multifunctional health-care regenerated cellulose fiber prepared in this embodiment was washed 30 times according to the washing method in Appendix C 4. Simplified Washing Conditions and Procedures of Standard FZ / T 73023-2006, the antibacterial rates against Staphylococcus aureus, Escherichia coli, and Candida albicans still reached 89.3%, 88.3%, and 90.5%, respectively; the antiviral activity values against influenza A virus and influenza B virus still reached 2.6 and 2.5, respectively; the ultraviolet protection factor (UPF) still reached 52, and the ultraviolet transmittance T (UVA) still reached 4.46%.

[0136] Comparative Example 1 Comparative Example 1 adopts the preparation method of the multifunctional health-care regenerated cellulose fiber of Example 3, with the difference that the preparation of the red iron oxide dispersion system is omitted, and red iron oxide is directly added in the preparation of the blended spinning solution; the rest of the process is the same.

[0137] After testing, the regenerated cellulose fiber prepared in Comparative Example 1 had an antibacterial rate of 90.4% against Staphylococcus aureus, an antibacterial rate against Escherichia coli, and an antibacterial rate against Candida albicans of 90.8%; the antiviral activity value against influenza A virus was 2.6, and the antiviral activity value against influenza B virus was 2.5; the ultraviolet protection factor (UPF) was 33, and the ultraviolet transmittance T (UVA) was 7.2%.

[0138] Comparative Example 2 Comparative Example 2 adopts the preparation method of the multifunctional health-care regenerated cellulose fiber of Example 3, with the difference that the addition of the low thermal conductivity porous silicate mineral powder is omitted; the rest of the process is the same.

[0139] After testing, the regenerated cellulose fiber prepared in Comparative Example 2 had an antibacterial rate of 86.1% against Staphylococcus aureus, an antibacterial rate against Escherichia coli, and an antibacterial rate against Candida albicans of 86.5%; the antiviral activity value against influenza A virus was 2.1, and the antiviral activity value against influenza B virus was 2.1; the ultraviolet protection factor (UPF) was 51, and the ultraviolet transmittance T (UVA) was 4.32%.

[0140] Comparative Example 3 Comparative Example 3 adopts the preparation method of the multifunctional health-care regenerated cellulose fiber of Example 3, with the difference that the mixing of n-alkane and plant essential oil is omitted, and the plant essential oil is directly mixed with the low thermal conductivity porous silicate mineral powder and then modified. The rest of the process is the same.

[0141] After testing, the regenerated cellulose fiber prepared in Comparative Example 3 had an antibacterial rate of 86.7% against Staphylococcus aureus, an antibacterial rate against Escherichia coli, and an antibacterial rate against Candida albicans of 87.7%; the antiviral activity value against influenza A virus was 2.2, and the antiviral activity value against influenza B virus was 2.1; the ultraviolet protection factor (UPF) was 53, and the ultraviolet transmittance T (UVA) was 4.26%.

[0142] Unless otherwise specified, all percentages used in the present invention are by mass.

[0143] Finally, it should be noted that the above descriptions are merely preferred embodiments of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art will be able to modify the technical solutions described in the aforementioned embodiments or substitute equivalents for some of the technical features. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention shall be included within the scope of protection of the present invention.

Claims

1. A method for preparing a multifunctional health-care regenerated cellulose fiber, characterized in that: The method comprises the following steps: preparing a plant essential oil dispersion system, preparing a red iron oxide dispersion system, preparing a blended spinning solution, and spinning; The preparation of the plant essential oil dispersion system includes the following steps: preparation and modification of an oily blend powder containing the plant essential oil; The preparation of the oily blend powder containing plant essential oil comprises the following steps: uniformly mixing molten n-alkane and plant essential oil to obtain the plant essential oil oily blend; then mixing low thermal conductivity porous silicate mineral powder and the plant essential oil oily blend, and ultrasonically treating the mixture to obtain the plant essential oil oily blend powder; In the modification treatment, the dispersant, the coupling agent, the oily blend powder containing the plant essential oil and deionized water are ground and dispersed to obtain a plant essential oil dispersion system.

2. The method for preparing the multifunctional health-care regenerated cellulose fiber according to claim 1, characterized in that: The plant essential oil is at least one of the following: lavender essential oil, peppermint essential oil, coral essential oil, isatis root essential oil, thyme essential oil, melaleuca oil, cinnamon essential oil, clove essential oil, eucalyptus essential oil, tea tree essential oil, camellia seed oil, oregano essential oil; The n-alkane is a mixture of n-eicosane, n-heneicosane and n-tricosane; The low thermal conductivity porous silicate mineral powder is one of the following: mica powder, diatomaceous earth, kaolin, sepiolite, and zeolite.

3. The method for preparing the multifunctional health-care regenerated cellulose fiber according to claim 2, characterized in that: The mass ratio of the plant essential oil to the normal alkane is 1-2:1; The mass ratio of n-eicosane, n-heneicosane and n-tricosane is 1:1-2:2-3; The mass ratio of the low thermal conductivity porous silicate mineral powder to the plant essential oil oily blend is 1:1-2.

4. The method for preparing the multifunctional health-care regenerated cellulose fiber according to claim 1, characterized in that: In the modification treatment, the dispersant is one of the following: sodium dodecylbenzenesulfonate and sodium methylene bisnaphthalenesulfonate; the coupling agent is one of the following: silane coupling agent kh-570, silane coupling agent kh-560, coupling agent A-151, coupling agent A-171; The mass ratio of the dispersant, the coupling agent and the oily blend powder containing plant essential oil is 8-12:2-5:

100.

5. The method for preparing the multifunctional health-care regenerated cellulose fiber according to claim 1, characterized in that: The preparation of the iron oxide red dispersion system comprises the following steps: grinding and dispersing a dispersant, a defoaming agent, a coupling agent, nano iron oxide red, and deionized water to obtain a nano iron oxide red aqueous dispersion system; then adding gelatin and gum arabic to the nano iron oxide red aqueous dispersion system, dispersing the mixture evenly, adjusting the pH to acidic, and stirring for reaction; adding transglutaminase, adjusting the pH to alkaline, and stirring for reaction; and using a thickener to adjust the viscosity to 25-35s to obtain the iron oxide red dispersion system.

6. The method for preparing the multifunctional health-care regenerated cellulose fiber according to claim 5, characterized in that: In the preparation of the iron oxide red dispersion system, the dispersant is sodium dodecylbenzenesulfonate or sodium methylene bisnaphthalenesulfonate; the defoaming agent is polyoxypropylene glycerol ether or polyoxypropylene polyoxyethylene glycerol ether; the coupling agent is one of the following: silane coupling agent KH-570, silane coupling agent KH-560, coupling agent A-151, coupling agent A-171; The mass ratio of dispersant, defoaming agent, coupling agent and nano iron oxide red is 10-15:3-5:2-5:100; 7-8% by mass of gelatin and 7-8% by mass of gum arabic were added to the nano-iron oxide red aqueous dispersion system.

7. The method for preparing the multifunctional health-care regenerated cellulose fiber according to claim 1, characterized in that: The preparation of the blended spinning solution comprises uniformly mixing the plant essential oil dispersion system, the iron oxide red dispersion system and the spinning solution to obtain the blended spinning solution; The cellulose A content in the spinning solution is 8.90-9.25 wt%; The amount of the plant essential oil dispersion system added is 5-9% of the mass of cellulose alpha in the spinning solution; The added amount of the iron oxide red dispersion system is 3-6% of the mass of the type A cellulose in the spinning solution.

8. The method for preparing the multifunctional health-care regenerated cellulose fiber according to claim 1, characterized in that: The spinning comprises the steps of: using a blended spinning solution to be spun into a coagulation bath at 45-50°C for spinning; the obtained spun filaments are drawn to obtain a formed filament; and the formed filaments are post-treated to obtain multifunctional health-care regenerated cellulose fibers; The coagulation bath includes: 95-105 g / L of sulfuric acid, 310-330 g / L of sodium sulfate, 9.5-11.0 g / L of zinc sulfate, 5-8 g / L of acid bath auxiliary agent, 3-5 g / L of denaturant EBT, and the solvent is deionized water.

9. A multifunctional health-care regenerated cellulose fiber, characterized in that: The method is prepared according to any one of claims 1 to 8.

10. An application of the multifunctional health-care regenerated cellulose fiber according to claim 9, characterized in that: Application of the multifunctional health-care regenerated cellulose fiber in textile fabrics and / or non-woven fabrics.