Viscose large biological fiber with anti-allergy function and preparation method thereof

Abstract

The invention provides a viscose large biological fiber with an anti-allergy function and a preparation method thereof, and belongs to the field of viscose fibers. The preparation method of the viscose large biological fiber with the anti-allergy function comprises the following steps: preparing a molecular nest, preparing modified gel, coating and forming, preparing a spinning solution, and spinning and forming. According to the preparation method of the viscose large biological fiber with the anti-allergy function, the problem that the activity and the stability of adopted plant active ingredients are reduced due to the fact that the adopted plant active ingredients are affected by process environments, solvent ingredients and the like can be solved; meanwhile, the release characteristic of the plant active ingredients in the viscose fibers can be regulated and controlled according to needs, so that the plant active ingredients are released in a large dose within a short time or slowly released in a small dose within a long time, and then emergent repair or long-acting allergy relief of skin allergy areas is achieved.

Description

Technical Field

[0001] The present invention relates to the field of viscose fibers, in particular to a viscose large biological fiber with a soothing function and a preparation method thereof. Background Art

[0002] Viscose fiber is made from natural fibers. It undergoes alkalization, aging, and sulfonation to produce soluble cellulose xanthate, which is then dissolved in a dilute alkali solution to produce viscose liquid. Finally, it is produced by wet spinning. Viscose fiber is widely used in various textiles and apparel due to its excellent moisture absorption and breathability, high wearing comfort, ease of dyeing, low static charge, and excellent spinnability. As people's living standards improve, viscose is constantly being upgraded. However, due to factors such as its inherent properties and the simple preparation process, the performance of traditional viscose fiber is increasingly unable to meet the actual needs of consumers. Consumers demand more than just basic moisture absorption and breathability from viscose fiber; they also demand diversified and functionalized viscose fibers, such as antibacterial, antifouling, antioxidant, and UV protection. Functional viscose fiber has become the main development direction in recent years. Its functional improvement usually involves adding corresponding functional plant ingredients (such as functional particles and microcapsules containing plant active ingredients) during the preparation process of viscose fiber; or after the viscose fiber is prepared, it is further given different functions through post-treatment processes (such as spraying, soaking, etc.).

[0003] In the traditional viscose fiber preparation process, when plant active ingredients are used in the preparation of viscose fibers, the plant active ingredients are easily affected by the process environment, solvent components, etc. of viscose fiber preparation, thereby reducing their activity and stability, resulting in poor binding performance between the plant active ingredients and the viscose fibers. Not only can the stable functional modification of the viscose fibers not be achieved, but the physical properties of the viscose fibers will also be affected.

[0004] Furthermore, environmental factors such as ultraviolet rays, haze, dust and dry wind act on exposed skin for a long time, which can cause the skin to have allergic symptoms such as imbalance, dryness, itching, redness and swelling. It is of great significance and research value to provide a viscose biofiber with a soothing function. In the prior art, there are fewer fibers disclosed for having a soothing function. For example, Chinese patent CN117265684B discloses a preparation method and application of gentian viscose fibers with soothing effects. After the spinning solution is prepared using gentian extract and viscose stock solution, oat-β glucan, lignin and organic quaternary ammonium salt, the spinning solution is formed by coagulation bath spinning, drawing, washing and drying to obtain viscose fibers. However, on the one hand, in the preparation process of its viscose fibers, gentian extract is easily affected by the viscose stock solution solvent environment, coagulation bath solvent environment, process conditions and the like, which limits its modification effect on viscose fibers. On the other hand, when the skin is acutely allergic and needs emergency repair, the viscose fiber cannot release a large dose of plant active ingredients in a short period of time to achieve the purpose of emergency repair; when the skin allergy area needs continuous and long-lasting soothing, it cannot stably release plant active ingredients over a long period of time to achieve the purpose of long-lasting soothing; the soothing functionality of viscose fiber needs to be further improved. Summary of the Invention

[0005] In order to solve the technical problems existing in the prior art, the present invention provides a viscose large biofiber with soothing function and a preparation method thereof, which can avoid the problem that the activity and stability of the plant active ingredients used are reduced by the process environment, solvent components, etc.; at the same time, it can regulate the release characteristics of the plant active ingredients in the viscose fiber as needed, so as to realize the plant active ingredients in a short time, a large dose release or a long time, a small dose sustained release, thereby achieving emergency repair or long-term soothing of skin allergy areas.

[0006] In order to solve the above technical problems, the technical solutions adopted by the present invention are as follows: A method for preparing a viscose biofiber with a soothing function, comprising the following steps: preparing molecular nests, preparing modified gels, coating and molding, preparing spinning solution, and spinning and molding; The molecular nest is prepared by uniformly mixing mesoporous silica, 3-aminopropyltriethoxysilane, and an ethanol aqueous solution, stirring at 45-50° C., and then cooling to obtain a carrier dispersion; adding green tea extract, coral extract, and ginkgo leaf extract into deionized water and uniformly dispersing them to obtain an active ingredient solution; mixing the carrier dispersion and the active ingredient solution, stirring at room temperature, separating to obtain a solid, and drying to obtain the molecular nest; The modified gel is prepared by using N-vinylcaprolactam, N-hydroxyethyl acrylamide, acrylic acid, N,N-methylenebisacrylamide, sodium lauryl sulfate, and sodium bicarbonate as reaction raw materials in a solvent environment under the protection of an inert gas, and reacting at 68-70° C. in the presence of an initiator. The obtained reactant is dialyzed and dried to obtain the modified gel. The coating molding adopts modified gel to coat the molecular nest to obtain composite temperature-sensitive coated particles; The spinning solution is prepared by uniformly mixing the composite temperature-sensitive coated particles with the spinning solution to obtain a blended spinning solution; The blended spinning solution is spun into a fiber to produce a viscose biofiber with a soothing function.

[0007] Preferably, in the preparation of the molecular nest, the weight ratio of mesoporous silica, 3-aminopropyltriethoxysilane, and ethanol aqueous solution in the carrier dispersion is 10-12:1.5-1.9:70-75; The weight ratio of green tea extract, sarcandra glabra extract, ginkgo leaf extract and deionized water in the active ingredient liquid is 7-7.5:4.2-4.7:2-2.2:120-130; the particle size of the green tea extract is 80-100 mesh, and the extraction ratio is 10-20:1; the particle size of the sarcandra glabra extract is 80-100 mesh, and the extraction ratio is 10-20:1; the particle size of the ginkgo leaf extract is 80-100 mesh, and the extraction ratio is 10-20:1.

[0008] The weight ratio of the carrier dispersion liquid to the active ingredient liquid is 2.1-2.3:1.

[0009] Furthermore, the modified gel is prepared by adding N-vinylcaprolactam, N-hydroxyethylacrylamide, acrylic acid, N,N-methylenebisacrylamide, sodium lauryl sulfate, and sodium bicarbonate into deionized water, mixing them uniformly under the protection of inert gas, stirring, and heating to 68-70° C., adding a potassium persulfate aqueous solution, keeping the temperature for reaction for 5-7 hours, cooling, and obtaining a reactant; the reactant is dialyzed for 4-5 days through a dialysis bag with a molecular weight cutoff of 12-14 KDa, and then dried to obtain a modified gel.

[0010] Preferably, in the preparation of the modified gel, the weight ratio of N-vinylcaprolactam, N-hydroxyethyl acrylamide, acrylic acid, N,N-methylenebisacrylamide, sodium lauryl sulfate, sodium bicarbonate, and deionized water is 5-5.1:1.05-1.15:0.28-0.31:0.06-0.07:0.08-0.09:0.12-0.16:380-400; The concentration of the potassium persulfate aqueous solution is 1.2-1.3 wt %, and the volume ratio of the potassium persulfate aqueous solution to deionized water is 1:50-55.

[0011] Furthermore, the coating molding is performed by adding the modified gel into deionized water at 5-8°C and dispersing it evenly, then adding the molecular nest and stirring and heating it to 24-26°C at a heating rate of 0.2-0.3°C / min; then stirring and heating it to 37-38°C at a heating rate of 0.5-0.6°C / min. After keeping warm and stirring, the solid matter is separated and the solid matter is washed and dried to obtain composite temperature-sensitive coated particles.

[0012] Preferably, in the overmolding, the weight ratio of the modified gel to deionized water is 1:35-40; The weight ratio of the modified gel to the molecular nest is 4.5-5:1.

[0013] Furthermore, the spinning solution is prepared by adding the composite temperature-sensitive coated particles into deionized water at a temperature of 37-38° C. and dispersing them evenly to obtain a functionally modified solution; then the functionally modified solution, spinning solution, sodium carboxymethyl cellulose, 3-aminopropyltriethoxysilane, and sodium alginate are evenly mixed, and the mixture is filtered, degassed, and aged to obtain a blended spinning solution; The spinning molding comprises spraying the blended spinning solution into a coagulation bath at 42-43° C., and spinning molding to obtain primary fibers; the primary fibers are desulfurized, washed, oiled, and dried to obtain viscose large bio-fibers with soothing functions.

[0014] Preferably, in the preparation of the spinning solution, the weight ratio of the composite temperature-sensitive coated particles to deionized water in the functional modification solution is 1:14-15; The weight ratio of the functional modification solution, spinning solution, sodium carboxymethyl cellulose, 3-aminopropyltriethoxysilane, and sodium alginate is 10-11:88-92:0.3-0.4:0.9-1.1:0.4-0.5; The methyl cellulose content of the spinning solution is 9.1-9.3%, the total alkali content is 2.8-3.2%, and the viscosity is 35-40s.

[0015] Preferably, in the spinning process, the spinning speed is controlled to be 19-20 m / min, the spinning nozzle draft ratio is 4-6%, the inter-disk draft ratio is 11-13%, the three-bath draft ratio is 31-33%, the four-bath draft ratio is 10-12%, and the immersion length is 900-950 mm; The contents of the components in the coagulation bath are: 90-100 g / L of sulfuric acid, 180-210 g / L of sodium sulfate, 20-25 g / L of zinc sulfate, and 10-12 g / L of calcium chloride.

[0016] A viscose biofiber with a soothing function is prepared by adopting the above-mentioned preparation method.

[0017] Compared with the prior art, the present invention has the following beneficial effects: (1) The preparation method of the viscose biofiber with soothing function of the present invention comprises the following steps: in the preparation of molecular nests, 3-aminopropyltriethoxysilane is used to treat mesoporous silica to introduce amino groups to prepare a carrier dispersion; green tea extract, coral extract, and ginkgo leaf extract are dispersed in deionized water to prepare an active ingredient liquid; and the two are then mixed and loaded to prepare mesoporous silica loaded with plant active ingredients (i.e., molecular nests). In the preparation of modified gel, N-vinyl caprolactam NVCL is used as the main thermosensitive raw material in the presence of an initiator and a cross-linking agent, and is copolymerized with N-hydroxyethyl acrylamide HEAA and acrylic acid AAC to specifically adjust the lower critical solution temperature LCST of the thermosensitive gel to match the temperature range of the allergic skin area, thereby improving its subsequent coating performance for the molecular nests, and introducing carboxyl groups to further improve the binding performance of the modified gel with the molecular nests and the plant active ingredients loaded thereon. In the coating molding step, the modified gel molecular chains are first fully stretched in a low-temperature deionized water environment at 5-8°C before being placed into molecular nests. While slowly heating, the modified gel is uniformly coated on the outer surface of the molecular nests. The temperature is then further raised to a temperature exceeding the lower critical solution temperature (LCST) of the modified gel, causing the modified gel to shrink on the outer surface of the molecular nests, completing the coating molding process and producing composite thermosensitive coated particles. Then, in the spinning solution preparation step, a functional modified solution is prepared using the composite thermosensitive coated particles. This is then mixed with the spinning solution and its auxiliary materials to form a blended spinning solution. This blended spinning solution is then spun to produce a viscose biofiber with soothing properties. The aforementioned technical approaches work synergistically to prevent the activity and stability of the plant active ingredients from being affected by the process environment, solvent composition, and other factors. Furthermore, the release characteristics of the plant active ingredients within the viscose fiber can be adjusted as needed, enabling either a short, high-dose release or a long-term, low-dose, sustained release of the plant active ingredients, thereby achieving either immediate repair of allergic areas or long-term soothing.

[0018] (2) The viscose biofiber with soothing function of the present invention has a 2-hour release rate of catechins of 42.0-42.6%, a 2-hour release rate of rosmarinic acid of 37.4-38.2%, and a 2-hour release rate of ginkgolides of 29.8-30.1% at a temperature of 22°C; a 48-hour release rate of catechins of 82.7-83.2%, a 48-hour release rate of rosmarinic acid of 75.3-75.7%, and a 48-hour release rate of ginkgolides of 60.4-60.6%. The release rate of active ingredients in the fiber can be regulated by temperature, so as to achieve a large-dose release of plant active ingredients in a short time, thereby achieving an emergency repair function.

[0019] (3) The viscose biofiber with soothing function of the present invention has a 2-hour release rate of catechins of 5.8-6.1%, a 2-hour release rate of rosmarinic acid of 4.9-5.2%, and a 2-hour release rate of ginkgo lactones of 3.2-3.4% at a temperature of 36°C; a 48-hour release rate of catechins of 27.4-27.8%, a 48-hour release rate of rosmarinic acid of 23.7-24.0%, and a 48-hour release rate of ginkgo lactones of 17.9-18.1%. The release rate of the active ingredients in the fiber can be regulated by temperature, thereby achieving long-term stable controlled release of the plant active ingredients and thus achieving a long-term soothing function.

[0020] (4) The viscose biofiber with soothing function of the present invention has an antibacterial rate of 99.1-99.2% against Staphylococcus aureus, 97.5-98.0% against Escherichia coli, and 96.0-96.7% against Candida albicans; the DPPH free radical scavenging rate is 88.9-89.3%; ABTS + The free radical scavenging rate is 87.0-87.5%, and the cytotoxicity level in the in vitro cytotoxicity test is level 0.

[0021] (5) The viscose biofiber with soothing function of the present invention has a dry breaking strength of 2.99-3.07 cN / dtex, a wet breaking strength of 1.70-1.73 cN / dtex, a whiteness of 54.2-54.6%, and a defect point of 1.7-1.9 mg / 100 g. DETAILED DESCRIPTION

[0022] 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.

[0023] 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.

[0024] The embodiment of the present invention provides a method for preparing a viscose biofiber with a soothing function, which comprises the following steps: preparing molecular nests, preparing modified gels, coating and molding, preparing spinning solution, and spinning and molding.

[0025] The method for preparing the molecular nest comprises the following steps: adding mesoporous silica and 3-aminopropyltriethoxysilane to an ethanol aqueous solution with a volume concentration of 60-65%, ultrasonically dispersing for 20-30 minutes, heating to 45-50° C., stirring at this temperature for 2-3 hours, and cooling to room temperature to prepare a carrier dispersion liquid; adding green tea extract, coral extract, and ginkgo biloba extract to deionized water, stirring for 20-30 minutes, and preparing an active ingredient liquid; mixing the carrier dispersion liquid and the active ingredient liquid at a weight ratio of 2.1-2.3:1, stirring at room temperature for 4-6 hours, and centrifuging to obtain a solid; and transferring the solid to a vacuum drying oven, drying at 70-75° C. in a vacuum environment of 0.07-0.09 MPa to constant weight to prepare the molecular nest (i.e., mesoporous silica loaded with plant active ingredients), which is then set aside for use.

[0026] In the preparation of the molecular nest, in the carrier dispersion, the weight ratio of mesoporous silica, 3-aminopropyltriethoxysilane, and ethanol aqueous solution is 10-12:1.5-1.9:70-75.

[0027] In the active ingredient liquid, the weight ratio of green tea extract, coral reef extract, ginkgo leaf extract and deionized water is 7-7.5:4.2-4.7:2-2.2:120-130.

[0028] Among them, the preparation method of green tea extract is to use green tea as raw material, mix it with 10-12 times the extraction solvent (ethanol aqueous solution with a volume concentration of 60-65%), and then reflux extract at 70-75°C in a nitrogen and light-proof environment for 1-1.5 hours to obtain an extract; repeat the extraction 2-3 times, combine the multiple extracts and filter them, and then spray dry them to obtain the extract; or you can purchase green tea extract with an extraction ratio of 10-20:1 and a particle size of 80-100 mesh through conventional commercial channels.

[0029] The preparation method of the Sarcandra glabra extract is to use Sarcandra glabra as a raw material, mix it with 10-12 times the amount of an extraction solvent (an ethanol aqueous solution with a volume concentration of 60-65%), add 0.1wt% of citric acid, and extract under reflux at 60-65°C for 1-1.5 hours in a nitrogen atmosphere and in a dark environment to obtain an extract; repeat the extraction 2-3 times, combine the multiple extracts, filter, and then spray-dry to obtain the extract; or the Sarcandra glabra extract with an extraction ratio of 10-20:1 and a particle size of 80-100 mesh can be purchased through conventional commercial channels.

[0030] Ginkgo biloba extract is prepared by mixing ginkgo biloba with 10-12 times the volume of an extraction solvent (a 60-65% by volume acetone aqueous solution), and then extracting under reflux at 50-55°C for 1.5-2 hours in a nitrogen atmosphere and in a dark environment to obtain an extract. The extraction is repeated 2-3 times, and the multiple extracts are combined and filtered, and then spray-dried to obtain the extract. Alternatively, ginkgo biloba extract with an extraction ratio of 10-20:1 and a particle size of 80-100 mesh can be purchased through conventional commercial channels.

[0031] The method for preparing the modified gel comprises the following steps: adding N-vinyl caprolactam NVCL, N-hydroxyethyl acrylamide HEAA, acrylic acid AAC, N,N-methylenebisacrylamide MBA, sodium lauryl sulfate SDS, and sodium bicarbonate into a reactor containing deionized water; completely replacing the air in the reactor with nitrogen; stirring the mixture for 15-30 minutes while continuously introducing nitrogen to provide an atmosphere protection; then heating the mixture to 68-70°C at a heating rate of 0.5-0.8°C / min under stirring, maintaining the temperature and stirring for 30-40 minutes, and then adding a 1.2-1.3 wt% aqueous solution of potassium persulfate, maintaining the temperature and reacting for 5-7 hours, and cooling the mixture to room temperature to obtain a reactant; transferring the reactant into a dialysis bag with a molecular weight cutoff of 12-14 kDa, dialyzing the mixture for 4-5 days (changing the water every 8 hours), and freeze-drying the mixture after the dialysis is completed to obtain the modified gel for standby use.

[0032] In the preparation of the modified gel, the weight ratio of N-vinyl caprolactam NVCL, N-hydroxyethyl acrylamide HEAA, acrylic acid AAC, N,N-methylenebisacrylamide MBA, sodium lauryl sulfate SDS, sodium bicarbonate, and deionized water is 5-5.1:1.05-1.15:0.28-0.31:0.06-0.07:0.08-0.09:0.12-0.16:380-400; The volume ratio of the potassium persulfate aqueous solution to deionized water is 1:50-55.

[0033] The coating molding method comprises the following steps: introducing a predetermined amount of deionized water into a reactor, cooling the mixture to 5-8°C, and keeping the mixture warm; then adding the modified gel, stirring the mixture at 100-150 rpm for 40-50 minutes, adding the molecular nest, stirring the mixture and heating the mixture to 24-26°C at a heating rate of 0.2-0.3°C / min; then stirring the mixture and heating the mixture to 37-38°C at a heating rate of 0.5-0.6°C / min, keeping the mixture warm and stirring for 30-40 minutes, separating the solid matter, washing the solid matter with deionized water at a temperature of 37-38°C, and freeze-drying the solid matter to obtain the composite temperature-sensitive coated particles for later use.

[0034] In the overmolding process, the weight ratio of the modified gel to deionized water is 1:35-40; The weight ratio of the modified gel to the molecular nest is 4.5-5:1.

[0035] The method for preparing the spinning solution comprises the following steps: adding the composite temperature-sensitive coated particles into deionized water at a temperature of 37-38° C., stirring for 10-15 minutes, and obtaining a functionally modified solution; then uniformly mixing the functionally modified solution, spinning solution, sodium carboxymethyl cellulose, 3-aminopropyltriethoxysilane, and sodium alginate, filtering, degassing, and aging to obtain a blended spinning solution.

[0036] In the preparation of the spinning solution, the weight ratio of the composite temperature-sensitive coated particles to deionized water in the functional modification solution is 1:14-15; The weight ratio of the functional modification solution, spinning solution, sodium carboxymethyl cellulose, 3-aminopropyltriethoxysilane, and sodium alginate is 10-11:88-92:0.3-0.4:0.9-1.1:0.4-0.5; The methyl cellulose content of the spinning solution is 9.1-9.3%, the total alkali content is 2.8-3.2%, and the viscosity is 35-40s.

[0037] The spinning forming method comprises the following steps: introducing the blended spinning solution into a spinning machine, spraying the solution into a coagulation bath at 42-43° C., controlling the spinning speed to 19-20 m / min, setting the spinning nozzle draft ratio to 4-6%, the inter-disk draft ratio to 11-13%, the three-bath draft ratio to 31-33%, the four-bath draft ratio to 10-12%, and the immersion length to 900-950 mm; after spinning forming, primary fibers are obtained; and the primary fibers are desulfurized, washed, oiled, and dried to obtain viscose macro-biofibers with a soothing function.

[0038] In the spinning process, the contents of the components in the coagulation bath are: 90-100 g / L of sulfuric acid, 180-210 g / L of sodium sulfate, 20-25 g / L of zinc sulfate, and 10-12 g / L of calcium chloride.

[0039] The embodiment of the present invention also provides a viscose biofiber with a soothing function produced by the above method.

[0040] The present invention will be further described below with reference to some specific embodiments.

[0041] Example 1 This embodiment provides a method for preparing a viscose biofiber with a soothing function, specifically: 1. Preparation of molecular nests Mesoporous silica and 3-aminopropyltriethoxysilane were added to an ethanol aqueous solution with a volume concentration of 60%, ultrasonically dispersed for 20 minutes, heated to 45°C, stirred for 2 hours, and then cooled to room temperature to prepare a carrier dispersion liquid; green tea extract, coral extract, and ginkgo leaf extract were added to deionized water and stirred for 20 minutes to prepare an active ingredient liquid; the carrier dispersion liquid and the active ingredient liquid were mixed in a weight ratio of 2.1:1, stirred at room temperature for 4 hours, and centrifuged to obtain a solid; the solid was transferred to a vacuum drying oven and dried at 75°C to constant weight in a vacuum environment of 0.07 MPa to prepare a molecular nest (i.e., mesoporous silica loaded with plant active ingredients) for standby use.

[0042] Wherein, in the carrier dispersion, the weight ratio of mesoporous silica, 3-aminopropyltriethoxysilane and ethanol aqueous solution is 10:1.5:70.

[0043] In the active ingredient liquid, the weight ratio of green tea extract, sarcandra extract, ginkgo leaf extract, and deionized water is 7:4.2:2:120; the particle size of the green tea extract used in this embodiment is 100 mesh, and the extraction ratio is 20:1; the particle size of the sarcandra extract is 100 mesh, and the extraction ratio is 20:1; the particle size of the ginkgo leaf extract is 100 mesh, and the extraction ratio is 20:1.

[0044] 2. Preparation of modified gel N-vinyl caprolactam NVCL, N-hydroxyethyl acrylamide HEAA, acrylic acid AAC, N,N-methylenebisacrylamide MBA, sodium dodecyl sulfate SDS, and sodium bicarbonate were added to a reactor filled with deionized water. The air in the reactor was completely replaced with nitrogen. The mixture was stirred for 15 minutes while continuously flowing nitrogen to provide a protective atmosphere. The mixture was then heated to 68°C at a heating rate of 0.5°C / min under stirring, kept warm and stirred for 30 minutes, and then a 1.2 wt% aqueous solution of potassium persulfate was added. The mixture was kept warm for 5 hours and then cooled to room temperature to obtain a reactant. The reactant was transferred to a dialysis bag with a molecular weight cutoff of 12-14 kDa and dialyzed for 4 days (the water was changed every 8 hours). After dialysis, the mixture was freeze-dried to obtain a modified gel for later use. The modified gel prepared in this example had a lower critical solution temperature (LCST) of 34.1°C.

[0045] Among them, the weight ratio of N-vinylcaprolactam NVCL, N-hydroxyethylacrylamide HEAA, acrylic acid AAC, N,N-methylenebisacrylamide MBA, sodium lauryl sulfate SDS, sodium bicarbonate and deionized water is 5:1.05:0.28:0.06:0.08:0.12:380.

[0046] The volume ratio of the potassium persulfate aqueous solution to deionized water is 1:50.

[0047] 3. Overmolding A predetermined amount of deionized water was introduced into the reactor, cooled to 5°C, and kept warm; then the modified gel was added, stirred at 100 rpm for 40 minutes, and then the molecular nest was added, and the temperature was raised to 24°C at a heating rate of 0.2°C / min; then the temperature was raised to 37°C at a heating rate of 0.5°C / min, and kept warm and stirred for 30 minutes, and the solid was separated. The solid was washed with deionized water at 37°C and freeze-dried to obtain composite temperature-sensitive coated particles for later use.

[0048] The weight ratio of the modified gel to deionized water is 1:35.

[0049] The weight ratio of modified gel to molecular nest is 4.5:1.

[0050] 4. Preparation of spinning solution The composite thermosensitive coated particles were put into deionized water at a temperature of 37°C and stirred for 10 minutes to obtain a functional modified liquid; then the functional modified liquid, spinning solution, sodium carboxymethyl cellulose, 3-aminopropyltriethoxysilane, and sodium alginate were evenly mixed, filtered, degassed, and aged to obtain a blended spinning solution.

[0051] Among them, the weight ratio of the composite thermosensitive coated particles to deionized water in the functional modification liquid is 1:14.

[0052] The weight ratio of the functional modification liquid, the spinning solution, sodium carboxymethyl cellulose, 3-aminopropyltriethoxysilane and sodium alginate is 10:88:0.3:0.9:0.4.

[0053] The methyl cellulose content of the spinning solution is 9.2%, the total alkali content is 2.9%, and the viscosity is 37s.

[0054] 5. Spinning The blended spinning solution is introduced into the spinning machine and sprayed into a coagulation bath at 42°C. The spinning speed is controlled at 19m / min, the spinning nozzle draft ratio is 4%, the inter-disk draft ratio is 11%, the three-bath draft ratio is 31%, the four-bath draft ratio is 10%, and the immersion length is 900mm. After spinning and forming, primary fibers are obtained. The primary fibers are desulfurized, washed, oiled, and dried to obtain viscose large bio-fibers with soothing functions.

[0055] The contents of the components in the coagulation bath are as follows: 92 g / L sulfuric acid, 195 g / L sodium sulfate, 23 g / L zinc sulfate, and 10 g / L calcium chloride.

[0056] This embodiment also provides a viscose biofiber with a soothing function produced by the aforementioned method.

[0057] Example 2 This embodiment provides a method for preparing a viscose biofiber with a soothing function, specifically: 1. Preparation of molecular nests Mesoporous silica and 3-aminopropyltriethoxysilane were added to an ethanol aqueous solution with a volume concentration of 62%, ultrasonically dispersed for 25 minutes, heated to 48°C, stirred for 2.5 hours, and then cooled to room temperature to prepare a carrier dispersion; green tea extract, coral extract, and ginkgo leaf extract were added to deionized water and stirred for 25 minutes to prepare an active ingredient liquid; the carrier dispersion and the active ingredient liquid were mixed in a weight ratio of 2.2:1, stirred at room temperature for 5 hours, and centrifuged to obtain a solid; the solid was transferred to a vacuum drying oven and dried at 72°C to constant weight in a vacuum environment of 0.08 MPa to prepare a molecular nest (i.e., mesoporous silica loaded with plant active ingredients) for standby use.

[0058] Wherein, in the carrier dispersion, the weight ratio of mesoporous silica, 3-aminopropyltriethoxysilane and ethanol aqueous solution is 11:1.7:73.

[0059] In the active ingredient liquid, the weight ratio of green tea extract, sarcandra extract, ginkgo leaf extract, and deionized water is 7.3:4.5:2.1:125; the particle size of the green tea extract used in this embodiment is 100 mesh, and the extraction ratio is 20:1; the particle size of the sarcandra extract is 100 mesh, and the extraction ratio is 20:1; the particle size of the ginkgo leaf extract is 100 mesh, and the extraction ratio is 20:1.

[0060] 2. Preparation of modified gel N-vinyl caprolactam NVCL, N-hydroxyethyl acrylamide HEAA, acrylic acid AAC, N,N-methylenebisacrylamide MBA, sodium dodecyl sulfate SDS, and sodium bicarbonate were added to a reactor filled with deionized water. The air in the reactor was completely replaced with nitrogen. The mixture was stirred for 20 minutes while continuously purging nitrogen to provide a protective atmosphere. The mixture was then heated to 70°C at a heating rate of 0.6°C / min under stirring, kept stirring for 35 minutes, and then a 1.3 wt% aqueous solution of potassium persulfate was added. The mixture was kept warm for 6 hours and then cooled to room temperature to obtain a reactant. The reactant was transferred to a dialysis bag with a molecular weight cutoff of 12-14 kDa and dialyzed for 4.5 days (the water was changed every 8 hours). After dialysis, the mixture was freeze-dried to obtain a modified gel for later use. The modified gel prepared in this example had a lower critical solution temperature (LCST) of 34.3°C.

[0061] Among them, the weight ratio of N-vinylcaprolactam NVCL, N-hydroxyethylacrylamide HEAA, acrylic acid AAC, N,N-methylenebisacrylamide MBA, sodium lauryl sulfate SDS, sodium bicarbonate and deionized water is 5.1:1.1:0.3:0.065:0.085:0.14:390.

[0062] The volume ratio of the potassium persulfate aqueous solution to deionized water is 1:53.

[0063] 3. Overmolding A predetermined amount of deionized water was introduced into the reactor, cooled to 6°C, and kept warm; then the modified gel was added, stirred at 120 rpm for 45 minutes, and then the molecular nest was added, and the temperature was raised to 25°C at a heating rate of 0.2°C / min; then the temperature was raised to 38°C at a heating rate of 0.5°C / min, and kept warm and stirred for 35 minutes, and then the solid was separated. The solid was washed with deionized water at 38°C and freeze-dried to obtain composite temperature-sensitive coated particles for later use.

[0064] The weight ratio of the modified gel to deionized water is 1:37.

[0065] The weight ratio of modified gel to molecular nest is 4.8:1.

[0066] 4. Preparation of spinning solution The composite thermosensitive coated particles were put into deionized water at a temperature of 38°C and stirred for 12 minutes to obtain a functional modified liquid; then the functional modified liquid, spinning solution, sodium carboxymethyl cellulose, 3-aminopropyltriethoxysilane, and sodium alginate were evenly mixed, filtered, degassed, and aged to obtain a blended spinning solution.

[0067] Among them, the weight ratio of the composite thermosensitive coated particles to deionized water in the functional modification liquid is 1:14.5.

[0068] The weight ratio of the functional modification solution, the spinning solution, sodium carboxymethyl cellulose, 3-aminopropyltriethoxysilane and sodium alginate is 10.6:90:0.35:1:0.45.

[0069] The methyl cellulose content of the spinning solution is 9.2%, the total alkali content is 2.9%, and the viscosity is 37s.

[0070] 5. Spinning The blended spinning solution is introduced into the spinning machine and sprayed into a coagulation bath at 42°C. The spinning speed is controlled at 20m / min, the spinning nozzle draft ratio is 5%, the inter-disk draft ratio is 12%, the three-bath draft ratio is 32%, the four-bath draft ratio is 11%, and the immersion length is 950mm. After spinning and forming, primary fibers are obtained. The primary fibers are desulfurized, washed, oiled, and dried to obtain viscose large bio-fibers with soothing functions.

[0071] The contents of the components in the coagulation bath are as follows: 92 g / L sulfuric acid, 195 g / L sodium sulfate, 23 g / L zinc sulfate, and 10 g / L calcium chloride.

[0072] This embodiment also provides a viscose biofiber with a soothing function produced by the aforementioned method.

[0073] Example 3 This embodiment provides a method for preparing a viscose biofiber with a soothing function, specifically: 1. Preparation of molecular nests Mesoporous silica and 3-aminopropyltriethoxysilane were added to an ethanol aqueous solution with a volume concentration of 65%, ultrasonically dispersed for 30 minutes, heated to 50°C, stirred for 3 hours, and then cooled to room temperature to prepare a carrier dispersion liquid; green tea extract, coral extract, and ginkgo leaf extract were added to deionized water and stirred for 30 minutes to prepare an active ingredient liquid; the carrier dispersion liquid and the active ingredient liquid were mixed in a weight ratio of 2.3:1, stirred at room temperature for 6 hours, and centrifuged to obtain a solid; the solid was transferred to a vacuum drying oven and dried at 70°C to constant weight in a vacuum environment of 0.09 MPa to prepare a molecular nest (i.e., mesoporous silica loaded with plant active ingredients) for standby use.

[0074] In the carrier dispersion, the weight ratio of mesoporous silica, 3-aminopropyltriethoxysilane and ethanol aqueous solution is 12:1.9:75.

[0075] In the active ingredient liquid, the weight ratio of green tea extract, sarcandra extract, ginkgo leaf extract, and deionized water is 7.5:4.7:2.2:130; the particle size of the green tea extract used in this embodiment is 100 mesh, and the extraction ratio is 20:1; the particle size of the sarcandra extract is 100 mesh, and the extraction ratio is 20:1; the particle size of the ginkgo leaf extract is 100 mesh, and the extraction ratio is 20:1.

[0076] 2. Preparation of modified gel N-vinyl caprolactam NVCL, N-hydroxyethyl acrylamide HEAA, acrylic acid AAC, N,N-methylenebisacrylamide MBA, sodium dodecyl sulfate SDS, and sodium bicarbonate were added to a reactor filled with deionized water. The air in the reactor was completely replaced with nitrogen. The mixture was stirred for 30 minutes while continuously purging nitrogen to provide a protective atmosphere. The mixture was then heated to 70°C at a heating rate of 0.8°C / min under stirring, kept warm and stirred for 40 minutes, and then a 1.3 wt% aqueous solution of potassium persulfate was added. The mixture was kept warm for 7 hours and then cooled to room temperature to obtain a reactant. The reactant was transferred to a dialysis bag with a molecular weight cutoff of 12-14 kDa and dialyzed for 5 days (the water was changed every 8 hours). After dialysis, the mixture was freeze-dried to obtain a modified gel for later use. The modified gel prepared in this example had a lower critical solution temperature (LCST) of 34.6°C.

[0077] Among them, the weight ratio of N-vinylcaprolactam NVCL, N-hydroxyethylacrylamide HEAA, acrylic acid AAC, N,N-methylenebisacrylamide MBA, sodium lauryl sulfate SDS, sodium bicarbonate and deionized water is 5.1:1.15:0.31:0.07:0.09:0.16:400.

[0078] The volume ratio of the potassium persulfate aqueous solution to deionized water is 1:55.

[0079] 3. Overmolding A predetermined amount of deionized water was introduced into the reactor, cooled to 8°C, and kept warm; then the modified gel was added, stirred at 150 rpm for 50 minutes, and then the molecular nest was added, and the temperature was raised to 26°C at a heating rate of 0.3°C / min; then the temperature was raised to 38°C at a heating rate of 0.6°C / min, and kept warm and stirred for 40 minutes, and then the solid was separated. The solid was washed with deionized water at 38°C and freeze-dried to obtain composite temperature-sensitive coated particles for later use.

[0080] The weight ratio of the modified gel to deionized water is 1:40.

[0081] The weight ratio of modified gel to molecular nest is 5:1.

[0082] 4. Preparation of spinning solution The composite thermosensitive coated particles were put into deionized water at a temperature of 38°C and stirred for 15 minutes to obtain a functional modified liquid; then the functional modified liquid, spinning solution, sodium carboxymethyl cellulose, 3-aminopropyltriethoxysilane, and sodium alginate were evenly mixed, filtered, degassed, and aged to obtain a blended spinning solution.

[0083] The weight ratio of the composite thermosensitive coated particles to deionized water in the functional modification liquid is 1:15.

[0084] The weight ratio of the functional modification liquid, the spinning solution, sodium carboxymethyl cellulose, 3-aminopropyltriethoxysilane and sodium alginate is 11:92:0.4:1.1:0.5.

[0085] The methyl cellulose content of the spinning solution is 9.2%, the total alkali content is 2.9%, and the viscosity is 37s.

[0086] 5. Spinning The blended spinning solution is introduced into the spinning machine and sprayed into a coagulation bath at 43°C. The spinning speed is controlled at 20m / min, the spinning nozzle draft ratio is 6%, the inter-disk draft ratio is 13%, the three-bath draft ratio is 33%, the four-bath draft ratio is 12%, and the immersion length is 950mm. After spinning and forming, primary fibers are obtained. The primary fibers are desulfurized, washed, oiled, and dried to obtain viscose large bio-fibers with soothing functions.

[0087] The contents of the components in the coagulation bath are as follows: 92 g / L sulfuric acid, 195 g / L sodium sulfate, 23 g / L zinc sulfate, and 10 g / L calcium chloride.

[0088] This embodiment also provides a viscose biofiber with a soothing function produced by the aforementioned method.

[0089] Comparative Example 1 This comparative example adopts the technical solution of Example 2, with the following changes: the steps of preparing the modified gel and the coating molding are omitted, and the molecular nests (i.e., mesoporous silica loaded with plant active ingredients) obtained in the molecular nest preparation step are directly used in the spinning solution preparation step; specifically, the molecular nests are added to deionized water to prepare a functional modified liquid, and the weight ratio of the molecular nests to deionized water in the functional modified liquid is controlled to be 1:28.

[0090] Comparative Example 2 This comparative example adopts the technical solution of Example 2, with the following changes: 1) in the step of preparing molecular nests, the addition of 3-aminopropyltriethoxysilane is omitted; 2) in the step of preparing modified gel, the addition of N-hydroxyethyl acrylamide HEAA and acrylic acid AAC is omitted.

[0091] The lowest critical solution temperature (LCST) of the modified gel prepared in Comparative Example 2 was 31.2°C.

[0092] The release performance of the plant active ingredients (green tea extract, coral extract, and ginkgo leaf extract) of the viscose biofibers of Examples 1-3 and Comparative Examples 1-2 at 22°C was tested. Specifically, 5 g of the viscose biofibers of Examples 1-3 and Comparative Examples 1-2 were placed in a dialysis bag with a molecular weight cutoff of 1 KDa, and then immersed in 250 mL of the first absorption liquid at 22°C, shaken in a water bath at 100 rpm in the dark, and respectively mixed with 2 At 2 h and 48 h, the first absorption liquid was taken for detection and the contents of catechins, rosmarinic acid and ginkgolide in the first absorption liquid were recorded; then the viscose biofiber in the dialysis bag was taken out, chopped into pieces and placed in 250 mL of the second absorption liquid at a temperature of 22°C, and ultrasonically crushed and extracted for 60 min at this temperature, and the second absorption liquid was taken for detection and the contents of catechins, rosmarinic acid and ginkgolide in the second absorption liquid were recorded; the release rates of the representative active ingredients catechins, rosmarinic acid and ginkgolide at 2 h and 48 h were calculated respectively.

[0093] The first absorption liquid and the second absorption liquid have the same composition, using PBS buffer with a pH of 7.4 as the base solvent, and containing 10% by weight of ethanol, 0.1% by weight of Tween-80, and ascorbic acid with a concentration of 0.1 mmol / L.

[0094] The release rate of catechins at 2 h or 48 h was calculated as follows: [catechin content in the first absorption liquid at 2 h or 48 h / (catechin content in the first absorption liquid at 48 h + catechin content in the second absorption liquid after ultrasonic extraction)] × 100%.

[0095] The release rate of rosmarinic acid at 2 h or 48 h was calculated as follows: [rosmarinic acid content in the first absorption liquid at 2 h or 48 h / (rosmarinic acid content in the first absorption liquid at 48 h + rosmarinic acid content in the second absorption liquid after ultrasonic extraction)] × 100%.

[0096] The release rate of ginkgolide at 2 h or 48 h was calculated as follows: [ginkgolide content in the first absorption solution at 2 h or 48 h / (ginkgolide content in the first absorption solution at 48 h + ginkgolide content in the second absorption solution after ultrasonic extraction)] × 100%.

[0097] The specific results are shown in the following table:

[0098] Furthermore, the release performance of the plant active ingredients (green tea extract, coral extract, and ginkgo biloba extract) from the viscose biofibers of Examples 1-3 and Comparative Examples 1-2 was tested at 36°C. The specific method was the same as that for the release performance at 22°C, except that the temperature of the first and second absorption liquids was maintained at 36°C. The release rates of representative active ingredients, catechins, rosmarinic acid, and ginkgolides, at 2 and 48 hours are shown in the following table:

[0099] As can be seen, the method for preparing the allergy-relief viscose biofiber of the present invention involves treating mesoporous silica with 3-aminopropyltriethoxysilane to introduce amino groups during the molecular nest preparation step, creating a carrier dispersion. Green tea extract, coral extract, and ginkgo biloba extract are then dispersed in deionized water to create an active ingredient solution. The two are then mixed and loaded to produce mesoporous silica loaded with plant active ingredients (i.e., molecular nests). In the modified gel preparation step, N-vinylcaprolactam (NVCL) is used as the primary thermosensitive raw material and copolymerized with N-hydroxyethylacrylamide (HEAA) and acrylic acid (AAC) in the presence of an initiator and a crosslinker. This specifically adjusts the thermosensitive gel's lower critical solution temperature (LCST) to match the temperature range of sensitive skin areas, improving its subsequent encapsulation performance with the molecular nests. Carboxyl groups are introduced to further improve the binding of the modified gel to the molecular nests and the loaded plant active ingredients. In the coating molding step, the gel molecular chains are fully stretched in a low-temperature deionized water environment at 5-8°C. The gel is then placed into a molecular nest and uniformly coated onto the outer surface of the nest while slowly heating. The temperature is then further raised to a temperature exceeding the lower critical solution temperature (LCST) of the modified gel, causing the modified gel to shrink on the outer surface of the nest, completing the coating molding process and producing the composite thermosensitive coated particles. In the spinning solution preparation step, a functional modified solution is prepared using the composite thermosensitive coated particles. This solution is then mixed with the spinning solution and its auxiliary materials to form a blended spinning solution. The blended spinning solution is then spun to produce a viscose biofiber with a soothing effect.

[0100] The soothing viscose biofibers of Examples 1-3, at a temperature of 22°C (below the critical solution temperature, LCST), showed significantly higher release rates of plant active ingredients (such as catechins, rosmarinic acid, and ginkgolides) at 2 and 48 hours compared to the release rates at 36°C (slightly above the temperature of the allergic skin area). Fabrics made from these fibers can achieve high-dose, short-term release of plant active ingredients through temperature regulation, thereby achieving an emergency repair function. Subsequently, during prolonged contact with the skin, as the fabric gradually warms to skin temperature, the release of plant active ingredients from the fibers gradually decreases and stabilizes, transitioning to a long-term, low-dose, sustained release, thereby achieving a long-term soothing effect. In Comparative Example 1, where the modified gel and overmolding steps were omitted, the lack of the modified gel's encapsulation and controlled release effects on the molecular nests resulted in poor binding between the carrier and the plant active ingredients in the molecular nests. Consequently, the release rate was significantly affected by temperature and was significantly higher than that of Example 2. In Comparative Example 2, 3-aminopropyltriethoxysilane was omitted in the molecular nest preparation step, and N-hydroxyethylacrylamide HEAA and acrylic acid AAC were omitted in the modified gel preparation step. On the one hand, the lower critical solution temperature LCST of the gel could not be effectively increased. On the other hand, the binding performance with the plant active ingredients was reduced, resulting in an increase in the release rate of the plant active ingredients in a short period of time. In addition, in a temperature environment of 36°C, the excessive shrinkage of the gel may destroy the coating of the molecular nest, resulting in uncontrolled release of the plant active ingredients. Its release rate was significantly higher than that of Example 2, which exhibited long-term stable and controllable release.

[0101] Furthermore, the viscose large biofibers of Example 2 and Comparative Examples 1-2 were used for skin sensitivity tests. Specifically, the viscose large biofibers of Example 2 and Comparative Examples 1-2 were respectively spun into test fabrics. 20 Balb / c mice were selected as test subjects and randomly divided into 4 groups. The Balb / c mice were treated with 2,4-dinitrochlorobenzene at a concentration of 0.5wt% to cause erythema and edema allergic symptoms of substantially the same area. The following operations were performed on each group: In the first group, the test fabric of Example 2, which had been refrigerated at 10° C., was applied to the allergic area, completely covering the allergic area on the skin. The test fabric, which had been refrigerated at 10° C., was replaced every 8 hours.

[0102] In the second group, the test fabric of Example 2 at 36°C (similar to the skin surface temperature of the allergic area) was applied to the allergic area, completely covering the allergic area on the skin. The 36°C test fabric was replaced every 8 hours.

[0103] In the third group, the test fabric of Comparative Example 1, which had been refrigerated at 10°C, was applied to the allergic area and completely covered the allergic area on the skin. The test fabric, which had been refrigerated at 10°C, was replaced every 8 hours.

[0104] In the fourth group, the test fabric of Comparative Example 2, which had been refrigerated at 10°C, was applied to the allergic area and completely covered the allergic area on the skin. The test fabric, which had been refrigerated at 10°C, was replaced every 8 hours.

[0105] 24 hours after the application of the test fabric in each group, the soothing condition of the skin surface of each test subject was observed, and the number of test subjects who achieved each soothing effect (significant soothing, moderate soothing, mild soothing, and no soothing) was counted respectively; among them, significant soothing means that the reduction rate of erythema and / or edema area is ≥90%, moderate soothing means that the reduction rate of erythema and / or edema area is 50-90% (including 50%), mild soothing means that the reduction rate of erythema and / or edema area is 10-50%, and no soothing means that the reduction rate of erythema and / or edema area is ≤10%.

[0106] The specific results are shown in the following table:

[0107] After applying the test fabric for 48 hours, the sensitivity of the skin surface of each test subject was observed, and the number of test subjects who achieved different sensitivity effects (significant sensitivity, moderate sensitivity, mild sensitivity, and no sensitivity) was counted. The specific results are shown in the following table:

[0108] It can be seen that the test fabric made of pure viscose biofiber with soothing function of Example 2 and applied to the allergic area, after being refrigerated at 10°C, can not only have a cold compress and calming effect on allergic skin, but also can achieve a large dose release of plant active ingredients in a short period of time, thereby achieving an emergency repair function; compared with the test fabric of Example 2 applied to the allergic area at 36°C, it can achieve an ideal rapid soothing effect, and its soothing effect at 24h and 48h is significantly better. The test fabric made of pure viscose biofiber of Comparative Example 1 was applied to the allergic area. Because the plant active ingredients are affected by the viscose stock solution solvent environment, the coagulation bath solvent environment, and process conditions during the fiber preparation process, the binding effect of the fiber is not ideal, and its soothing effect on the allergic area is significantly worse than that of Example 2. The test fabric made purely from viscose large biofiber of Comparative Example 2 was applied to the allergic area. After the relevant technical means were omitted in the fiber preparation, the binding performance of the fiber and the plant active ingredients was reduced, and the stable controlled release of the plant active ingredients contained therein could not be achieved. Compared with Example 2, the soothing effect on the allergic area was reduced to a certain extent.

[0109] Furthermore, the antibacterial properties, antioxidant properties, and cytotoxicity levels of the viscose biofibers of Examples 1-3 and Comparative Examples 1-2 were tested. The antibacterial properties were tested in accordance with the relevant provisions of GB / T 20944.3-2008, "Evaluation of Antimicrobial Properties of Textiles - Part 3: Oscillation Method"; the cytotoxicity level was tested in accordance with the relevant provisions of the MTT method in GB / T 16886.5-2017, "Biological Evaluation of Medical Devices - Part 5: In Vitro Cytotoxicity Test"; and the antioxidant properties were tested using the DPPH method and the ABTS method, respectively.

[0110] The DPPH method specifically involves dissolving 2.5 mg of 1,1-diphenyl-2-trinitrophenylhydrazine (DPPH) in anhydrous ethanol and then diluting the volume to 100 mL to prepare a 25.0 mg / L DPPH ethanol solution. 2.0 g of the viscose biofibers from Examples 1-3 and Comparative Examples 1-2, respectively, are placed in an ultrasonic extraction bottle containing 50 mL of ethanol solution (50% by volume). After soaking at 25°C for 24 hours, ultrasonic extraction is performed for 20 minutes. The filtrate is then filtered and transferred to a rotary evaporator at a controlled temperature of 55°C and a vacuum of 0.085 MPa. The filtrate is then evaporated until it reaches 2 mL and diluted to 4 mL with ethanol solution (50% by volume) to serve as the test solution. Finally, 1 mL of the test solution was added to 2 mL of DPPH ethanol solution, mixed evenly, and allowed to stand in the dark for 10 min. The absorbance at a wavelength of 517 nm was detected using a spectrophotometer to calculate the DPPH free radical scavenging rate.

[0111] The specific method of the ABTS method is to take 200.0 mg of 2,2-azino-bis(3-ethyl-benzothiazole-6-sulfonic acid) diammonium salt ABTS and 34.4 mg of potassium persulfate and dissolve them in 50.0 mL of deionized water. After standing at room temperature in the dark for 24 hours, the ABTS mother solution is obtained. A certain amount of ABTS mother solution is taken and diluted with 95% ethanol solution to an absorbance of 0.70 at a wavelength of 734 nm to obtain an ABTS diluent. Then, the test solution is prepared (the specific method of preparing the test solution is the same as the preparation method of the test solution in the aforementioned DPPH free radical scavenging rate test). Finally, 0.5 mL of the test solution is added to 5 mL of the ABTS diluent, mixed evenly, and after standing in the dark for 10 minutes, the absorbance at a wavelength of 734 nm is detected by a spectrophotometer to calculate the ABTS. + Free radical scavenging rate.

[0112] The specific results are shown in the following table:

[0113] The plant active ingredients contained in the viscose large bio-fiber with soothing function of Examples 1-3 can achieve effective antibacterial and antioxidant effects, and can inhibit the growth of bacteria in the allergic skin areas while soothing the allergic skin areas; at the same time, it can also remove excess free radicals produced by skin allergies through its antioxidant function, reduce the oxidative stress of the skin, and assist in repairing the skin's barrier function; and the cytotoxicity level of the viscose large bio-fiber is all level 0, with low irritation to allergic skin, and is effectively suitable for skin soothing.

[0114] Furthermore, the dry breaking strength, wet breaking strength, whiteness, and defects of the viscose biofibers of Examples 1-3 and Comparative Examples 1-2 were tested. Whiteness was tested using a Datacolor SF600 colorimeter at 20°C and 65% relative humidity. The results are shown in the following table:

[0115] In the preparation of the viscose biofiber with soothing function of Examples 1-3, the composite temperature-sensitive coated particles used can not only impart soothing function to the fiber, but also further improve the mechanical properties of the viscose biofiber, have no adverse effect on whiteness, and have a low fiber defect content.

[0116] Unless otherwise specified, all percentages used in the present invention are by mass.

[0117] 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 viscose biofiber with a soothing function, characterized in that: The method comprises the following steps: preparing molecular nests, preparing modified gel, coating and molding, preparing spinning solution, and spinning and molding; The molecular nest is prepared by uniformly mixing mesoporous silica, 3-aminopropyltriethoxysilane, and an ethanol aqueous solution, stirring at 45-50° C., and then cooling to obtain a carrier dispersion; adding green tea extract, coral extract, and ginkgo leaf extract into deionized water and uniformly dispersing them to obtain an active ingredient solution; mixing the carrier dispersion and the active ingredient solution, stirring at room temperature, separating to obtain a solid, and drying to obtain the molecular nest; The modified gel is prepared by using N-vinylcaprolactam, N-hydroxyethyl acrylamide, acrylic acid, N,N-methylenebisacrylamide, sodium lauryl sulfate, and sodium bicarbonate as reaction raw materials in a solvent environment under the protection of an inert gas, and reacting at 68-70° C. in the presence of an initiator. The obtained reactant is dialyzed and dried to obtain the modified gel. The coating molding adopts modified gel to coat the molecular nest to obtain composite temperature-sensitive coated particles; The spinning solution is prepared by uniformly mixing the composite temperature-sensitive coated particles with the spinning solution to obtain a blended spinning solution; The blended spinning solution is spun into a fiber to produce a viscose biofiber with a soothing function.

2. The method for preparing the viscose biofiber with soothing function according to claim 1, characterized in that: In the preparation of the molecular nest, the weight ratio of mesoporous silica, 3-aminopropyltriethoxysilane and ethanol aqueous solution in the carrier dispersion is 10-12: 1.5-1.9:70-75； The weight ratio of green tea extract, coral extract, ginkgo leaf extract and deionized water in the active ingredient liquid is 7-7.5:4.2-4.7:2-2.2:120-130; The weight ratio of the carrier dispersion liquid to the active ingredient liquid is 2.1-2.3:

1.

3. The method for preparing the viscose biofiber with soothing function according to claim 1, characterized in that: The modified gel is prepared by adding N-vinylcaprolactam, N-hydroxyethylacrylamide, acrylic acid, N,N-methylenebisacrylamide, sodium lauryl sulfate, and sodium bicarbonate into deionized water, mixing them uniformly under the protection of inert gas, stirring, heating to 68-70° C., adding a potassium persulfate aqueous solution, keeping the temperature for reaction for 5-7 hours, cooling, and obtaining a reactant; and dialyzing the reactant through a dialysis bag with a molecular weight cutoff of 12-14 kDa for 4-5 days, and then drying to obtain the modified gel.

4. The method for preparing the viscose biofiber with soothing function according to claim 3, characterized in that: In the preparation of the modified gel, the weight ratio of N-vinylcaprolactam, N-hydroxyethyl acrylamide, acrylic acid, N,N-methylenebisacrylamide, sodium lauryl sulfate, sodium bicarbonate, and deionized water is 5-5.1:1.05-1.15:0.28-0.31:0.06-0.07:0.08-0.09:0.12-0.16:380-400; The concentration of the potassium persulfate aqueous solution is 1.2-1.3 wt %, and the volume ratio of the potassium persulfate aqueous solution to deionized water is 1:50-55.

5. The method for preparing the viscose biofiber with soothing function according to claim 1, characterized in that: The coating molding comprises the following steps: putting the modified gel into deionized water at 5-8°C and dispersing it evenly, then putting the molecular nest into the water, stirring and heating it to 24-26°C at a heating rate of 0.2-0.3°C / min; then stirring and heating it to 37-38°C at a heating rate of 0.5-0.6°C / min, keeping the temperature and stirring, separating and obtaining a solid, and washing and drying the solid to obtain composite temperature-sensitive coated particles.

6. The method for preparing the viscose biofiber with soothing function according to claim 5, characterized in that: In the overmolding process, the weight ratio of the modified gel to deionized water is 1:35-40; The weight ratio of the modified gel to the molecular nest is 4.5-5:

1.

7. The method for preparing the viscose biofiber with soothing function according to claim 1, characterized in that: The spinning solution is prepared by adding the composite temperature-sensitive coated particles into deionized water at a temperature of 37-38° C. and dispersing them uniformly to obtain a functionally modified solution; the functionally modified solution, spinning solution, sodium carboxymethyl cellulose, 3-aminopropyltriethoxysilane, and sodium alginate are uniformly mixed, and the mixture is filtered, degassed, and aged to obtain a blended spinning solution; The spinning molding comprises spraying the blended spinning solution into a coagulation bath at 42-43° C., and spinning molding to obtain primary fibers; the primary fibers are desulfurized, washed, oiled, and dried to obtain viscose large bio-fibers with soothing functions.

8. The method for preparing the viscose biofiber with soothing function according to claim 7, characterized in that: In the preparation of the spinning solution, the weight ratio of the composite temperature-sensitive coated particles to deionized water in the functional modification solution is 1:14-15; The weight ratio of the functional modification solution, spinning solution, sodium carboxymethyl cellulose, 3-aminopropyltriethoxysilane, and sodium alginate is 10-11:88-92:0.3-0.4:0.9-1.1:0.4-0.5; The methyl cellulose content of the spinning solution is 9.1-9.3%, the total alkali content is 2.8-3.2%, and the viscosity is 35-40s.

9. The method for preparing the viscose biofiber with soothing function according to claim 7, characterized in that: In the spinning process, the spinning speed is controlled to be 19-20 m / min, the spinning nozzle draft ratio is 4-6%, the inter-disk draft ratio is 11-13%, the three-bath draft ratio is 31-33%, the four-bath draft ratio is 10-12%, and the immersion length is 900-950 mm; The contents of the components in the coagulation bath are: 90-100 g / L of sulfuric acid, 180-210 g / L of sodium sulfate, 20-25 g / L of zinc sulfate, and 10-12 g / L of calcium chloride.

10. A viscose biofiber with soothing function, characterized in that: The method is prepared according to any one of claims 1 to 9.

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