Viscose large biological fiber with soothing function and preparation method thereof

Abstract

The application provides viscose large biofibers with soothing function and a preparation method thereof, and belongs to the field of viscose fibers. The preparation method of the viscose large biofibers with soothing function comprises the following steps: preparing a molecular nest, preparing a modified gel, coating and forming, preparing a spinning solution, and spinning and forming. The preparation method of the viscose large biofibers with soothing function can avoid the problem that the plant active ingredients are affected by process environment, solvent components and the like, and the activity and stability of the plant active ingredients are reduced; meanwhile, the release characteristics of the plant active ingredients in the viscose fibers can be regulated according to needs, the plant active ingredients are released in a large dose in a short time or a small dose in a long time, and thus the emergency repair or long-acting soothing of the skin allergic area is achieved.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of viscose fibers, in particular to a viscose large bio fiber with a soothing function and a preparation method thereof. BACKGROUND

[0002] Viscose fiber is a soluble cellulose xanthate prepared by taking natural fiber as raw material, through alkalization, aging, sulfonation and other processes, then dissolving in dilute alkali solution to prepare viscose liquid, and finally wet spinning. Due to its good moisture absorption and air permeability, high comfort, easy dyeing, not easy to generate static electricity, and good spinnability, viscose fiber is widely used in various textiles, clothing and other fields. With the improvement of people's living standards, viscose is constantly updated and replaced. Due to the influence of its inherent characteristics and single preparation process, the performance of traditional viscose fiber is more and more unable to meet the actual needs of market consumers. People not only require viscose fiber to have basic moisture absorption and air permeability, but also require its diversification and functionalization, such as antibacterial, antifouling, antioxidant, anti-ultraviolet and other functions. Functional viscose fiber has become the main development direction in recent years. The functional improvement is usually to add corresponding functional plant ingredients (such as functional particles, microcapsules containing plant active ingredients) during the preparation of viscose fiber; or after the preparation of viscose fiber is completed, further give viscose fiber different functions through post-processing process (such as spraying, soaking, etc.).

[0003] In the traditional preparation process of viscose fiber, when plant active ingredients are used in the preparation of viscose fiber, the plant active ingredients are easily affected by the process environment, solvent composition and other factors during the preparation of viscose fiber, which reduces the activity and stability, resulting in poor combination performance of plant active ingredients and viscose fiber. Not only can't realize the stable functional modification of viscose fiber, but also affect the physical properties of viscose fiber.

[0004] Further, environmental factors such as ultraviolet rays, smog, dust and dry wind, etc. act on the exposed skin for a long time, which can cause skin imbalance, dryness, itching, redness and other allergic symptoms. It is of great significance and research value to provide a viscose large biological fiber with soothing function. There are few disclosures in the prior art for fibers with soothing function. For example, Chinese patent CN117265684B discloses a preparation method and application of a gentian viscose fiber with soothing effect. The gentian extract, viscose stock solution, oat-beta glucan, lignin and organic quaternary ammonium salt are combined to form a spinning solution, and then the spinning solution is formed into a viscose fiber through a coagulation bath, drawing, washing and drying. However, on the one hand, during the preparation process of the viscose fiber, the gentian extract is easily affected by the solvent environment of the viscose stock solution, the coagulation bath solvent environment and the process conditions, which limits its modification effect on the viscose fiber. On the other hand, when the skin needs emergency repair due to acute allergy, the viscose fiber cannot release a large dose of plant active ingredients in a short time to achieve the purpose of emergency repair. When the skin allergy position needs long-acting soothing, the viscose fiber also cannot stably release plant active ingredients in a long time to achieve the purpose of long-acting soothing. The soothing function of the viscose fiber needs to be further improved. SUMMARY

[0005] To solve the technical problems in the prior art, the present application provides a viscose large biological fiber with soothing function and a preparation method thereof, which can avoid the problem that the plant active ingredients are affected by process environment, solvent composition, etc. and reduce the activity and stability; at the same time, the release characteristics of the plant active ingredients in the viscose fiber can be regulated as needed to achieve short-time large-dose release or long-time small-dose slow release of the plant active ingredients, thereby achieving emergency repair or long-acting soothing of the skin allergy area.

[0006] To solve the above technical problems, the technical solutions adopted by the present application are as follows:

[0007] A preparation method of a viscose large biological fiber with soothing function, comprising the following steps: preparing a molecular nest, preparing a modified gel, coating and forming, preparing a spinning solution, and spinning and forming;

[0008] In the preparation of the molecular nest, mesoporous silica, 3-aminopropyltriethoxysilane and ethanol aqueous solution are uniformly mixed, and after 45-50℃ incubation and stirring, the mixture is cooled to obtain a carrier dispersion liquid. The green tea extract, Sarcandra glabra extract and ginkgo leaf extract are uniformly dispersed in deionized water to obtain an active ingredient solution. The carrier dispersion liquid and the active ingredient solution are mixed and stirred at room temperature, and the solid material is separated and dried to obtain the molecular nest.

[0009] The modified gel is prepared by using N-vinyl caprolactam, N-hydroxyethyl acrylamide, acrylic acid, N,N-methylene bisacrylamide, sodium dodecyl sulfate and sodium bicarbonate as raw materials, under the protection of inert gas, at 68-70 DEG C, and then the reaction product is obtained by dialysis and drying.

[0010] The coating forming is performed by using the modified gel to coat the molecular nest, so as to obtain the composite temperature-sensitive coated particles.

[0011] The spinning solution is prepared by uniformly mixing the composite temperature-sensitive coated particles and the spinning solution, so as to obtain the blended spinning solution.

[0012] The blended spinning solution is formed by spinning, so as to obtain the viscose large bio-fiber with the soothing function.

[0013] Preferably, in the preparation of the molecular nest, the weight ratio of mesoporous silica, 3-aminopropyl triethoxysilane and ethanol aqueous solution in the carrier dispersion solution is 10-12:1.5-1.9:70-75.

[0014] The weight ratio of green tea extract, Sarcandra glabra extract, ginkgo leaf extract and deionized water in the active ingredient solution 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.

[0015] The weight ratio of the carrier dispersion solution and the active ingredient solution is 2.1-2.3:1.

[0016] Further, the modified gel is prepared by adding N-vinyl caprolactam, N-hydroxyethyl acrylamide, acrylic acid, N,N-methylene bisacrylamide, sodium dodecyl sulfate and sodium bicarbonate into deionized water, uniformly mixing, stirring and heating to 68-70 DEG C under the protection of inert gas, adding potassium persulfate aqueous solution, and then incubating for 5-7 h to obtain the reaction product; the reaction product is dialyzed in a dialysis bag with a molecular weight cut-off of 12-14 KDa for 4-5 d, and then dried to obtain the modified gel.

[0017] Preferably, in the preparation of the modified gel, the weight ratio of N-vinyl caprolactam, N-hydroxyethyl acrylamide, acrylic acid, N,N-methylene bisacrylamide, sodium dodecyl 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.

[0018] The concentration of the potassium persulfate aqueous solution is 1.2-1.3wt%, and the volume ratio of the potassium persulfate aqueous solution to deionized water is 1:50-55.

[0019] Further, in the coating forming, the modified gel is uniformly dispersed in deionized water at 5-8℃, and then is put into a molecular nest, and is stirred and heated to 24-26℃ at a heating rate of 0.2-0.3℃ / min; then is stirred and heated to 37-38℃ at a heating rate of 0.5-0.6℃ / min, and after heat preservation and stirring, a solid is separated and obtained, and the solid is washed and dried to prepare the composite temperature-sensitive coated particles.

[0020] Preferably, in the coating forming, the weight ratio of the modified gel to deionized water is 1:35-40;

[0021] The weight ratio of the modified gel to the molecular nest is 4.5-5:1.

[0022] Further, in the preparation of the spinning solution, the composite temperature-sensitive coated particles are uniformly dispersed in deionized water at a temperature of 37-38℃ to obtain a functional modified liquid; then the functional modified liquid, a spinning stock solution, sodium carboxymethyl cellulose, 3-aminopropyl triethoxysilane and sodium alginate are uniformly mixed, and are filtered, defoamed and aged to prepare a blended spinning solution.

[0023] In the spinning forming, the blended spinning solution is sprayed into a coagulation bath at 42-43℃, and after the spinning forming, a primary fiber is prepared; and the primary fiber is desulfurized, washed, oiled and dried to prepare the viscose large bio-fiber with the soothing function.

[0024] Preferably, in the preparation of the spinning solution, the weight ratio of the composite temperature-sensitive coated particles to deionized water in the functional modified liquid is 1:14-15;

[0025] The weight ratio of the functional modified liquid, the spinning stock solution, sodium carboxymethyl cellulose, 3-aminopropyl triethoxysilane and sodium alginate is 10-11:88-92:0.3-0.4:0.9-1.1:0.4-0.5.

[0026] The content of methylcellulose in the spinning stock solution is 9.1-9.3%, the total alkali content is 2.8-3.2%, and the viscosity is 35-40s.

[0027] Preferably, in the spinning forming, the spinning speed is controlled to be 19-20m / min, the spinning nozzle draft ratio is 4-6%, the inter-disc 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 900-950mm.

[0028] The content of each component in the coagulation bath is: 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.

[0029] A viscose large biological fiber with a soothing function is prepared by the method.

[0030] Compared with the prior art, the method has the following beneficial effects:

[0031] (1) In the method for preparing the viscose large biological fiber with a soothing function, in the preparation of the molecular nest step, 3-aminopropyl triethoxysilane is used to treat mesoporous silica to introduce amino groups, and a carrier dispersion liquid is prepared; green tea extract, Sarcandra glabra extract and ginkgo leaf extract are dispersed in deionized water to prepare an active ingredient liquid; then the two are mixed and loaded to prepare mesoporous silica loaded with plant active ingredients (i.e., the molecular nest). In the preparation of the modified gel step, N-vinyl caprolactam (NVCL) is used as the main temperature-sensitive material to copolymerize with N-hydroxyethyl acrylamide (HEAA) and acrylic acid (AAC) in the presence of an initiator and a crosslinking agent, so as to adjust the low critical solution temperature (LCST) of the temperature-sensitive gel to match the temperature range of the allergic skin region, improve the subsequent coating performance of the temperature-sensitive gel on the molecular nest, and introduce carboxyl groups to further improve the binding performance of the modified gel, the molecular nest and the plant active ingredients loaded thereon. In the coating and forming step, the modified gel molecular chain is fully stretched in a low-temperature deionized water environment at 5-8 DEG C, and then the molecular nest is put into the deionized water, and the modified gel is uniformly coated on the outer surface of the molecular nest while slowly heating, and then the temperature is further increased to be higher than the low critical solution temperature (LCST) of the modified gel, so that the modified gel shrinks on the outer surface of the molecular nest, the coating and forming are completed, and a composite temperature-sensitive coated particle is prepared. Then in the preparation of the spinning solution step, the functional modified liquid is prepared by using the composite temperature-sensitive coated particle, and then the functional modified liquid is mixed with the spinning stock solution and its auxiliary materials to prepare a blended spinning solution; the blended spinning solution is spun to form a viscose large biological fiber with a soothing function. The above technical means cooperate with each other and work synergistically, so that the problem of reduction in activity and stability of the plant active ingredients due to the influence of process environment and solvent components can be avoided; at the same time, the release characteristics of the plant active ingredients in the viscose fiber can be regulated according to needs, so that the plant active ingredients are released in a large dose in a short time or released in a small dose for a long time, and then the skin allergic area is urgently repaired or long-acting soothing is achieved.

[0032] (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.

[0033] (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.

[0034] (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.

[0035] (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

[0036] 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.

[0037] It is to be noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments in accordance with the present application. As used herein, "first," "second," and / or the like are used merely as labels to facilitate explanation of the exemplary skilled in the art will understand that the use of the terms "first," "second," and / or the like is not to imply that the particular features so designated must be in any given order or be executed in any particular order, and the like. Additionally, it will be understood that when using terms such as "contain" and / or "include," that these terms are meant to encompass the items listed thereafter, and / or equivalents thereof, unless specifically stated otherwise.

[0038] The application provides a preparation method of viscose large biological fiber with soothing function, which comprises the following steps: preparing a molecular nest, preparing a modified gel, coating and forming, preparing a spinning solution, and spinning and forming.

[0039] The method for preparing the molecular nest comprises the following steps: putting mesoporous silica and 3-aminopropyl triethoxysilane into an ethanol aqueous solution with a volume concentration of 60-65%, ultrasonic dispersion for 20-30 min, heating to 45-50℃, and stirring for 2-3 h, then cooling to room temperature to obtain a carrier dispersion liquid; putting green tea extract, coralline extract and ginkgo leaf extract into deionized water, stirring for 20-30 min to obtain an active ingredient liquid; mixing the carrier dispersion liquid and the active ingredient liquid with a weight ratio of 2.1-2.3:1, stirring at room temperature for 4-6 h, and centrifugal separation to obtain a solid; transferring the solid to a vacuum drying oven, drying in a vacuum degree of 0.07-0.09 MPa at 70-75℃ until constant weight to obtain the molecular nest (i.e. mesoporous silica loaded with plant active ingredients), ready for use.

[0040] In the preparation of the molecular nest, the weight ratio of mesoporous silica, 3-aminopropyl triethoxysilane and the ethanol aqueous solution in the carrier dispersion liquid is 10-12:1.5-1.9:70-75.

[0041] In the active ingredient liquid, the weight ratio of green tea extract, coralline extract, ginkgo leaf extract and deionized water is 7-7.5:4.2-4.7:2-2.2:120-130.

[0042] The preparation method of the green tea extract is as follows: mixing green tea with 10-12 times of extraction solvent (ethanol aqueous solution with a volume concentration of 60-65%) in a nitrogen and light-proof environment, and refluxing extraction at 70-75℃ for 1-1.5 h to obtain an extraction liquid; repeating the extraction for 2-3 times, combining the extraction liquids, filtering, and then spray drying to obtain the green tea extract; or the green tea extract with an extraction ratio of 10-20:1 and a particle size of 80-100 mesh can be purchased through a conventional market channel.

[0043] The preparation method of the extract of Sarcandra glabra is that Sarcandra glabra is used as raw material, mixed with 10-12 times of extraction solvent (60-65% (volume concentration) ethanol aqueous solution), 0.1wt% of citric acid is added, and then the mixture is extracted at 60-65℃ for 1-1.5h under nitrogen and in the dark. The extract is obtained. The extraction is repeated for 2-3 times. The multiple extracts are combined, filtered, and then spray-dried to obtain the extract of Sarcandra glabra. Alternatively, the extract of Sarcandra glabra with an extraction ratio of 10-20:1 and a particle size of 80-100 mesh can be purchased through a conventional commercial channel.

[0044] The extract of Ginkgo biloba leaves is prepared by using Ginkgo biloba leaves as raw material, mixing with 10-12 times of extraction solvent (60-65% (volume concentration) acetone aqueous solution), and then extracting at 50-55℃ for 1.5-2h under nitrogen and in the dark. The extract is obtained. The extraction is repeated for 2-3 times. The multiple extracts are combined, filtered, and then spray-dried to obtain the extract of Ginkgo biloba leaves. Alternatively, the extract of Ginkgo biloba leaves with an extraction ratio of 10-20:1 and a particle size of 80-100 mesh can be purchased through a conventional commercial channel.

[0045] The preparation method of the modified gel is that N-vinyl caprolactam NVCL, N-hydroxyethyl acrylamide HEAA, acrylic acid AAC, N,N-methylene bisacrylamide MBA, sodium dodecyl sulfate SDS, and sodium bicarbonate are put into a reaction kettle containing deionized water. The air in the reaction kettle is completely replaced with nitrogen. The mixture is stirred for 15-30min under the protection of nitrogen atmosphere. Then the temperature is raised to 68-70℃ at a rate of 0.5-0.8℃ / min under stirring. After stirring at 68-70℃ for 30-40min, a 1.2-1.3wt% potassium persulfate aqueous solution is continuously added. After 5-7h of incubation, the reaction mixture is cooled to room temperature. The reaction mixture is transferred into a dialysis bag with a molecular weight cut-off of 12-14KDa. Dialysis is performed for 4-5d (water is changed every 8h). After dialysis, the modified gel is obtained by freeze-drying.

[0046] In the preparation of the modified gel, the weight ratio of N-vinyl caprolactam NVCL, N-hydroxyethyl acrylamide HEAA, acrylic acid AAC, N,N-methylene bisacrylamide MBA, sodium dodecyl 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.

[0047] The volume ratio of the potassium persulfate aqueous solution to deionized water is 1:50-55.

[0048] The method for the coating molding is that a predetermined amount of deionized water is introduced into a reaction kettle, cooled to 5-8 DEG C, and incubated; then the modified gel is added, stirred at 100-150 rpm for 40-50 min, and then the molecular nest is continuously added, and the stirring temperature is raised to 24-26 DEG C at a temperature raising rate of 0.2-0.3 DEG C / min; then the stirring temperature is raised to 37-38 DEG C at a temperature raising rate of 0.5-0.6 DEG C / min, and incubated and stirred for 30-40 min, and then the solid product is separated, and the solid product is washed with deionized water at a temperature of 37-38 DEG C, and then freeze-dried to obtain the composite temperature-sensitive coated particles.

[0049] In the coating molding, the weight ratio of the modified gel to the deionized water is 1:35-40;

[0050] The weight ratio of the modified gel to the molecular nest is 4.5-5:1.

[0051] The method for preparing the spinning solution is that the composite temperature-sensitive coated particles are added into deionized water at a temperature of 37-38 DEG C, and stirred for 10-15 min to obtain the functional modification liquid; then the functional modification liquid, the spinning stock solution, sodium carboxymethyl cellulose, 3-aminopropyl triethoxysilane, and sodium alginate are uniformly mixed, filtered, and then degassed and aged to obtain the blended spinning solution.

[0052] In the preparation of the spinning solution, the weight ratio of the composite temperature-sensitive coated particles to the deionized water in the functional modification liquid is 1:14-15;

[0053] The weight ratio of the functional modification liquid, the spinning stock solution, sodium carboxymethyl cellulose, 3-aminopropyl triethoxysilane, and sodium alginate is 10-11:88-92:0.3-0.4:0.9-1.1:0.4-0.5;

[0054] The content of methyl cellulose in the spinning stock solution is 9.1-9.3%, the total alkali content is 2.8-3.2%, and the viscosity is 35-40 s.

[0055] The method for the spinning molding is that the blended spinning solution is introduced into a spinning machine, sprayed into a coagulation bath at a temperature of 42-43 DEG C, and 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; after the spinning molding, the primary fiber is obtained; and the primary fiber is subjected to desulfurization, washing, oiling, and drying to obtain the viscose large biofiber with the soothing function.

[0056] In the spinning molding, the content of each component in the coagulation bath is: sulfuric acid 90-100 g / L, sodium sulfate 180-210 g / L, zinc sulfate 20-25 g / L, and calcium chloride 10-12 g / L.

[0057] The application further provides the viscose large bio-fiber with the soothing function prepared by the method.

[0058] The application will be further described in combination with some specific embodiments.

[0059] Embodiment 1

[0060] The embodiment provides a preparation method of viscose large bio-fiber with soothing function, and specifically relates to the following steps.

[0061] 1. Preparation of molecular nest

[0062] Mesoporous silica and 3-aminopropyl triethoxysilane are put into an ethanol aqueous solution with a volume concentration of 60%, and ultrasonic dispersion is performed for 20 min; the temperature is increased to 45 DEG C, and the stirring is performed for 2 h; then the temperature is cooled to room temperature; the carrier dispersion liquid is prepared; green tea extract, coralline extract and ginkgo leaf extract are put into deionized water, and stirring is performed for 20 min; the active ingredient liquid is prepared; the weight ratio of the carrier dispersion liquid and the active ingredient liquid is 2.1:1; the stirring is performed at room temperature for 4 h; the solid is obtained by centrifugal separation; the solid is transferred into a vacuum drying oven; the drying is performed at 75 DEG C until the constant weight under the condition of 0.07 MPa vacuum degree; the molecular nest (i.e. mesoporous silica loaded with plant active ingredients) is prepared, and is ready for use.

[0063] In the carrier dispersion liquid, the weight ratio of mesoporous silica, 3-aminopropyl triethoxysilane and the ethanol aqueous solution is 10:1.5:70.

[0064] In the active ingredient liquid, the weight ratio of green tea extract, coralline extract, ginkgo leaf extract and deionized water is 7:4.2:2:120; the particle size of the green tea extract used in the embodiment is 100 mesh, and the extraction ratio is 20:1; the particle size of the coralline 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.

[0065] 2. Preparation of modified gel

[0066] N-vinyl caprolactam NVCL, N-hydroxyethyl acrylamide HEAA, acrylic acid AAC, N,N-methylene bisacrylamide MBA, sodium dodecyl sulfate SDS, sodium bicarbonate were put into a reaction kettle containing deionized water, the air in the reaction kettle was completely replaced with nitrogen, and the mixture was stirred for 15 min under the condition of continuously supplying nitrogen to provide an atmosphere protection; then under stirring, the temperature was raised to 68℃ at a rate of 0.5℃ / min, and after 30 min of incubation and stirring, 1.2wt% potassium persulfate aqueous solution was continuously added, and after 5h of incubation and reaction, it was cooled to room temperature to obtain a reaction product; the reaction product was transferred to a dialysis bag with a molecular weight cut-off of 12-14KDa, dialyzed for 4d (water was changed every 8h), and after dialysis, it was freeze-dried to obtain a modified gel, which was used as needed; detection showed that the lowest critical solution temperature LCST of the modified gel prepared in this embodiment was 34.1℃.

[0067] The weight ratio of N-vinyl caprolactam NVCL, N-hydroxyethyl acrylamide HEAA, acrylic acid AAC, N,N-methylene bisacrylamide MBA, sodium dodecyl sulfate SDS, sodium bicarbonate, and deionized water is 5:1.05:0.28:0.06:0.08:0.12:380.

[0068] The volume ratio of potassium persulfate aqueous solution to deionized water is 1:50.

[0069] 3, coating forming

[0070] A predetermined amount of deionized water was introduced into the reaction kettle and cooled to 5℃ for incubation; then the modified gel was added, and after 40 min of stirring at 100rpm, the molecular nest was continuously added, and the temperature was raised to 24℃ at a rate of 0.2℃ / min under stirring; then the temperature was raised to 37℃ at a rate of 0.5℃ / min under stirring, and after 30 min of incubation and stirring, the solid was separated; the solid was washed with deionized water at a temperature of 37℃, and then freeze-dried to obtain a composite temperature-sensitive coated particle, which was used as needed.

[0071] The weight ratio of the modified gel to deionized water is 1:35.

[0072] The weight ratio of the modified gel to the molecular nest is 4.5:1.

[0073] 4, preparation of spinning solution

[0074] The composite temperature-sensitive coated particle was added to deionized water at a temperature of 37℃, and stirred for 10 min to obtain a functional modification liquid; then the functional modification liquid, the spinning stock solution, sodium carboxymethyl cellulose, 3-aminopropyl triethoxysilane, and sodium alginate were mixed uniformly, filtered, and then degassed, aged to obtain a blended spinning solution.

[0075] The weight ratio of the composite temperature-sensitive coated particles in the functional modification liquid to deionized water is 1:14.

[0076] The weight ratio of the functional modification liquid, the spinning dope, sodium carboxymethyl cellulose, 3-aminopropyl triethoxysilane and sodium alginate is 10:88:0.3:0.9:0.4.

[0077] The content of methyl cellulose in the spinning dope is 9.2%, the total alkali content is 2.9%, and the viscosity is 37 s.

[0078] 5. Spinning forming

[0079] The blended spinning liquid is introduced into a spinning machine and sprayed into a coagulation bath at 42℃, the spinning speed is controlled to be 19 m / 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 900 mm; after the spinning forming, the primary fiber is prepared; the primary fiber is subjected to desulfurization, washing, oiling and drying to prepare the viscose large bio-fiber with soothing function.

[0080] The content of each component in the coagulation bath is: sulfuric acid 92 g / L, sodium sulfate 195 g / L, zinc sulfate 23 g / L, and calcium chloride 10 g / L.

[0081] The embodiment also provides the viscose large bio-fiber with soothing function prepared by the method.

[0082] Embodiment 2

[0083] The embodiment provides a preparation method of a viscose large bio-fiber with soothing function, and specifically relates to the following steps:

[0084] 1. Preparing a molecular nest

[0085] Mesoporous silica and 3-aminopropyl triethoxysilane are put into an ethanol aqueous solution with a volume concentration of 62%, ultrasonic dispersion is performed for 25 min, the temperature is increased to 48℃, and after 2.5 h of constant temperature stirring, the temperature is cooled to room temperature to prepare a carrier dispersion liquid; green tea extract, Sarcandra glabra extract and ginkgo leaf extract are put into deionized water and stirred for 25 min to prepare an active ingredient liquid; the weight ratio of the weight ratio of the carrier dispersion liquid and the active ingredient liquid is 2.2:1, the carrier dispersion liquid and the active ingredient liquid are mixed and stirred at room temperature for 5 h, and centrifugal separation is performed to obtain a solid; the solid is transferred into a vacuum drying oven, dried at 72℃ under a vacuum degree of 0.08 MPa until the weight is constant, and a molecular nest (i.e., mesoporous silica loaded with plant active ingredients) is prepared.

[0086] The weight ratio of mesoporous silica, 3-aminopropyl triethoxysilane and the ethanol aqueous solution in the carrier dispersion liquid is 11:1.7:73.

[0087] The weight ratio of green tea extract, Sarcandra glabra extract, ginkgo leaf extract, and deionized water in the active ingredient solution 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 glabra 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.

[0088] 2. Preparation of modified gel

[0089] N-vinyl caprolactam NVCL, N-hydroxyethyl acrylamide HEAA, acrylic acid AAC, N,N-methylene bisacrylamide MBA, sodium dodecyl sulfate SDS, and sodium bicarbonate were put into a reaction kettle containing deionized water, the air in the reaction kettle was completely replaced with nitrogen, and the mixture was stirred for 20 min under the condition of continuous nitrogen atmosphere protection. Then, under stirring, the temperature was raised to 70°C at a rate of 0.6°C / min, and after 35 min of incubation and stirring, a 1.3 wt% potassium persulfate aqueous solution was continuously added. After 6 h of incubation and reaction, the reaction mixture was cooled to room temperature. The reaction mixture was transferred to a dialysis bag with a molecular weight cut-off of 12-14 KDa, dialyzed for 4.5 d (water was changed every 8 h), and then freeze-dried after dialysis to obtain the modified gel, which was ready for use. The lowest critical solution temperature LCST of the modified gel prepared in this embodiment was 34.3°C.

[0090] The weight ratio of N-vinyl caprolactam NVCL, N-hydroxyethyl acrylamide HEAA, acrylic acid AAC, N,N-methylene bisacrylamide MBA, sodium dodecyl sulfate SDS, sodium bicarbonate, and deionized water is 5.1:1.1:0.3:0.065:0.085:0.14:390.

[0091] The volume ratio of potassium persulfate aqueous solution to deionized water is 1:53.

[0092] 3. Coating molding

[0093] A predetermined amount of deionized water was introduced into the reaction kettle and cooled to 6°C for incubation. Then, the modified gel was added, and after 45 min of stirring at 120 rpm, the molecular nest was continuously added. The temperature was raised to 25°C at a rate of 0.2°C / min under stirring. Then, the temperature was raised to 38°C at a rate of 0.5°C / min under stirring, and after 35 min of incubation and stirring, the solid was separated. The solid was washed with deionized water at a temperature of 38°C, and then freeze-dried to obtain the composite temperature-sensitive coated particles, which were ready for use.

[0094] The weight ratio of the modified gel to deionized water is 1:37.

[0095] The weight ratio of the modified gel to the molecular nest is 4.8:1.

[0096] 4. Preparation of the spinning solution

[0097] The composite temperature-sensitive coated particles are put into deionized water at a temperature of 38 DEG C and stirred for 12 min to obtain a functional modification liquid; then the functional modification liquid, the spinning stock solution, sodium carboxymethyl cellulose, 3-aminopropyl triethoxysilane and sodium alginate are uniformly mixed, filtered, defoamed and aged to obtain a blended spinning solution.

[0098] The weight ratio of the composite temperature-sensitive coated particles to the deionized water in the functional modification liquid is 1:14.5.

[0099] The weight ratio of the functional modification liquid, the spinning stock solution, sodium carboxymethyl cellulose, 3-aminopropyl triethoxysilane and sodium alginate is 10.6:90:0.35:1:0.45.

[0100] The content of methyl cellulose in the spinning stock solution is 9.2%, the total alkali content is 2.9% and the viscosity is 37 s.

[0101] 5. Spinning forming

[0102] The blended spinning solution is introduced into a spinning machine and sprayed into a coagulation bath at a temperature of 42 DEG C, the spinning speed is controlled at 20 m / 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 950 mm; after the spinning forming, a primary fiber is obtained; the primary fiber is desulfurized, washed, oiled and dried to obtain a viscose large biofiber with a soothing function.

[0103] The content of each component in the coagulation bath is as follows: sulfuric acid 92 g / L, sodium sulfate 195 g / L, zinc sulfate 23 g / L and calcium chloride 10 g / L.

[0104] The embodiment also provides the viscose large biofiber with a soothing function prepared by the method.

[0105] Example 3

[0106] The embodiment provides a preparation method of a viscose large biofiber with a soothing function, and specifically relates to the following steps.

[0107] 1. Preparation of the molecular nest

[0108] The mesoporous silica, 3-aminopropyl triethoxysilane and 65% volume concentration of ethanol aqueous solution were put into a beaker, and ultrasonic dispersion was performed for 30 min. The beaker was heated to 50℃, and the mixture was stirred for 3 h. Then, the beaker was cooled to room temperature to obtain a carrier dispersion liquid. The green tea extract, the Sarcandra glabra extract and the ginkgo leaf extract were put into deionized water, and stirred for 30 min to obtain an active ingredient liquid. The carrier dispersion liquid and the active ingredient liquid were mixed at a weight ratio of 2.3:1, and stirred at room temperature for 6 h. The solid was obtained by centrifugal separation. The solid was transferred into a vacuum drying oven, and dried at 70℃ under a vacuum degree of 0.09 MPa until the weight was constant to obtain a molecular nest (i.e. the mesoporous silica loaded with the plant active ingredients), which was ready for use.

[0109] In the carrier dispersion liquid, the weight ratio of the mesoporous silica, 3-aminopropyl triethoxysilane and ethanol aqueous solution was 12:1.9:75.

[0110] In the active ingredient liquid, the weight ratio of the green tea extract, the Sarcandra glabra extract, the ginkgo leaf extract and deionized water was 7.5:4.7:2.2:130. The particle size of the green tea extract used in the example was 100 mesh, and the extraction ratio was 20:1. The particle size of the Sarcandra glabra extract was 100 mesh, and the extraction ratio was 20:1. The particle size of the ginkgo leaf extract was 100 mesh, and the extraction ratio was 20:1.

[0111] 2. Preparation of modified gel

[0112] The N-vinyl caprolactam NVCL, N-hydroxyethyl acrylamide HEAA, acrylic acid AAC, N,N-methylene bisacrylamide MBA, sodium dodecyl sulfate SDS and sodium bicarbonate were put into a reaction kettle containing deionized water. The air in the reaction kettle was completely replaced by nitrogen. The mixture was stirred for 30 min under the protection of nitrogen atmosphere. Then, the mixture was heated to 70℃ at a heating rate of 0.8℃ / min under stirring. After stirring at 70℃ for 40 min, a 1.3wt% potassium persulfate aqueous solution was continuously added. After reaction at 70℃ for 7 h, the reaction mixture was cooled to room temperature to obtain a reaction product. The reaction product was transferred into a dialysis bag with a molecular weight cut-off of 12-14 KDa. Dialysis was performed for 5 d (water was changed every 8 h). After dialysis, the dialysis bag was freeze-dried to obtain a modified gel, which was ready for use. The lowest critical solution temperature LCST of the modified gel prepared in the example was 34.6℃.

[0113] In the example, the weight ratio of the N-vinyl caprolactam NVCL, N-hydroxyethyl acrylamide HEAA, acrylic acid AAC, N,N-methylene bisacrylamide MBA, sodium dodecyl sulfate SDS, sodium bicarbonate and deionized water was 5.1:1.15:0.31:0.07:0.09:0.16:400.

[0114] The volume ratio of the potassium persulfate aqueous solution to the deionized water is 1:55.

[0115] 3. Coating molding

[0116] A predetermined amount of deionized water was introduced into the reaction kettle and cooled to 8℃, and then the modified gel was added, stirred at 150 rpm for 50 min, and then the molecular nest was continuously added, and the temperature was raised to 26℃ at a temperature raising rate of 0.3℃ / min, and then the temperature was raised to 38℃ at a temperature raising rate of 0.6℃ / min, and after 40 min of temperature maintaining and stirring, the solid product was separated, washed with deionized water at a temperature of 38℃, and then freeze-dried to obtain the composite temperature-sensitive coated particles.

[0117] The weight ratio of the modified gel to the deionized water is 1:40.

[0118] The weight ratio of the modified gel to the molecular nest is 5:1.

[0119] 4. Preparation of a spinning solution

[0120] The composite temperature-sensitive coated particles were added into deionized water at a temperature of 38℃, and stirred for 15 min to obtain a functional modification liquid, and then the functional modification liquid, the spinning stock solution, sodium carboxymethyl cellulose, 3-aminopropyl triethoxysilane and sodium alginate were uniformly mixed, filtered, and then deaerated and aged to obtain the blended spinning solution.

[0121] The weight ratio of the composite temperature-sensitive coated particles to the deionized water in the functional modification liquid is 1:15.

[0122] The weight ratio of the functional modification liquid, the spinning stock solution, sodium carboxymethyl cellulose, 3-aminopropyl triethoxysilane and sodium alginate is 11:92:0.4:1.1:0.5.

[0123] The content of methyl cellulose in the spinning stock solution is 9.2%, the total alkali content is 2.9%, and the viscosity is 37 s.

[0124] 5. Spinning molding

[0125] The blended spinning solution was introduced into a spinning machine, sprayed into a coagulation bath at a temperature of 43℃, and the spinning speed was controlled to be 20 m / min, the spinning nozzle draft ratio was 6%, the inter-disk draft ratio was 13%, the three-bath draft ratio was 33%, the four-bath draft ratio was 12%, and the immersion length was 950 mm; after the spinning molding, the primary fiber was obtained; and the primary fiber was subjected to desulfurization, washing, oiling and drying to obtain the viscose large biofiber with a soothing function.

[0126] The content of each component in the coagulation bath is: sulfuric acid 92 g / L, sodium sulfate 195 g / L, zinc sulfate 23 g / L, and calcium chloride 10 g / L.

[0127] The embodiment also provides the viscose large bio-fiber with the soothing function prepared by the method.

[0128] Comparative Example 1

[0129] The comparative example adopts the technical solution of the embodiment 2, and the change is that: the preparation of the modified gel is omitted, the step of coating is omitted, and the molecular nest prepared in the step of preparing the molecular nest (i.e. the mesoporous silica loaded with the plant active ingredient) is directly used in the step of preparing the spinning solution; specifically, the molecular nest is put into deionized water to prepare a function-modified liquid, and the weight ratio of the molecular nest to the deionized water in the function-modified liquid is controlled to be 1:28.

[0130] Comparative Example 2

[0131] The comparative example adopts the technical solution of the embodiment 2, and the change is that: 1) in the step of preparing the molecular nest, the addition of 3-aminopropyl triethoxysilane is omitted; 2) in the step of preparing the modified gel, the addition of N-hydroxyethyl acrylamide HEAA and acrylic acid AAC is omitted.

[0132] Among them, the lowest critical solution temperature LCST of the modified gel prepared in the comparative example 2 is 31.2℃.

[0133] The release performance of the plant active ingredients (green tea extract, Sarcandra glabra extract, ginkgo leaf extract) of the viscose large bio-fiber in the embodiments 1-3 and the comparative examples 1-2 under the temperature condition of 22℃ is detected, specifically: 5g of the viscose large bio-fiber in the embodiments 1-3 and the comparative examples 1-2 is respectively placed in a dialysis bag with a molecular weight cut-off of 1KDa, then immersed into a first absorption liquid 250mL with a temperature of 22℃, and oscillated in a dark condition at 100rpm in a water bath, and the content of catechin, rosmarinic acid and ginkgolide in the first absorption liquid is detected and recorded at 2h and 48h respectively; then the viscose large bio-fiber in the dialysis bag is taken out, cut and placed in a second absorption liquid 250mL with a temperature of 22℃, and ultrasonic broken extraction is carried out for 60min, and the content of catechin, rosmarinic acid and ginkgolide in the second absorption liquid is detected and recorded; the release rate of the representative active ingredients catechin, rosmarinic acid and ginkgolide at 2h and 48h is calculated respectively.

[0134] Among them, the first absorption liquid and the second absorption liquid have the same composition, which is a PBS buffer with a pH of 7.4 as a basic solvent, and contains 10% by weight of ethanol, 0.1% by weight of Tween-80, and 0.1mmol / L of ascorbic acid.

[0135] The release rate of catechin at 2h or 48h is calculated as follows: [catechin content in the first absorption liquid at 2h or 48h / (catechin content in the first absorption liquid at 48h + catechin content in the second absorption liquid after ultrasonic crushing extraction)] x 100%.

[0136] The release rate of rosmarinic acid at 2h or 48h is calculated as follows: [rosmarinic acid content in the first absorption liquid at 2h or 48h / (rosmarinic acid content in the first absorption liquid at 48h + rosmarinic acid content in the second absorption liquid after ultrasonic crushing extraction)] x 100%.

[0137] The release rate of ginkgolide at 2h or 48h is calculated as follows: [ginkgolide content in the first absorption liquid at 2h or 48h / (ginkgolide content in the first absorption liquid at 48h + ginkgolide content in the second absorption liquid after ultrasonic crushing extraction)] x 100%.

[0138] The specific results are shown in the following table:

[0139]

[0140] Further, the release performance of the plant active ingredients (green tea extract, Sarcandra glabra extract, ginkgo leaf extract) of the viscose large biological fibers of Examples 1-3 and Comparative Examples 1-2 at a temperature of 36℃ was detected, and the specific method was the same as the release performance at a temperature of 22℃ as described above, except that the temperature of the first absorption liquid and the second absorption liquid was maintained at 36℃. The release rates of representative active ingredients catechin, rosmarinic acid and ginkgolide at 2h and 48h are shown in the following table:

[0141]

[0142] It can be seen that the preparation method of the viscose large bio-fiber with soothing function has the following steps: in the preparation of the molecular nest step, 3-aminopropyl triethoxysilane is used to treat mesoporous silica to introduce amino groups, and a carrier dispersion liquid is prepared; green tea extract, coralline extract and ginkgo leaf extract are dispersed in deionized water to prepare an active ingredient liquid; then the two are mixed and loaded to prepare mesoporous silica loaded with plant active ingredients (i.e. molecular nest). In the preparation of the modified gel step, N-vinyl caprolactam NVCL is used as the main temperature-sensitive material to copolymerize with N-hydroxyethyl acrylamide HEAA and acrylic acid AAC in the presence of an initiator and a crosslinking agent, so as to match the low critical solution temperature LCST of the temperature-sensitive gel with the temperature range of the allergic skin area, improve the subsequent coating performance of the molecular nest, and introduce carboxyl groups to further improve the binding performance of the modified gel, the molecular nest and the plant active ingredients loaded thereon. In the coating forming step, the gel molecular chain is fully stretched in a low-temperature deionized water environment of 5-8℃, and then the molecular nest is put in, which is uniformly coated on the outer surface of the molecular nest while slowly heating, and then further heated to above the low critical solution temperature LCST of the modified gel, so that the modified gel shrinks on the outer surface of the molecular nest, the coating forming is completed, and the composite temperature-sensitive coated particles are prepared. Then in the preparation of the spinning liquid step, the composite temperature-sensitive coated particles are used to prepare a functional modified liquid, which is mixed with the spinning stock solution and its auxiliary materials to prepare a blended spinning liquid; the blended spinning liquid is spun to prepare the viscose large bio-fiber with soothing function.

[0143] The plant active ingredients (such as catechin, rosmarinic acid, ginkolide, etc.) in the viscose macro-biofibers with soothing function of Examples 1-3 are significantly higher in release rate at 2h and 48h under the temperature condition of 22℃ which is lower than the critical solution temperature LCST than that under the temperature condition of 36℃ which is slightly higher than the temperature of the allergic skin area, the fabric made of the same can realize the large-dose release of the plant active ingredients in a short time through temperature regulation, and then realize the emergency repair function; then in the process of long-time contact with the skin, the fabric made of the same is gradually warmed up to the skin temperature, the release amount of the plant active ingredients in the fiber gradually decreases and tends to be stable, and changes to long-time small-dose sustained release, and then realizes the long-acting soothing function. After omitting the modification gel and the coating forming step in Comparative Example 1, the combination performance of the carrier and the plant active ingredients in the molecular nest is poor due to the lack of the coating and controlled release effect of the modification gel on the molecular nest, the release rate is greatly affected by the temperature, and the release rate is significantly higher than that of Example 2. After omitting 3-aminopropyl triethoxysilane in the preparation of the molecular nest step and N-hydroxyethyl acrylamide HEAA and acrylic acid AAC in the preparation of the modification gel step in Comparative Example 2, on the one hand, the low critical solution temperature LCST of the gel cannot be effectively improved, and on the other hand, the combination performance with the plant active ingredients is reduced, leading to the increase of the release rate of the plant active ingredients in a short time, and in the temperature environment of 36℃, the coating of the gel on the molecular nest may be damaged due to excessive shrinkage, leading to the loss of control of the release of the plant active ingredients, and the release rate is significantly higher than that of the long-acting stable and controllable release of Example 2.

[0144] Further, the skin soothing test was carried out on the viscose macro-biofibers of Example 2 and Comparative Examples 1-2 respectively, specifically: the test fabrics were made by pure spinning of the viscose macro-biofibers of Example 2 and Comparative Examples 1-2 respectively, 20 Balb / c mice were selected as test objects, and randomly divided into 4 groups, and the allergic symptoms of redness and edema with basically the same area were caused on the Balb / c mice by treating them with 2,4-dinitrochlorobenzene with a concentration of 0.5wt%, and then the following operations were carried out on the corresponding groups:

[0145] The test fabric of Example 2 after 10℃ cold storage was applied to the allergic area and completely covered the allergic area on the skin, and the test fabric after 10℃ cold storage was replaced every 8h.

[0146] The test fabric of Example 2 at 36℃ (close to the skin surface temperature of the allergic area) was applied to the allergic area and completely covered the allergic area on the skin, and the test fabric at 36℃ was replaced every 8h.

[0147] The test fabric of Comparative Example 1 after 10℃ cold storage was applied to the allergic area and completely covered the allergic area on the skin, and the test fabric after 10℃ cold storage was replaced every 8h.

[0148] Group 4, the test fabric of Comparative Example 2 after 10°C refrigeration was applied to the allergic area and completely covered the allergic area on the skin, and the test fabric after 10°C refrigeration was replaced every 8h.

[0149] After the test fabric was applied to each group for 24h, the skin surface of each test subject was observed for soothing, and the number of test subjects achieving each soothing effect (significant soothing, moderate soothing, mild soothing, and no soothing) was counted. Significant soothing was a reduction rate of erythema and / or edema area ≥ 90%, moderate soothing was a reduction rate of erythema and / or edema area of 50-90% (including 50%), mild soothing was a reduction rate of erythema and / or edema area of 10-50%, and no soothing was a reduction rate of erythema and / or edema area ≤ 10%.

[0150] The specific results are shown in the following table:

[0151]

[0152] After the test fabric was applied to each group for 48h, the skin surface of each test subject was observed for soothing, and the number of test subjects achieving each soothing effect (significant soothing, moderate soothing, mild soothing, and no soothing) was counted. The specific results are shown in the following table:

[0153]

[0154] It can be seen that the test fabric made of the soothing viscose large bio-fiber of Example 2 was applied to the allergic area, and after the test fabric was treated by 10°C refrigeration, it not only played a cold compress calming effect on the allergic skin, but also achieved a large dose release of plant active ingredients in a short time, thereby achieving an emergency repair function. Compared with the test fabric of Example 2 at 36°C applied to the allergic area, it achieved an ideal rapid soothing effect, and its soothing effect at 24h and 48h was significantly better. The test fabric made of viscose large bio-fiber of Comparative Example 1 applied to the allergic area, due to the influence of the viscose original solution solvent environment, the coagulation bath solvent environment, and the process conditions during fiber preparation, the combination effect of the fiber and the plant active ingredients was not ideal, and its soothing effect on the allergic area was significantly worse than that of Example 2. The test fabric made of viscose large bio-fiber of Comparative Example 2 applied to the allergic area, after omitting the related technical means during fiber preparation, the combination performance of the fiber and the plant active ingredients was reduced, and stable controlled release of the plant active ingredients contained therein could not be achieved, and its soothing effect on the allergic area was reduced to some extent compared with Example 2.

[0155] Further, the antibacterial performance, antioxidant performance, cytotoxicity grade of the viscose macro-biofibers of Examples 1-3 and Comparative Examples 1-2 are respectively tested. The antibacterial performance is tested according to the relevant provisions in GB / T20944.3-2008 “Evaluation of antibacterial properties of textiles Part 3: Shake method”; the cytotoxicity grade is tested according to the relevant provisions in MTT method in GB / T16886.5-2017 “Biological evaluation of medical devices Part 5: In vitro cytotoxicity tests”; and the antioxidant performance is tested by DPPH method and ABTS method respectively.

[0156] The specific method of the DPPH method is as follows: 1,1-diphenyl-2-trinitrobenzene hydrazine DPPH 2.5 mg is dissolved in anhydrous ethanol and diluted to 100 mL to prepare a DPPH ethanol solution with a concentration of 25.0 mg / L. 2.0 g of viscose macro-biofibers of Examples 1-3 and Comparative Examples 1-2 are respectively put into an ultrasonic extraction bottle containing 50 mL of ethanol solution (volume concentration 50%) and soaked at 25°C for 24 h, and then ultrasonic extraction is performed for 20 min. Then, the filtrate is obtained by filtration, transferred to a rotary evaporator, and controlled at a rotary evaporation temperature of 55°C and a rotary evaporation vacuum degree of 0.085 MPa. When the rotary evaporation of the filtrate is stopped at 2 mL, it is diluted with an ethanol solution (volume concentration 50%) to 4 mL as a test solution. Finally, 1 mL of the test solution is added to 2 mL of the DPPH ethanol solution, mixed uniformly, and placed in the dark for 10 min. The absorbance at a wavelength of 517 nm is detected by a spectrophotometer, and the DPPH· free radical scavenging rate is calculated.

[0157] The specific method of the ABTS method is as follows: 2,2-azino-bis(3-ethyl-benzothiazoline-6-sulfonic acid) diammonium salt ABTS 200.0 mg and potassium persulfate 34.4 mg are dissolved in 50.0 mL of deionized water, and after being placed in the dark at room temperature for 24 h, an ABTS mother liquor is obtained. A certain amount of the ABTS mother liquor is diluted with an ethanol solution with a volume concentration of 95% to an absorbance value of 0.70 at a wavelength of 734 nm to obtain an ABTS diluent. Then, a test solution is prepared (the specific method of preparing the test solution is the same as that in the DPPH· free radical scavenging rate detection method described above). Finally, 0.5 mL of the test solution is added to 5 mL of the ABTS diluent, mixed uniformly, and placed in the dark for 10 min. The absorbance at a wavelength of 734 nm is detected by a spectrophotometer, and the ABTS· free radical scavenging rate is calculated. +

[0158] The specific results are shown in the following table:

[0159]

[0160] ​The plant active ingredients contained in the viscose large biofibers with soothing function of embodiments 1-3 can achieve effective antibacterial and antioxidant effects, can soothe the skin allergic area while inhibiting the growth of bacteria in the skin allergic area; at the same time, the antioxidant function can also remove excess free radicals generated by skin allergy, reduce skin oxidative stress, and assist in repairing the skin barrier function; and the cytotoxicity grade of the viscose large biofibers is all 0, the irritability to allergic skin is low, and it is effectively applicable to skin soothing.

[0161] Further, the dry breaking strength, wet breaking strength, whiteness and defects of the viscose large biofibers of embodiments 1-3 and comparative examples 1-2 were detected respectively. The whiteness was detected by DatacolorSF600 colorimeter under the conditions of temperature 20℃ and relative humidity 65%. The specific results are shown in the following table:

[0162]

[0163] In the preparation of the viscose large biofibers with soothing function of embodiments 1-3, the composite temperature-sensitive coated particles used can further improve the mechanical properties of the viscose large biofibers while imparting soothing function to the fibers, and have no adverse effect on whiteness, and low fiber defect content.

[0164] Unless otherwise specified, the percentages used in the present application are mass percentages.

[0165] Finally, it should be noted that: the above only describes the preferred embodiments of the present application and is not intended to limit the present application, although the present application has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions recorded in the foregoing embodiments, or make equivalent replacement for some technical features. Any modification, equivalent replacement, improvement, etc. within the spirit and principles of the present application shall be included in the protection scope of the present application.

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 comprises the following steps: adding the modified gel into deionized water at 5-8°C and dispersing the gel uniformly; then adding the molecular nest; heating the gel to 24-26°C at a heating rate of 0.2-0.3°C / min with stirring; then heating the gel to 37-38°C at a heating rate of 0.5-0.6°C / min with stirring; and separating the gel to obtain a solid matter after heat preservation and stirring. The solid matter is then washed and dried to obtain the composite temperature-sensitive coated particles. In the overmolding process, the weight ratio of the modified gel to deionized water is 1:35-40; The weight ratio of modified gel to molecular nest is 4.5-5:1; 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 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.

6. The method for preparing the viscose biofiber with soothing function according to claim 5, 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.

7. The method for preparing the viscose biofiber with soothing function according to claim 5, 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.

8. A viscose biofiber with soothing function, characterized in that: The method is prepared according to any one of claims 1 to 7.

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