Method for preparing degradable lyocell fiber having artemisia argyi microcapsule slow-release function

Abstract

The present invention belongs to the technical field of the preparation of artificial fibers. Disclosed is a method for preparing a degradable lyocell fiber having an Artemisia argyi microcapsule slow-release function. The method comprises the steps of: preparing raw materials used for the preparation of Artemisia argyi essential oil microcapsules; preparing Artemisia argyi essential oil microcapsules; preparing a nanoporous material; preparing an Artemisia argyi essential oil microcapsule nanoporous composite material; and putting the Artemisia argyi essential oil microcapsule nanoporous composite material, an aqueous solution of N-methylmorpholine-N-oxide and cotton pulp into a reaction kettle, performing vacuum stirring to obtain a spinning solution, then introducing the spinning solution into a screw extruder, extruding same out into a metering pump by means of the screw extruder, then making same enter a spinning assembly of a spinning box from the metering pump, discharging same from a spinneret plate of the spinning assembly to obtain a fiber melt, sequentially subjecting the fiber melt to cooling, washing with alcohol, washing with water and drying, then subjecting same to oiling, re-drying and a corona treatment, and finally performing setting, so as to obtain a finished product. The method has the advantages whereby porous structures can be formed inside and outside the fiber, and the good effect of slow release of Artemisia argyi microcapsules can be maintained; and the fiber has yang warming and anti-microbial effects.

Description

Preparation method of degradable lyocell fiber with mugwort microcapsule sustained-release function Technical Field

[0001] The invention belongs to the technical field of artificial fiber preparation, and particularly relates to a method for preparing degradable lyocell fiber with mugwort microcapsule sustained-release function. Background Art

[0002] Because the particle size of mugwort microcapsules is typically less than 1 micron, they are often referred to as mugwort microcapsules, also known as mugwort essential oil microcapsules. Mugwort essential oil is a plant essential oil, a natural substance extracted from the herbaceous plant mugwort. Capsules with a particle size of 10-1000 nm are called nano-sized mugwort essential oil microcapsules. The content of alcohols, alkenes, aldehydes, ketones, esters, and other compounds (also known as compounds) in mugwort essential oil extracted from different origins varies. By incorporating mugwort essential oil into yarn and fabrics through technical means, it can impart antibacterial, mildew-proofing, and health-promoting properties to fabrics such as lyocell. Due to its inherent volatility, mugwort essential oil is currently commonly used in a core-shell encapsulated form, combining the essential oil with a shell polymer to form mugwort microcapsules. These microcapsules are then applied to the yarn through post-finishing to achieve sustained release of the essential oil.

[0003] Lyocell fiber, made from pulp from renewable plant fibers such as bamboo and wood, is considered one of the most valuable products in the history of man-made fibers over the past half century, combining the excellent properties of both natural and synthetic fibers. Lyocell is considered environmentally friendly and biodegradable because the production process involves no chemical reactions and uses non-toxic solvents.

[0004] With the continuous improvement of people's living standards and the growing awareness of green, healthy, and environmental protection, the demand for green, environmentally friendly, and natural textiles is growing. Typical, but not limited, examples of textile fabrics with health benefits currently available on the market include antibacterial bamboo fiber, biodegradable polylactic acid (PLA) fiber, and skin-friendly soy protein fiber. Lyocell fiber, hailed as a highly sought-after green fiber of the 21st century, is a regenerated cellulose fiber produced through a wet spinning process (abbreviated as "wet spinning") using N-methylmorpholine-N-oxide (NMMO, also written as NMO) as a solvent. It is naturally degradable upon disposal, without impacting soil, water, or air. Furthermore, since the amine oxide solvent used in the spinning process is recyclable at a rate of 99.5%, it not only saves resources and reduces costs, but also possesses extremely low toxicity, eliminating any environmental impact.

[0005] Plant-based functional fibers based on lyocell have been a focus of recent attention in the textile industry. Plant-based cellulose fibers, such as isatis root, mugwort, and ginger, are already available on the market. These fibers, produced by blending plant ingredients into a viscose base or by adding additives during the post-printing and dyeing finishing process, offer various functional properties, such as deodorizing, antibacterial, and thermoregulating properties, and are highly sought after by consumers. However, these fibers also have numerous drawbacks. For example, functional fibers made by adding ground plant ingredients to cellulose fibers struggle to achieve the desired slow release of their active ingredients during use. For example, functional fibers made by encapsulating polymer microcapsules or adding porous polymers to cellulose fibers often fail to meet environmentally friendly and biodegradable requirements. Furthermore, additives added to cellulose fibers often rely on the attachment of these additives, making it difficult to maintain their desired functionality over time. As clothing made from these fibers is worn longer or more frequently, especially with increasing washes, these functional properties gradually diminish or even disappear. Furthermore, since the addition of additives during the fabric finishing process results in significant waste, this approach has gradually fallen out of favor in the industry. Given the shortcomings of the aforementioned prior art, and not limited to the aforementioned, there is a positive interest in exploring how to make Lyocell fibers not only possess the antibacterial and sustained-release properties of mugwort, but also enable the release of mugwort essential oil from the mugwort microcapsules through the porous structure of the fibers through friction and compression during use, and achieve a long-lasting sustained-release effect, even after repeated washings, while maintaining excellent deodorizing, warming, and antibacterial properties. The technical solutions described below were developed in this context. Summary of the Invention

[0006] In view of the shortcomings of the existing technology, the task of the present invention is to provide a method for preparing a degradable lyocell fiber with a sustained-release function of mugwort microcapsules. The degradable lyocell fiber with a sustained-release function of mugwort microcapsules prepared by this method can durably maintain the sustained-release effect of mugwort essential oil and durably maintain good warming and antibacterial functions. After being made into clothing, the functions will not be lost due to the extension of the wearing time, the increase in the number of wearing times and / or the number of washing times. It can also naturally degrade after being discarded, thereby reflecting a good green environmental protection effect.

[0007] The task of the present invention is accomplished by a method for preparing a degradable lyocell fiber with a sustained-release function of wormwood microcapsules, comprising the following steps:

[0008] A) preparing raw materials for preparing wormwood essential oil microcapsules, wherein the wormwood essential oil microcapsules include a core material and a wall material, wherein the core material is a mixture of wormwood essential oil and tea tree essential oil mixed in a mass ratio, and the wall material is a mixture of hydroxypropyl cellulose and porous starch mixed in a mass ratio, to obtain raw materials for preparing wormwood essential oil microcapsules;

[0009] B) preparing wormwood essential oil microcapsules, first adding the mixture obtained by step A) and the mixture to a dispersed emulsion and mixing, and controlling the mass percent concentration of the mixture in the dispersed emulsion and the mass percent concentration of the mixture in the dispersed emulsion to obtain a liquid to be sprayed, then spraying the liquid to be sprayed into a medium in a spraying manner, so that the solvent in the liquid to be sprayed is precipitated from the mixture, and controlling the temperature of the spraying device to obtain wormwood essential oil microcapsules;

[0010] C) preparing a nanoporous material by first adding a mixture of far-infrared ceramic powder and diatomaceous earth to a grinding device, grinding it with an etchant added to the grinding device, controlling the mass ratio of the far-infrared ceramic powder to the diatomaceous earth, the mass ratio of the mixture of the far-infrared ceramic powder and diatomaceous earth to the etchant, and controlling the grinding speed and grinding time of the grinding device to obtain a grind, filtering the grind through a filter screen, neutralizing the grind with acid, and rinsing the grind, and then filtering the grind through a filter membrane to obtain a filtered aqueous solution, filtering the filtered aqueous solution again to obtain a solid mixture, and finally introducing the solid mixture into a dryer for drying, while controlling the drying temperature and drying time of the dryer to obtain the nanoporous material;

[0011] D) preparing wormwood essential oil microcapsule nanoporous composite material, first by step B) the wormwood essential oil microcapsules obtained and by step C) the nanoporous material obtained are introduced into a stirred vessel filled with a dispersant aqueous solution and equipped with a stirrer and stir evenly, and control the mass percentage of the wormwood essential oil microcapsules in the dispersant aqueous solution and the mass percentage of the nanoporous material in the dispersant aqueous solution, control the stirring speed and stirring time of the stirrer of the stirred vessel, proceed to drying in a drying machine, and control the drying temperature and drying time of the drying machine, exit the drying machine, and obtain the wormwood essential oil microcapsule nanoporous composite material;

[0012] E) preparing a finished product, first, the wormwood essential oil microcapsule nanoporous composite material obtained in step D), an N-methylmorpholine-N-oxide (NMMO) aqueous solution, and cotton pulp are added to a reactor in a mass ratio of 3:11-12:1-3, and vacuum stirred while controlling the vacuum stirring time and the temperature of the reactor to obtain a spinning solution, and then the spinning solution is introduced into a screw extruder, extruded by the screw extruder to a metering pump, and then from the metering pump into a spinning assembly of a spinning box and out of a spinneret of the spinning assembly to obtain a fiber melt, and the fiber melt is sequentially cooled, washed with alcohol, washed with water, and dried, and then oiled, dried again and corona treated, and finally shaped while controlling the fiber tension and the shaping temperature during the shaping process to obtain a finished product, i.e., a biodegradable lyocell fiber with a sustained-release function of wormwood microcapsules and a flavin content of 17.5-19.7 mg / g.

[0013] In a specific embodiment of the present invention, the wormwood essential oil and tea tree essential oil mixed in step A) are mixed in a mass ratio of 3-6:1; the hydroxypropyl cellulose and porous starch mixed in a mass ratio are mixed in a mass ratio of 2-3:1; the mass percentage of isoeupretinoic acid in the wormwood essential oil is 3-3.5%; and the porous starch is an enzymatically prepared porous starch.

[0014] In another specific embodiment of the present invention, the step B) of controlling the mass percentage concentration of the mixture in the dispersed emulsion is to control the mass percentage concentration to 3-5%; the step of controlling the mass percentage concentration of the mixture in the dispersed emulsion is to control the mass percentage concentration to 3.5-6%; the medium is water; and the step of controlling the temperature of the spray device is to control the temperature of the spray device to 50-70°C.

[0015] In another specific embodiment of the present invention, the dispersed emulsion is composed of the following raw materials in the following proportions by mass: 1-2% nonionic surfactant and / or preservative, 4-7% solvent, and the balance water.

[0016] In another specific embodiment of the present invention, the nonionic surfactant is Tween and Span; the preservative is chitosan; and the solvent is a mixture of ethylene glycol having a mass percentage concentration greater than 99% and glycerol having a mass percentage concentration greater than 99.5% in a volume ratio of 1:1.

[0017] In another specific embodiment of the present invention, the mass ratio of the far-infrared ceramic powder to the diatomaceous earth in step C) is controlled to be 1:1.5-4; the mass ratio of the mixture of the far-infrared ceramic powder and the diatomaceous earth to the etchant is controlled to be 70-120:8-11; the grinding speed and grinding time of the grinding device are controlled to be 500-1100 rpm and 20-80 min; the mesh size of the filter used for filtration is 200 mesh; the acid neutralization is carried out with HCl. Neutralized to pH 7-8; the soaking is to soak the weakly alkaline material obtained after filtering through the filter and neutralizing with acid for 5-10 minutes at a volume ratio of 1:10-20 to water, and the aqueous solution obtained after soaking is filtered using a filter membrane, the filter membrane is a nylon 66 filter membrane with a pore size of 0.5 μm, and the re-filtration of the filtered aqueous solution is to filter the filtered aqueous solution using a filter membrane with a pore size of 0.1 μm; the drying temperature and drying time of the drying machine are controlled to be 40-60°C and 60-120 minutes respectively, and the drying machine is a drum dryer.

[0018] In a more specific embodiment of the present invention, the etchant is a mixture of a dispersant and caustic soda in a mass ratio of 8.5-10:0.5-1, and the dispersant is ethylene glycol with a mass percentage concentration greater than 99%.

[0019] In a further specific embodiment of the present invention, the step D) of controlling the mass percentage of the wormwood essential oil microcapsules in the dispersant aqueous solution is to control the mass percentage to 10-20%, and the controlling the mass percentage of the nanoporous material in the dispersant aqueous solution is to control the mass percentage to 20-40%; the controlling the stirring speed and stirring time of the stirrer is to control the stirring speed to 1000-2000 rpm and the stirring time to 30-40 min; the controlling the drying temperature and drying time of the dryer is to control the drying temperature and drying time of the dryer to 50-70 ° C and 60-120 min, respectively, and the dryer is a drum dryer.

[0020] In yet another specific embodiment of the present invention, the dispersant aqueous solution is a Tween aqueous solution with a mass percentage concentration of 1-2%.

[0021] In yet another specific embodiment of the present invention, the mass percentage concentration of the N-methylmorpholine-N-oxide aqueous solution in step E) is 85-90%; the vacuum stirring time is controlled to be 30-90 minutes; the temperature of the reactor is controlled to be 100-110°C; the corona treatment is performed using a generator with a voltage of 1000-2000 volts and a power of 5-20W; the tension of the fiber during the setting process is controlled to be 5-50N, and the setting temperature is controlled to be 120-130°C; and the content of isoeutaxanthin in the biodegradable lyocell fiber with sustained-release function of wormwood microcapsules is 10-20 mg / g.

[0022] The technical effect of the technical solution provided by the present invention is that: since the mixture and the mixture of step A are sequentially used as the core material and wall material of the mugwort essential oil microcapsules, the mixture and the mixture are made into mugwort essential oil microcapsules in step B, the nanoporous material is made in step C, and then the mugwort essential oil microcapsule nanoporous composite material is made in step D, and finally the mugwort essential oil microcapsule nanoporous composite material, NMMO and cotton pulp are made into a spinning solution and spun into a degradable lyocell fiber with mugwort microcapsule sustained-release function in step E, a porous structure can be formed inside and outside the fiber, so that the excellent effect of the slow release of the mugwort microcapsules can be maintained for a long time; since mugwort is a purely yang substance and has a good effect on eliminating some viruses and bacteria, the fiber prepared by the present invention has a warming and antibacterial effect after being made into fabrics and clothing. DETAILED DESCRIPTION Example 1:

[0023] A) preparing a raw material for preparing wormwood essential oil microcapsules, the wormwood essential oil microcapsules comprising a core material and a wall material, the core material being a mixture of wormwood essential oil containing 3.5% isoeutaxanthin and tea tree essential oil in a mass ratio of 3:1, preferably mixed with a mixing device, and the wall material being a mixture of hydroxypropyl cellulose and porous starch prepared by an enzymatic method in a mass ratio of 2:1, preferably mixed with a mixing device, to obtain the raw material for preparing wormwood essential oil microcapsules;

[0024] B) preparing wormwood essential oil microcapsules, first adding the mixture obtained by step A) and the mixture to the dispersed emulsion and mixing, and controlling the mass percentage concentration of the mixture in the dispersed emulsion to be 5%, and controlling the mass percentage concentration of the mixture in the dispersed emulsion to be 3.5%, the dispersed emulsion described in this step is composed of the following raw materials in percentage ratio: Tween 1%, a mixture of ethylene glycol having a mass percentage concentration greater than 99% and glycerol having a mass percentage concentration greater than 99.5% in a volume ratio of 1:1 7%, and the remainder being water (using purified water) to obtain a spray liquid, and then spraying the aforementioned spray liquid into a medium serving as water in a spraying manner, so that the solvent (i.e., a mixture of ethylene glycol having a mass percentage concentration greater than 99% and glycerol having a mass percentage concentration greater than 99.5% in a volume ratio of 1:1) is precipitated from the mixture, and the temperature of the aforementioned spray device is controlled to 70° C. to obtain wormwood essential oil microcapsules;

[0025] C) preparing a nanoporous material, first adding a mixture of far-infrared ceramic powder obtained from a commercial channel and diatomaceous earth at a mass ratio of 1:3 to a grinding device, and grinding together with an etchant added to the grinding device, controlling the mass ratio of the far-infrared ceramic powder and diatomaceous earth mixture to the etchant to be 120:8, and controlling the grinding speed and grinding time of the grinding device to be 500 rpm and 80 minutes, respectively, to obtain a grind material, which is sequentially filtered through a 200-mesh filter (i.e., first through a filter), and then neutralizing the filtered material through the 200-mesh filter with HCl (hydrochloric acid) to a pH of 7-8 to obtain a weakly alkaline material, and then the weakly alkaline material is further filtered through a 200-mesh filter. The alkaline material is soaked with water at a volume ratio of 1:10 for 10 minutes. After the soaking, an aqueous solution is obtained, which is filtered through a nylon 66 filter membrane with a pore size of 0.5 μm to obtain a filtered aqueous solution. The filtered aqueous solution is filtered again through a filter membrane with a pore size of 0.1 μm to obtain a solid mixture. Finally, the solid mixture is introduced into a dryer for drying to obtain a nanoporous material. The drying temperature and drying time of the dryer in this step are controlled to 40° C. and 120 minutes, respectively. The dryer is a drum dryer. The etchant in this step is a mixture of ethylene glycol with a mass percentage concentration greater than 99% and caustic soda at a mass ratio of 8.5:1.

[0026] D) prepare wormwood essential oil microcapsule nanoporous composite material, first by step B) wormwood essential oil microcapsules obtained and by step C) nanoporous material obtained are introduced into a stirred vessel filled with a dispersant aqueous solution and equipped with a stirrer to stir evenly, go out of the stirred vessel and proceed to drying in a drying machine, go out of the drying machine, obtain the wormwood essential oil microcapsule nanoporous composite material, the mass percent control of the wormwood essential oil microcapsules in the described dispersant aqueous solution is 10%, the mass percent control of the nanoporous material in the dispersant aqueous solution is 30%, the stirring speed and the stirring time of the described stirred vessel are respectively controlled to 1000rpm and 40min, the baking temperature and the baking time of the described drying machine are respectively controlled to 50 DEG C and 120min, the described drying machine is a drum dryer, and the described dispersant aqueous solution is a Tween aqueous solution with a mass percent concentration of 1%;

[0027] E) preparing a finished product, first, the wormwood essential oil microcapsule nanoporous composite material obtained in step D), an 85% by mass concentration of N-methylmorpholine-N-oxide (NMMO (also abbreviated as NMO) aqueous solution, and cotton pulp in a mass ratio of 3:12:1 are placed in a reactor and vacuum stirred, the vacuum stirring time and the temperature of the reactor are controlled at 90 minutes and 100° C., respectively, to obtain a spinning solution, and then the spinning solution is introduced into a screw extruder, extruded by the screw extruder to a metering pump, and then discharged from the metering pump. The fiber melt enters the spinning assembly of the spinning box and exits the spinneret of the spinning assembly of the spinning box to obtain a fiber melt. The fiber melt is sequentially cooled by side blowing or ring blowing, washed with alcohol, washed with water, oiled and dried again, and then subjected to corona treatment. The voltage used for the corona treatment is 2000 volts and the power is 5W. Finally, the fiber is shaped at a temperature of 120°C, and the fiber tension during the shaping process is controlled to be 50N, thereby obtaining a biodegradable lyocell fiber with a wormwood microcapsule sustained-release function and a flavonoid content of 19.7 mg / g. Example 2:

[0028] A) preparing a raw material for preparing wormwood essential oil microcapsules, the wormwood essential oil microcapsules comprising a core material and a wall material, the core material being a mixture of wormwood essential oil having a mass percentage content of 3% isoeupretinoic acid and tea tree essential oil in a mass ratio of 6:1, preferably mixed with a mixing device, and the wall material being a mixture of hydroxypropyl cellulose and porous starch prepared by an enzymatic method in a mass ratio of 2.5:1, preferably mixed with a mixing device, to obtain the raw material for preparing wormwood essential oil microcapsules;

[0029] B) preparing wormwood essential oil microcapsules, first adding the mixture obtained in step A) and the mixture to the dispersed emulsion and mixing, and controlling the mass percentage concentration of the mixture in the dispersed emulsion to be 4%, and controlling the mass percentage concentration of the mixture in the dispersed emulsion to be 5%, the dispersed emulsion described in this step is composed of the following raw materials in percentage ratio: 0.75% Span, 0.75% Tween, 6% of a mixture of ethylene glycol having a mass percentage concentration greater than 99% and glycerol having a mass percentage concentration greater than 99.5% in a volume ratio of 1:1, and the remainder being water (using purified water) to obtain a spray liquid, and then spraying the aforementioned spray liquid into a medium consisting of water to allow the solvent (i.e., a mixture of ethylene glycol having a mass percentage concentration greater than 99% and glycerol having a mass percentage concentration greater than 99.5% in a volume ratio of 1:1) to precipitate from the mixture, and controlling the temperature of the aforementioned spray device to be 50° C. to obtain wormwood essential oil microcapsules;

[0030] C) preparing a nanoporous material, first adding a mixture of far-infrared ceramic powder obtained from a commercial channel and diatomaceous earth at a mass ratio of 1:1.5 to a grinding device, and grinding together with an etchant added to the grinding device, wherein the mass ratio of the far-infrared ceramic powder and diatomaceous earth mixture to the etchant is controlled to be 70:11, and the grinding speed and grinding time of the grinding device are controlled to be 750 rpm and 65 minutes, respectively, to obtain a grind. The grind is sequentially filtered through a 200-mesh filter (i.e., first through a filter), and then the filtered material after the 200-mesh filter is neutralized with HCl (hydrochloric acid) to a pH of 7-8 to obtain a weakly alkaline material, and then The weakly alkaline material is soaked with water at a volume ratio of 1:20 for 7 minutes, and an aqueous solution is obtained after the soaking. The aqueous solution is filtered through a nylon 66 filter membrane with a pore size of 0.5 μm to obtain a filtered aqueous solution. The filtered aqueous solution is filtered again through a filter membrane with a pore size of 0.1 μm to obtain a solid mixture. Finally, the solid mixture is introduced into a dryer for drying to obtain a nanoporous material. The drying temperature and drying time of the dryer in this step are controlled to 60° C. and 60 minutes, respectively. The dryer is a drum dryer. The etchant in this step is a mixture of ethylene glycol with a mass percentage concentration greater than 99% and caustic soda in a mass ratio of 10:0.8;

[0031] D) prepare wormwood essential oil microcapsule nanoporous composite material, first by step B) the wormwood essential oil microcapsules obtained and by step C) the nanoporous material obtained are introduced into a stirred vessel filled with a dispersant aqueous solution and equipped with a stirrer to stir evenly, go out of the stirred vessel and proceed to drying in a drying machine, go out of the drying machine, obtain the wormwood essential oil microcapsule nanoporous composite material, the mass percent control of the wormwood essential oil microcapsules in the described dispersant aqueous solution is 20%, the mass percent control of the nanoporous material in the dispersant aqueous solution is 20%, the stirring speed and the churning time of the described stirred vessel are respectively controlled to 2000rpm and 30min, the baking temperature and the baking time of the described drying machine are respectively controlled to 70 ℃ and 60min, the described drying machine is a drum dryer, and the described dispersant aqueous solution is that the mass percent concentration is 1.4% Tween aqueous solution;

[0032] E) preparing a finished product, first, the wormwood essential oil microcapsule nanoporous composite material obtained in step D), a 90% by mass concentration of N-methylmorpholine-N-oxide (NMMO (also abbreviated as NMO) aqueous solution, and cotton pulp in a mass ratio of 3:11:2 are put into a reactor and vacuum stirred, the vacuum stirring time and the temperature of the reactor are controlled at 75 minutes and 102° C., respectively, to obtain a spinning solution, and then the spinning solution is introduced into a screw extruder, extruded by the screw extruder to a metering pump, and then the metering pump is used to pump the spinning solution. The fiber melt enters the spinning assembly of the spinning box and exits the spinneret of the spinning assembly of the spinning box to obtain a fiber melt. The fiber melt is sequentially cooled by side blowing or ring blowing, washed with alcohol, washed with water, oiled and dried again, and then subjected to corona treatment. The voltage used for the corona treatment is 1000 volts and the power is 20 W. Finally, the fiber is shaped at a temperature of 130°C, and the fiber tension during the shaping process is controlled to be 5N, thereby obtaining a biodegradable lyocell fiber with a wormwood microcapsule sustained-release function and a flavonoid content of 17.5 mg / g. Example 3:

[0033] A) preparing a raw material for preparing wormwood essential oil microcapsules, the wormwood essential oil microcapsules comprising a core material and a wall material, the core material being a mixture of wormwood essential oil containing 3.2% isoeutaxanthin and tea tree essential oil in a mass ratio of 4:1, preferably mixed with a mixing device, and the wall material being a mixture of hydroxypropyl cellulose and porous starch prepared by an enzymatic method in a mass ratio of 3:1, preferably mixed with a mixing device, to obtain the raw material for preparing wormwood essential oil microcapsules;

[0034] B) preparing wormwood essential oil microcapsules, first adding the mixture obtained by step A) and the mixture to the dispersed emulsion and mixing, and controlling the mass percentage concentration of the mixture in the dispersed emulsion to be 3%, controlling the mass percentage concentration of the mixture in the dispersed emulsion to be 6%, the dispersed emulsion described in this step is composed of the following raw materials in percentage ratio: 2% chitosan, a mixture of ethylene glycol having a mass percentage concentration greater than 99% and glycerol having a mass percentage concentration greater than 99.5% in a volume ratio of 1:1 mixed 4%, and the remainder being water (using purified water) to obtain a liquid to be sprayed, and then spraying the aforementioned liquid to be sprayed into a medium served by water in a spraying manner, so that the solvent (i.e., a mixture of ethylene glycol having a mass percentage concentration greater than 99% and glycerol having a mass percentage concentration greater than 99.5% in a volume ratio of 1:1 mixed) is precipitated from the mixture, and controlling the temperature of the aforementioned spray device to be 60° C. to obtain wormwood essential oil microcapsules;

[0035] C) preparing a nanoporous material, first adding a mixture of far-infrared ceramic powder obtained from a commercial channel and diatomaceous earth at a mass ratio of 1:4 to a grinding device, and grinding together with an etchant added to the grinding device, wherein the mass ratio of the far-infrared ceramic powder and diatomaceous earth mixture to the etchant is controlled to be 85:10, and the grinding speed and grinding time of the grinding device are controlled to be 900 rpm and 40 minutes, respectively, to obtain a grind. The grind is filtered through a 200-mesh filter (i.e., firstly), and then the filtered material after the 200-mesh filter is neutralized with HCl (hydrochloric acid) to a pH of 7-8 to obtain a weakly alkaline material, and then the weakly alkaline material is filtered through a 200-mesh filter. The alkaline material is soaked with water at a volume ratio of 1:13 for 5 minutes. After the soaking, an aqueous solution is obtained, which is filtered through a nylon 66 filter membrane with a pore size of 0.5 μm to obtain a filtered aqueous solution. The filtered aqueous solution is filtered again through a filter membrane with a pore size of 0.1 μm to obtain a solid mixture. Finally, the solid mixture is introduced into a dryer for drying to obtain a nanoporous material. The drying temperature and drying time of the dryer in this step are controlled to 55° C. and 80 minutes, respectively. The aforementioned dryer is a drum dryer. The etchant in this step is a mixture of ethylene glycol with a mass percentage concentration greater than 99% and caustic soda in a mass ratio of 9.5:0.6;

[0036] D) prepare wormwood essential oil microcapsule nanoporous composite material, first by step B) wormwood essential oil microcapsules obtained and by step C) nanoporous material obtained are introduced into a stirred vessel filled with a dispersant aqueous solution and equipped with a stirrer and stir evenly, go out of the stirred vessel and proceed to drying in a drying machine, go out of the drying machine, obtain wormwood essential oil microcapsule nanoporous composite material, the mass percent control of the wormwood essential oil microcapsules in the described dispersant aqueous solution is 13%, the mass percent control of the nanoporous material in the dispersant aqueous solution is 40%, the stirring speed and the mixing time of the described stirred vessel are respectively controlled to 1500rpm and 35min, the baking temperature and the baking time of the described drying machine are respectively controlled to 40 ℃ and 90min, the described drying machine is a drum dryer, and the described dispersant aqueous solution is that the mass percent concentration is 1.7% Tween aqueous solution;

[0037] E) preparing a finished product, first, the wormwood essential oil microcapsule nanoporous composite material obtained in step D), an 88% by mass concentration of N-methylmorpholine-N-oxide (NMMO (also abbreviated as NMO) aqueous solution, and cotton pulp in a mass ratio of 3:11.8:3 are put into a reactor and vacuum stirred, the vacuum stirring time and the temperature of the reactor are controlled at 50 minutes and 105° C., respectively, to obtain a spinning solution, and then the spinning solution is introduced into a screw extruder, extruded by the screw extruder to a metering pump, and then The fiber melt is pumped into the spinning assembly of the spinning box and exits the spinning assembly of the spinning box to obtain a fiber melt. The fiber melt is sequentially cooled by side blowing or ring blowing, washed with alcohol, washed with water, oiled and dried again, and then subjected to corona treatment. The voltage used for the corona treatment is 1800 volts and the power is 10 W. Finally, the fiber is shaped at a temperature of 124°C, and the fiber tension during the shaping process is controlled at 15 N to obtain a biodegradable lyocell fiber with a wormwood microcapsule sustained-release function and a flavonoid content of 18.2 mg / g. Example 4:

[0038] A) preparing a raw material for preparing wormwood essential oil microcapsules, the wormwood essential oil microcapsules comprising a core material and a wall material, the core material being a mixture of wormwood essential oil containing 3.4% isoeutaxanthin and tea tree essential oil in a mass ratio of 5:1, preferably mixed with a mixing device, and the wall material being a mixture of hydroxypropyl cellulose and porous starch prepared by an enzymatic method in a mass ratio of 2.2:1, preferably mixed with a mixing device, to obtain the raw material for preparing wormwood essential oil microcapsules;

[0039] B) preparing wormwood essential oil microcapsules, first adding the mixture obtained by step A) and the mixture to the dispersed emulsion and mixing, and controlling the mass percentage concentration of the mixture in the dispersed emulsion to be 4.5%, controlling the mass percentage concentration of the mixture in the dispersed emulsion to be 4%, the dispersed emulsion described in this step is composed of the following raw materials in percentage ratio: Tween 0.6%, Span 0.6%, chitosan 0.6%, a mixture of ethylene glycol having a mass percentage concentration greater than 99% and glycerol having a mass percentage concentration greater than 99.5% in a volume ratio of 1:1 5%, and the remainder being water (using purified water) to obtain a spray liquid, and then spraying the aforementioned spray liquid into a medium served by water in a spraying manner, so that the solvent (i.e., a mixture of ethylene glycol having a mass percentage concentration greater than 99% and glycerol having a mass percentage concentration greater than 99.5% in a volume ratio of 1:1) is precipitated from the mixture, and the temperature of the aforementioned spray device is controlled to 65°C to obtain wormwood essential oil microcapsules;

[0040] C) preparing a nanoporous material, first adding a mixture of far-infrared ceramic powder obtained from a commercial channel and diatomaceous earth at a mass ratio of 1:2 to a grinding device, and grinding together with an etchant added to the grinding device, controlling the mass ratio of the far-infrared ceramic powder and diatomaceous earth mixture to the etchant to be 105:9, and controlling the grinding speed and grinding time of the grinding device to be 1100 rpm and 20 minutes, respectively, to obtain a grind. The grind was sequentially filtered through a 200-mesh filter (i.e., firstly), and then the filtered material after being filtered through the 200-mesh filter was neutralized with HCl (hydrochloric acid) to a pH of 7-8 to obtain a weakly alkaline material, and then The weakly alkaline material is soaked with water at a volume ratio of 1:16 for 8 minutes. After the soaking, an aqueous solution is obtained, which is filtered through a nylon 66 filter membrane with a pore size of 0.5 μm to obtain a filtered aqueous solution. The filtered aqueous solution is filtered again through a filter membrane with a pore size of 0.1 μm to obtain a solid mixture. Finally, the solid mixture is introduced into a dryer for drying to obtain a nanoporous material. The drying temperature and drying time of the dryer in this step are controlled to 45° C. and 100 minutes, respectively. The aforementioned dryer is a drum dryer. The etchant in this step is a mixture of ethylene glycol with a mass percentage concentration greater than 99% and caustic soda in a mass ratio of 9:0.5;

[0041] D) prepare wormwood essential oil microcapsule nanoporous composite material, first by step B) the wormwood essential oil microcapsules obtained and by step C) the nanoporous material obtained are introduced into a stirred vessel filled with a dispersant aqueous solution and equipped with a stirrer to stir evenly, go out of the stirred vessel and proceed to drying in a drying machine, go out of the drying machine, obtain the wormwood essential oil microcapsule nanoporous composite material, the mass percent control of the wormwood essential oil microcapsules in the described dispersant aqueous solution is 17%, the mass percent control of the nanoporous material in the dispersant aqueous solution is 25%, the stirring speed and the mixing time of the described stirred vessel are respectively controlled to 1800rpm and 25min, the baking temperature and the baking time of the described drying machine are respectively controlled to 55 DEG C and 110min, the described drying machine is a tumble dryer, and the described dispersant aqueous solution is that the mass percent concentration is 2% of the Tween aqueous solution;

[0042] E) preparing a finished product, first, the wormwood essential oil microcapsule nanoporous composite material obtained in step D), an 86% by mass concentration of N-methylmorpholine-N-oxide (NMMO (also abbreviated as NMO) aqueous solution, and cotton pulp in a mass ratio of 3:11.6:2.5 are put into a reactor and vacuum stirred, the vacuum stirring time and the temperature of the reactor are controlled at 30 minutes and 110° C., respectively, to obtain a spinning solution, and then the spinning solution is introduced into a screw extruder, extruded by the screw extruder to a metering pump, and then automatically metered. The fiber melt is sequentially cooled by side blowing or ring blowing, washed with alcohol, washed with water, oiled and dried again, and then subjected to corona treatment. The voltage used for corona treatment is 1400 volts and the power is 16 W. Finally, the fiber is shaped at a temperature of 127°C, and the fiber tension during the shaping process is controlled at 35 N to obtain a biodegradable lyocell fiber with a wormwood microcapsule sustained-release function and a flavonoid content of 18.6 mg / g.

[0043] Isoeupretinoic acid, also known as zeuratin, is primarily found in the Asteraceae plant Artemisia argyi. It has the effects of dissipating heat and relieving pain, warming the meridians and stopping bleeding, and inhibiting tumor growth. The technical indicators of the degradable lyocell fibers with sustained-release wormwood microcapsules obtained in Examples 1 to 4, such as washability, were primarily verified by their wearability after being processed into fabrics. Therefore, the fibers of the present invention were cut into short fibers, spun, and then woven into fabrics using an air-jet loom. The fabric parameters were: warp and weft count 80 s *80 s , yarn count is 210*175, weight is 125g / m 2 The sustained-release function of the mugwort microcapsules of the fiber of the present invention is demonstrated by testing the content of isoeutaxanthin in the fabric after multiple washings. The washing test is conducted in accordance with GB / T8629-2017 "Household Washing and Drying Procedure for Textile Testing":

[0044] The following table shows the washability test data of the active ingredient (isoeupatoria flavescens) in yarns made from fibers and fabrics woven from the yarns.

[0045]

[0046] The applicant provides the following explanations on the above forms:

[0047] 1. According to the GB / T19277 biodegradation-composting method, the 180-day biodegradation rate exceeds 90%, indicating that the yarn made from the fiber obtained by the method of the present invention and the fabric woven from the yarn have excellent biodegradability and are environmentally friendly.

[0048] 2. The woven fabrics described in the table are obtained by sequentially sizing the warp yarn, loading the cloth roller, threading, adjusting the needle plate and weaving the yarn made of the lyocell fiber with the slow-release function of mugwort microcapsules obtained by the method of the present invention on a sizing machine.

[0049] 3, the active ingredient of Artemisia argyi effect is mainly isoeupretinoic acid, so the Artemisia argyi effective content of measuring fiber, mainly is exactly to measure the content of isoeupretinoic acid in the clothing made of yarn, in the form, according to the taking process of product, yarn is woven into fabric by testing the content change of fabric isoeupretinoic acid after its washing, determines effect.Fiber isoeupretinoic acid content of the present invention can reach 18.2-19.7mg / g, in making fabric process, because warp yarn will pass through sizing, fabric will pass through printing and dyeing processing desizing and bleaching finishing after being woven, causes process part active ingredient isoeupretinoic acid to discharge, and content decreases.From the isoeupretinoic acid content change analysis under different embodiments in the form, after 20 washings, fabric content still can reach 8.5-9.3g / mg, possesses a state of fabric washability and slow release.

[0050] 4. The data for isoeutaxanthin content in the table was obtained by gas chromatography-mass spectrometry (GC-MS) chromatography at the request of the applicant and commissioned by Shanghai Standard Inspection Product Testing Co., Ltd. The test report number is ST22100208, and the testing period is from October 21, 2022, to October 28, 2022.

Claims

1. A method for preparing a degradable lyocell fiber with sustained-release function of wormwood microcapsules, characterized in that: The following steps are involved: A) preparing a raw material for preparing wormwood essential oil microcapsules, wherein the wormwood essential oil microcapsules include a core material and a wall material, wherein the core material is a mixture of wormwood essential oil and tea tree essential oil mixed in a mass ratio, and the wall material is a mixture of hydroxypropyl cellulose and porous starch mixed in a mass ratio, to obtain a raw material for preparing wormwood essential oil microcapsules; B) preparing wormwood essential oil microcapsules, first adding the mixture obtained in step A) and the mixture into the dispersed emulsion and mixing them, and controlling the mass percentage concentration of the mixture in the dispersed emulsion and the mass percentage concentration of the mixture in the dispersed emulsion to obtain a liquid to be sprayed, and then spraying the liquid to be sprayed into the medium in a spraying manner, so that the solvent in the liquid to be sprayed is precipitated from the mixture, and controlling the temperature of the spraying device to obtain wormwood essential oil microcapsules; C) preparing a nanoporous material, first adding a mixture of far-infrared ceramic powder and diatomaceous earth into a grinding device, grinding it with an etchant added to the grinding device, and controlling the mass ratio of the far-infrared ceramic powder to the diatomaceous earth, the mass ratio of the mixture of the far-infrared ceramic powder and the diatomaceous earth to the etchant, and controlling the grinding speed and grinding time of the grinding device to obtain a grind, filtering it through a filter screen, acid neutralization and leaching it in sequence, and then filtering it with a filter membrane to obtain a filtered aqueous solution, filtering the filtered aqueous solution again to obtain a solid mixture, and finally introducing the solid mixture into a dryer for drying, and controlling the drying temperature and drying time of the dryer to obtain the nanoporous material; D) preparing a nanoporous composite material of wormwood essential oil microcapsules, firstly introducing the wormwood essential oil microcapsules obtained by step B) and the nanoporous material obtained by step C) into a stirring container filled with a dispersant aqueous solution and equipped with a stirrer, stirring evenly, and controlling the mass percentage of the wormwood essential oil microcapsules in the dispersant aqueous solution and the mass percentage of the nanoporous material in the dispersant aqueous solution, controlling the stirring speed and stirring time of the stirrer of the stirring container, taking out of the stirring container and transferring to a drying machine for drying, and controlling the drying temperature and drying time of the drying machine, and taking out of the drying machine, to obtain the nanoporous composite material of wormwood essential oil microcapsules; E) preparing a finished product, firstly, the wormwood essential oil microcapsule nanoporous composite material obtained in step D), N-methylmorpholine-N-oxide aqueous solution and cotton pulp are put into a reactor in a mass ratio of 3:11-12:1-3, and vacuum stirring is performed, and the vacuum stirring time and the temperature of the reactor are controlled to obtain a spinning solution, and then the spinning solution is introduced into a screw extruder, extruded from the screw extruder to a metering pump, and then from the metering pump into a spinning assembly of a spinning box, and out of a spinneret of the spinning assembly to obtain a fiber melt, and the fiber melt is sequentially cooled, washed with alcohol, washed with water and dried, and then oiled, dried again and corona treated, and finally shaped, and the fiber tension in the shaping process is controlled and the shaping temperature is controlled to obtain a finished product, i.e., a degradable lyocell fiber with a wormwood microcapsule sustained-release function and a content of 17.5-19.7 mg / g of isoeilflavin.

2. The method for preparing the degradable lyocell fiber with sustained-release function of wormwood microcapsules according to claim 1, characterized in that: The wormwood essential oil and tea tree essential oil described in step A) are mixed in a mass ratio of 3-6:1; the hydroxypropyl cellulose and porous starch are mixed in a mass ratio of 2-3:1; the mass percentage of isoeuvreflavin in the wormwood essential oil is 3-3.5%; and the porous starch is a porous starch prepared by an enzymatic method.

3. The method for preparing the degradable lyocell fiber with sustained-release function of wormwood microcapsules according to claim 1, characterized in that: The step B) of controlling the mass percentage concentration of the mixture in the dispersed emulsion is to control the mass percentage concentration to 3-5%; the step of controlling the mass percentage concentration of the mixture in the dispersed emulsion is to control the mass percentage concentration to 3.5-6%; the medium is water; the step of controlling the temperature of the spray device is to control the temperature of the spray device to 50-70°C.

4. The method for preparing the degradable lyocell fiber with sustained-release function of wormwood microcapsules according to claim 1 or 3, characterized in that: The dispersed emulsion is composed of the following raw materials in proportion by mass percentage: 1-2% of nonionic surfactant and / or preservative, 4-7% of solvent, and the rest of water.

5. The method for preparing the degradable lyocell fiber with sustained-release function of wormwood microcapsules according to claim 4, characterized in that: The nonionic surfactant is Tween and Span; the preservative is chitosan; and the solvent is a mixture of ethylene glycol with a mass percentage concentration greater than 99% and propylene glycol with a mass percentage concentration greater than 99.5% in a volume ratio of 1:

1.

6. The method for preparing the degradable lyocell fiber with sustained-release function of wormwood microcapsules according to claim 1, characterized in that: The mass ratio of the far-infrared ceramic powder to diatomaceous earth in step C) is controlled to be 1:1.5-4; the mass ratio of the mixture of the far-infrared ceramic powder and diatomaceous earth to the etchant is controlled to be 70-120:8-11; the grinding speed and grinding time of the grinding device are controlled to be 500-1100rpm and 20-80min; the mesh size of the filter used for filtering is 200 mesh; the acid neutralization refers to neutralization with HCl to pH7-8; The soaking is to soak the weakly alkaline material obtained after filtering through the filter and neutralizing with acid for 5-10 minutes at a volume ratio of 1:10-20 to water, and the aqueous solution obtained after soaking is filtered using a filter membrane, the filter membrane is a nylon 66 filter membrane with a pore size of 0.5μm, and the filtering of the filtered aqueous solution again is to filter the filtered aqueous solution using a filter membrane with a pore size of 0.1μm; the controlling of the drying temperature and drying time of the dryer is to control the drying temperature and drying time to 40-60℃ and 60-120min respectively, and the dryer is a drum dryer.

7. The method for preparing the degradable lyocell fiber with sustained-release function of wormwood microcapsules according to claim 6, characterized in that: The etchant is a mixture of a dispersant and caustic soda in a mass ratio of 8.5-10:0.5-1, and the dispersant is ethylene glycol with a mass percentage concentration greater than 99%.

8. The method for preparing the degradable lyocell fiber with sustained-release function of wormwood microcapsules according to claim 1, characterized in that: The step D) of controlling the mass percentage of the wormwood essential oil microcapsules in the dispersant aqueous solution is to control the mass percentage to 10-20%, and the step of controlling the mass percentage of the nanoporous material in the dispersant aqueous solution is to control the mass percentage to 20-40%; the step of controlling the stirring speed and stirring time of the stirrer is to control the stirring speed to 1000-2000rpm and the stirring time to 30-40min; the step of controlling the drying temperature and drying time of the dryer is to control the drying temperature and drying time of the dryer to 50-70°C and 60-120min, respectively, and the dryer is a drum dryer.

9. The method for preparing the degradable lyocell fiber with sustained-release function of wormwood microcapsules according to claim 1 or 8, characterized in that: The dispersant aqueous solution is a Tween aqueous solution with a mass percentage concentration of 1-2%.

10. The method for preparing the degradable lyocell fiber with sustained-release function of wormwood microcapsules according to claim 1, characterized in that: The mass percentage concentration of the N-methylmorpholine-N-oxide aqueous solution in step E) is 85-90%; the vacuum stirring time is controlled to be 30-90 minutes; the temperature of the reactor is controlled to be 100-110°C; the corona treatment is carried out using a generator with a voltage of 1000-2000 volts and a power of 5-20W; the tension of the fiber in the shaping process is controlled to be 5-50N, and the shaping temperature is controlled to be 120-130°C; the content of isoeilin in the degradable lyocell fiber with the sustained-release function of wormwood microcapsules is 10-20 mg / g.

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