阅读说明：本技术 一种珍珠中药防湿疹再生纤维素纤维及其制备方法 (Pearl traditional Chinese medicine eczema-prevention regenerated cellulose fiber and preparation method thereof ) 是由 刘训林 钱晓燕 于 2020-06-10 设计创作，主要内容包括：本发明提供了一种珍珠中药防湿疹再生纤维素纤维及其制备方法。所述珍珠中药防湿疹再生纤维素纤维包括以下重量百分比的组分：珍珠粉2-5.5wt％和中药提取物2-3wt％。所述中药提取物为50-70wt％的苦参碱,20-40wt％的地肤子皂苷和5-10wt％的葛根素。本发明的珍珠中药防湿疹再生纤维素纤维,珍珠粉分散性好,不易团聚,且能由亲水性变为亲油性。通过制备微胶囊将珍珠粉和中药提取物包覆起来,微胶囊尺寸小,不影响纺丝,且能避免纺丝过程中强酸强碱对中药提取物成分的破坏。本发明的纤维具有防湿疹和保健护肤的功能,经过反复水洗后,依然能发挥功效。(The invention provides pearl traditional Chinese medicine eczema-preventing regenerated cellulose fiber and a preparation method thereof. The pearl traditional Chinese medicine eczema-preventing regenerated cellulose fiber comprises the following components in percentage by weight: 2-5.5 wt% of pearl powder and 2-3 wt% of traditional Chinese medicine extract. The traditional Chinese medicine extract comprises 50-70 wt% of matrine, 20-40 wt% of kochiae saponin and 5-10 wt% of puerarin. The pearl traditional Chinese medicine eczema-preventing regenerated cellulose fiber has good pearl powder dispersibility, is not easy to agglomerate, and can be changed from hydrophilicity to lipophilicity. The pearl powder and the traditional Chinese medicine extract are coated by preparing the microcapsule, the microcapsule has small size, does not influence spinning, and can avoid the damage of strong acid and strong alkali to the components of the traditional Chinese medicine extract in the spinning process. The fiber has the functions of eczema prevention and health care and skin care, and can still exert the effect after repeated washing.)

1. The pearl traditional Chinese medicine eczema-preventing regenerated cellulose fiber is characterized by comprising pearl powder and a traditional Chinese medicine extract, wherein the addition amounts of the pearl traditional Chinese medicine eczema-preventing regenerated cellulose fiber and the traditional Chinese medicine extract respectively account for 2-5.5 wt% and 2-3 wt% of a spinning solution.

2. The pearl Chinese medicine eczema-preventing regenerated cellulose fiber as claimed in claim 1, wherein the Chinese medicine extract is 50-70 wt% of matrine, 20-40 wt% of kochia saponins and 5-10 wt% of puerarin.

3. The preparation method of the pearl Chinese medicinal anti-eczema regenerated cellulose fiber according to any one of claims 1 or 2, which is characterized by comprising the following steps:

s1, adding a traditional Chinese medicine extract into water according to the amount of 0.5-2g/ml to prepare a water phase, uniformly mixing vegetable oil and an emulsifier to prepare an oil phase, and adding the water phase into the oil phase under the stirring condition to prepare a traditional Chinese medicine extract micro-emulsion;

s2, coarsely crushing pearls, adding water, stirring to form slurry of 25-40%, feeding the slurry into a high-pressure tank, pressurizing by steam, entering an expansion cavity, quickly reducing the pressure to be normal, repeating for at least three times, and grinding to obtain pearl powder;

s3, dispersing a cross-linking agent and a cross-linking catalyst in water to form a cross-linking agent solution, heating polyethylene glycol to 60-80 ℃ to melt, mixing the pearl powder and the Chinese medicinal extract microemulsion, dispersing the mixture in the molten polyethylene glycol, stirring for 5-12h, immersing the mixture in the cross-linking agent solution, and drying to obtain a mixture with an inner layer of the pearl powder and the Chinese medicinal extract and an outer layer of the polyethylene glycol cross-linking layer;

and S4, melting the raw materials for producing the regenerated cellulose fibers into spinning solution, injecting the mixture obtained in the step S3 into the spinning solution, and mixing, spinning, drafting and shaping to obtain a finished product.

4. The method for preparing the pearl Chinese medicinal anti-eczema regenerated cellulose fiber according to claim 3, wherein in the step S1, the emulsifier is an emulsifier with HLB value of 3-6.

5. The method for preparing the pearl Chinese medicinal anti-eczema regenerated cellulose fiber according to the claim 3, wherein in the step S1, the weight percentage of each component is 20-40% of water phase, 0.5-2% of emulsifier and the balance of oil phase.

6. The preparation method of the pearl Chinese medicinal anti-eczema regenerated cellulose fiber according to claim 3, characterized in that in step S2, the fineness of the pearl powder is D95 ≤ 0.1 μm.

7. The method for preparing the pearl Chinese medicine anti-eczema regenerated cellulose fiber as claimed in claim 3, wherein in step S3, the molecular weight of the polyethylene glycol is 400-600-.

8. The method for preparing the pearl Chinese medicine anti-eczema regenerated cellulose fiber according to the claim 3, wherein in the step S3, the crosslinking catalyst is dibutyltin dilaurate.

9. The preparation method of the pearl Chinese medicine anti-eczema regenerated cellulose fiber according to the claim 3, characterized in that in the step S3, the cross-linking agent is any one or more of triisocyanate and toluene diisocyanate.

10. The preparation method of the pearl Chinese medicinal anti-eczema regenerated cellulose fiber according to claim 3, wherein the mixing addition amount of the pearl powder and the Chinese medicinal extract, the mass ratio of the polyethylene glycol to the cross-linking agent to the cross-linking catalyst is 100: (1-5): (20-30): (0.26-0.6): (0.01-0.02).

Technical Field

The invention relates to the technical field of textile fibers, and particularly relates to pearl traditional Chinese medicine eczema-preventing regenerated cellulose fibers and a preparation method thereof.

Background

The clothes and eating habits are closely related to the life of people. In the textile field, people have not only satisfied comfortable and beautiful appearance, but also actively developed healthy and environment-friendly functional textiles, and have successively introduced many textiles with health care and medical functions, such as promoting blood circulation, relieving itching and diminishing inflammation, whitening and resisting ultraviolet rays, and the like.

CN102493207A relates to a preparation method of regenerated cellulose fabric with calming and health care functions. Adding sweet orange essential oil into polyurethane and water, stirring, adding the microcapsule solution, stirring fully, adding a dispersing agent, a binder and a softening agent, and stirring to obtain the sweet orange essential oil microcapsule finishing agent. The sweet orange essential oil microcapsule finishing agent is coated on the regenerated cellulose fabric after being treated by a spraying method, a padding method or a dipping method. By adopting the adding method, after the fabric is washed and worn for a long time, the sweet orange essential oil microcapsule finishing agent is not firmly combined with the fabric.

CN110747627A discloses a preparation method and application of a super-hydrophobic perfume slow-release cotton fiber. By sol-gel processing of TiO₂Modifying the particles on the surface of the cotton fiber, growing MOF crystals on the surface of the cotton fiber by an in-situ growth method, and soaking the prepared composite material in a normal heptane solution containing menthol and low surface energy substances to prepare the super-hydrophobic perfume slow-release cotton fiber. The method provided by the invention regulates and controls TiO on the surface of the cotton fiber₂The deposition amount of the particles and the MOF crystals can effectively regulate and control the roughness of the surface of the material, and further regulate and control the hydrophobic property of the slow-release cotton fiber. Will pass through TiO₂The particles and MOF-modified cotton fibers were immersed in a n-heptane solution containing menthol and PDMS. PDMS has good film forming propertyNot only has certain barrier function on the release of menthol and improves the slow release performance, but also has certain barrier function on TiO₂The particles and MOF crystals are effectively protected, and TiO is effectively inhibited₂The particles and MOF crystals fall off from the surface of the cotton fiber, so that the use stability of the material is obviously improved, and the excellent slow release performance of the material is ensured. The retention rate of the slow-release cotton fiber to the menthol spice after being washed by water is still 97.07 percent, which is obviously higher than the retention rate of the slow-release cotton fiber to the menthol after being washed by water, which is 27.92 percent. But incorporating TiO on cotton fibers₂Particles and MOF crystals, can affect wearer comfort.

The pearl has bright color, contains chitin, various amino acids, and various microelements such as manganese, zinc, copper and selenium, and can be used as ornament, skin care product and medicinal product. The compendium of materia medica records that pearl is coated on the surface, makes people moist and good in color, is coated on hands and feet, and is peeled and furled. Pearl, being cold in nature, sweet and salty in taste, enters heart and lung meridians, and has the effects of relieving heart and arresting convulsion, clearing liver and removing nebula, and promoting the production of organism and detoxification. The pearl particles have far infrared radiation function, and can promote the expansion of epidermal capillary vessels and improve the microcirculation of human bodies when contacting with human bodies. After the pearl powder is added in the spinning process, due to the particle size and the agglomeration of the pearl powder, the pearl powder is easy to settle, so that the spinneret orifices are blocked by the pearl powder or the prepared fiber pearl powder is not uniformly distributed.

Radix sophorae flavescentis, fructus kochiae and radix puerariae are common traditional Chinese medicines. Ku Shen is bitter and cold in nature. Has the functions of clearing heat, drying dampness, killing parasites and promoting urination. Can be used for treating dysentery, hematochezia, jaundice, hematuria, leucorrhea with red and white discharge, pudendal swelling, pudendal pruritus, eczema, and skin pruritus. Matrine extracted from radix Sophorae Flavescentis has antiinflammatory and antiallergic effects. Di Fu Zi is pungent, bitter and cold in nature. It can be used for treating lower abdomen pain, pudendal pruritus, leukorrhagia, rubella, eczema, and skin pruritus. Has the effects of clearing heat, promoting diuresis, dispelling wind and relieving itching. The saponin in Kochiae fructus extract has anti-itch and anti-inflammatory effects. Kudzuvine root, sweet, pungent and cool, has the effects of relieving muscles and reducing fever and promoting eruption. Puerarin has tranquilizing effect. The three components are added into the fiber to contact with human skin, so that the traditional Chinese medicine effect can be exerted, and skin itch and allergy can be relieved. However, the spinning process needs strong acid and strong alkali treatment, which can affect the effective components of the traditional Chinese medicine.

Disclosure of Invention

In view of the above, the invention aims to provide a pearl Chinese medicinal eczema-prevention regenerated cellulose fiber and a preparation method thereof, by adding pearl powder and extracts of Chinese medicinal herbs of sophora flavescens, fructus kochiae and radix puerariae into a spinning stock solution, the problems that the pearl powder is large in particle size and easy to agglomerate and Chinese medicinal ingredients are easy to damage by acid and alkali in the prior art are solved, so that the prepared fiber can exert the effects of pearls and Chinese medicaments, and the product quality is not influenced.

In order to achieve the purpose, the technical scheme of the invention is realized as follows:

a pearl Chinese medicinal anti-eczema regenerated cellulose fiber comprises pearl powder and Chinese medicinal extracts, and the addition amounts of the pearl powder and the Chinese medicinal extracts respectively account for 2-5.5 wt% and 2-3 wt% of a spinning solution.

Further, the traditional Chinese medicine extract comprises 50-70 wt% of matrine, 20-40 wt% of kochiae saponin and 5-10 wt% of puerarin.

The invention also provides a preparation method of the pearl traditional Chinese medicine eczema-prevention regenerated cellulose fiber, which comprises the following steps:

s1, adding a traditional Chinese medicine extract into water according to the amount of 0.5-2g/ml to prepare a water phase, uniformly mixing vegetable oil and an emulsifier to prepare an oil phase, and adding the water phase into the oil phase under the stirring condition to prepare a traditional Chinese medicine extract micro-emulsion;

s2, adding water into the coarsely crushed pearl powder, stirring the pearl powder into slurry of which the concentration is 25-40%, feeding the slurry into a high-pressure tank, pressurizing the slurry by steam, feeding the slurry into an expansion cavity, quickly reducing the pressure to be normal, repeating the steps for at least three times, and grinding the slurry to obtain the pearl powder;

s3, dispersing part of a cross-linking agent and a cross-linking catalyst in water to form a cross-linking agent solution, heating polyethylene glycol to 60-80 ℃ for melting, mixing the pearl powder and the Chinese medicine extract microemulsion, dispersing the mixture in the molten polyethylene glycol, stirring for 5-12h, immersing the mixture in the cross-linking agent solution, and drying to obtain a mixture with an inner layer of the pearl powder and the Chinese medicine extract and an outer layer of the polyethylene glycol cross-linking layer;

s4, dissolving chitosan in an acetic acid solution, adding the mixture prepared in the step S3 and the rest of the cross-linking agent into the chitosan acetic acid solution for cross-linking, and drying to obtain microcapsules, wherein the inner layer is pearl powder and a traditional Chinese medicine extract, the middle layer is polyethylene glycol cross-linked, and the outermost layer is chitosan cross-linked;

s5, melting the raw materials for producing the regenerated cellulose fibers into spinning solution, injecting the microcapsules obtained in the step S4 into the spinning solution, and mixing, spinning, drafting and shaping to obtain a finished product.

Further, in step S1, the emulsifier has an HLB value of 3 to 6.

Further, in step S1, the weight percentages of the components are 20-40% of water phase, 0.5-2% of emulsifier and the balance of oil phase.

Further, in step S2, the fineness of the pearl powder reaches D95 not more than 0.1 μm.

Further, in step S3, the molecular weight of the polyethylene glycol is 400-600.

Further, in step S3, the crosslinking catalyst is dibutyltin dilaurate.

Further, in the steps S3-S4, the crosslinking agent is any one or more of triisocyanate and toluene diisocyanate. Dimethylol dihydroxyethylene urea is also generally used as a crosslinking agent, but since it causes yellowing of the fiber product, it is possible to select a tri-isocyanate or a toluene di-isocyanate as a crosslinking agent.

Further, the mass ratio of the cross-linking agent in the step S3 to the cross-linking agent in the step S4 is 1: (2-3).

Further, in step S4, the mass ratio of the chitosan to the acetic acid solution is 1: (4-10).

Furthermore, the mixing addition amount of the pearl powder and the traditional Chinese medicine extract, the mass ratio of the polyethylene glycol, the chitosan, the cross-linking agent and the cross-linking catalyst is 100: (1-5): (20-30): (0.5-2): (0.01-0.02).

The regenerated cellulose fiber is regenerated cellulose short fiber or filament obtained by spinning with spinning solution prepared by mixing one or more of wood pulp, bamboo pulp or cotton pulp, and is specifically viscose, bamboo fiber or modal.

Compared with the prior art, the pearl traditional Chinese medicine eczema-preventing regenerated cellulose fiber has the following advantages:

(1) by adopting the pearl pulverization method, the pearl powder has ideal effects in the aspects of stability, particle size distribution and dispersibility, the pearl powder is not easy to agglomerate and is uniformly dispersed, and the prepared fiber has good quality.

(2) The invention prepares the traditional Chinese medicine extract matrine, belvedere fruit saponin and puerarin into micro emulsion, then mixes the micro emulsion with pearl parts and coats the micro emulsion with polyethylene glycol, in order to improve the coating effect, chitosan crosslinking is adopted to carry out secondary coating, and the prepared pearl powder and the traditional Chinese medicine extract are microcapsules with an inner layer, polyethylene glycol is a middle layer and chitosan is an outer layer. The average size of the microcapsule is about 2.5 mu m, and the microcapsule does not influence the spinning process and the properties of a finished product when added into fibers. Meanwhile, the traditional Chinese medicine extract is prevented from being influenced by acid and alkali in the spinning process.

(3) The compatibility of polyethylene glycol and pearl is good, the polyethylene glycol is coated on the surface of pearl powder to enhance the lipophilicity of the pearl powder, the polyethylene glycol and the pearl powder are combined more firmly through the chemical crosslinking effect, and the prepared pearl traditional Chinese medicine eczema-preventing regenerated cellulose fiber is easier to be close to the skin so as to achieve the function of beautifying the skin.

(4) Matrine, kochia saponin and puerarin are added into the fiber, and the regenerated cellulose fiber containing pearl traditional Chinese medicine for preventing eczema can still release effective components after being repeatedly washed for 50 times, has the effects of sterilizing and relieving itching and has the function of preventing eczema.

Detailed Description

The invention will be further illustrated with reference to specific embodiments. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Furthermore, it should be understood that various changes or modifications to the invention may be made by those skilled in the art after reading the disclosure of the present invention, and these changes or modifications also fall within the scope of the protection of the present application.

The traditional Chinese medicine extracts of matrine, belvedere fruit saponin and puerarin are extracted and prepared from radix sophorae flavescentis, belvedere fruit and radix puerariae according to the prior art.

Example 1

Preparation of pearl powder

Selecting and cleaning raw material pearls, mixing the raw material pearls with water, putting the mixture into a stirring ball mill, and coarsely crushing the pearls to about 5 mu m by means of generated pressure and shearing force. Then adding water and stirring to obtain 25-40% slurry, feeding into a high-pressure tank of high-pressure expansion equipment, pressurizing the slurry by using steam, then feeding into an expansion cavity by using an expansion valve, recovering to conventional condition, and repeating at least three times. Repeating high-pressure expansion for many times, namely decompressing to conventional conditions, expanding pearl layers, loosening easily, and grinding by using a jet milling technology or a wet grinding and crushing method. The fineness of the obtained pearl powder reaches D95 ≤ 0.1 μm, and the dispersity is greater than 90%.

If the particle size of the powder added into the fiber is larger, the powder not only blocks the machine in the spinning process, but also influences the quality of the prepared fiber. By adopting the crushing method of the invention, the fineness of the pearl powder is D95 not more than 0.1 μm, the particle size is smaller, and the addition amount of the pearl powder in the fiber can be increased. And along with the increase of times of high-pressure expansion and decompression to conventional conditions, the powder is easier to crush to the nanometer level, and the powder obtained is finer.

Example 2

Mixing 1.95kg matrine, 0.9kg Kochiae fructus saponin and 0.15kg puerarin, adding into 3L water, mixing 6.9kg palm oil and 0.1kg triglyceride with HLB of 5 to prepare oil phase, adding the water phase into the oil phase under stirring to prepare the Chinese medicinal extract microemulsion. 4kg of pearl is pulverized according to the pulverization method of the embodiment 1 to prepare the pearl powder, and the fineness of the pearl powder is D95 which is less than or equal to 0.1 mu m.

0.02kg of toluene diisocyanate and 0.7g of dibutyltin dilaurate are dispersed in water to form a cross-linking agent solution, 0.21kg of polyethylene glycol with the molecular weight of 400 is heated to 60 ℃ for melting, the pearl powder and the Chinese medicinal extract microemulsion are mixed and then dispersed in the molten polyethylene glycol, the mixture is immersed in the cross-linking agent solution after being stirred for 12 hours, and the mixture with the inner layer of the pearl powder and the Chinese medicinal extract microemulsion and the outer layer of the polyethylene glycol cross-linking layer is obtained after drying, and the average size is 2.0 mu m.

Melting raw materials for producing regenerated cellulose fibers into spinning solution, and injecting the mixture into the spinning solution, wherein the dosage of pearl powder in the mixture is 4% of the fiber spinning solution, and the dosage of traditional Chinese medicine extract is 3% of the fiber spinning solution. The spinning and post-treatment processes are carried out according to the conventional process of viscose fibers.

Example 3

Mixing 1kg of matrine, 0.8kg of broom cypress fruit saponin and 0.2kg of puerarin, adding the mixture into 2L of water to prepare a water phase, uniformly mixing 2.9kg of soybean oil and 0.1kg of sucrose ester with HLB of 6 to prepare an oil phase, and adding the water phase into the oil phase under the condition of stirring to prepare the traditional Chinese medicine extract microemulsion. 5.5kg of pearl is pulverized according to the pulverization method of the embodiment 1 to prepare the pearl powder, and the fineness of the pearl powder is D95 which is less than or equal to 0.1 mu m.

Dispersing 0.02kg of triisocyanate and 0.7g of dibutyltin dilaurate in water to form a cross-linking agent solution, heating 0.075kg of polyethylene glycol with the molecular weight of 600 to 60 ℃ for melting, mixing the traditional Chinese medicine extract microemulsion and pearl powder, dispersing in the molten polyethylene glycol, stirring for 5h, immersing in the cross-linking agent solution, and drying to obtain a mixture with an inner layer of the pearl powder and the traditional Chinese medicine extract microemulsion and an outer layer of a polyethylene glycol cross-linking layer.

Dissolving 1.5kg of chitosan in 6kg of acetic acid solution, adding the prepared mixture and 0.02kg of triisocyanate into the chitosan acetic acid solution for crosslinking, and drying to obtain the micro-emulsion with the inner layer of pearl powder and Chinese medicinal extract, the middle layer of polyethylene glycol crosslinked and the outermost layer of chitosan crosslinked micro-capsule. The average size of the microcapsules was 2.1 μm.

Melting raw materials for producing regenerated cellulose fibers into spinning solution, and injecting the microcapsules into the spinning solution, wherein the dosage of the pearl powder in the microcapsules is 5.5% of the spinning solution, and the dosage of the traditional Chinese medicine extract is 2% of the spinning solution. The spinning and post-treatment processes are carried out according to the conventional process of viscose fibers.

Example 4

Mixing 2.1kg matrine, 0.6kg Kochiae fructus saponin and 0.3kg puerarin, adding into 6L water, mixing 23.85kg corn oil and 0.15kg Tween with HLB of 3 to prepare oil phase, adding the water phase into the oil phase under stirring to prepare the Chinese medicinal extract microemulsion. Pulverizing 2kg Margarita according to the pulverizing method of example 1 to obtain Margarita powder with fineness D95 no more than 0.1 μm.

Dispersing 0.03kg of triisocyanate and 1g of dibutyltin dilaurate in water to form a cross-linking agent solution, heating 0.25kg of polyethylene glycol with the molecular weight of 600 to 70 ℃ for melting, mixing the pearl powder and the Chinese medicinal extract microemulsion, dispersing in the molten polyethylene glycol, stirring for 10h, immersing in the cross-linking agent solution, and drying to obtain a mixture with an inner layer being the pearl powder and Chinese medicinal extract microemulsion and an outer layer being the polyethylene glycol cross-linking layer.

Dissolving 1.5kg of chitosan in 15kg of acetic acid solution, adding the prepared mixture and 0.07kg of triisocyanate into the chitosan acetic acid solution for crosslinking, and drying to obtain the micro-emulsion with the inner layer of pearl powder and Chinese medicinal extract, the middle layer of polyethylene glycol crosslinked and the outermost layer of chitosan crosslinked micro-capsule. The average size of the microcapsules was 1.9 μm.

Melting raw materials for producing regenerated cellulose fibers into spinning solution, and injecting the microcapsules into the spinning solution, wherein the dosage of the pearl powder in the microcapsules is 2% of the spinning solution, and the dosage of the traditional Chinese medicine extract is 3% of the spinning solution. The spinning and post-treatment processes are carried out according to the conventional process of viscose fibers.

Example 5

Mixing 1.95kg matrine, 0.9kg Kochiae fructus saponin and 0.15kg puerarin, adding into 3L water, mixing 6.9kg palm oil and 0.1kg triglyceride with HLB of 5 to prepare oil phase, adding the water phase into the oil phase under stirring to prepare the Chinese medicinal extract microemulsion. 4kg of pearl is pulverized according to the pulverization method of the embodiment 1 to prepare the pearl powder, and the fineness of the pearl powder is D95 which is less than or equal to 0.1 mu m.

0.02kg of toluene diisocyanate and 0.7g of dibutyltin dilaurate are dispersed in water to form a cross-linking agent solution, 0.21kg of polyethylene glycol with the molecular weight of 400 is heated to 60 ℃ for melting, the pearl powder and the Chinese medicinal extract microemulsion are mixed and then dispersed in the molten polyethylene glycol, the mixture is immersed in the cross-linking agent solution after being stirred for 12 hours, and the mixture with the inner layer of the pearl powder and the Chinese medicinal extract microemulsion and the outer layer of the polyethylene glycol cross-linking layer is obtained after drying.

Dissolving 1.75kg of chitosan in 14kg of acetic acid solution, adding the prepared mixture and 0.05kg of toluene diisocyanate into the chitosan acetic acid solution for crosslinking, and drying to obtain the microcapsule with the inner layer of pearl powder and Chinese medicinal extract microemulsion, the middle layer of polyethylene glycol crosslinked and the outermost layer of chitosan crosslinked. The average size of the microcapsules was 2.5 μm.

Melting raw materials for producing regenerated cellulose fibers into spinning solution, and injecting the microcapsules into the spinning solution, wherein the dosage of the pearl powder in the microcapsules is 4% of the spinning solution, and the dosage of the traditional Chinese medicine extract is 3% of the spinning solution. The spinning and post-treatment processes are carried out according to the conventional process of viscose fibers.

Example 5 differs from example 2 in that example 2 is not crosslinked with chitosan.

Comparative example 1

The compound plant traditional Chinese medicine antibacterial itching-relieving regenerated cellulose fiber is prepared according to the method of CN110359112A example 1.

Comparative example 2

Mixing 1.95kg matrine, 0.9kg Kochiae fructus saponin and 0.15kg puerarin, adding into 3L water, mixing 6.9kg palm oil and 0.1kg triglyceride with HLB of 5 to prepare oil phase, adding the water phase into the oil phase under stirring to prepare the Chinese medicinal extract microemulsion. 4kg of pearl is pulverized according to the pulverization method of the embodiment 1 to prepare the pearl powder, and the fineness of the pearl powder is D95 which is less than or equal to 0.1 mu m.

0.07kg of toluene diisocyanate and 0.7g of dibutyltin dilaurate are dispersed in water to form a cross-linking agent solution, 0.21kg of polyethylene glycol with the molecular weight of 400, 1.75kg of chitosan and 14kg of acetic acid solution are mixed, the pearl powder and the Chinese medicinal extract microemulsion are mixed and dispersed in the mixed solution, stirred for 12 hours and immersed in the cross-linking agent solution, and the microcapsule with the inner layer being the pearl powder and the Chinese medicinal extract microemulsion and the outer layer being the polyethylene glycol and chitosan cross-linking layer is obtained after drying. The average size of the microcapsules was 5 μm.

Melting raw materials for producing regenerated cellulose fibers into spinning solution, and injecting the microcapsules into the spinning solution, wherein the dosage of the pearl powder in the microcapsules is 4% of the spinning solution, and the dosage of the traditional Chinese medicine extract is 3% of the spinning solution. The spinning and post-treatment processes are carried out according to the conventional process of viscose fibers.

Comparative example 2 is different from example 5 in that comparative example 2 is prepared by mixing chitosan and polyethylene glycol and then crosslinking the mixture. Instead of independently crosslinking the pearl powder coated by polyethylene glycol and the microemulsion of the traditional Chinese medicine extract, and adding chitosan for crosslinking.

Comparative example 3

4kg of pearl is pulverized according to the pulverization method of the embodiment 1 to prepare the pearl powder, and the fineness of the pearl powder is D95 which is less than or equal to 0.1 mu m.

0.02kg of toluene diisocyanate and 0.7g of dibutyltin dilaurate are dispersed in water to form a cross-linking agent solution, 0.21kg of polyethylene glycol with the molecular weight of 400 is heated to 60 ℃ for melting, the pearl powder is dispersed in the molten polyethylene glycol, stirred for 12h and immersed in the cross-linking agent solution, and a mixture with the inner layer of pearl powder and the outer layer of polyethylene glycol cross-linked layer is obtained after drying.

Dissolving 1.75kg of chitosan in 14kg of acetic acid solution, adding the prepared mixture and 0.05kg of toluene diisocyanate into the chitosan acetic acid solution for crosslinking, and drying to obtain the microcapsule with the pearl powder as the inner layer, the polyethylene glycol crosslinking as the middle layer and the chitosan crosslinking as the outermost layer. The average size of the microcapsules was 1.5 μm.

Melting raw materials for producing regenerated cellulose fibers into spinning solution, injecting the microcapsules into the spinning solution, wherein the dosage of pearl powder in the microcapsules is 4% of the fiber spinning solution, and performing spinning and post-treatment according to the conventional process of viscose fibers.

The difference between the comparative example 3 and the example 5 is that the traditional Chinese medicine extracts of matrine, kochiae fructus saponin and puerarin are not added in the comparative example 3.

The oil absorption values were measured after mixing and dispersing the pearl powders of examples 2 to 5 and comparative examples 2 to 3 and the microemulsion of the herb extracts in polyethylene glycol for 5 to 12 hours, before immersing in the solution of the cross-linking agent. The oil absorption value of the pearl powder of example 1 was measured. The agglomeration property test method is to place the powder in deionized water for 6 months and then observe the agglomeration property. Specific performance indexes are shown in table 1.

TABLE 1

Group of	Oil absorption number (ml/100g)	Agglomeration property
			Example 1	75	Slight agglomeration
Example 2	36	No agglomeration and uniform dispersion
			Example 3	38	No agglomeration and uniform dispersion
Example 4	30	No agglomeration and uniform dispersion
			Example 5	35	No agglomeration and uniform dispersion
Comparative example 2	49	Agglomerated into small particles with precipitates
			Comparative example 3	30	No agglomeration and uniform dispersion

The pearl powder of example 1 has a small particle size but is poor in lipophilicity. The pearl powder of examples 2-5 was added with polyethylene glycol and mixed with a microemulsion of the extracts of the Chinese herbs, the microemulsion being a water-in-oil system. The pearl powder is equivalent to be contacted with the oil phase of the microemulsion. The pearl powder is changed from hydrophilicity to lipophilicity after being treated, and the oil absorption value is reduced. The polyethylene glycol and vegetable oil can react with the hydroxyl of the pearl powder to change the hydrophilicity into lipophilicity, the affinity with human skin is better, and the polyethylene glycol is adsorbed on the surface of the pearl powder to prevent the growth and aggregation of pearl powder crystals. The traditional Chinese medicine extract can enter the micropore structure of the pearl, so that the overall density of pearl powder can be reduced, the pearl powder is prevented from settling, the pearl powder provides a barrier for the traditional Chinese medicine extract, and the influence of acid and alkali on the effective components of the traditional Chinese medicine in the spinning process is reduced. In comparative example 2, chitosan and polyethylene glycol were added simultaneously, and a part of the pearl powder was not coated with polyethylene glycol but with chitosan, and the hydrophilicity of the chitosan-coated pearl powder was not improved, and the fiber prepared was poor in affinity to human skin.

The microcapsules prepared in the embodiments 2 to 5 have uniform particle sizes, the average size is less than or equal to 2.5 microns, and the physical and mechanical properties of the fiber finished product meet the standard of GB/T14463-. The microcapsules of comparative example 2 had an average size of 5 μm and a size larger than those of examples 2 to 5. The reason may be that, in comparative example 2 in which chitosan and polyethylene glycol were added at the same time, a part of the pearl powder was not coated with polyethylene glycol but with chitosan. The structure of polyethylene glycol and the affinity of pearl powder are good, aggregation and growth can be inhibited after coating, and the part of pearl powder coated by chitosan is easy to agglomerate, so that the size of the prepared microcapsule is increased. The oversize causes problems such as blockage in the spinning process. The fiber prepared in comparative example 2 also has reduced quality, and the physical and mechanical properties do not meet the GB/T14463-2008 standard.

Test for relieving itching

80 mice are taken, male and female halves are randomly divided into 8 groups, 10 mice are taken, and the groups are respectively a negative control group (comparative example 3, namely no traditional Chinese medicine extract is added), an example 2 group, an example 3 group, an example 4 group, an example 5 group, a comparative example 1 group, a comparative example 2 group and a positive control group (a certain brand of compound dermatitis ointment for treating eczema on the market). In the positive control group, the compound dermatitis ointment was uniformly applied to ordinary viscose fibers (i.e., the fibers did not contain traditional Chinese medicines), and the content of the ointment per unit area was the same as the content of the traditional Chinese medicine extract per unit area of the fibers prepared in example 5.

The mouse had a 2cmx3cm size depilated in the back and neck, and 24 hours later the administration of each of: each group of fiber products was measured to 3 × 3cm and coated on the mouse depilatory site. After 30min, 4-aminopyridine mg/kg (4-AP is prepared into 0.5% solution by using normal saline, and the solution is diluted into 0.01% solution by using the normal saline before the experiment) is injected subcutaneously into the back of the neck of each mouse, and the times of body licking of the mice within 10min are immediately observed (the mice have the behavior of repeatedly twisting the head and licking the back of two sides, namely the body licking reaction, and the mice continuously lick the body to cause transient pause, and the counting is carried out once for the body licking). The method comprises the following steps: the licking body must lick the back hairless area (fiber product coating area) for more than 5 times continuously, and only the head twisting or other parts licking are not counted; short pause requirement: the user needs to move, such as walk, stretch head, stand or smell things, and the like, and the time is not considered; repeatedly twisting head, licking hands or washing face without pause. The results are shown in Table 2.

TABLE 2

Note: p < 0.05 compared to the negative control group.

As can be seen from Table 2, the pearl Chinese medicinal anti-eczema regenerated cellulose fibers in the embodiments 2 to 5 have an inhibiting effect on skin pruritus caused by excessive release of histamine from skin mast cells due to 4-AP. Meanwhile, the preparation method of the invention is also demonstrated that the effective components of the traditional Chinese medicine are not damaged by strong acid and strong base in the spinning process, and the effect of the traditional Chinese medicine can be exerted. In the fiber of the comparative example 1, the content of the compound traditional Chinese medicine extract is up to 20%, and the times of licking the body are more than those of the fibers of the examples 2 to 5. The reason may be that the effective ingredients of the chinese medicine are damaged or lost much during the spinning process using the method of comparative example 1, and the effect is weakened.

Bacteriostatic activity

Eczema is an inflammatory skin disease with obvious exudation tendency, and the microbial detection rate of the eczema is obviously higher than that of normal skin, and is mainly staphylococcus aureus, candida and the like. Samples of examples 2 to 5 and comparative examples 1 to 3 were taken to examine the bacteriostatic rate. The representative bacteria selected are staphylococcus aureus and candida albicans. The bacteriostatic rate of the prepared fiber and the bacteriostatic effect after washing for 50 times are detected according to an oscillation method in the antibacterial performance of the textile of GB/T20944.3-2008, and the results are shown in Table 3.

TABLE 3

Function of pearl

The pearl has far infrared emission function, and can promote blood circulation of body surface and absorption and metabolism of cells, and promote absorption of effective components of Chinese medicinal materials. The long-term close-fitting wearing is beneficial to the health of people and promotes microcirculation. GB/T30127-2013 is adopted to detect the anti-eczema regenerated cellulose fiber of the prepared pearl traditional Chinese medicine and the far infrared performance after the pearl traditional Chinese medicine is repeatedly washed by water for 50 times, and the results are shown in Table 4.

TABLE 4

As shown in tables 3-4, the pearl traditional Chinese medicine eczema-preventing regenerated cellulose fiber prepared in the embodiments 3-5 of the invention has the bacteriostasis rate of 93.2-96.2% on staphylococcus aureus, and the bacteriostasis rate is 91.8-94.1% after repeated washing for 50 times. The bacteriostasis rate to candida albicans is 94.1-96.4%, and the bacteriostasis rate after repeated washing for 50 times is 92.6-93.4%. The far infrared emissivity is 0.90-0.95%, the far infrared radiation temperature is 1.8-2.0 ℃, and after repeated washing for 50 times, the far infrared emissivity is 0.89-0.93%, and the far infrared radiation temperature is 1.6-1.9 ℃. Therefore, the pearl Chinese medicine eczema-preventing regenerated cellulose fiber can exert the respective effects of the Chinese medicine and the pearl, the repeated water-based performance is reduced less, and the effective components can be slowly released for a long time. The microcapsule coated with the pearl powder and the microemulsion of the traditional Chinese medicine extract is not cross-linked and coated by chitosan in the example 2, and the microcapsule coated with the pearl powder and the microemulsion of the traditional Chinese medicine extract in the comparative example 2 is prepared by adopting a cross-linking process after mixing polyethylene glycol and chitosan, and after repeated washing for 50 times, the bacteriostatic effect on staphylococcus aureus and candida albicans is reduced more, and the far infrared emissivity and the far infrared radiation temperature are reduced more. Probably, the microcapsules are easily damaged in the water washing process, the pearl powder and the traditional Chinese medicine extract are suddenly released, and the effect is reduced more, which is lower than that of the embodiment 3-5. The fiber of the comparative example 1 has no far infrared function because no pearl is added, and the bacteriostasis rate is reduced more after washing. Therefore, the traditional Chinese medicine anti-eczema fibers of the embodiments 3 to 5 have the function of slowly releasing the effective components for a long time.

The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.