Anti-erythra regenerated cellulose fiber containing pearl traditional Chinese medicine and preparation method thereof

文档序号:93941 发布日期:2021-10-12 浏览:28次 中文

阅读说明:本技术 一种含珍珠中药的防红疹再生纤维素纤维及其制备方法 (Anti-erythra regenerated cellulose fiber containing pearl traditional Chinese medicine 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:本发明提供了一种含珍珠中药的防红疹再生纤维素纤维及其制备方法。所述含珍珠中药的防红疹再生纤维素纤维包括珍珠粉2-5.5wt%,中药提取物2-5wt%。所述中药提取物为80-90%的青蒿素及其衍生物和10-20%的冰片。本发明的含珍珠中药的防红疹再生纤维素纤维,珍珠粉分散性好,不易团聚。通过制备微胶囊将青蒿素及其衍生物和冰片包覆起来,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青蒿素及其衍生物和冰片的破坏。本发明的纤维具有护肤、防红疹的功能,经过反复水洗后,依然能发挥功效。(The invention provides a regenerated cellulose fiber containing pearl Chinese medicaments for preventing erythra and a preparation method thereof. The regenerated cellulose fiber containing pearl Chinese medicine for preventing erythra comprises 2-5.5 wt% of pearl powder and 2-5 wt% of Chinese medicine extract. The Chinese medicinal extract comprises 80-90% of artemisinin and its derivatives and 10-20% of borneol. The anti-erythra regenerated cellulose fiber containing the pearl traditional Chinese medicine has good pearl powder dispersibility and is not easy to agglomerate. The artemisinin and the derivatives thereof and the borneol 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 artemisinin and the derivatives thereof and the borneol in the spinning process. The fiber of the invention has the functions of skin care and preventing erythra, and can still exert the effect after being repeatedly washed by water.)

1. The anti-erythra regenerated cellulose fiber containing the pearl traditional Chinese medicine is characterized by comprising pearl powder and a traditional Chinese medicine extract, wherein the addition amounts of the pearl powder and the traditional Chinese medicine extract respectively account for 2-5.5 wt% and 2-5 wt% of a spinning solution.

2. The anti-erythra regenerated cellulose fiber containing pearl Chinese herbal medicines according to claim 1, wherein the Chinese herbal medicine extract is 80-90% of artemisinin and derivatives thereof and 10-20% of borneol.

3. The method for preparing the regenerated cellulose fiber containing pearl Chinese medicine for preventing erythra according to any one of claims 1 or 2, characterized by comprising the following steps: (1) pulverizing Margarita, adding water, stirring to obtain slurry, feeding into a high pressure tank, pressurizing with steam, rapidly decompressing in an expansion chamber, repeating for at least three times, and grinding to obtain Margarita powder; (2) preparing traditional Chinese medicine extract microcapsules; (3) preparing blended spinning solution; (4) spinning and post-processing.

4. The preparation method according to claim 3, wherein the preparation of the microcapsule of the herbal extract in step (2) comprises the steps of:

s1, dissolving chitosan in an acetic acid solution with the mass concentration of 0.5-2% to prepare a chitosan acetic acid solution with the mass concentration of 1-2%;

s2, crushing the traditional Chinese medicine extract artemisinin, the derivative thereof and the ice product, uniformly dispersing the crushed extract artemisinin, the derivative thereof and the ice product with citric acid and an emulsifier into water, adding the mixture into the chitosan acetic acid solution, then adding sodium citrate, and carrying out high-speed emulsification treatment for 15-30min at the rotating speed of 10000-15000r/min to obtain microcapsules taking the traditional Chinese medicine extract emulsion as a core material and chitosan as a wall material;

s3, adding sodium alginate into the microcapsule with the chitosan as the wall material, stirring at the speed of 200-800r/min, adjusting the pH value to 6-7, mixing with the aqueous solution of calcium chloride, standing, and then adding a cross-linking agent to react for 1-2h to obtain the microcapsule with the traditional Chinese medicine extract as the core material and the chitosan/sodium alginate as the wall material.

5. The preparation method according to claim 3, wherein the fineness of the pearl powder in step (1) reaches D95 ≤ 0.1 μm.

6. The preparation method of claim 4, wherein in steps S1-S3, the mass ratio of the chitosan to the Chinese herbal medicine extract to the sodium alginate to the sodium citrate to the citric acid is 1: (5-18): (1-5): (0.5-1.5): (0.1-0.2).

7. The method according to claim 4, wherein the chitosan has a molecular weight of 30 to 80 ten thousand in step S1.

8. The method according to claim 4, wherein in step S2, the volume ratio of the water for dispersing the herbal extract and the chitosan acetic acid solution is 1: (3-6).

9. The method according to claim 4, wherein in step S2, the emulsifier is an oil-in-water emulsifier with HLB value in the range of 9-15, and the amount is 3-10% of the extract of Chinese medicinal materials.

10. The preparation method according to claim 4, wherein in step S3, the crosslinking agent is at least one of formaldehyde, glutaraldehyde and epichlorohydrin, and the amount of the crosslinking agent is 2-4% of the total weight of the chitosan and sodium alginate.

Technical Field

The invention relates to the technical field of textile fibers, and particularly relates to a regenerated cellulose fiber containing pearl traditional Chinese medicines and capable of preventing erythema and a preparation method of the regenerated cellulose fiber.

Background

Health and environmental protection are the subjects of recent years, and people pay attention to the health and environmental protection in all aspects of life. The clothed people are closely related to the lives of everyone. In the field of textiles, the fabric not only needs to meet the requirements of people on warm keeping and comfort, but also has a health-care function. Therefore, various functional textiles come out endlessly, such as textiles with the functions of resisting bacteria and removing mites, preserving moisture, resisting static electricity, bringing cool feeling and the like. The textiles are fashionable and healthy, and therefore become top-quality products pursued by people.

In order to achieve the functional effect of textiles, it is generally necessary to pass the following techniques: firstly, in the fabric after-finishing process, the additive with special function is finished on the fabric in a manner of dipping, coating or drying, but by adopting the after-finishing manner, the additive and the fabric are not firmly combined, and the additive with special function is easy to fall off from the textile in the long-term wearing and washing processes, so that the function is greatly weakened; secondly, the fiber is treated to a certain extent in the production process of the fiber, and additives with special functions are added into the fiber. In this way, the additive can be bonded to the textile more firmly, but the influence of acid and alkali in the fiber preparation process on the additive and the size of the additive need to be considered.

CN101343780A discloses a viscose fiber containing aloe and a preparation method thereof, wherein an aloe extract is directly mixed with a viscose spinning solution, and substances such as amino acids contained in aloe can be damaged in a strong alkali process, so that a large amount of effective substances are lost, and the skin-care and moisture-retention effects are weakened.

CN107604455A discloses a method for preparing Chinese herbal medicine fiber, which comprises the steps of forming folium artemisiae argyi drug microcapsules by interfacial polymerization of folium artemisiae argyi extract, an emulsifier and a dispersant, blending the prepared Chinese herbal medicine fiber with regenerated cellulose solution, and developing the Chinese herbal medicine folium artemisiae argyi fiber with a slow release effect by a wet spinning process. The method can realize effective combination of Chinese herbal medicine and textile, and the medicinal components can be slowly released into human body through absorption and respiration of skin. However, the influence of the size of the Chinese herbal medicine microcapsules on the spinning process is not considered.

Margarita is produced from mollusk such as Margarita and nacre, and is a mineral produced by endocrine function. Because of the characteristics of bright color, soft texture, containing various substances beneficial to the human body and the like, the natural plant extract can be widely applied to ornaments and health care products. The pearl is rich in various amino acids, and contains microelements such as iron, zinc, manganese, selenium, etc. Can be used for tranquilizing and allaying excitement, sterilizing and disinfecting, stopping bleeding and promoting tissue regeneration in pharmacy, and can be used in skin care products for maintaining beauty, keeping young, preventing aging, keeping the skin white and fine and the like. When human skin sweats, the sweat can unbalance the ph value of the skin, resulting in the invasion of external bacteria. Calcium carbonate contained in the pearl can react with lactic acid in sweat to regulate acid-base balance of skin, so that the skin becomes soft and glossy, and the aims of maintaining physiological balance of the skin and protecting the skin are fulfilled.

The artemisinin is sesquiterpene lactone peroxide separated from artemisia annua L, and its derivatives mainly include dihydroartemisinin, artesunate, artemether and arteether, and are specific medicine for treating malaria and also have antifungal and immunoregulatory effects. Zhenghongyan and the like find that the artemisinin residue powder and decoction have different degrees of inhibition effects on partial fungi, and the artemisinin mother liquor with the concentration of 5 percent has very strong inhibition effects on the fungi, which are equivalent to 5 percent of benzoic acid and salicylic acid. Eczema is a common dermatological disease, probably because of the imbalance of Th1/Th2, Guoqing and the like, after peripheral blood T lymphocytes of chronic eczema patients are cultured in vitro with artesunate with different concentrations, the IgE level of the supernatant is detected by enzyme linked immunosorbent assay, and the changes of Th1 and Th2 are detected by a flow cytometer method. The result shows that the artesunate can inhibit the expression of Th1 of peripheral blood lymphocytes of patients with chronic eczema, promote the expression of Th2, is in certain dose dependence, and simultaneously can inhibit the IgE secretion of the peripheral blood lymphocytes of the patients with chronic eczema. Therefore, the immunosuppressive and immunomodulatory effects of artesunate can be used for treating eczema. In order to investigate the clinical practical value of artesunate, the clinical observation and analysis were conducted on 90 patients with skin disease treated by artesunate, wherein 35 cases of eczema, 6 cases of atopic dermatitis, 8 cases of erythema multiforme, 12 cases of solar exanthema multiforme, 15 cases of psoriasis vulgaris, 6 cases of summer blistering disease and 8 cases of dermatomyositis were conducted. The artesunate is used for intravenous drip, the adult dose is 60mg/d, and the pediatric dose is 1.2mg/(kg d). No oral medicine is added in the treatment process, and the treatment effect of different degrees is achieved after 14 days of treatment, and the effect is particularly ideal for eczema, polymorphous light eruption and dermatomyositis.

The Borneolum can be obtained by extracting resin and volatile oil of Borneolum of Agaricaceae, or synthesized by chemical method with Camphora, turpentine, etc. or crystallized from leaf of blumea balsamifera of Compositae. Has the effects of opening orifices, dissipating stagnated fire, removing nebula, improving eyesight, reducing swelling and relieving pain, and can be used as an auxiliary component of some medicaments. It has refreshing effect and is helpful for tranquilizing and relieving itching.

Disclosure of Invention

In view of the above, the present invention aims to provide a regenerated cellulose fiber containing pearl traditional Chinese medicine and a preparation method thereof. The purpose of health and skin care is achieved by adding pearl, artemisinin and derivatives thereof and borneol into the fiber, and the problems that the effective components are easily weakened by acid and alkali and cannot be released continuously and stably in the prior art are solved.

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

a regenerated cellulose fiber containing Margarita and Chinese medicinal materials for preventing erythra comprises Margarita powder and Chinese medicinal extract, the addition amounts of which are 2-5.5 wt% and 2-5 wt% of spinning solution, respectively.

Further, the traditional Chinese medicine extract comprises 80-90% of artemisinin and derivatives thereof and 10-20% of borneol. The artemisinin and the derivatives thereof have certain treatment effect on various skin diseases, and the artemisinin and the derivatives thereof are added into the fibers, so that the anti-inflammatory and bactericidal effects are achieved, and the skin condition of a patient with eczema is improved. The ice product has refreshing effect, eczema is usually accompanied with skin pruritus, and 10-20% of borneol is added into artemisinin and derivatives thereof for tranquilizing and relieving itching.

The preparation method of the regenerated cellulose fiber containing pearl traditional Chinese medicine for preventing the erythema comprises the following steps:

(1) pulverizing Margarita, adding water, stirring to obtain slurry, feeding into a high pressure tank, pressurizing with steam, rapidly decompressing in an expansion chamber, repeating for at least three times, and grinding to obtain Margarita powder; (2) preparing traditional Chinese medicine extract microcapsules; (3) preparing blended spinning solution; (4) spinning and post-processing.

On the other hand, the invention also provides a preparation method of the traditional Chinese medicine extract microcapsule, which comprises the following steps:

s1, dissolving chitosan in an acetic acid solution with the mass concentration of 0.5-2% to prepare a chitosan acetic acid solution with the mass concentration of 1-2%;

s2, crushing the traditional Chinese medicine extract artemisinin, the derivative thereof and the ice product, uniformly dispersing the crushed extract artemisinin, the derivative thereof and the ice product with citric acid and an emulsifier into water, adding the mixture into the chitosan acetic acid solution, then adding sodium citrate, and carrying out high-speed emulsification treatment for 15-30min at the rotating speed of 10000-15000r/min to obtain microcapsules taking the traditional Chinese medicine extract emulsion as a core material and chitosan as a wall material;

s3, adding sodium alginate into the microcapsule with the chitosan as the wall material, stirring at the speed of 200-800r/min, adjusting the pH value to 6-7, mixing with the aqueous solution of calcium chloride, standing, and then adding a cross-linking agent to react for 1-2h to obtain the microcapsule with the traditional Chinese medicine extract as the core material and the chitosan/sodium alginate as the wall material.

Furthermore, in the step (1), the fineness of the pearl powder reaches D95 which is less than or equal to 0.1 μm.

Further, in step S1-3, the mass ratio of the chitosan, the traditional Chinese medicine extract, the sodium alginate, the sodium citrate and the citric acid is 1: (5-18): (1-5): (0.5-1.5): (0.1-0.2).

Further, in step S1, the chitosan has a molecular weight of 30 to 80 ten thousand.

Further, in step S2, the volume ratio of the water for dispersing the herbal extract to the chitosan acetic acid solution is 1: (3-6).

Further, in step S2, the emulsifier is an oil-in-water emulsifier with HLB value in the range of 9-15, and the dosage is 3-10% of the Chinese medicinal extract.

Further, in step S3, the mass concentration of calcium chloride in the aqueous solution of calcium chloride is 3 to 5%.

Further, in step S3, the crosslinking agent is at least one of formaldehyde, glutaraldehyde and epichlorohydrin, and the amount of the crosslinking agent is 2-4% of the total weight of the chitosan and sodium alginate.

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 invention has the following advantages:

(1) after the pearls are crushed and pretreated, the pearl powder is prepared into slurry to be blended with the cellulose spinning solution, the pearl powder has ideal effects on 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 anti-erythra regenerated cellulose fiber containing pearl traditional Chinese medicines is easier to be close to skin so as to achieve the function of beautifying the skin, and pearl contains various amino acids, has the functions of far infrared performance and the like, and has the anti-erythra function when being added into the fiber.

(3) The artemisinin and the derivatives thereof and the borneol are emulsified into nano-scale emulsion to be used as a core material, and the chitosan/sodium alginate is used as a wall material, so that the prepared microcapsule has small size, and the spinning process and the properties of a finished product cannot be influenced when the microcapsule is added into fibers. Simultaneously, the artemisinin and the derivatives thereof and the borneol are prevented from being influenced by acid and alkali in the spinning process.

(4) The fiber is added with artemisinin and derivatives thereof and borneol, and the anti-erythra regenerated cellulose fiber containing pearl traditional Chinese medicines can still release effective components after being repeatedly washed for 50 times, has bactericidal effect and provides a method for improving eczema for patients with 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.

Experimental example 1 pulverization of pearls

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. Feeding the obtained coarsely crushed pearl slurry into a high-pressure tank of high-pressure expansion equipment, pressurizing the pearl slurry by steam, entering an expansion cavity through an expansion valve, recovering to the conventional condition, and repeating for 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 pearl powder has larger grain diameter, the machine can be blocked in the spinning process, and the quality of the prepared fiber is influenced. By adopting the crushing method of the invention, the fineness of the pearl powder is D95 not more than 0.1 mu m, the particle size is in nanometer level, and the addition amount of the pearl powder in the fiber can be increased. And with the increase of times of high-pressure expansion and decompression to conventional conditions, the pearl is easier to be crushed to the nanometer level, and the obtained pearl powder is finer.

Experimental example 2 pretreatment of pearls

The influence of the pretreatment mode on the improvement of the lipophilicity and the dispersibility of the pearl powder is further explored by pretreating the crushed pearl powder. The pearl powder is a hydrophilic and oleophobic substance, has large specific surface area and is easy to agglomerate, so the pearl powder is added into the fiber to be made into a textile, and the absorption effect of the skin is poor. If the pearl powder can change hydrophilicity into lipophilicity, the pearl powder can be better contacted with human skin, and is more beneficial to exerting the efficacy of the pearl. Meanwhile, the more uniform the pearl powder is dispersed, the more favorable the spinning process and the quality of the fiber are.

Adding water into pulverized Margarita powder to obtain 20-35% slurry, and pre-treating by adding span 80, polyethylene glycol 400 and vegetable oil such as palm oil and corn oil into Margarita slurry. The addition amounts of span 80, polyethylene glycol 400 and vegetable oil are 0.5-0.8%, 0.3-0.5% and 0.6-2% of the dry weight of the pearl powder respectively. The vegetable oil contains unsaturated fatty glyceride, and can generate physical adsorption with pearl hydroxyl after being added into pearl powder to form a coating layer and inhibit secondary aggregation of pearl powder. Meanwhile, the span 80, the polyethylene glycol 400 and the vegetable oil act synergistically, so that the repulsion force on the surface of the pearl powder is increased, the dispersibility and the stability are improved, the surface of the pearl powder is changed from hydrophilicity to lipophilicity, and the affinity of the pretreated pearl to the skin is enhanced.

The oleophylic property testing method comprises the following steps: the pearl powder is put into deionized water, the water is still completely transparent after stirring, and then the pearl powder is put into white oil, no particles float on the surface, which shows that the obtained pearl powder has good lipophilicity. The agglomeration property is measured by placing the pearl powder in deionized water for 6 months and observing the agglomeration property. Specific amounts of addition and performance indices are shown in table 1.

TABLE 1

As can be seen from Table 1, the pearl powders of groups 1-4 have good lipophilicity, good dispersibility and are not easy to agglomerate after being treated by span 80, polyethylene glycol 400 and vegetable oil. The pearl powder of the control group 1 is added with only vegetable oil, which can improve lipophilicity, but has poor dispersibility and is easy to agglomerate. The pearl powder of the control group 2 was not treated at all, was poor in lipophilicity and easily agglomerated.

The regenerated cellulose fiber containing pearl Chinese medicine for preventing erythra in the following examples adopts the crushing and pretreatment method of pearl in experimental examples 1-2.

Experimental example 3 research on preparation process of microcapsule of Chinese medicinal extract

The process study of preparing microcapsules by using artemisinin and its derivatives and borneol as the extracts of Chinese herbs is explored through the following examples and comparative examples. The artemisinin and the derivatives thereof are extracted from the artemisia annua plant by adopting the existing extraction method. The ice product is purchased from the market.

Example 1

1kg of chitosan with the molecular weight of 30 ten thousand is dissolved in 100L of acetic acid solution with the mass concentration of 0.5 percent. Pulverizing 4kg of artemisinin and its derivatives and 1kg of ice, adding 0.1kg of citric acid and 0.15kg of tween with HLB value of 13, uniformly dispersing in 33L of water, adding into the acetic acid solution, and adding 0.5kg of sodium citrate. Mixing, and emulsifying at 10000r/min for 20min to obtain microcapsule with traditional Chinese medicine extract emulsion as core material and chitosan as wall material.

1kg of sodium alginate is mixed into the microcapsule with the chitosan as the wall material, the mixture is stirred at the speed of 500r/min, and the pH value is adjusted to 6 by using sodium hydroxide. Then pouring the mixture into a calcium chloride solution with the mass concentration of 5%, mixing, standing for two days, adding 0.08kg of glutaraldehyde, reacting for 2 hours to obtain the microcapsule with the traditional Chinese medicine extract emulsion as a core material and the chitosan/sodium alginate as a wall material, wherein the average particle size of the microcapsule is 2.5 microns, and the proportion of the microcapsule with the particle size larger than 4 microns is 5%.

Example 2

0.3kg of chitosan with the molecular weight of 50 ten thousand is dissolved in 10L of acetic acid solution with the mass concentration of 2 percent. Pulverizing 4.8kg of artemisinin and its derivatives and 0.6kg of ice product, adding 0.06kg of citric acid and 0.54kg of egg yolk lecithin, uniformly dispersing in 1.67L of water, adding into the acetic acid solution, and adding 0.45kg of sodium citrate. And (3) after mixing, carrying out high-speed emulsification treatment for 15min at the rotating speed of 30000r/min to obtain the microcapsule taking the traditional Chinese medicine extract emulsion as a core material and chitosan as a wall material.

1.5kg of sodium alginate is mixed into water and then added into the microcapsule taking chitosan as the wall material, the mixture is stirred at the speed of 200r/min, and the pH value is adjusted to 7 by sodium hydroxide. Then pouring a calcium chloride solution with the mass concentration of 3% for mixing, standing for one day, adding 0.04kg of formaldehyde, standing for 2 hours to obtain the microcapsule with the traditional Chinese medicine extract emulsion as a core material and the chitosan/sodium alginate as a wall material, wherein the average particle size of the microcapsule is 2.0 microns, and the proportion of the microcapsule with the particle size larger than 4 microns is 3%.

Experimental example 3

2kg of chitosan with the molecular weight of 80 ten thousand is dissolved in 100L of acetic acid solution with the mass concentration of 2 percent. Pulverizing 17kg of artemisinin and its derivatives and 3kg of ice, adding 0.3kg of citric acid and 1kg of sucrose fatty acid ester with HLB value of 11, uniformly dispersing in 20L of water, adding into the acetic acid solution, and adding 2kg of sodium citrate. And (3) after mixing, carrying out high-speed emulsification treatment for 30min at the rotating speed of 30000r/min to obtain the microcapsule taking the traditional Chinese medicine extract emulsion as a core material and chitosan as a wall material.

Mixing 6kg of sodium alginate into water, adding the mixture into the microcapsule with chitosan as a wall material, stirring the mixture at the speed of 400r/min, and adjusting the pH value to 6 by using sodium hydroxide. Then pouring a calcium chloride solution with the mass concentration of 4%, standing for one day, adding 0.24kg of epoxy chloropropane, reacting for 2h to obtain the microcapsule with the traditional Chinese medicine extract emulsion as a core material and the chitosan/sodium alginate as a wall material, wherein the average particle size of the microcapsule is 1.8 mu m, and the proportion of the microcapsule with the particle size of more than 4 mu m is 3%.

Comparative example 1

The procedure, operating conditions and parameters of comparative example 1 were the same as those of example 3. Except that no citric acid is added in the process of emulsifying the traditional Chinese medicine extract.

Comparative example 2

The procedure, operating conditions and parameters of comparative example 2 were the same as those of example 3. Except that no sodium citrate is added in the process of emulsifying the traditional Chinese medicine extract.

Comparative example 3

The procedure, operating conditions and parameters of comparative example 3 were the same as those of example 3. Except that no calcium chloride solution was added during the preparation of the microcapsules.

Comparative example 4

The procedure, operating conditions and parameters of comparative example 4 were the same as those of example 3. Except that no epichlorohydrin crosslinking was added during the preparation of the microcapsules.

Observing the appearance of the traditional Chinese medicine extract emulsion during preparation, measuring the particle size of the emulsion, and the stability under the centrifugation condition of 5000r/min and 30 min. The results are shown in Table 2.

TABLE 2

Serial number Appearance of the product Particle size (nm) Centrifugal stability
Example 1 Uniform milky white color 600 Not delaminating
Example 2 Uniform milky white color 750 Not delaminating
Example 3 Uniform milky white color 750 Not delaminating
Comparative example 1 Uniform milky white color 1000 Layering
Comparative example 2 Uniform milky white color 1000 Layering
Comparative example 3 Uniform milky white color 800 Not delaminating
Comparative example 4 Uniform milky white color 850 Not delaminating

As can be seen from Table 2, in the preparation process of the traditional Chinese medicine extract emulsions of examples 1-3 and comparative examples 3-4, the particle size of the emulsion obtained after emulsification is between 600 and 850nm by adding citric acid into the traditional Chinese medicine extract and adding sodium citrate into the chitosan acetic acid solution, and the emulsion has stable properties and does not generate layering after centrifugation. Comparative example 1 no citric acid was added during emulsification, comparative example 2 no sodium citrate was added during emulsification, the particle size of the prepared emulsion was 1000nm, and delamination occurred after centrifugation. Presumably, in the emulsification process, citric acid is added into the core material traditional Chinese medicine extract, and sodium citrate is added into the wall material, so that citric acid and sodium citrate can be respectively combined with the hydrophilic end and the lipophilic end of the emulsifier, which is beneficial to stabilizing the surface of the emulsion and not easy to aggregate and grow, and therefore, the particle size of the emulsion is smaller.

The embedding rates of the microcapsules prepared in examples 1 to 3 and comparative examples 1 to 4 were calculated. The embedding rate (the content of the core material of the emulsion of the traditional Chinese medicine extract in the prepared microcapsule/the feeding amount of the core material) is 100 percent. The results are shown in Table 3.

TABLE 3

As is clear from Table 3, the microcapsules of examples 1 to 3 had an encapsulation efficiency of 91.0 to 93.2%. The embedding rates of comparative examples 1-2 were 88.3% and 85.1%, respectively, probably because the particle size of the core emulsion was large, and therefore the embedding rate was affected. The addition of the sodium citrate is not only beneficial to emulsification, but also can perform complex coacervation with the chitosan in the emulsification process, so that the chitosan wall material and the core material are combined more firmly, and the embedding rate is improved. The microcapsule wall materials of examples 1-3 adopt a combination of ionic crosslinking and chemical crosslinking. The protonated chitosan and sodium citrate are subjected to electrostatic interaction, and sodium alginate and calcium ions are crosslinked, but the ionic crosslinking is usually not stable enough, so that the crosslinking agent is used for crosslinking between molecules and in molecules of the chitosan and sodium alginate to form a network structure. By adopting the combined crosslinking mode, the embedding rate of the traditional Chinese medicine extract emulsion can be improved, for example, the comparative examples 2-4 are all single crosslinking modes, and the embedding rate is lower than that of the examples 1-3. Meanwhile, after the microcapsule is added into the spinning solution, the compactness of the microcapsule is good, the tolerance to acid and alkali is improved in the spinning process, and the traditional Chinese medicine extract can be protected from the influence of the acid and alkali. In the experimental process, chitosan and sodium alginate after ion crosslinking can realize crosslinking only by using 2-4% of chemical crosslinking agent. The chemical cross-linking agent glutaraldehyde has certain side effect on human body, and the invention can reduce the usage amount of the chemical cross-linking agent.

Preparation of fibers

Pearl powder having D95 ≤ 0.1 μm was prepared according to the pearl pulverization and pretreatment methods of experimental examples 1-2. According to the process method of the traditional Chinese medicine extract microcapsule of the experimental example 3, the microcapsule with the traditional Chinese medicine extract as the core material and chitosan/sodium alginate as the wall material is prepared. Preparing the pearl powder into slurry with pearl powder solid content of 20-25% according to the dosage of the pearl powder being 2-5.5% of the viscose fiber spinning solution, injecting the traditional Chinese medicine extract embedded in the microcapsule into the viscose fiber spinning solution according to the dosage of the traditional Chinese medicine extract being 2-5% of the viscose fiber spinning solution, and mixing. The spinning and post-treatment process is carried out according to the conventional process of viscose staple fiber. The prepared fiber meets the standard of GB/T14463-. Therefore, the pearl powder and the traditional Chinese medicine extract which are added by the preparation method of the invention can not influence the performance of the fiber. Of course, the viscose filaments can also be produced according to conventional processes, which are not described in detail again. Specific feed ratios are shown in table 4.

TABLE 4

Pharmacological experiment-anti-inflammatory experiment

The experimental method comprises the following steps: 50 mice were randomly divided into 5 groups of 10 mice each, and divided into a negative control group, an example 4 group, an experimental example 5 group, an experimental example 6 group and a positive drug 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 the traditional Chinese medicine extract), and the content of the ointment per unit area was the same as that of the traditional Chinese medicine extract per unit area of the fibers prepared in example 4. The fiber products of examples 4-6 and the positive control group were coated on the right ear of the mouse at a size of 2cm × 2cm, and the negative control group was coated with distilled water on the front and rear sides of the right ear of the mouse. After 1h of administration, 0.03ml of xylene is uniformly smeared on the right and the front sides of the right ear of a mouse to cause inflammation, and after 2h, the mouse is dislocated and killed, and the thickness of the two ears is measured. The swelling degree (mm) is the difference between the thicknesses of both ears, and the swelling inhibition (%) (negative control group ear thickness difference-sample group ear thickness difference)/negative control group ear thickness difference. The results are shown in Table 5.

TABLE 5

Group of Number of animals (only) Swelling degree (mm) Swelling inhibition ratio (%)
Negative control group 10 0.158±0.042
Positive control group 10 0.059±0.078* 62.66
Example 4 10 0.069±0.049** 56.33
Example 5 10 0.082±0.052** 48.10
Example 6 10 0.091±0.058** 42.41

Note: p < 0.01, P < 0.05, compared to the negative control group.

As can be seen from table 5, the experimental group and the positive control group both reduced the effect of ear swelling of mice caused by xylene compared to the negative control group, and had statistical differences. The inhibition rate of swelling of the positive control group was 62.66%, the amounts of the Chinese herbal extracts of examples 4-6 were 5%, 3% and 2%, respectively, and the inhibition rates were 56.33%, 48.10% and 42.41%, respectively. Therefore, the artemisinin, the derivatives thereof and the ice product are added in the process before spinning, and the prepared fiber has the effect of inhibiting inflammation and improving the erythra.

Bacteriostatic activity

The skin of the patient with erythra has higher microbial detection rate than normal skin, and is usually associated with certain bacteria and fungi. Samples of examples 4-5 and comparative examples 5-7 were taken to determine the inhibition rate against Candida albicans. The bacteriostatic rate of the prepared fiber on candida albicans and the bacteriostatic effect of the fiber after being washed for 50 times are detected according to an oscillation method in the antibacterial performance of the textile in GB/T20944.3-2008, and the results are shown in Table 6.

TABLE 6

The anti-erythra regenerated cellulose fiber prepared by the pearl-containing traditional Chinese medicines in the embodiments 4-6 of the invention has a bacteriostatic rate of 95.2-99.9% against candida albicans, and the bacteriostatic rate is reduced less after 50 times of water washing. In the preparation process of comparative examples 5 to 7, the wall material of the microcapsule of the traditional Chinese medicine extract is crosslinked, which is different from that in examples 4 to 6, and the bacteriostasis rate is reduced more after 50 times of water washing. The possible reasons are that the wall material is damaged and the effective components of the traditional Chinese medicine extract are lost in the process of repeatedly washing the fiber by a single ionic crosslinking mode or a chemical crosslinking mode.

With reference to tables 5-6, it can be seen that, with the method of the present invention, firstly, the content ratio of artemisinin, its derivatives and ice in the extract of Chinese herbs has the effects of anti-inflammation and sterilization, and the effect of preventing erythra is exerted; secondly, the preparation of the microcapsule can protect the components of the traditional Chinese medicine extract, reduce the loss and the damage of strong acid and strong base in the spinning post-treatment process, and the prepared fiber can play the effects of artemisinin, derivatives thereof and borneol; finally, the microcapsule adopts a mode of combining ionic crosslinking and chemical crosslinking, so that the wall material is more compact, the wall material is still not damaged after being washed by water for 50 times, the active ingredients of the core material traditional Chinese medicine extract can still be released, and the slow release effect is achieved.

Performance of pearl

GB/T30127-2013 is adopted to detect the far infrared performance of the anti-erythema regenerated cellulose fiber of the prepared pearl-containing traditional Chinese medicine, and the result is shown in Table 7.

TABLE 7

As can be seen from Table 7, the regenerated cellulose fiber for preventing erythema of the pearl-containing traditional Chinese medicines of examples 4 to 6 of the present invention has a far infrared emissivity of 0.90 to 0.93%, a far infrared radiation temperature of 1.6 to 1.9 ℃, and a far infrared property. After repeated washing for 50 times, the far infrared emissivity is 0.88-0.91%, the far infrared radiation temperature is 1.5-1.7 ℃, the far infrared performance is still maintained, and the reduction is small.

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.

11页详细技术资料下载
上一篇:一种医用注射器针头装配设备
下一篇:一种珍珠中药防湿疹再生纤维素纤维及其制备方法

网友询问留言

已有0条留言

还没有人留言评论。精彩留言会获得点赞!

精彩留言,会给你点赞!