CN117344399B

CN117344399B - Large biological polyester fiber containing plant active ingredients and preparation method thereof

Info

Publication number: CN117344399B
Application number: CN202311639245.4A
Authority: CN
Inventors: 黄效华; 池姗; 刘彦明
Original assignee: Qingdao Baicao New Material Co ltd; Zhongke Textile Research Institute Qingdao Co ltd; Weifang Ruiyin Textile Technology Co ltd; Bestee Material Tsingtao Co Ltd
Current assignee: Qingdao Baicao New Material Co ltd; Zhongke Textile Research Institute Qingdao Co ltd; Weifang Ruiyin Textile Technology Co ltd; Bestee Material Tsingtao Co Ltd
Priority date: 2023-12-04
Filing date: 2023-12-04
Publication date: 2024-03-19
Anticipated expiration: 2043-12-04
Also published as: CN117344399A

Abstract

The invention provides a large biological polyester fiber containing plant active ingredients and a preparation method thereof, belonging to the field of polyester fibers. The preparation method of the large biological polyester fiber containing the plant active ingredients comprises the following steps: extracting main components, extracting auxiliary components, preparing a first modifier, preparing a second modifier, preparing functional master batch and spinning. According to the preparation method of the large biological polyester fiber containing the plant active ingredients, the effective modification of the polyester fiber can be realized by adopting a plurality of plant active ingredients, and the main ingredients and the auxiliary ingredients in the plurality of plant active ingredients can be matched under the condition of optimal proportioning dosage for a long time, so that the improvement, the alleviation and the prevention of eczema are realized, and the long-term effectiveness is good.

Description

Large biological polyester fiber containing plant active ingredients and preparation method thereof

Technical Field

The invention relates to the field of polyester fibers, in particular to a large biological polyester fiber containing plant active ingredients and a preparation method thereof.

Background

Polyester fiber, also called polyester fiber, is polyester high polymer fiber obtained by spinning polyester formed by polycondensation of organic dibasic acid and dihydric alcohol. The polyester fiber has a series of excellent properties such as high breaking strength and elastic modulus, moderate rebound resilience, excellent heat setting effect, good heat resistance and light resistance and the like.

The melting point of the polyester fiber is about 255 ℃, the glass transition temperature is about 70 ℃, the shape is stable in the production and application processes, the fabric can be leveled after being washed without ironing or slightly ironing, and the washing wearability is good. In addition, the polyester fiber has excellent resistance (such as organic solvent resistance, soap resistance, detergent resistance, bleaching liquid resistance, oxidant resistance and the like), better corrosion resistance and stable performance in weak acid, alkali and other environments. Therefore, the polyester fiber has a wide application range. Meanwhile, with the rapid development of the petroleum industry, a richer and cheaper raw material is provided for the production of the polyester fiber, and the rapid development of chemical, mechanical and automatic control technology in recent years ensures that the polyester fiber gradually realizes short-cut, continuous, automatic and high-speed in the processes of raw material production, fiber forming, processing modification, spinning and the like. Therefore, the polyester fiber is the synthetic fiber variety with the highest development speed and highest yield.

With the development of organic synthesis, polymer science and polyester fiber industry, various functional polyester fibers with different characteristics have been developed in the prior art; such as high-strength polyester fiber, high-elastic polyester fiber, plant component modified fiber, inorganic component modified fiber, etc. The large biological polyester fiber, namely the large biological functional polyester fiber, is prepared by adding a certain amount of functional materials (such as plant components and inorganic components) which can act on human bodies or other organisms into a polymer of polyester high polymer, so as to realize the functional modification of the polyester fiber, thereby endowing the polyester fiber with one or more functions. In recent years, the variety of the biological functional polyester fiber at home and abroad is various, and the biological functional polyester fiber is continuously promoted to be new, and has wide application prospect. Therefore, the large biological functional polyester fiber becomes the development focus of the polyester fiber field in the future, and has important significance for the research and development and expansion of the functionality of the polyester fiber.

Eczema is a skin inflammatory reaction with severe itching caused by various internal and external factors, and has the characteristics of polymorphism, symmetry, itching, easy repeated attack and the like. The etiology of eczema is complex, usually as a result of interaction between internal and external causes. Internal causes such as chronic digestive system diseases, mental stress, insomnia, excessive fatigue, mood changes, endocrine dyscrasia, infection, metabolic disorder, etc.; external factors such as living environment, climate change, food, etc. may cause eczema. At the same time, external stimuli such as sunlight, cold, dryness, heat, hot water scalding, and various animal fur, plants, cosmetics, soaps may induce eczema. In recent years, the incidence rate of eczema is about 15-20%, and children and adults are likely to suffer from eczema, so that daily work and study of people are seriously affected. In addition, in the prior art, hormone western medicines are mostly adopted to treat eczema, so that the side effect is large, the eczema cannot be radically treated, and the repeated attacks of the eczema cannot be prevented or prevented. Meanwhile, in the prior art, the treatment method of externally applying the gauze impregnated with the Chinese medicinal liquid to the eczema part is also provided, but the gauze is inconvenient to use, has poor air permeability after absorbing the liquid, and can also stimulate the eczema to aggravate the illness state.

In order to solve the above-mentioned drawbacks, the inventors hope to develop a large biological polyester fiber containing plant active ingredients, and functionally modify the polyester fiber by adopting plant active ingredients capable of mutually cooperating to improve or alleviate eczema, so as to realize effective exertion and long-acting slow release of the plant active ingredients on the large biological polyester fiber, and finally realize effective improvement, alleviation and prevention effects on eczema. Meanwhile, the functionally modified large biological polyester fiber can be prepared into downstream products such as bandages, medical patches, vests, bellyband and underwear, and the targeted improvement, alleviation and prevention of eczema are realized by matching various plant active ingredients of the large biological polyester fiber in a slow release manner, and the side effects of external application western medicines or plant active ingredients are avoided.

However, the inventors have found that the following problems exist in the modification of polyester fibers by blending various plant active ingredients: firstly, after the polyester fiber is functionally modified by adopting a plurality of plant active ingredients, the release efficiency is inconsistent due to the different properties of main ingredients and auxiliary ingredients in the plurality of plant active ingredients, and the main ingredients and the auxiliary ingredients cannot be effectively matched, so that ideal improvement, alleviation and prevention effects on eczema cannot be realized. Secondly, the combination property of various plant active ingredients and polyester fibers is different, the stability is not ideal, when the polyester fibers are influenced by external factors (such as water washing, high temperature, high humidity, illumination and the like), the loss rates of the various plant active ingredients are different, the various plant active ingredients in the polyester fibers can not be matched under the condition of optimal proportioning dosage, and further the long-term improvement, alleviation and prevention effects of the large biological polyester fibers on eczema are influenced, and the long-term effectiveness is poor. Thirdly, in the functional modification and spinning process of polyester fibers, the various plant active ingredients are greatly influenced by the technological conditions such as the properties of fiber raw materials, melt spinning ingredients, temperature and the like, and are easy to lose efficacy, and main ingredients and auxiliary ingredients in the various plant active ingredients cannot be effectively matched under the condition of optimal proportioning dosage, so that ideal improvement, alleviation and prevention effects on eczema cannot be realized.

Disclosure of Invention

In order to solve the technical problems in the prior art, the invention provides the large biological polyester fiber containing the plant active ingredients and the preparation method thereof, which can effectively modify the polyester fiber by adopting a plurality of plant active ingredients, and the main ingredients and auxiliary ingredients in the plurality of plant active ingredients can be matched under the condition of optimal proportioning dosage for a long time, thereby realizing targeted improvement, alleviation and prevention effects on eczema and having good long-term effectiveness.

In order to solve the technical problems, the technical scheme adopted by the invention is as follows:

a preparation method of a large biological polyester fiber containing plant active ingredients comprises the following steps: extracting main components, extracting auxiliary components, preparing a first modifier, preparing a second modifier, preparing functional master batch and spinning.

The method for extracting the main components comprises cleaning stem and leaf of fructus Cnidii, placing in an environment with vacuum degree of 0.01-0.02MPa, controlling drying temperature to 65-75deg.C, and keeping temperature and pressure until the moisture content of stem and leaf of fructus Cnidii is 4-6wt%; then transferring into a superfine pulverizer, controlling superfine pulverizing temperature to 38-42 ℃ and rotational speed to 4000-4500rpm, pulverizing to 1800-2000 mesh, and obtaining fructus Cnidii micropowder; then putting the cnidium fruit micro powder into a supercritical carbon dioxide extraction device, introducing carbon dioxide at an introducing rate of 12-16kg/h, and controlling the pressure in the supercritical carbon dioxide extraction device to be 10-12MPa; then heating to 40-45deg.C at a heating rate of 0.5-0.7deg.C/min, and extracting under heat and pressure for 5-6 hr to obtain extract of main component.

The stem and leaf of the cnidium fruit adopted in the step of extracting the main components is warm in nature and pungent in taste, and has the effects of eliminating dampness and dispelling wind, clearing heat and detoxicating, diminishing inflammation and relieving itching. The prepared large biological polyester fiber containing plant active ingredients can be used as a monarch drug.

The method for extracting auxiliary components comprises cleaning radix Clematidis, radix Saposhnikoviae, herba Taraxaci, and folium Bambusae, respectively, placing in an environment with vacuum degree of 0.01-0.02MPa, controlling drying temperature to 65-75deg.C, and keeping temperature and pressure until water content is 4-6wt%; then transferring the dried radix clematidis, radix saposhnikoviae, dandelion and bamboo leaves into an air flow pulverizer, mixing and pulverizing to 100-150 meshes, transferring into a superfine pulverizer, controlling the superfine pulverizing temperature to 38-42 ℃ and the rotating speed to 4000-4500rpm, and pulverizing to 1800-2000 meshes to obtain mixed plant micropowder; then the mixed plant micro powder is put into a supercritical carbon dioxide extraction device, carbon dioxide is introduced at the introducing rate of 16-20kg/h, and the pressure in the supercritical carbon dioxide extraction device is controlled to be 13-15MPa; then heating to 40-45deg.C at a heating rate of 0.5-0.7deg.C/min, and extracting under heat and pressure for 5-6 hr to obtain auxiliary component extract.

In the auxiliary extraction components, the weight ratio of the radix clematidis to the radix saposhnikoviae to the dandelion to the bamboo leaves is 10-12:7-8:1-1.5:0.8-1.2.

The clematis root adopted in the step of extracting the auxiliary components is warm in nature, pungent and salty in taste, and has the effects of dispelling wind and removing dampness, and dredging collaterals and relieving pain. The prepared large biological polyester fiber containing plant active ingredients can be used as ministerial drug to assist monarch drug.

Radix Saposhnikoviae, slightly warm in nature, pungent and sweet in taste, has effects of dispelling pathogenic wind, relieving exterior syndrome, eliminating dampness, relieving pain, and relieving spasm. The prepared large biological polyester fiber containing plant active ingredients is used as an adjuvant and matched with a monarch drug to play a role.

Dandelion is cold in nature, sweet in taste and slightly bitter in flavor, and has the effects of clearing heat and detoxicating, dispelling wind and dissipating heat. The prepared large biological polyester fiber containing plant active ingredients can be used as a drug to be matched with other drugs.

Bamboo leaves are cold in nature, sweet and light in taste, and have the effects of clearing heat, calming, resisting bacteria and diminishing inflammation. The prepared large biological polyester fiber containing plant active ingredients can be used as a drug to be matched with other drugs.

The preparation of the first modifier comprises the following steps: preparing a composite carrier, modifying and loading.

The method for preparing the composite carrier comprises the steps of putting titanyl sulfate into deionized water with the weight of 80-100 times, stirring at normal temperature until the titanyl sulfate is completely dissolved, then mixing the solution with phosphate buffer solution and absolute ethyl alcohol, and stirring at normal temperature for 1-2 hours to obtain mixed solution; simultaneously, in the stirring process, the pH value of the mixed solution is controlled to be within the range of 6.5-6.8 by adopting sodium hydroxide solution; adding macroporous nano silicon dioxide with the weight of 0.1-0.15 times of that of the mixed solution after stirring at normal temperature, regulating the pH value to 2-2.5 by adopting hydrochloric acid solution after ultrasonic dispersion uniformly, heating to 550-600 ℃ at the heating rate of 5-7 ℃/min, preserving heat for 1.5-2.5h, naturally cooling to 25-30 ℃, preserving heat and standing for 10-12h, filtering out solid matters, washing the solid matters by adopting deionized water with the volume of 8-10 times for 2-3 times, continuously washing the solid matters by adopting absolute ethyl alcohol with the volume of 8-10 times, and then placing the solid matters in the environment with the vacuum degree of 0.04-0.05MPa, and drying to constant weight at the temperature of 80-90 ℃ to obtain the composite carrier.

In the preparation of the composite carrier, the pH value of the phosphate buffer solution is 6.5-6.8;

in the mixed solution, the weight ratio of deionized water, phosphate buffer solution and absolute ethyl alcohol is 6-7:10-12:7-8;

the concentration of the sodium hydroxide solution is 0.6 to 0.7 weight percent;

the concentration of the hydrochloric acid solution is 0.2-0.25mol/L.

The modification treatment method comprises the steps of putting the composite carrier into an electrolytic tank containing electrolyte with the volume of 20-25 times, controlling the modification voltage to be 1.6-1.7V/cm, carrying out electric modification treatment for 1.5-2 hours, separating out solid matters, washing the solid matters by using deionized water with the volume of 8-10 times, and drying at the temperature of 80-90 ℃ to constant weight under the environment with the vacuum degree of 0.04-0.05MPa to obtain the modified composite carrier.

In the modification treatment, the electrolyte is calcium chloride aqueous solution with the mass concentration of 0.03-0.035%.

The loading method comprises the steps of putting the modified composite carrier into 10-12 times of loading liquid in parts by weight, uniformly dispersing by ultrasonic, vacuumizing to a vacuum degree of 0.085-0.095MPa under stirring, maintaining the vacuum for 40-60min, breaking the vacuum, pressurizing to 3-4MPa, maintaining the pressure for 1-2h, and recovering to normal pressure; then heating to 35-40 ℃, stirring at 30-60rpm for 18-20h, and filtering out solid matters; washing solid with 8-10 times of deionized water, placing in a vacuum degree of 0.01-0.02MPa, drying at 75-85deg.C to constant weight, and grinding uniformly to obtain the first modifier.

In the loading, the preparation method of the loading liquid comprises the steps of adding main component extracts, tetradecyl dimethyl betaine, sodium carboxymethyl cellulose and a silane coupling agent kH-550 into an ethanol solution, and uniformly dispersing to obtain the preparation;

in the loading liquid, the weight ratio of the main components of extract, tetradecyl dimethyl betaine, sodium carboxymethyl cellulose, a silane coupling agent KH-550 and ethanol solution is 20-22:0.06-0.07:0.1-0.12:0.5-0.6:55-60;

the volume concentration of the ethanol solution is 50-55%.

Adding auxiliary component extracts, sodium dodecyl sulfate and fatty alcohol polyoxyethylene ether AEO-9 into deionized water, uniformly dispersing by ultrasonic, heating to 45-55 ℃ at a heating rate of 1-1.5 ℃/min under a stirring condition, and carrying out heat preservation and stirring for 30-40min to obtain core material liquid; adding starch octenyl succinate, carrageenan and sodium alginate into deionized water, heating to 40-50 ℃, and carrying out ultrasonic emulsification uniformly to obtain wall material liquid; then the core material liquid is put into wall material liquid with the volume of 1.8-2 times, after ultrasonic dispersion is carried out for 30-50min, the primary homogenizing pressure is controlled to be 12-15MPa, and after primary homogenizing is carried out for 5-10 min; controlling the secondary homogenizing pressure to 25-28MPa, carrying out secondary homogenizing for 5-10min, and spray drying to obtain the second modifier.

In the preparation of the second modifier, in the core material liquid, the weight ratio of auxiliary components of extract, sodium dodecyl sulfate, fatty alcohol polyoxyethylene ether AEO-9 and deionized water is 20-22:0.15-0.25:0.08-0.12:50-60;

in the wall material liquid, the weight ratio of the octenyl succinic acid starch ester to the carrageenan to the sodium alginate to the deionized water is 1.5-2:0.6-0.8:0.05-0.06:160-180.

The method for preparing the functional master batch comprises the steps of uniformly mixing polyester chips, a first modifier, sodium stearate, polytrimethylene terephthalate and an antioxidant 1790, putting into a double-screw extruder, and carrying out melting, extrusion and granulation to obtain a first functional master batch; and uniformly mixing polyester chips, a second modifier, sodium stearate, polytrimethylene terephthalate and an antioxidant 1790, putting into a double-screw extruder, and melting, extruding and granulating to obtain the second functional master batch.

In the preparation of the functional master batch, in the first functional master batch, the weight ratio of polyester chips, a first modifier, sodium stearate, polytrimethylene terephthalate and an antioxidant 1790 is 80-90:10-11:0.5-0.6:1.2-1.5:1-1.2;

in the second functional master batch, the weight ratio of the polyester chips to the second modifier to the sodium stearate to the polytrimethylene terephthalate to the antioxidant 1790 is 80-90:19-21:0.5-0.6:1.2-1.5:1-1.2.

The spinning method comprises the steps of uniformly mixing polyester chips, first functional master batches and second functional master batches, putting into a double-screw extruder, performing melt extrusion and metering, introducing into a spinning machine for spinning, controlling the spinning temperature to be 270-275 ℃, controlling the spinning speed to be 3500-3800m/min, controlling the drafting temperature to be 160-170 ℃ after preparing fibers, controlling the drafting multiple to be 3.2-3.3 times, and performing primary drafting; controlling the drafting temperature to be 110-120 ℃ and the drafting multiple to be 2-2.2 times, and oiling and winding after secondary drafting to prepare the large biological polyester fiber containing plant active ingredients.

In the spinning, the weight ratio of the polyester chips to the first functional master batch to the second functional master batch is 100:4-5:6.5-7.5.

A large biological polyester fiber containing plant active components is prepared by the preparation method.

Compared with the prior art, the invention has the beneficial effects that:

(1) The preparation method of the large biological polyester fiber containing plant active ingredients comprises the steps of extracting principal ingredients of the cnidium monnieri, treating the principal ingredients, and extracting the principal ingredients by supercritical carbon dioxide to obtain principal ingredient extract containing the principal ingredients of the plant active ingredients of the cnidium monnieri; extracting auxiliary components of radix Clematidis, radix Saposhnikoviae, herba Taraxaci, and herba Lophatheri, and extracting with supercritical carbon dioxide to obtain auxiliary component extract containing other medicinal plant active components; in the preparation of the first modifier, macroporous nano silicon dioxide and porous titanium dioxide are combined in an in-situ generation mode, so that the loading and controlled release performance of the active ingredients of the monarch drug plants are improved, and the active ingredients of the plants can be matched within the effective proportioning dosage range for a long time; meanwhile, the composite carrier is subjected to hydroxylation electric modification treatment by combining modification treatment, so that on one hand, the loading and controlled release performance of the active ingredients of the monarch medicine plants are further improved, on the other hand, the combination performance of the first modifier and the polyester fibers is improved, and the stability of the first modifier in the polyester fibers is improved; in the preparation of the second modifier, coating the core material liquid containing the plant extract as an auxiliary component by adopting a composite wall material; after the first modifier and the second modifier are respectively adopted to prepare the functional master batches, the first functional master batches and the second functional master batches are matched to be used in the spinning preparation of the polyester fibers, so that the problem that after the polyester fibers are functionally modified by adopting various plant active ingredients, the release efficiency is inconsistent due to the fact that the main ingredients (monarch ingredients) and auxiliary ingredients (ministerial drugs, adjuvant drugs and drug ingredients) in the various plant active ingredients are different in nature, and the main ingredients and the auxiliary ingredients cannot be effectively matched can be effectively avoided; meanwhile, the combination property of various plant active ingredients and the polyester fiber is good, the stability is high, the loss is not easy, the various plant active ingredients in the polyester fiber can be matched under the condition of optimal proportioning dosage for a long time, the improvement, alleviation and prevention effects on corresponding symptoms are stable, and the long-term effectiveness is good; meanwhile, the condition that various plant active ingredients fail in the functional modification and spinning processes of the polyester fiber can be effectively avoided.

(2) In the large biological polyester fiber containing plant active ingredients, the first modifier is prepared from the main component extract containing the principal component of the monarch drug plant active ingredients; the preparation method is combined with a second modifier prepared from auxiliary component extracts of ministerial drugs radix clematidis, adjuvant drugs radix sileris, messenger drugs dandelion and messenger drugs bamboo leaves, and different treatment methods in preparing the first modifier and preparing the second modifier are adopted aiming at the characteristics and the matching relation of the active components of each plant, so that the effective controlled release of the active components of different plants in the modified active components is realized, the release efficiency of the active components of each plant in polyester fiber is consistent, and the modified active components can be matched within the effective proportioning dosage range for a long time, so that the targeted improvement, alleviation and prevention of eczema are realized; experiments prove that the traditional Chinese medicine composition can effectively eliminate or obviously relieve chronic eczema for patients suffering from chronic eczema, has no recurrence or aggravation during application, and has the total of obvious efficiency and effective efficiency up to 100%; at the same time, eczema does not relapse or aggravate within 30 days of stopping administration.

(3) The large biological polyester fiber containing the plant active ingredient has good antibacterial function besides the aim of improving, relieving and preventing eczema, and the antibacterial rate of the large biological polyester fiber to staphylococcus aureus is 99.9-99.7%, the antibacterial rate to escherichia coli is 99.1-99.2%, and the antibacterial rate to candida albicans is 95.2-95.7% through detection.

(4) The large biological polyester fiber containing the plant active ingredients has good combination property and stability of various plant active ingredients and polyester fiber, is not easy to run off when being influenced by external factors (such as water washing, high temperature, high humidity, illumination and the like), and has good long-term effectiveness; through experiments, after the large biological polyester fiber containing the plant active ingredient is washed with 60 ℃ high temperature water for 15 times and is air-dried under illumination, the antibacterial rate of the large biological polyester fiber to staphylococcus aureus still can reach 93.9-94.4%, the antibacterial rate to escherichia coli still can reach 93.1-93.4%, and the antibacterial rate to candida albicans still can reach 88.9-89.8%.

(5) The large biological polyester fiber containing the plant active ingredients can be effectively combined with the large biological polyester fiber, so that the modified polyester fiber can be functionally modified, the physical properties of the modified polyester fiber are prevented from being reduced, and the physical properties of the polyester fiber are effectively maintained; according to detection, the breaking strength of the large biological polyester fiber containing the plant active ingredient is 5.4-5.7cN/dtex, the breaking elongation is 24-25%, the dry heat shrinkage at 180 ℃ is 3-3.5%, and the defect content is 3.4-3.7mg/100g.

(6) The large biological polyester fiber containing the plant active ingredients can be prepared into downstream products such as bandages, patches, vests, bellies, undergarments and the like in downstream application, can realize targeted improvement and alleviation of corresponding diseases, simultaneously avoid bad stimulation of various plant active ingredients to intestines and stomach, liver and the like of a human body by oral administration, and further expand the application range of the large biological polyester fiber.

Detailed Description

Specific embodiments of the present invention will now be described in order to provide a clearer understanding of the technical features, objects and effects of the present invention.

Example 1

A preparation method of a large biological polyester fiber containing plant active ingredients specifically comprises the following steps:

1. extracting main ingredient

Cleaning stem leaves of fructus Cnidii, placing in an environment with vacuum degree of 0.01MPa, controlling drying temperature to 65deg.C, and keeping temperature and pressure until the moisture content of stem leaves of fructus Cnidii is 4wt%; then transferring into a superfine pulverizer, controlling the superfine pulverizing temperature to 38 ℃ and the rotating speed to 4000rpm, and pulverizing to 1800 meshes to obtain the fructus cnidii micropowder; then putting the cnidium fruit micro powder into a supercritical carbon dioxide extraction device, introducing carbon dioxide at an introducing rate of 12kg/h, and controlling the pressure in the supercritical carbon dioxide extraction device to be 10MPa; then heating to 40 ℃ at a heating rate of 0.5 ℃/min, and preserving heat and pressure for 5 hours to prepare the extract of the main component.

2. Extracting auxiliary components

Cleaning radix Clematidis, radix Saposhnikoviae, herba Taraxaci, and folium Bambusae, respectively, placing in an environment with vacuum degree of 0.01MPa, controlling drying temperature to 65deg.C, and keeping temperature and pressure until water content is 4wt%; then transferring the dried radix clematidis, radix saposhnikoviae, dandelion and bamboo leaves into an air flow pulverizer, mixing and pulverizing to 100 meshes, transferring into a superfine pulverizer, controlling the superfine pulverizing temperature to 38 ℃, controlling the rotating speed to 4000rpm, and pulverizing to 1800 meshes to obtain mixed plant micro powder; then the mixed plant micro powder is put into a supercritical carbon dioxide extraction device, carbon dioxide is introduced at the introducing rate of 16kg/h, and the pressure in the supercritical carbon dioxide extraction device is controlled to be 13MPa; then heating to 40 ℃ at a heating rate of 0.5 ℃/min, and preserving heat and pressure for 5 hours to prepare the auxiliary component extract.

Wherein the weight ratio of radix clematidis, radix sileris, dandelion to bamboo leaves is 10:7:1:0.8.

3. Preparation of the first modifier

1) Preparation of composite Carriers

Adding titanyl sulfate into deionized water with the weight 80 times of that of the solution, stirring at normal temperature until the titanyl sulfate is completely dissolved, then mixing the solution with phosphate buffer solution and absolute ethyl alcohol, and stirring at normal temperature for 1h to obtain a mixed solution; simultaneously, in the stirring process, the pH value of the mixed solution is controlled to be within the range of 6.5-6.8 by adopting sodium hydroxide solution; adding macroporous nano silicon dioxide with the weight of 0.1 time of the mixed solution after stirring at normal temperature, regulating the pH value to 2 by adopting a hydrochloric acid solution after ultrasonic dispersion is uniform, heating to 550 ℃ at a heating rate of 5 ℃/min, preserving heat for 1.5 hours, naturally cooling to 25 ℃, preserving heat and standing for 10 hours, filtering out solid matters, washing the solid matters by adopting deionized water with the volume of 8 times for 2 times, continuously washing the solid matters by adopting absolute ethyl alcohol with the volume of 8 times, and then placing the solid matters in an environment with the vacuum degree of 0.04MPa, and drying at 80 ℃ to constant weight to obtain the composite carrier.

Wherein the pH value of the phosphate buffer solution is 6.5.

In the mixed solution, the weight ratio of deionized water, phosphate buffer solution and absolute ethyl alcohol is 6:10:7.

The concentration of the sodium hydroxide solution was 0.6wt%.

The concentration of the hydrochloric acid solution was 0.2mol/L.

2) Modification treatment

Putting the composite carrier into an electrolytic cell containing 20 times of electrolyte, controlling the modification voltage to be 1.6V/cm, performing electric modification treatment for 1.5 hours, separating out solid matters, washing the solid matters by 8 times of deionized water, and drying at 80 ℃ to constant weight under the environment of 0.04MPa of vacuum degree to obtain the modified composite carrier.

Wherein the electrolyte is calcium chloride aqueous solution with the mass concentration of 0.03 percent.

3) Load(s)

Putting the modified composite carrier into 10 times of load liquid in parts by weight, uniformly dispersing by ultrasonic, vacuumizing to a vacuum degree of 0.085MPa under stirring, maintaining the vacuum for 40min, breaking the vacuum, pressurizing to 3MPa, maintaining the pressure for 1h, and recovering to normal pressure; then heating to 35 ℃, stirring at 30rpm for 18 hours, and filtering out solid matters; and (3) washing the solid by 8 times of deionized water, placing in an environment with the vacuum degree of 0.01MPa, drying at 75 ℃ to constant weight, and grinding uniformly to obtain the first modifier.

The preparation method of the loading solution comprises the steps of adding the main components of extract, tetradecyl dimethyl betaine, sodium carboxymethyl cellulose and a silane coupling agent kH-550 into ethanol solution, and uniformly dispersing.

In the loading liquid, the weight ratio of the main components of the extract, tetradecyl dimethyl betaine, sodium carboxymethyl cellulose, a silane coupling agent KH-550 and an ethanol solution is 20:0.06:0.1:0.5:55.

The volume concentration of the ethanol solution was 50%.

4. Preparation of the second modifier

Adding the auxiliary component extract, sodium dodecyl sulfate and fatty alcohol polyoxyethylene ether AEO-9 into deionized water, uniformly dispersing by ultrasonic, heating to 45 ℃ at a heating rate of 1 ℃/min under a stirring condition, and carrying out heat preservation and stirring for 30min to obtain a core material liquid; adding starch octenyl succinate, carrageenan and sodium alginate into deionized water, heating to 40 ℃, and carrying out ultrasonic emulsification uniformly to obtain wall material liquid; then the core material liquid is put into wall material liquid with the volume of 1.8 times, after ultrasonic dispersion is carried out for 30min, the primary homogenizing pressure is controlled to be 12MPa, and after primary homogenizing is carried out for 5 min; controlling the secondary homogenizing pressure to 25MPa, carrying out secondary homogenizing for 5min, and spray drying to obtain the second modifier.

Wherein, in the core material liquid, the weight ratio of the auxiliary component extract to the sodium dodecyl sulfate to the fatty alcohol polyoxyethylene ether AEO-9 to the deionized water is 20:0.15:0.08:50.

In the wall material liquid, the weight ratio of the octenyl succinic acid starch ester to the carrageenan to the sodium alginate to the deionized water is 1.5:0.6:0.05:160.

5. Preparation of functional masterbatch

Uniformly mixing polyester chips, a first modifier, sodium stearate, polytrimethylene terephthalate and an antioxidant 1790, putting into a double-screw extruder, and melting, extruding and granulating to obtain first functional master batch; and uniformly mixing polyester chips, a second modifier, sodium stearate, polytrimethylene terephthalate and an antioxidant 1790, putting into a double-screw extruder, and melting, extruding and granulating to obtain the second functional master batch.

In the first functional master batch, the weight ratio of polyester chips, a first modifier, sodium stearate, polytrimethylene terephthalate and an antioxidant 1790 is 80:10:0.5:1.2:1.

In the second functional master batch, the weight ratio of the polyester chips to the second modifier to the sodium stearate to the polytrimethylene terephthalate to the antioxidant 1790 is 80:19:0.5:1.2:1.

6. Spinning process

Uniformly mixing polyester chips, first functional master batches and second functional master batches, putting into a double-screw extruder, performing melt extrusion, metering, introducing into a spinning machine for spinning, controlling the spinning temperature to be 270 ℃, controlling the spinning speed to be 3500m/min, preparing fibers, controlling the drafting temperature to be 160 ℃, and performing primary drafting, wherein the drafting multiple is 3.2 times; controlling the drafting temperature to 110 ℃ and the drafting multiple to 2 times, and oiling and winding after the secondary drafting, so as to prepare the large biological polyester fiber containing the plant active ingredients.

The weight ratio of the polyester chips to the first functional master batch to the second functional master batch is 100:4:6.5.

Example 2

1. extracting main ingredient

Cleaning stem leaves of fructus Cnidii, placing in an environment with vacuum degree of 0.015MPa, controlling drying temperature to 70deg.C, and keeping temperature and pressure until the moisture content of stem leaves of fructus Cnidii is 5wt%; then transferring into a superfine pulverizer, controlling the superfine pulverizing temperature to 40 ℃ and the rotating speed to 4300rpm, and pulverizing to 1900 meshes to obtain the fructus cnidii micropowder; then putting the cnidium fruit micro powder into a supercritical carbon dioxide extraction device, introducing carbon dioxide at an introducing rate of 15kg/h, and controlling the pressure in the supercritical carbon dioxide extraction device to be 11MPa; then heating to 42 ℃ at a heating rate of 0.6 ℃/min, and preserving heat and pressure for 5.5 hours to prepare the extract of the main component.

2. Extracting auxiliary components

Cleaning radix Clematidis, radix Saposhnikoviae, herba Taraxaci, and folium Bambusae respectively, placing in an environment with vacuum degree of 0.015MPa, controlling drying temperature to 70deg.C, and keeping temperature and pressure until water content is 5wt%; then transferring the dried radix clematidis, radix saposhnikoviae, dandelion and bamboo leaves into an air flow pulverizer, mixing and pulverizing to 120 meshes, transferring into a superfine pulverizer, controlling the superfine pulverizing temperature to 40 ℃ and the rotating speed to 4300rpm, and pulverizing to 1900 meshes to obtain mixed plant micro powder; then the mixed plant micro powder is put into a supercritical carbon dioxide extraction device, carbon dioxide is introduced at the introducing rate of 18kg/h, and the pressure in the supercritical carbon dioxide extraction device is controlled to be 14MPa; then heating to 42 ℃ at a heating rate of 0.6 ℃/min, and preserving heat and pressure for 5.5 hours to prepare the auxiliary component extract.

Wherein the weight ratio of radix clematidis to radix saposhnikoviae to dandelion to bamboo leaves is 11:7.5:1.3:1.

3. Preparation of the first modifier

1) Preparation of composite Carriers

Adding titanyl sulfate into deionized water with the weight being 90 times that of the titanyl sulfate, stirring at normal temperature until the titanyl sulfate is completely dissolved, then mixing the solution with phosphate buffer solution and absolute ethyl alcohol, and stirring at normal temperature for 1.5 hours to obtain a mixed solution; simultaneously, in the stirring process, the pH value of the mixed solution is controlled to be within the range of 6.5-6.8 by adopting sodium hydroxide solution; adding macroporous nano silicon dioxide with the weight of 0.13 times of the mixed solution after stirring at normal temperature, regulating the pH value to 2.3 by adopting a hydrochloric acid solution after ultrasonic dispersion is uniform, heating to 570 ℃ at a heating rate of 6 ℃/min, naturally cooling to 28 ℃ after heat preservation for 2 hours, filtering out a solid matter after heat preservation and standing for 11 hours, washing the solid matter by adopting deionized water with the volume of 9 times for 3 times, continuously washing the solid matter by adopting absolute ethyl alcohol with the volume of 9 times, and then placing the solid matter in an environment with the vacuum degree of 0.045MPa, and drying at 85 ℃ to constant weight to obtain the composite carrier.

Wherein the pH value of the phosphate buffer solution is 6.6.

In the mixed solution, the weight ratio of deionized water, phosphate buffer solution and absolute ethyl alcohol is 6.5:11:7.5.

The concentration of sodium hydroxide solution was 0.65wt%.

The concentration of the hydrochloric acid solution was 0.22mol/L.

2) Modification treatment

Putting the composite carrier into an electrolytic cell containing 23 times of volume electrolyte, controlling the modification voltage to be 1.65V/cm, carrying out electric modification treatment for 1.8 hours, separating out solid matters, washing the solid matters by 9 times of volume deionized water, and drying at 85 ℃ to constant weight under the environment of 0.045MPa of vacuum degree to obtain the modified composite carrier.

Wherein the electrolyte is calcium chloride aqueous solution with the mass concentration of 0.033 percent.

3) Load(s)

Putting the modified composite carrier into 11 times of load liquid in parts by weight, uniformly dispersing by ultrasonic, vacuumizing to a vacuum degree of 0.09MPa under stirring, maintaining the vacuum for 50min, breaking the vacuum, pressurizing to 3.5MPa, maintaining the pressure for 1.5h, and recovering to normal pressure; then heating to 38 ℃, stirring at 50rpm for 19 hours, and filtering out solid matters; and (3) washing the solid by using 9 times of deionized water, placing the solid in an environment with the vacuum degree of 0.015MPa, drying at 80 ℃ to constant weight, and grinding uniformly to obtain the first modifier.

In the loading solution, the weight ratio of the main components of the extract, tetradecyl dimethyl betaine, sodium carboxymethyl cellulose, a silane coupling agent KH-550 and an ethanol solution is 21:0.065:0.11:0.55:57.

The volume concentration of the ethanol solution was 52%.

4. Preparation of the second modifier

Adding the auxiliary component extract, sodium dodecyl sulfate and fatty alcohol polyoxyethylene ether AEO-9 into deionized water, uniformly dispersing by ultrasonic, heating to 50 ℃ at a heating rate of 1.3 ℃/min under a stirring condition, and carrying out heat preservation and stirring for 35min to obtain a core material liquid; adding starch octenyl succinate, carrageenan and sodium alginate into deionized water, heating to 45 ℃, and carrying out ultrasonic emulsification uniformly to obtain wall material liquid; then the core material liquid is put into wall material liquid with the volume of 1.9 times, after ultrasonic dispersion is carried out for 40min, the primary homogenizing pressure is controlled to be 14MPa, and after primary homogenizing is carried out for 7 min; controlling the secondary homogenizing pressure to 26MPa, carrying out secondary homogenizing for 8min, and spray drying to obtain the second modifier.

Wherein, in the core material liquid, the weight ratio of the auxiliary component extract to the sodium dodecyl sulfate to the fatty alcohol polyoxyethylene ether AEO-9 to the deionized water is 21:0.2:0.1:55.

In the wall material liquid, the weight ratio of the octenyl succinic acid starch ester to the carrageenan to the sodium alginate to the deionized water is 1.8:0.7:0.055:170.

5. Preparation of functional masterbatch

In the first functional master batch, the weight ratio of the polyester chips to the first modifier to the sodium stearate to the polytrimethylene terephthalate to the antioxidant 1790 is 85:10.5:0.55:1.3:1.1.

In the second functional master batch, the weight ratio of the polyester chips to the second modifier to the sodium stearate to the polytrimethylene terephthalate to the antioxidant 1790 is 85:20:0.55:1.3:1.1.

6. Spinning process

Uniformly mixing polyester chips, first functional master batches and second functional master batches, putting into a double-screw extruder, performing melt extrusion, metering, introducing into a spinning machine for spinning, controlling the spinning temperature to 272 ℃, controlling the spinning speed to 3700m/min, preparing fibers, controlling the drafting temperature to 165 ℃, controlling the drafting multiple to 3.25 times, and performing primary drafting; controlling the drafting temperature to 115 ℃ and the drafting multiple to 2.1 times, and oiling and winding after the secondary drafting, so as to prepare the large biological polyester fiber containing the plant active ingredient.

The weight ratio of the polyester chips to the first functional master batch to the second functional master batch is 100:4.5:7.

Example 3

1. extracting main ingredient

Cleaning stem leaves of fructus Cnidii, placing in an environment with vacuum degree of 0.02MPa, controlling drying temperature to 75deg.C, and keeping temperature and pressure until the moisture content of stem leaves of fructus Cnidii is 6wt%; then transferring into a superfine pulverizer, controlling the superfine pulverizing temperature to be 42 ℃, controlling the rotating speed to be 4500rpm, and pulverizing to 2000 meshes to obtain fructus cnidii micropowder; then putting the cnidium fruit micro powder into a supercritical carbon dioxide extraction device, introducing carbon dioxide at an introducing rate of 16kg/h, and controlling the pressure in the supercritical carbon dioxide extraction device to be 12MPa; then heating to 45 ℃ at a heating rate of 0.7 ℃/min, and preserving heat and pressure for extraction for 6 hours to obtain the extract of the main component.

2. Extracting auxiliary components

Cleaning radix Clematidis, radix Saposhnikoviae, herba Taraxaci, and folium Bambusae, respectively, placing in an environment with vacuum degree of 0.02MPa, controlling drying temperature to 75deg.C, and keeping temperature and pressure until water content is 6wt%; then transferring the dried radix clematidis, radix saposhnikoviae, dandelion and bamboo leaves into an air flow pulverizer, mixing and pulverizing to 150 meshes, transferring into a superfine pulverizer, controlling the superfine pulverizing temperature to 42 ℃ and the rotating speed to 4500rpm, and pulverizing to 2000 meshes to obtain mixed plant micro powder; then the mixed plant micro powder is put into a supercritical carbon dioxide extraction device, carbon dioxide is introduced at the introducing rate of 20kg/h, and the pressure in the supercritical carbon dioxide extraction device is controlled to be 15MPa; then heating to 45 ℃ at a heating rate of 0.7 ℃/min, and preserving heat and pressure for extraction for 6 hours to obtain auxiliary component extracts.

Wherein the weight ratio of radix clematidis to radix saposhnikoviae to dandelion to bamboo leaves is 12:8:1.5:1.2.

3. Preparation of the first modifier

1) Preparation of composite Carriers

Adding titanyl sulfate into deionized water with the weight 100 times of that of the titanyl sulfate, stirring at normal temperature until the titanyl sulfate is completely dissolved, then mixing the solution with phosphate buffer solution and absolute ethyl alcohol, and stirring at normal temperature for 2 hours to obtain a mixed solution; simultaneously, in the stirring process, the pH value of the mixed solution is controlled to be within the range of 6.5-6.8 by adopting sodium hydroxide solution; adding macroporous nano silicon dioxide with the weight of 0.15 times of that of the mixed solution after stirring at normal temperature, regulating the pH value to 2.5 by adopting a hydrochloric acid solution after ultrasonic dispersion is uniform, heating to 600 ℃ at a heating rate of 7 ℃/min, preserving heat for 2.5 hours, naturally cooling to 30 ℃, preserving heat and standing for 12 hours, filtering out solid matters, washing the solid matters with 10 times of deionized water for 3 times, continuously washing the solid matters with 10 times of absolute ethyl alcohol, and then placing the solid matters in an environment with the vacuum degree of 0.05MPa, and drying at 90 ℃ to constant weight to obtain the composite carrier.

Wherein the pH value of the phosphate buffer solution is 6.8.

In the mixed solution, the weight ratio of deionized water, phosphate buffer solution and absolute ethyl alcohol is 7:12:8.

The concentration of the sodium hydroxide solution was 0.7wt%.

The concentration of the hydrochloric acid solution was 0.25mol/L.

2) Modification treatment

Putting the composite carrier into an electrolytic cell containing 25 times of volume electrolyte, controlling the modification voltage to be 1.7V/cm, carrying out electric modification treatment for 2 hours, separating out solid matters, washing the solid matters by adopting 10 times of volume deionized water, and drying at 90 ℃ to constant weight under the environment of 0.05MPa of vacuum degree to obtain the modified composite carrier.

Wherein the electrolyte is calcium chloride aqueous solution with the mass concentration of 0.035 percent.

3) Load(s)

Putting the modified composite carrier into 12 times of load liquid in weight part, uniformly dispersing by ultrasonic, vacuumizing to a vacuum degree of 0.095MPa under stirring, maintaining the vacuum for 60min, breaking the vacuum, pressurizing to 4MPa, maintaining the pressure for 2h, and recovering to normal pressure; then heating to 40 ℃, stirring at 60rpm for 20 hours, and filtering out solid matters; and (3) washing the solid by adopting deionized water with the volume of 10 times, placing the solid in an environment with the vacuum degree of 0.02MPa, drying at the temperature of 85 ℃ to constant weight, and grinding uniformly to obtain the first modifier.

In the loading liquid, the weight ratio of the main components of the extract, tetradecyl dimethyl betaine, sodium carboxymethyl cellulose, a silane coupling agent KH-550 and an ethanol solution is 22:0.07:0.12:0.6:60.

The volume concentration of the ethanol solution was 55%.

4. Preparation of the second modifier

Adding the auxiliary component extract, sodium dodecyl sulfate and fatty alcohol polyoxyethylene ether AEO-9 into deionized water, uniformly dispersing by ultrasonic, heating to 55 ℃ at a heating rate of 1.5 ℃/min under the stirring condition, and carrying out heat preservation and stirring for 40min to obtain a core material liquid; adding starch octenyl succinate, carrageenan and sodium alginate into deionized water, heating to 50 ℃, and carrying out ultrasonic emulsification uniformly to obtain wall material liquid; then the core material liquid is put into wall material liquid with the volume of 2 times, after ultrasonic dispersion is carried out for 50min, the primary homogenizing pressure is controlled to be 15MPa, and after primary homogenizing is carried out for 10 min; controlling the secondary homogenizing pressure to 28MPa, carrying out secondary homogenizing for 10min, and spray drying to obtain the second modifier.

Wherein, in the core material liquid, the weight ratio of the auxiliary component extract to the sodium dodecyl sulfate to the fatty alcohol polyoxyethylene ether AEO-9 to the deionized water is 22:0.25:0.12:60.

In the wall material liquid, the weight ratio of the octenyl succinic acid starch ester to the carrageenan to the sodium alginate to the deionized water is 2:0.8:0.06:180.

5. Preparation of functional masterbatch

In the first functional master batch, the weight ratio of polyester chips, a first modifier, sodium stearate, polytrimethylene terephthalate and an antioxidant 1790 is 90:11:0.6:1.5:1.2.

In the second functional master batch, the weight ratio of the polyester chips to the second modifier to the sodium stearate to the polytrimethylene terephthalate to the antioxidant 1790 is 90:21:0.6:1.5:1.2.

6. Spinning process

Uniformly mixing polyester chips, first functional master batches and second functional master batches, putting into a double-screw extruder, performing melt extrusion, metering, introducing into a spinning machine for spinning, controlling the spinning temperature to be 275 ℃, controlling the spinning speed to be 3800m/min, preparing fibers, controlling the drawing temperature to be 170 ℃, and drawing multiple to be 3.3 times, and performing primary drawing; controlling the drafting temperature to 120 ℃ and the drafting multiple to 2.2 times, and oiling and winding after the secondary drafting, so as to prepare the large biological polyester fiber containing the plant active ingredient.

The weight ratio of the polyester chips to the first functional master batch to the second functional master batch is 100:5:7.5.

Comparative example 1

The preparation method of the large biological polyester fiber containing the plant active ingredient in the embodiment 2 is adopted, and the difference is that: 1) Omitting the step of extracting main components, and in the step of extracting auxiliary components, washing, drying, mixing and crushing stem and leaf of cnidium fruit, clematis root, divaricate saposhnikovia root, dandelion and bamboo leaf together, and extracting by supercritical carbon dioxide to obtain a mixed extract; and controlling the weight ratio of stem and leaf of cnidium fruit, clematis root, ledebouriella root, dandelion and bamboo leaf to be 32:11:7.5:1.3:1. 2) The step of preparing the second modifier is omitted, and the mixed extract described above is used in the loading step of preparing the first modifier instead of the main component extract.

Comparative example 2

The preparation method of the large biological polyester fiber containing the plant active ingredient in the embodiment 2 is adopted, and the difference is that: 1) The main component extract is used for preparing a second modifier, and then a first functional master batch is prepared; 2) The auxiliary component extract is used in the first modifier preparation step; then preparing a second functional master batch; 3) In the spinning step, the weight ratio of the polyester chips to the first functional master batch to the second functional master batch is controlled to be 100:6.5:5.5.

Comparative example 3

The preparation method of the large biological polyester fiber containing the plant active ingredient in the embodiment 2 is adopted, and the difference is that: in the preparation of the first modifier, the preparation of the composite carrier and the modification treatment are omitted, and macroporous nano silicon dioxide with the same specification is adopted to replace the modified composite carrier to carry out the relevant treatment of the loading step.

The breaking strength, breaking elongation, 180 ℃ dry heat shrinkage and defect content of the large biological polyester fibers containing the plant active ingredients prepared in examples 1-3 and comparative examples 1-3 are respectively detected. The specific detection results are as follows:

it can be seen that in the large biological polyester fiber containing the plant active ingredient, the first modifier and the second modifier can be effectively combined with the large biological polyester fiber, so that the modified polyester fiber can be functionally modified, and meanwhile, the physical property of the modified polyester fiber is prevented from being reduced, and the physical property of the polyester fiber is effectively maintained. The degradation of the physical properties of the polyester fiber in comparative example 3 is more remarkable, because the combination property of the first modifier and the polyester fiber is reduced after relevant technical means are omitted, the defect content is high, and the breaking strength is reduced to a certain extent.

Further, the large biological polyester fibers containing the plant active ingredients of examples 1-3 and comparative examples 1-3 were blended with spandex to prepare test bandages, and the content of the large biological polyester fibers containing the plant active ingredients in each test bandage was controlled to 92wt% and the content of spandex was controlled to 8wt%.

120 volunteers aged over 10 years and suffering from chronic eczema were selected, and the number of men and women in the volunteers was controlled to be half of each other. 120 volunteers were randomized into 6 groups and each half of men and women within each group was controlled.

Wherein, 1-3 groups correspond to the application of the test bandages of examples 1-3, and 4-6 groups correspond to the application of the test bandages of comparative examples 1-3, respectively. The specific application method is that after skin of the eczema area is cleaned with warm water every day, the test bandage is fixed on the chronic eczema area, the test bandage is kept fixed for at least 10 hours every day, and the application is continued for 42 days. Meanwhile, during the continuous application, the test bandages were subjected to a conventional water wash once per day. Investigation of the application effect (effective, ineffective) of each test bandage, and statistics of the corresponding number of people; and the number of significant and effective volunteers who had recurrent or aggravated eczema during the period of administration and within 30 days of cessation of administration was counted.

Wherein, the effect is that the eczema in the fixed area of the test bandage is effectively eliminated, and no recurrence is generated during the application period.

Effectively, eczema in the fixed area of the test bandage is obviously relieved, and no aggravation is caused during application.

The ineffectiveness is that there is no significant difference in chronic eczema of the skin in the area where the test bandages were fixed compared to before the test bandages were not applied.

The specific test results are as follows:

it can be seen that the first modifier is prepared from the extract of the main component containing the plant active ingredient of the monarch drug in the large biological polyester fiber containing the plant active ingredient; the preparation method is combined with a second modifier prepared from auxiliary component extracts of ministerial drugs radix clematidis, adjuvant drugs radix sileris, messenger drugs dandelion and messenger drugs bamboo leaves, and different treatment methods in preparing the first modifier and preparing the second modifier are adopted aiming at the characteristics and the matching relation of the active components of each plant, so that the effective controlled release of the active components of different plants in the modified active components is realized, the release efficiency of the active components of each plant in polyester fiber is consistent, and the modified active components can be matched within the effective proportioning dosage range for a long time, so that the targeted improvement, alleviation and prevention of eczema are realized; in addition, in the test process, the test bandages can still achieve the effects after being applied by conventional water washing for many times, and the plant active ingredients in the large biological polyester fiber containing the plant active ingredients have good bonding performance with the polyester fiber, high stability, difficult loss and good long-term effectiveness. As can be seen from comparative example 1, the process for preparing the modifier by loading after mixing all the plant active ingredients (i.e. mixing the monarch drug with other ingredients) is characterized in that, on one hand, the polyester fiber has different properties of each plant active ingredient, inconsistent release efficiency, and unsatisfactory blending effect of each plant active ingredient, which is particularly characterized by reduced number of significant effects, improved inefficiency, and increased number of people who relapse or aggravate eczema after stopping applying the test bandages. As can be seen from comparative example 2, after the main component extract containing the active ingredients of the monarch drug plants is treated by adopting the method for preparing the second modifier, the first functional master batch is prepared; preparing a second functional master batch by adopting a method for preparing a first modifier to treat auxiliary component extracts containing ministerial drugs of radix clematidis, adjuvant drugs of radix sileris, guiding drugs of dandelion and guiding drugs of bamboo leaf plant active components; the change of the plant active ingredients in the first modifier and the second modifier can not effectively and stably regulate and control the release efficiency of each plant active ingredient, so that each plant active ingredient can not be matched under the condition of optimal proportioning dosage for a long time, and further, the chronic eczema can not be effectively improved and relieved, and the method is particularly characterized by reducing the number of significant effects, improving the inefficiency and increasing the number of recurrent or aggravated eczema after stopping applying the test bandages. As can be seen from comparative example 3, in the preparation of the first modifier, the macroporous nano silicon dioxide and the porous titanium dioxide are combined in an in-situ generation mode, so that the loading and controlled release performance of the active ingredients of the monarch drug plants are effectively improved, and other active ingredients of the monarch drug plants can be matched with the active ingredients of the monarch drug plants within an effective proportioning dosage range for a long time; meanwhile, the composite carrier is subjected to hydroxylation electric modification treatment in combination with modification treatment, so that on one hand, the loading and controlled release performance of the active ingredients of the monarch medicine plants are further improved, and the stable and effective release of the active ingredients of the monarch medicine plants in the large biological polyester fibers is maintained; on the other hand, the combination property of the first modifier and the polyester fiber is improved, and the stability of the first modifier in the polyester fiber is improved; thereby ensuring the targeted alleviation, improvement and prevention of eczema. Comparative example 3 the improvement and alleviation effect on chronic eczema was significantly reduced after omitting the related technical means.

Further, according to GB/T20944.3-2008, evaluation of antibacterial Properties of textiles, section 3: the antibacterial properties of the large biosurfactant polyester fibers containing the plant active ingredients of examples 1 to 3 and comparative examples 1 to 3 were tested according to the content of antibacterial properties specified in the vibration method, and the specific test results are as follows:

the large biological polyester fiber containing the plant active ingredient has good antibacterial function besides the targeted improvement and alleviation of eczema. As can be seen from comparative example 3, in the preparation of the first modifier, the preparation of the composite carrier and the modification treatment were omitted, and the main component extract had poor loading effect on the carrier, and was easily lost during the subsequent functional treatment of the polyester fiber, so that the antibacterial performance was reduced.

Further, the large biological polyester fibers containing the plant active ingredients of examples 1 to 3 and comparative examples 1 to 3 were spun into a fabric, and then cut into 20cm×20cm water-washed samples. Respectively putting the water washing samples into a washing machine, setting the water temperature of the washing water to be 60 ℃, taking the washing water as water for washing once for 30min, and after the washing is finished, putting the water washing samples into a temperature environment of 35 ℃, and continuously radiating the water washing samples to be completely dried by adopting a 100W xenon lamp; and repeating the washing and airing operations for 15 times, and respectively carrying out antibacterial property tests on all the washing samples by adopting the antibacterial property detection method.

The specific test results are as follows:

it can be seen that in the large biological polyester fiber containing the plant active ingredients, the combination property of each plant active ingredient and the large biological polyester fiber is good, the stability is good, the plant active ingredient is not easy to run off after being washed with water for many times and the illumination factor is influenced, and the long-term effectiveness is good. As can be seen from comparative example 1, after omitting the preparation of the second modifier, the treatment mode of the plant active ingredients is single, and the antibacterial effect can not be realized by the combination of multiple ingredients; and a plurality of plant active ingredients are loaded on the carrier, and the loss condition of the plant active ingredients exists in the water washing and airing processes. As can be seen from comparative example 2, the treatment method of the plant active ingredients is changed, and the performance of improving and relieving eczema by mutually matching the plant active ingredients is affected, but the stability of the large biological polyester fiber is affected less, and the antibacterial performance is not greatly different from that of example 2 after the large biological polyester fiber is washed and dried for many times. As can be seen from comparative example 3, in the preparation of the first modifier, the loading effect and stability of the active ingredients of the monarch drug on the carrier are affected after the preparation of the composite carrier and the modification treatment are omitted, and the stability of the first modifier in the polyester fiber is also degraded, so that the degradation of the antibacterial property is obvious after the multi-time washing and the drying.

In summary, it can be seen that the preparation method of the large biological polyester fiber containing plant active ingredients of the invention prepares the main component extract containing the plant active ingredients of the monarch drug by extracting the main component of the monarch drug fructus cnidii and extracting the main component by supercritical carbon dioxide; extracting auxiliary components of radix Clematidis, radix Saposhnikoviae, herba Taraxaci, and herba Lophatheri, and extracting with supercritical carbon dioxide to obtain auxiliary component extract containing other medicinal plant active components; in the preparation of the first modifier, macroporous nano silicon dioxide and porous titanium dioxide are combined in an in-situ generation mode, so that the loading and controlled release performance of the active ingredients of the monarch drug plants are improved, and the active ingredients of the plants can be matched within the effective proportioning dosage range for a long time; meanwhile, the modification treatment is combined, and the hydroxylation treatment of the composite carrier is carried out, so that on one hand, the loading and controlled release performance of the active ingredients of the monarch medicine plant is further improved, on the other hand, the combination performance of the first modifier and the polyester fiber is improved, and the stability of the first modifier in the polyester fiber is improved; in the preparation of the second modifier, coating the core material liquid containing the plant extract as an auxiliary component by adopting a composite wall material; after the first modifier and the second modifier are respectively adopted to prepare the functional master batches, the first functional master batches and the second functional master batches are matched to be used in the spinning preparation of the polyester fibers, so that the problem that after the polyester fibers are functionally modified by adopting various plant active ingredients, the release efficiency is inconsistent due to the fact that the main ingredients (monarch ingredients) and auxiliary ingredients (ministerial drugs, adjuvant drugs and drug ingredients) in the various plant active ingredients are different in nature, and the main ingredients and the auxiliary ingredients cannot be effectively matched can be effectively avoided; meanwhile, the combination property of various plant active ingredients and the polyester fiber is good, the stability is high, the loss is not easy, the various plant active ingredients in the polyester fiber can be matched under the condition of optimal proportioning dosage for a long time, the improvement, alleviation and prevention effects on corresponding symptoms are stable, and the long-term effectiveness is good; meanwhile, the condition that various plant active ingredients fail in the functional modification and spinning processes of the polyester fiber can be effectively avoided.

The percentages used in the present invention are mass percentages unless otherwise indicated.

Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. The preparation method of the large biological polyester fiber containing the plant active ingredients is characterized by comprising the following steps: extracting main components, extracting auxiliary components, preparing a first modifier, preparing a second modifier, preparing functional master batches and spinning;

the method for extracting the main components comprises the steps of cleaning, drying and crushing stems and leaves of the cnidium fruit to prepare the cnidium fruit micro powder; extracting fructus Cnidii micropowder with supercritical carbon dioxide to obtain main component extract;

the method for extracting the auxiliary components comprises the steps of respectively cleaning, drying, mixing and crushing radix clematidis, radix saposhnikoviae, dandelion and bamboo leaves to obtain mixed plant micro powder; extracting the mixed plant micropowder with supercritical carbon dioxide to obtain auxiliary component extract;

The preparation of the first modifier comprises the following steps: preparing a composite carrier, modifying and loading;

the method for preparing the composite carrier comprises the steps of adding titanyl sulfate into deionized water with the weight of 80-100 times, stirring until the titanyl sulfate is completely dissolved, then mixing the solution with phosphate buffer solution and absolute ethyl alcohol, and stirring at normal temperature to obtain a mixed solution; in the normal temperature stirring process, controlling the pH value of the mixed solution to be in the range of 6.5-6.8; continuously adding macroporous nano silicon dioxide with the weight of 0.1-0.15 times of that of the mixed solution, uniformly dispersing by ultrasonic, regulating the pH value to 2-2.5, heating to 550-600 ℃ at the heating rate of 5-7 ℃/min, preserving heat for 1.5-2.5h, naturally cooling to 25-30 ℃, preserving heat and standing for 10-12h, filtering out solid matters, washing the solid matters by deionized water and absolute ethyl alcohol in sequence, and carrying out vacuum drying to obtain a composite carrier;

the modification treatment method comprises the steps of putting the composite carrier into electrolyte, controlling the modification voltage to be 1.6-1.7V/cm, performing electric modification treatment for 1.5-2h, separating out solid matters, washing the solid matters with deionized water, and performing vacuum drying to obtain a modified composite carrier;

In the modification treatment, the electrolyte is calcium chloride aqueous solution, and the mass concentration of calcium chloride in the electrolyte is 0.03-0.035%;

the volume ratio of the composite carrier to the electrolyte is 1:20-22;

the loading method comprises the steps of putting the modified composite carrier into loading liquid, uniformly dispersing by ultrasonic, vacuumizing to a vacuum degree of 0.085-0.095MPa under stirring, maintaining the vacuum for 40-60min, breaking the vacuum, pressurizing to 3-4MPa, maintaining the pressure for 1-2h, and recovering to normal pressure; then heating to 35-40 ℃, preserving heat and stirring for 18-20h, and filtering out solid matters; washing the solid by deionized water, vacuum drying, and grinding uniformly to obtain a first modifier;

in the loading, the loading liquid is prepared by adding main components of extract, tetradecyl dimethyl betaine, sodium carboxymethyl cellulose and a silane coupling agent kH-550 into an ethanol solution and uniformly dispersing;

in the load, the weight ratio of the modified composite carrier to the load liquid is 1:10-12;

the volume concentration of the ethanol solution is 50-55%;

The method for preparing the second modifier comprises the steps of adding auxiliary component extracts, sodium dodecyl sulfate and fatty alcohol polyoxyethylene ether AEO-9 into deionized water, and emulsifying uniformly to obtain core material liquid; adding starch octenyl succinate, carrageenan and sodium alginate into deionized water, and performing ultrasonic emulsification uniformly to obtain wall material liquid; then, the core material liquid is put into the wall material liquid, and after primary homogenization and secondary homogenization, the second modifier is prepared by spray drying;

in the preparation of the second modifier, the volume ratio of the core material liquid to the wall material liquid is 1:1.8-2 times;

the primary homogenizing pressure is 12-15MPa, and the primary homogenizing time is 5-10min;

the pressure of secondary homogenization is 25-28MPa, and the time of secondary homogenization is 5-10min;

in the core material liquid, the weight ratio of the auxiliary component extract to the sodium dodecyl sulfate to the fatty alcohol polyoxyethylene ether AEO-9 to the deionized water is 20-22:0.15-0.25:0.08-0.12:50-60;

in the wall material liquid, the weight ratio of the octenyl succinic acid starch ester to the carrageenan to the sodium alginate to the deionized water is 1.5-2:0.6-0.8:0.05-0.06:160-180;

the method for preparing the functional master batch comprises the steps of uniformly mixing polyester chips, a first modifier, sodium stearate, polytrimethylene terephthalate and an antioxidant 1790, and carrying out melting, extrusion and granulation to obtain a first functional master batch; uniformly mixing polyester chips, a second modifier, sodium stearate, polytrimethylene terephthalate and an antioxidant 1790, and melting, extruding and granulating to obtain a second functional master batch;

In the first functional master batch, the weight ratio of the polyester chips to the first modifier to the sodium stearate to the polytrimethylene terephthalate to the antioxidant 1790 is 80-90:10-11:0.5-0.6:1.2-1.5:1-1.2;

in the second functional master batch, the weight ratio of the polyester chips to the second modifier to the sodium stearate to the polytrimethylene terephthalate to the antioxidant 1790 is 80-90:19-21:0.5-0.6:1.2-1.5:1-1.2;

the spinning method comprises the steps of mixing the first functional master batch, the second functional master batch and polyester chips, and preparing the large biological polyester fiber containing plant active ingredients through melt extrusion, spinning, primary drawing, secondary drawing, oiling and winding;

in the spinning, the spinning temperature is controlled to be 270-275 ℃, and the spinning speed is controlled to be 3500-3800m/min;

the temperature of primary draft is 160-170 ℃, and the primary draft multiple is 3.2-3.3 times;

the temperature of the secondary drafting is 110-120 ℃, and the secondary drafting multiple is 2-2.2 times;

the weight ratio of the polyester chips to the first functional master batch to the second functional master batch is 100:4-5:6.5-7.5.

2. The method for preparing the large biological polyester fiber containing plant active ingredients according to claim 1, wherein in the extraction of the main ingredients, the introducing rate of carbon dioxide is controlled to be 12-16kg/h in the supercritical carbon dioxide extraction process; and controlling the supercritical carbon dioxide extraction pressure to be 10-12MPa, the supercritical carbon dioxide extraction temperature to be 40-45 ℃ and the supercritical carbon dioxide extraction time to be 5-6h.

3. The method for preparing the large biological polyester fiber containing plant active ingredients according to claim 1, wherein in the extraction auxiliary ingredients, the introducing rate of carbon dioxide is controlled to be 16-20kg/h in the supercritical carbon dioxide extraction process; controlling the supercritical carbon dioxide extraction pressure to be 13-15MPa, the supercritical carbon dioxide extraction temperature to be 40-45 ℃ and the supercritical carbon dioxide extraction time to be 5-6h;

the weight ratio of the radix clematidis to the radix saposhnikoviae to the dandelion to the bamboo leaves is 10-12:7-8:1-1.5:0.8-1.2.

4. A large biological polyester fiber containing plant active ingredients, characterized in that the large biological polyester fiber is prepared by the preparation method of any one of claims 1 to 3.