Bionylon fiber containing plant-active component and method for preparing the same

Abstract

To provide a bionylon fiber containing a plant-active component and to provide a method for preparing the same.SOLUTION: A method for preparing a bionylon fiber containing a plant-active component includes the steps of: extracting a first component; extracting a second component; preparing a first active component; preparing a second active component; preparing a functional masterbatch; and conducting spinning.EFFECT: The method according to the present invention for preparing the bionylon fiber containing the plant-active component can effectively modify nylon fibers, ensuring good stability of various plant-active components in the bionylon fiber. The bionylon fiber contains various plant-active components at optimal ratios over the long term, thereby targeting and improving or alleviating corresponding diseases with good long-term efficacy. Additionally, the method effectively avoids the adverse effects of high doses of plant-derived active components on low doses, and solves the problem of low-dose plant-derived active components being prone to loss.SELECTED DRAWING: None

Description

Technical Field

[0001] The present invention relates to the technical field of bio nylon fibers, and particularly to bio nylon fibers containing plant active ingredients and a method for preparing the same.

Background Art

[0002] Nylon fiber is called Polyamide in English, nylon in scientific name, and also Nylon. It is the first synthetic fiber to appear in the world. The most prominent advantages of nylon fiber are excellent wear resistance and good elasticity compared to other fibers, and the elastic recovery rate of nylon fiber can even rival that of wool. Adding several nylon fibers to blended fabrics can significantly improve the wear resistance of the fabrics. When nylon fiber is stretched to 103 - 106%, the elastic recovery rate reaches 100%. At the same time, nylon fiber can withstand tens of thousands of bends without breaking. Among the synthetic fibers commercially available in the prior art, nylon fiber ranks second only to polypropylene fiber (polypropylene). As a result, nylon fiber can be processed into thin, soft, and smooth threads and woven into beautiful and durable fiber products. Similar to polyester fiber, nylon fiber is also resistant to corrosion, insects, and mold. The filaments of nylon fiber can be used for socks, underwear, shirts, trainers, ski shirts, Mackintosh, etc. Short fibers can be blended with cotton, wool, and viscose fibers to provide excellent wear resistance and strength. Also, it can be used as nylon buckles, carpets, and decorative fabrics. For industrial use, it is mainly used for curtains, conveyor belts, fishing nets, cables, etc.

[0003] With the progress of science and technology and the improvement of people's living standards, the functionality of nylon fibers can gradually no longer meet the requirements of practical application, and people are paying more and more attention to the improvement of the functionality of nylon fibers. In recent years, varieties of functional nylon fibers at home and abroad have been continuously introducing new and broad application prospects. Various functional nylon fibers with different characteristics have been developed. For example, acid-resistant nylon fibers, antioxidant nylon fibers, antistatic nylon elastic yarns, antibacterial nylon fibers, skin-care nylon fibers, anti-radiation nylon fibers, etc. Therefore, researching the functionality of nylon fibers and expanding their application fields is of great significance.

[0004] Therefore, in order to expand the performance and application areas of nylon fibers, the inventor of the present invention has developed bio-nylon fibers containing plant active ingredients, adopted plant active ingredients that can cooperate with each other to exert the functions of removing wind, relieving pain, and reducing inflammation to improve the functionality of nylon fibers, and aims to realize the effective exertion of the plant active ingredients and the long-term sustained release of macro-bio-nylon fibers. At the same time, the bio-nylon fibers after functional modification can be made into downstream underwear products such as bandages, joint sleeves, shoulder pads, waist pads, and even vests through the percutaneous absorption and sustained release of the plant active ingredients of macro-biotic nylon fibers, achieving targeted improvement and relief of corresponding diseases and avoiding direct irritation of the gastrointestinal tract by the plant active ingredients taken orally.

[0005] However, when using various plant active ingredients in the modification process of nylon fibers, the inventors found the following problems: First, after functionally modifying nylon fibers with various plant active ingredients, the main components, auxiliary components, etc. in the various plant active ingredients cannot effectively cooperate, and it is impossible to effectively achieve the ideal functions of wind, pain, anti-inflammatory, and improvement of the pain relief effect of rheumatoid arthritis. Second, there are differences in the stability of various plant active ingredients in nylon fibers. The loss rates of different plant active ingredients in nylon fibers are different, and the loss amounts when affected by external factors (such as washing, high temperature, high humidity, light, etc.) are different. As a result, various plant active ingredients in nylon fibers cannot cooperate under optimal formulation conditions, affecting the stability of the pain relief effect of bio-nylon fibers on rheumatoid pain and resulting in unsatisfactory long-term effects. Third, in the process of functionally modifying nylon fibers with various plant active ingredients, the addition amount of the main plant active ingredients (such as the king drug ingredients) is large, and the influence on the small-dose auxiliary plant active ingredients (minister drug ingredients) is significant. In the process of functionally treating nylon fibers with small-dose auxiliary plant active ingredients, they are easily lost and cannot reach the effective amount. Moreover, each plant active ingredient cannot effectively act, and ultimately, an ideal improvement and relief effect on rheumatoid pain cannot be obtained.

Summary of the Invention

[0006] In order to solve the technical problems existing in the prior art, the present invention provides a bio-nylon fiber containing plant active ingredients and a preparation method thereof, which can effectively modify nylon fibers with various plant active ingredients, realize the effective exertion and long-term sustained release of plant active ingredients in the bio-nylon fiber, have good stability of various plant active ingredients in the bio-nylon fiber, enable various plant active ingredients in the bio-nylon fiber to cooperate under optimal formulation conditions for a long time to achieve targeted improvement and relief of corresponding diseases, have good long-term effects, and at the same time, can effectively avoid the adverse effects of large-dose plant active ingredients on small-dose plant active ingredients and avoid the problem that small-dose plant active ingredients are easily lost.

[0007] To solve the above technical problems, the present invention adopts the following technical solutions.

[0008] The preparation method of bio-nylon fiber containing plant active ingredients includes each step of first component extraction, second component extraction, preparation of the first active ingredient, preparation of the second active ingredient, preparation of the functional masterbatch, and spinning.

[0009] In the step of extracting the first component, after rinsing the whole herb of Portulaca oleracea with 4 to 8 times the volume of deionized water, it is placed in a vacuum drying box, the degree of vacuum is controlled at 0.01 to 0.02 MPa, the vacuum drying temperature is 60 to 70 °C, and the whole herb of Portulaca oleracea is dried until the water content is 4 to 6 wt%. Then it is transferred to an ultrafine pulverizer, the ultrafine pulverization temperature is controlled at 38 to 42 °C, and it is pulverized to 1800 to 2000 mesh to prepare the first active ingredient fine powder. Then the first active ingredient fine powder is put into 5 to 6 times the volume of ethanol aqueous solution, stirred and heated to 40 to 50 °C, kept warm and stirred for 5 to 6 h, then ultrasonically extracted for 20 to 30 min. Subsequently, it is heated to 55 to 65 °C, kept warm and stirred for 20 to 30 min, then ultrasonically extracted for 10 to 20 min. The solid matter is filtered to obtain the primary extract. The solid matter is put into 3 to 4 times the volume of ethanol aqueous solution, stirred and heated to 55 to 65 °C, kept warm and stirred for 20 to 30 min, then ultrasonically extracted for 10 to 20 min. The solid matter is filtered to obtain the secondary extract. The primary extract and the secondary extract are combined and left in an environment with a vacuum degree of 0.04 to 0.05 MPa, and vacuum concentrated to 30 to 35% of the original volume at 65 to 75 °C to prepare the first component liquid.

[0010] In the step of extracting the first component, the volume concentration of ethanol in the ethanol aqueous solution is 65 to 75%. The ultrasonic frequency of ultrasonic extraction is 40 to 45 kHz, and the ultrasonic power is 350 to 450 W.

[0011] The Portulaca oleracea adopted in the step of extracting the first component is warm in nature, bitter in taste, clears dampness, relaxes tendons and activates glue, and has the effects of detoxifying and relieving pain. In the prepared bio-nylon fiber containing plant active ingredients, it functions as a king medicine.

[0012] In the step of extracting the second component, mugwort, Patrinia villosa, and safflower are rinsed with 4 to 8 times the volume of deionized water respectively, then placed in a vacuum drying box, the degree of vacuum is controlled at 0.01 to 0.02 MPa, the vacuum drying temperature is 60 to 70 °C, dried until the moisture content reaches 4 to 6 wt%, transferred mugwort, Patrinia villosa, and safflower into an airflow pulverizer, mixed and pulverized to 100 to 150 mesh, then placed in an ultrafine pulverizer, the ultrafine pulverization temperature is controlled at 38 to 42 °C, pulverized to 1800 to 2000 mesh to prepare the second active ingredient fine powder. Then, the second active ingredient fine powder is put into an ethanol aqueous solution with 5 to 6 times the volume, stirred and heated to 40 to 50 °C, kept warm and stirred for 5 to 6 h, then ultrasonically extracted for 20 to 30 min, continuously heated to 55 to 65 °C, kept warm and stirred for 20 to 30 min, then ultrasonically extracted for 10 to 20 min, the solid matter is filtered to obtain the primary extract. The solid matter is put into an ethanol aqueous solution with 3 to 4 times the volume, stirred and heated to 55 to 65 °C, kept warm and stirred for 20 to 30 min, then ultrasonically extracted for 10 to 20 min, the solid matter is filtered to obtain the secondary extract. The primary extract and the secondary extract are combined and left in an environment with a degree of vacuum of 0.04 to 0.05 MPa, vacuum concentrated to 30 to 35% of the original volume at 65 to 75 °C to prepare the second component liquid.

[0013] In the step of extracting the second component, the weight ratio of mugwort, Patrinia villosa, and safflower is 10 to 12:6 to 7:0.6 to 0.8. The volume concentration of ethanol in the ethanol aqueous solution is 65 to 75%. The ultrasonic frequency of ultrasonic extraction is 40 to 45 kHz, and the ultrasonic power is 350 to 450 W.

[0014] The mugwort adopted in the step of extracting the second component is warm in nature and bitter in taste, has the efficacy of warming the meridians and collaterals, dispelling wind, and removing dampness, promotes the absorption of inflammation, and also has effects such as sterilization. In the bio-nylon fiber containing the prepared plant active ingredient, it functions as an assistant to the monarch drug as a ministerial drug.

[0015] The extended herb is warm in nature, slightly sweet in taste, with astringency, and has the effects of dispelling wind, alleviating pain, relaxing tendons, and activating glue. In the bio-nylon fiber containing the prepared plant active ingredient, it functions as an adjuvant drug in cooperation with the king drug.

[0016] Safflower is warm in nature, pungent and bitter in taste, and has the effect of activating blood circulation and removing stasis. In the bio-nylon fiber containing the prepared plant active ingredient, it functions as a minister drug in cooperation with other drugs.

[0017] The step of preparing the first active ingredient includes each step of primary treatment, secondary treatment, and loading.

[0018] In the step of the primary treatment, according to the weight part ratio of 2 - 3:1, nanomesoporous silica and perlite are put into a high-speed mixer, the mixing rotation speed is controlled at 700 - 800 rpm, mixed for 5 - 10 min to prepare the primary powder. Then the primary powder is put into toluene with a volume 20 - 22 times that of the primary powder, uniformly dispersed by ultrasonic waves, and then under stirring conditions, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane and γ-aminopropyltrimethoxysilane are added, stirred for 30 - 40 min, then heated to 80 - 90 °C with stirring, kept warm and stirred for 10 - 12 h, the solid is separated, the solid is washed 2 - 3 times with anhydrous ethanol with a volume 4 - 6 times that of the solid, and then dried at 60 - 70 °C for 8 - 10 h to prepare the primary treated product.

[0019] In the step of the primary treatment, the particle size of the nanomesoporous silica is 200 - 250 nm, the specific surface area is 550 - 600 m 2 / g, the pore volume is 0.62 - 0.66 cm 2 / g, The weight ratio of the primary powder, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, and γ-aminopropyltrimethoxysilane is 8 - 10:1 - 2:0.8 - 1.

[0020] In the secondary treatment, the primary treated product is put into a secondary treatment liquid with a volume 13 to 15 times that of the primary treated product, stirred for 10 to 12 hours, then the solid matter is separated, washed with deionized water with a volume 8 to 10 times that of the primary treated product, and then the solid matter is dried to a certain weight using a constant temperature drying box to prepare a secondary treated product.

[0021] In the step of the secondary treatment, the secondary treatment liquid is a deionized aqueous solution in which sodium thioglycolate is dissolved. In the secondary treatment liquid, the content of sodium thioglycolate is 8 to 10 wt%.

[0022] In the step of the loading, the first component liquid and sodium dodecylbenzenesulfonate are put into an ethanol solution, stirred for 10 to 20 minutes, then the secondary treated product is continuously put in and uniformly dispersed, then evacuated to a vacuum degree of 0.09 to 0.095 MPa, the vacuum is maintained for 30 to 50 minutes, then returned to atmospheric pressure, heated to 35 to 40 °C, kept warm and stirred for 20 to 24 hours, then the solid matter is filtered and put into a vacuum drying box, the vacuum degree is controlled to 0.02 to 0.03 MPa, the vacuum drying temperature is 70 to 80 °C, and vacuum dried until the water content is 1 to 1.5 wt% to prepare the first active ingredient.

[0023] In the step of the loading, the weight ratio of the first component liquid, sodium dodecylbenzenesulfonate, the secondary treated product, and the ethanol solution is 16 to 18: 0.05 to 0.06: 7 to 8: 50 to 60. The volume concentration of ethanol in the ethanol aqueous solution is 50 to 60%.

[0024] The step of preparing the second active ingredient is to put the second component liquid, sodium carboxymethyl cellulose, and maltodextrin into deionized water, heat it up to 40 - 50 °C, emulsify it uniformly with ultrasonic waves to prepare a second component emulsion, put gum arabic and guar gum into deionized water, heat it up to 50 - 60 °C, stir it uniformly to prepare a coating solution, then put the second component emulsion into 1.8 - 2.2 times the volume of the coating solution, disperse it with ultrasonic waves for 1.5 - 2.5 h, cool it to 4 - 6 °C, keep it warm and stand still for 2 - 4 h, filter the solid matter and put it into a vacuum drying box, control the vacuum degree to 0.05 - 0.06 MPa, the vacuum drying temperature is 70 - 80 °C, vacuum dry until the water content reaches 1 - 1.5 wt% to prepare the second active ingredient.

[0025] In the step of preparing the second active ingredient, the weight ratio of the second component liquid, sodium carboxymethyl cellulose, maltodextrin, and deionized water in the second component emulsion is 16 - 18:0.4 - 0.5:1 - 1.5:50 - 60. The weight ratio of gum arabic, guar gum, and deionized water in the coating solution is 20 - 25:0.8 - 1:150 - 160.

[0026] The step of preparing the functional masterbatch is to uniformly mix nylon 66 slices, the first active ingredient, antioxidant 1790, and sodium stearate, then put them into a screw extruder, control the temperature to 260 - 265 °C, keep it warm and melt it, then extrude and granulate to prepare the first functional masterbatch. At the same time, uniformly mix nylon 66 slices, the second active ingredient, antioxidant 1790, and sodium stearate, then put them into a screw extruder, control the temperature to 260 - 265 °C, keep it warm and melt it, then extrude and granulate to prepare the second functional masterbatch.

[0027] In the step of preparing the functional masterbatch, the weight ratio of nylon 66 slices, the first active ingredient, antioxidant 1790, and sodium stearate in the first functional masterbatch is 80 - 90:10 - 11:1 - 1.2:0.7 - 0.8. The weight ratio of nylon 66 slices, the second functional masterbatch, antioxidant 1790, and sodium stearate in the second functional masterbatch is 80 - 90:20 - 22:1 - 1.2:0.7 - 0.8.

[0028] In the spinning step, after uniformly mixing nylon 66 slices, the first functional masterbatch, and the second functional masterbatch, control the melting temperature at 260 - 265°C. After extrusion and melting, control the spinning speed at 1600 - 1800 m / min with a screw spinning machine. After spinning to prepare fibers, perform stretching, oil application, and winding to prepare bio-nylon fibers containing plant active ingredients.

[0029] In the spinning step, the weight ratio of nylon 66 slices, the first functional masterbatch, and the second functional masterbatch is 100:4 - 5:7 - 8.

[0030] The bio-nylon fibers containing plant active ingredients are prepared by the above preparation method.

Advantages of the Invention

[0031] Compared with the prior art, the present invention has the following beneficial effects. (1) The preparation method of the bio-nylon fiber containing the plant active ingredient of the present invention is to prepare a first component liquid containing the main plant active ingredient by extracting the first component from the garden balsam, which is the king medicine, and extract the second component from mugwort, which is the minister medicine, the spreading plantain, which is the adjuvant medicine, and safflower, which is the minister medicine, to prepare a second component liquid containing the auxiliary plant active ingredient. During the preparation process of the first active ingredient, after preparing the primary powder using aminosilane and performing amino modification, the primary treated product is subsequently subjected to sulfhydryl modification treatment using sodium thioglycolate, and then the first component liquid containing the main plant active ingredient is supported. During the preparation process of the second active ingredient, the second component emulsion containing the auxiliary plant active ingredient is subjected to coating treatment. After preparing the functional masterbatch using the first active ingredient and the second active ingredient respectively, it is used for the functional modification treatment of nylon fiber. During the functional modification process of nylon fiber, it can effectively avoid the problems that the addition amount of the main plant active ingredient (such as the king medicine component) is large and the influence on the small-dose auxiliary plant active ingredient (such as the minister medicine component) is large, and during the functional treatment process of nylon fiber, the small-dose auxiliary plant active ingredient is easily lost and cannot reach the effective amount. As a result, the problem that each plant active ingredient cannot cooperate effectively can be effectively avoided. In the prepared bio-nylon fiber containing the plant active ingredient, the main component and the auxiliary component among the various plant active ingredients contained can cooperate effectively to achieve the targeted improvement and relief of the corresponding symptoms. At the same time, the stability of the various plant active ingredients in the nylon fiber is good, it is not easily lost, the loss amount of each active ingredient can be controlled within the allowable range of efficacy, the various plant active ingredients in the nylon fiber can be formulated under the optimal formulation conditions for a long time, the effect of improving and relieving the corresponding symptoms is stable, and the long-term effect is good. (2) In the bio-nylon fiber containing the plant active ingredients of the present invention, the first active ingredient containing the garden balsam ingredient which is the sovereign drug, and the second active ingredient containing mugwort which is the ministerial drug, knotweed which is the adjuvant drug, and safflower which is the ministerial drug are combined, and effective release control of each plant active ingredient in the first active ingredient and the second active ingredient can be realized by different treatment methods, and each plant active ingredient can be effectively formulated within the effective amount formulation range for a long period of time, thereby realizing improvement and relief for rheumatic pain. According to the test, for patients with rheumatic pain, soft tissue rheumatic pain can be effectively removed or significantly relieved, there is no recurrence or deterioration during the sticking period, and the total of the apparent efficiency and the effective efficiency is at most 100%. On the other hand, after stopping the sticking, there is no recurrence or deterioration of rheumatic pain during a period of 7 days. (3) The bio-nylon fiber containing the plant active ingredients of the present invention can not only achieve targeted improvement and relief for rheumatic pain, but also has a good antibacterial function. As a result of detection, the bacterial inhibition rate of the bio-nylon fiber against Staphylococcus aureus reaches 99.7 - 99.8%, the bacterial inhibition rate against Escherichia coli reaches 99.0 - 99.1%, the bacterial inhibition rate against Klebsiella pneumoniae reaches 98.0 - 98.3%, and the bacterial inhibition rate against Candida albicans reaches 95.7 - 96.0%. (4) In the bio-nylon fiber containing the plant active ingredients of the present invention, various plant active ingredients are firmly bound to the nylon fiber, the stability of each plant active ingredient in the nylon fiber is good, it is not easily lost due to the influence of external factors (such as washing, high temperature, high humidity, light, etc.), and the long-term effect is good. As a result of the test, the bio-nylon fiber of the plant active ingredients of the present invention, after standing for 960 h under continuous light conditions in an environment of 42°C and 75% relative humidity, the bacterial inhibition rate against Staphylococcus aureus still reaches 92.5 - 93.0%, the bacterial inhibition rate against Escherichia coli still reaches 91.7 - 92.1%, the bacterial inhibition rate against Klebsiella pneumoniae still reaches 90.8 - 91.1%, and the bacterial inhibition rate against Candida albicans still reaches 88.6 - 89.2%. (5) The bio-nylon fiber containing the plant active ingredient of the present invention has various plant active ingredients effectively bonded to the bio-nylon fiber, which can avoid the reduction of the physical properties of the modified nylon fiber while functionally modifying the nylon fiber. As a result of detection, the breaking strength of the bio-nylon fiber containing the plant active ingredient of the present invention is 5.6 to 5.9 cN / dtex, and the elongation at break is 24 to 25%. (6) The bio-nylon fiber containing the plant active ingredient of the present invention can be used as downstream applications such as bandages, joint covers, shoulder pads, lumbar pads, and even underwear products such as vests. While avoiding the adverse effects on the human intestine, stomach, and liver caused by oral ingestion of various plant active ingredients, it can achieve targeted improvement and relief of corresponding diseases, and further expand the application range of bio-nylon fibers.

Embodiments for Carrying Out the Invention

[0032] In order to more clearly explain the technical features, objectives, and effects of the present invention, specific embodiments of the present invention will be described. <Example 1> The preparation method of the bio-nylon fiber containing the plant active ingredient is specifically as follows. 1. First component extraction After rinsing the whole plant of Impatiens balsamina with 4 volumes of deionized water, it was placed in a vacuum drying box. The vacuum degree was controlled at 0.01 MPa, and the vacuum drying temperature was 60 °C. The whole plant of Impatiens balsamina was dried until the moisture content reached 4 wt%. Then it was transferred to an ultrafine grinder, and the ultrafine grinding temperature was controlled at 38 °C and ground to 1800 mesh to prepare the first active ingredient fine powder. Then the first active ingredient fine powder was put into 5 volumes of ethanol aqueous solution, stirred and heated to 40 °C, kept warm and stirred for 5 h, then ultrasonically extracted for 20 min. Subsequently, it was heated to 55 °C, kept warm and stirred for 20 min, then ultrasonically extracted for 10 min. The solid was filtered to obtain the primary extract. The solid was put into 3 volumes of ethanol aqueous solution, stirred and heated to 55 °C, kept warm and stirred for 20 min, then ultrasonically extracted for 10 min. The solid was filtered to obtain the secondary extract. The primary extract and the secondary extract were combined and left in an environment with a vacuum degree of 0.04 MPa, and vacuum concentrated to 30% of the original volume at 65 °C to prepare the first component solution. Here, the volume concentration of ethanol in the ethanol aqueous solution is 65%. The ultrasonic frequency of the ultrasonic extraction is 40 kHz, and the ultrasonic power is 350 W.

[0033] 2. Extraction of the second component After rinsing mugwort, Patrinia villosa, and safflower with deionized water four times their volume respectively, place them in a vacuum drying box, control the vacuum degree to 0.01 MPa, the vacuum drying temperature is 60 °C, dry until the moisture content reaches 4 wt%, transfer mugwort, Patrinia villosa, and safflower into an airflow pulverizer, mix and pulverize to 100 mesh, then put them into an ultrafine pulverizer, control the ultrafine pulverization temperature to 38 °C, pulverize to 1800 mesh to prepare the second active ingredient fine powder. Then, put the second active ingredient fine powder into an ethanol aqueous solution five times its volume, stir and heat up to 40 °C, keep stirring for 5 h, then perform ultrasonic extraction for 20 min. Subsequently, heat up to 55 °C, keep stirring for 20 min, then perform ultrasonic extraction for 10 min. Filter the solid matter to obtain the primary extract. Put the solid matter into an ethanol aqueous solution three times its volume, stir and heat up to 55 °C, keep stirring for 20 min, then perform ultrasonic extraction for 10 min. Filter the solid matter to obtain the secondary extract. Combine the primary extract and the secondary extract, place them in an environment with a vacuum degree of 0.04 MPa, and vacuum concentrate at 65 °C to 30% of the original volume to prepare the second component solution. Here, the weight ratio of mugwort, Patrinia villosa, and safflower is 10:6:0.6. The volume concentration of ethanol in the ethanol aqueous solution is 65%. The ultrasonic frequency of ultrasonic extraction is 40 kHz, and the ultrasonic power is 350 W.

[0034] 3. Preparation of the first active ingredient 1) Primary treatment According to the weight part ratio of 2:1, put nanomesoporous silica and perlite into a high-speed mixer, control the mixing rotation speed to 700 rpm, mix for 5 min to prepare the primary powder. Then, put the primary powder into toluene 20 times its volume, disperse it uniformly by ultrasonic, and then, under stirring conditions, add N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane and γ-aminopropyltrimethoxysilane, stir for 30 min, then stir and heat up to 80 °C, keep stirring for 10 h, then separate the solid matter, wash the solid matter twice with absolute ethanol four times its volume, and dry at 60 °C for 8 h to prepare the primary treated product. Here, the particle size of nanomesoporous silica is 200 nm, and the specific surface area is 550 m 2 / g, and the pore volume is 0.62 cm 2 / g. The weight ratio of the primary powder, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, and γ-aminopropyltrimethoxysilane is 8:1:0.8. 2) Secondary treatment The primary treated product is put into 13 times the volume of the secondary treatment liquid, stirred for 10 h, then the solid is separated, washed with 8 times the volume of deionized water, and then the solid is dried to a constant weight in a constant temperature drying box to prepare the secondary treated product. Here, the secondary treatment liquid is a deionized aqueous solution in which sodium thioglycolate is dissolved. In the secondary treatment liquid, the content of sodium thioglycolate is 8 wt%. 3) Loading The first component liquid and sodium dodecylbenzenesulfonate are put into an ethanol solution, stirred for 10 min, then the secondary treated product is continuously added and uniformly dispersed, then evacuated to a vacuum degree of 0.09 MPa, the vacuum is maintained for 30 min, then returned to atmospheric pressure, heated to 35 °C, kept warm and stirred for 20 h, then the solid is filtered and put into a vacuum drying box, the vacuum degree is controlled to 0.02 MPa, the vacuum drying temperature is 70 °C, and vacuum dried until the moisture content reaches 1 wt% to prepare the first active ingredient. Here, the weight ratio of the first component liquid, sodium dodecylbenzenesulfonate, the secondary treated product, and the ethanol solution is 16:0.05:7:50. The volume concentration of ethanol in the ethanol aqueous solution is 50%.

[0035] 4. Preparation of the second active ingredient Put the second component liquid, sodium carboxymethyl cellulose, and maltodextrin into deionized water, heat up to 40 °C, and emulsify uniformly with ultrasonic waves to prepare the second component emulsion. Put gum arabic and guar gum into deionized water, heat up to 50 °C, and stir uniformly to prepare the coating solution. Then, put the second component emulsion into 1.8 times the volume of the coating solution, disperse with ultrasonic waves for 1.5 h, cool to 4 °C, keep warm and stand for 2 h, filter the solid matter, put it into a vacuum drying box, control the vacuum degree to 0.05 MPa, the vacuum drying temperature is 70 °C, and vacuum dry until the water content reaches 1 wt% to prepare the second active ingredient. Here, the weight ratio of the second component liquid, sodium carboxymethyl cellulose, maltodextrin, and deionized water in the second component emulsion is 16:0.4:1:50. The weight ratio of gum arabic, guar gum, and deionized water in the coating solution is 20:0.8:150.

[0036] 5. Preparation of the functional masterbatch After uniformly mixing nylon 66 slices, the first active ingredient, antioxidant 1790, and sodium stearate, put them into a screw extruder, control the temperature to 260 °C, keep warm and melt, then extrude and granulate to prepare the first functional masterbatch. At the same time, after uniformly mixing nylon 66 slices, the second active ingredient, antioxidant 1790, and sodium stearate, put them into a screw extruder, control the temperature to 260 °C, keep warm and melt, then extrude and granulate to prepare the second functional masterbatch. Here, the weight ratio of nylon 66 slices, the first active ingredient, antioxidant 1790, and sodium stearate in the first functional masterbatch is 80:10:1:0.7. The weight ratio of nylon 66 slices, the second active ingredient, antioxidant 1790, and sodium stearate in the second functional masterbatch is 80:20:1:0.7.

[0037] 6. Spinning After uniformly mixing nylon 66 slices, the first functional masterbatch, and the second functional masterbatch, control the melting temperature at 260 °C. After extrusion and melting, control the spinning speed at 1600 m / min with a screw spinning machine. After spinning to prepare fibers, perform stretching, oil application, and winding to prepare bio-nylon fibers containing plant active ingredients. Here, the weight ratio of nylon 66 slices, the first functional masterbatch, and the second functional masterbatch is 100:4:7. The bio-nylon fibers containing plant active ingredients in this example are prepared by the above preparation method.

[0038] <Example 2> The preparation method of bio-nylon fibers containing plant active ingredients is specifically as follows. 1. First component extraction Rinse the whole plant of Portulaca oleracea with 6 times the volume of deionized water, then put it into a vacuum drying box, control the vacuum degree at 0.015 MPa, the vacuum drying temperature is 65 °C, dry the whole plant of Portulaca oleracea until the moisture content reaches 5 wt%, then transfer it to an ultrafine pulverizer, control the ultrafine pulverization temperature at 40 °C, pulverize it to 1900 mesh to prepare the first active ingredient fine powder. Then put the first active ingredient fine powder into 5.5 times the volume of ethanol aqueous solution, stir and heat up to 45 °C, keep stirring for 5.5 h, then perform ultrasonic extraction for 25 min. Subsequently, heat up to 60 °C, keep stirring for 25 min, then perform ultrasonic extraction for 15 min. Filter the solid matter to obtain the primary extract. Put the solid matter into 3.5 times the volume of ethanol aqueous solution, stir and heat up to 60 °C, keep stirring for 25 min, then perform ultrasonic extraction for 15 min. Filter the solid matter to obtain the secondary extract. Combine the primary extract and the secondary extract, place them in an environment with a vacuum degree of 0.045 MPa, and vacuum concentrate at 70 °C to 32% of the original volume to prepare the first component liquid. Here, the volume concentration of ethanol in the ethanol aqueous solution is 70%. The ultrasonic frequency of ultrasonic extraction is 42 kHz, and the ultrasonic power is 400 W.

[0039] 2. Second component extraction After rinsing mugwort, Patrinia villosa, and safflower with six times their volume of deionized water respectively, place them in a vacuum drying box, control the vacuum degree to 0.015 MPa, the vacuum drying temperature is 65 °C, dry until the moisture content reaches 5 wt%, transfer mugwort, Patrinia villosa, and safflower into an airflow pulverizer, mix and pulverize to 120 mesh, then put them into an ultrafine pulverizer, control the ultrafine pulverization temperature to 40 °C, pulverize to 1900 mesh to prepare the second active ingredient fine powder. Then, put the second active ingredient fine powder into 5.5 times its volume of ethanol aqueous solution, stir and heat up to 45 °C, keep stirring for 5.5 h, then perform ultrasonic extraction for 25 min, continue to heat up to 60 °C, keep stirring for 25 min, then perform ultrasonic extraction for 15 min, filter the solid matter to obtain the primary extract. Put the solid matter into 3.5 times its volume of ethanol aqueous solution, stir and heat up to 60 °C, keep stirring for 25 min, then perform ultrasonic extraction for 15 min, filter the solid matter to obtain the secondary extract. Combine the primary extract and the secondary extract, place them in an environment with a vacuum degree of 0.045 MPa, and vacuum concentrate at 70 °C to 32% of the original volume to prepare the second component liquid. Here, the weight ratio of mugwort, Patrinia villosa, and safflower is 11:6.5:0.7. The volume concentration of ethanol in the ethanol aqueous solution is 70%. The ultrasonic frequency of ultrasonic extraction is 42 kHz, and the ultrasonic power is 400 W.

[0040] 3. Preparation of the first active ingredient 1) Primary treatment According to the weight part ratio of 2.5:1, put nanomesoporous silica and perlite into a high-speed mixer, control the mixing rotation speed to 750 rpm, mix for 8 min to prepare the primary powder. Then, put the primary powder into 21 times its volume of toluene, disperse it uniformly by ultrasonic, and then, under stirring conditions, add N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane and γ-aminopropyltrimethoxysilane, stir for 35 min, then stir and heat up to 85 °C, keep stirring for 11 h, then separate the solid matter, wash the solid matter three times with 5 times its volume of absolute ethanol, and dry at 65 °C for 9 h to prepare the primary treated product. Here, the particle size of the nanomesoporous silica is 220 nm, and the specific surface area is 590 m2 / g, and the pore volume is 0.65 cm 2 / g. The weight ratio of the primary powder, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, and γ-aminopropyltrimethoxysilane is 9:1.5:0.9. 2) Secondary treatment The primary treated product is put into 14 times the volume of the secondary treatment liquid, stirred for 11 h, then the solid is separated, washed with 9 times the volume of deionized water, and then the solid is dried to a constant weight in a constant temperature drying box to prepare the secondary treated product. Here, the secondary treatment liquid is an aqueous deionized solution in which sodium thioglycolate is dissolved. In the secondary treatment liquid, the content of sodium thioglycolate is 9 wt%. 3) Loading The first component liquid and sodium dodecylbenzenesulfonate are put into an ethanol solution, stirred for 15 min, then the secondary treated product is continuously added and uniformly dispersed, then evacuated to a vacuum degree of 0.092 MPa, the vacuum is maintained for 40 min, then returned to atmospheric pressure, heated to 38 °C, and kept warm and stirred for 22 h, then the solid is filtered and put into a vacuum drying box, the vacuum degree is controlled to 0.025 MPa, the vacuum drying temperature is 75 °C, and vacuum dried until the moisture content is 1.2 wt% to prepare the first active ingredient. Here, the weight ratio of the first component liquid, sodium dodecylbenzenesulfonate, the secondary treated product, and the ethanol solution is 17:0.055:7.5:55. The volume concentration of ethanol in the ethanol aqueous solution is 55%.

[0041] 4. Preparation of the second active ingredient The second component liquid, sodium carboxymethyl cellulose, and maltodextrin are added to deionized water, heated to 45°C, and emulsified uniformly by ultrasonic waves to prepare the second component emulsion. Gum arabic and guar gum are added to deionized water, heated to 55°C, and stirred uniformly to prepare the coating solution. Then, the second component emulsion is added to twice the volume of the coating solution, ultrasonically dispersed for 2 h, cooled to 5°C, and allowed to stand at a constant temperature for 3 h. The solids are filtered and placed in a vacuum drying box. The vacuum degree is controlled to 0.055 MPa, the vacuum drying temperature is 75°C, and vacuum drying is carried out until the water content reaches 1.2 wt% to prepare the second active ingredient. Here, the weight ratio of the second component liquid, sodium carboxymethyl cellulose, maltodextrin, and deionized water in the second component emulsion is 17:0.45:1.3:55. The weight ratio of gum arabic, guar gum, and deionized water in the coating solution is 22:0.9:155.

[0042] 5. Preparation of the functional masterbatch Nylon 66 slices, the first active ingredient, antioxidant 1790, and sodium stearate are uniformly mixed and then put into a screw extruder. The temperature is controlled to 263°C, kept warm and melted, and then extruded and granulated to prepare the first functional masterbatch. At the same time, nylon 66 slices, the second active ingredient, antioxidant 1790, and sodium stearate are uniformly mixed and then put into a screw extruder. The temperature is controlled to 263°C, kept warm and melted, and then extruded and granulated to prepare the second functional masterbatch. Here, the weight ratio of nylon 66 slices, the first active ingredient, antioxidant 1790, and sodium stearate in the first functional masterbatch is 85:10.5:1.1:0.75. The weight ratio of nylon 66 slices, the second active ingredient, antioxidant 1790, and sodium stearate in the second functional masterbatch is 85:21:1.1:0.75.

[0043] 6. Spinning After uniformly mixing nylon 66 slices, the first functional masterbatch, and the second functional masterbatch, the melting temperature is controlled at 263 °C. After extrusion and melting, the spinning speed is controlled at 1700 m / min with a screw spinning machine. After spinning to prepare fibers, stretching, applying an oil agent, and winding are carried out to prepare bio-nylon fibers containing plant active ingredients. Here, the weight ratio of nylon 66 slices, the first functional masterbatch, and the second functional masterbatch is 100:4.7:7.5. The bio-nylon fibers containing plant active ingredients in this example are prepared by the above preparation method.

[0044] <Example 3> The preparation method of bio-nylon fibers containing plant active ingredients is specifically as follows. 1. First component extraction After rinsing the whole herb of Portulaca oleracea with 8 times the volume of deionized water, put it into a vacuum drying box, control the vacuum degree at 0.02 MPa, the vacuum drying temperature is 70 °C, dry the whole herb of Portulaca oleracea until the moisture content reaches 6 wt%, then transfer it into an ultrafine pulverizer, control the ultrafine pulverization temperature at 42 °C, pulverize it to 2000 mesh to prepare the first active ingredient fine powder. Then put the first active ingredient fine powder into 6 times the volume of ethanol aqueous solution, stir and heat up to 50 °C, keep warm and stir for 6 h, then carry out ultrasonic extraction for 30 min. Subsequently, heat up to 65 °C, keep warm and stir for 30 min, then carry out ultrasonic extraction for 20 min. Filter the solid matter to obtain the primary extract. Put the solid matter into 4 times the volume of ethanol aqueous solution, stir and heat up to 65 °C, keep warm and stir for 30 min, then carry out ultrasonic extraction for 20 min. Filter the solid matter to obtain the secondary extract. Combine the primary extract and the secondary extract, place it in an environment with a vacuum degree of 0.05 MPa, and vacuum concentrate at 75 °C to 35% of the original volume to prepare the first component solution. Here, the volume concentration of ethanol in the ethanol aqueous solution is 75%. The ultrasonic frequency of ultrasonic extraction is 45 kHz, and the ultrasonic power is 450 W.

[0045] 2. Second component extraction After rinsing mugwort, Patrinia scabiosaefolia, and safflower with 8 times their volume of deionized water respectively, place them in a vacuum drying box, control the vacuum degree to 0.02 MPa, the vacuum drying temperature is 70 °C, dry until the moisture content reaches 6 wt%, transfer mugwort, Patrinia scabiosaefolia, and safflower into an airflow pulverizer, mix and pulverize to 150 mesh, then put them into an ultrafine pulverizer, control the ultrafine pulverization temperature to 42 °C, pulverize to 2000 mesh to prepare the second active ingredient fine powder. Then, put the second active ingredient fine powder into 6 times its volume of ethanol aqueous solution, stir and heat up to 50 °C, keep warm and stir for 6 h, then extract with ultrasonic for 30 min. Subsequently, continue to heat up to 65 °C, keep warm and stir for 30 min, then extract with ultrasonic for 20 min, filter the solid matter to obtain the primary extract. Put the solid matter into 4 times its volume of ethanol aqueous solution, stir and heat up to 65 °C, keep warm and stir for 30 min, then extract with ultrasonic for 20 min, filter the solid matter to obtain the secondary extract. Combine the primary extract and the secondary extract, place them in an environment with a vacuum degree of 0.05 MPa, and vacuum concentrate at 75 °C to 35% of the original volume to prepare the second component liquid. Here, the weight ratio of mugwort, Patrinia scabiosaefolia, and safflower is 12:7:0.8. The volume concentration of ethanol in the ethanol aqueous solution is 75%. The ultrasonic frequency of ultrasonic extraction is 45 kHz, and the ultrasonic power is 450 W.

[0046] 3. Preparation of the first active ingredient 1) Primary treatment According to the weight part ratio of 3:1, put nanomesoporous silica and perlite into a high-speed mixer, control the mixing rotation speed to 800 rpm, mix for 10 min to prepare the primary powder. Then, put the primary powder into 22 times its volume of toluene, disperse it uniformly with ultrasonic, and then, under stirring conditions, add N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane and γ-aminopropyltrimethoxysilane, stir for 40 min, then stir and heat up to 90 °C, keep warm and stir for 12 h, then separate the solid matter, wash the solid matter 3 times with 6 times its volume of absolute ethanol, and dry at 70 °C for 10 h to prepare the primary treated product. Here, the particle size of nanomesoporous silica is 200 - 250 nm, and the specific surface area is 550 - 600 m2 / g, and the pore volume is 0.62 - 0.66 cm 2 / g. The weight ratio of the primary powder, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, and γ-aminopropyltrimethoxysilane is 10:2:1. 2) Secondary treatment The primary treated product is put into 15 times the volume of the secondary treatment solution, stirred for 12 h, then the solid is separated, washed with 10 times the volume of deionized water, and then the solid is dried to a constant weight in a constant temperature drying box to prepare the secondary treated product.

[0047] Here, the secondary treatment solution is a deionized aqueous solution in which sodium thioglycolate is dissolved. In the secondary treatment solution, the content of sodium thioglycolate is 10 wt%. 3) Loading The first component solution and sodium dodecylbenzenesulfonate are put into an ethanol solution, stirred for 20 min, then the secondary treated product is continuously added and uniformly dispersed, then evacuated to a vacuum degree of 0.095 MPa, the vacuum is maintained for 50 min, then returned to atmospheric pressure, heated to 40 °C, kept warm and stirred for 24 h, then the solid is filtered and put into a vacuum drying box, the vacuum degree is controlled to 0.03 MPa, the vacuum drying temperature is 80 °C, and vacuum dried until the moisture content is 1.5 wt% to prepare the first active ingredient. Here, the weight ratio of the first component solution, sodium dodecylbenzenesulfonate, the secondary treated product, and the ethanol solution is 18:0.06:8:60. The volume concentration of ethanol in the ethanol aqueous solution is 60%.

[0048] 4. Preparation of the second active ingredient The second component liquid, sodium carboxymethyl cellulose, and maltodextrin are added to deionized water, heated to 50°C, emulsified uniformly by ultrasonic waves to prepare the second component emulsion. Gum arabic and guar gum are added to deionized water, heated to 60°C, stirred uniformly to prepare the coating liquid. Then, the second component emulsion is added to 2.2 times the volume of the coating liquid, dispersed by ultrasonic waves for 2.5 h, cooled to 6°C, kept warm and allowed to stand for 4 h. The solid matter is filtered and placed in a vacuum drying box. The vacuum degree is controlled to 0.06 MPa, the vacuum drying temperature is 80°C, and vacuum drying is carried out until the water content reaches 1.5 wt% to prepare the second active ingredient. Here, the weight ratio of the second component liquid, sodium carboxymethyl cellulose, maltodextrin, and deionized water in the second component emulsion is 18:0.5:1.5:60. The weight ratio of gum arabic, guar gum, and deionized water in the coating liquid is 25:1:160.

[0049] 5. Preparation of Functional Masterbatch Nylon 66 slices, the first active ingredient, antioxidant 1790, and sodium stearate are uniformly mixed and then put into a screw extruder. The temperature is controlled to 265°C, kept warm and melted, and then extruded and granulated to prepare the first functional masterbatch. At the same time, nylon 66 slices, the second active ingredient, antioxidant 1790, and sodium stearate are uniformly mixed and then put into a screw extruder. The temperature is controlled to 265°C, kept warm and melted, and then extruded and granulated to prepare the second functional masterbatch. Here, the weight ratio of nylon 66 slices, the first active ingredient, antioxidant 1790, and sodium stearate in the first functional masterbatch is 90:11:1.2:0.8. The weight ratio of nylon 66 slices, the second active ingredient, antioxidant 1790, and sodium stearate in the second functional masterbatch is 90:22:1.2:0.8.

[0050] 6. Spinning After uniformly mixing nylon 66 slices, the first functional masterbatch, and the second functional masterbatch, control the melting temperature at 265 °C. After extrusion and melting, control the spinning speed at 1800 m / min with a screw spinning machine. After spinning to prepare fibers, perform stretching, oil application, and winding to prepare bio-nylon fibers containing plant active ingredients. Here, the weight ratio of nylon 66 slices, the first functional masterbatch, and the second functional masterbatch is 100:5:8. The bio-nylon fibers containing plant active ingredients in this example are prepared by the above preparation method.

[0051] <Comparative Example 1> Adopt the preparation method of the bio-nylon fibers containing plant active ingredients in Example 2, and the differences are as follows: 1) Omit the first component extraction step. In the second component extraction step, use balsam with mugwort, elsholtzia splendens, and safflower for the subsequent extraction step to prepare the total component liquid, and control the weight ratio of balsam, mugwort, elsholtzia splendens, and safflower at 30:11:6.5:0.7. 2) Omit the preparation step of the second active ingredient, and the prepared total component liquid is used in the loading step of the first active ingredient preparation.

[0052] <Comparative Example 2> Adopt the preparation method of the bio-nylon fibers containing plant active ingredients in Example 2, and the differences are as follows: 1) Use the first component liquid in the preparation step of the second active ingredient, and then prepare the first functional masterbatch. 2) Use the second component liquid in the preparation step of the first active ingredient, and then prepare the second functional masterbatch. 3) In the spinning step, control the weight ratio of nylon 66 slices, the first functional masterbatch, and the second functional masterbatch at 100:6:6.5.

[0053] <Comparative Example 3> The preparation method of the bio-nylon fiber containing the plant active ingredient of Example 2 was adopted, and the differences are as follows: 1) In the preparation step of the first active ingredient, the primary powder prepared by the primary treatment was adopted instead of the secondary treatment product and used in the loading step. 2) In the preparation step of the second active ingredient, after the second component emulsion was put into the coating solution and ultrasonically dispersed, the second active ingredient was prepared by spray drying.

[0054] The bio-nylon fiber containing the plant active ingredient of Examples 1 to 3 and spandex were blended to prepare a test bandage, and the content of the bio-nylon fiber containing the plant active ingredient in each test bandage was controlled to 94 wt% and the spandex content was controlled to 6 wt%.

[0055] 120 volunteers aged 30 to 50 suffering from rheumatic pain (such as rheumatic lumbocrural pain, rheumatic arthralgia, rheumatic neck and shoulder pain, etc.) were selected, and the number of male and female volunteers was controlled to be half and half. The 120 volunteers were randomly divided into 6 groups, and the number of male and female in each group was controlled to be half and half.

[0056] Among them, groups 1 to 3 corresponded to the application of the test bandages of Examples 1 to 3 respectively, and groups 4 to 6 corresponded to the application of the test bandages of Comparative Examples 1 to 3 respectively. The specific application method was that after cleaning the skin of the rheumatic pain site every day, the test bandage was fixed on the rheumatic pain site, and the test bandage was continuously fixed for more than 12 h every day and continuously applied for 42 days. At the same time, during the continuous application period, the test bandage was washed with water regularly once every 2 days. The application effect (obvious effect, effective, ineffective) of each test bandage was investigated, the corresponding number of people was counted, and the number of volunteers with obvious effects and recurrence or exacerbation of effective rheumatic pain was counted during the application period and within 7 days after the application was stopped.

[0057] Here, the obvious effect means that the rheumatic pain in the fixed area of the test bandage is effectively removed and does not recur during the application period.

[0058] "Effective" means that the rheumatoid pain at the test bandage fixation site is significantly relieved and does not worsen during the application period.

[0059] "Ineffective" means that there is no significant difference in the rheumatoid pain at the test bandage fixation site compared to the case where the test bandage is not applied. The specific test results are as follows: JPEG2025090009000001.jpg48170

[0060] As can be seen from the above table, in the bio-nylon fiber containing the plant active ingredient of the present invention, the first active ingredient containing the garden balsam ingredient which is the sovereign drug, mugwort which is the ministerial drug, the spreading plant which is the adjuvant drug, and the second active ingredient containing safflower which is the ministerial drug are combined, and by different treatment methods, the controlled release of each plant active ingredient in the first active ingredient and the second active ingredient is realized, ensuring that each active ingredient is effectively formulated within the effective dose blending range for a long period of time, and further realizing the improvement and relief of rheumatic pain. Also, during the test process, the test bandage can achieve the above effects no matter how many times conventional washing is performed. That is, the binding property between the plant active ingredient in the bio-nylon fiber containing the plant active ingredient of the present invention and the nylon fiber is good, and good long-term effectiveness can be maintained. As can be seen from Comparative Example 1, in the manufacturing method of performing loading after mixing all the plant active ingredients, the blending effect of each plant active ingredient is not ideal. On the other hand, the addition amount of the sovereign drug ingredient is large, and the influence on the adjuvant drug and ministerial drug ingredients with small addition amounts is large, affecting the exertion of the efficacy of the adjuvant drug and ministerial drug, and thus the blending effect of each plant active ingredient is not good. Specifically, the number of people with obvious effects decreases, the inefficiency increases, and after stopping the application of the test bandage, the number of people with recurrence or exacerbation of rheumatic pain increases. As can be seen from Comparative Example 2, after treating the first component liquid containing the garden balsam ingredient which is the sovereign drug by the preparation method of the second active ingredient to prepare the first functional masterbatch, and treating the second component liquid containing mugwort which is the ministerial drug, the spreading plant which is the adjuvant drug, and the safflower ingredient which is the ministerial drug by the preparation method of the first active ingredient to prepare the second functional masterbatch, because the treatment methods for different components change, the release amount of each component cannot be effectively and stably adjusted with the bio-nylon fiber. As a result, each active ingredient cannot cooperate within the effective dose blending range, and thus rheumatic pain cannot be effectively improved and relieved. Specifically, the number of people with obvious effects decreases, the inefficiency increases, and after stopping the application of the test bandage, the number of people with recurrence or exacerbation of rheumatic pain increases.As can be seen from Comparative Example 3, in the preparation process of the first active ingredient, after preparing primary powder using aminosilane for amino modification, subsequently performing sulfhydryl modification treatment on the primary treated product using sodium thioglycolate can realize effective loading and release control of the garden balsam component, which is the monarch drug in the first active ingredient. At the same time, combined with the coating treatment during the preparation of the second active ingredient, it can improve the coating and release control effects of mugwort, which is the ministerial drug in the second active ingredient, Patrinia villosa Juss., which is the adjuvant drug, and safflower component, which is the ministerial drug. As a result, each active ingredient can cooperate within the effective amount blending range. Since the related technical means were omitted in Comparative Example 3, the effect of realizing the improvement and relief of rheumatic pain decreased to a certain extent.

[0061] Furthermore, in accordance with the antibacterial-related content stipulated in GB / T20944.3-2008 "Evaluation of Antibacterial Properties of Textiles - Part 3: Vibration Method", antibacterial performance tests were conducted on the bio-nylon fibers containing the plant active ingredients of Examples 1 to 3 and Comparative Examples 1 to 3 respectively. The specific test results are as follows: JPEG2025090009000002.jpg52170

[0062] As can be seen from the above table, the bio-nylon fibers containing the plant active ingredients of the present invention can not only achieve the targeted improvement and relief of the above-mentioned rheumatic pain, but also have good antibacterial functions. As can be seen from Comparative Example 1 and Comparative Example 2, even if the treatment method of the plant active ingredient is changed, the influence on the antibacterial performance of the bio-nylon fiber is small. As can be seen from Comparative Example 3, omitting the synergistic modification treatment of amino groups and sulfhydryls of the primary powder or changing the coating process of the second active ingredient will affect the loading or coating effect of each plant active ingredient and is likely to be lost during the subsequent functional treatment process of the nylon fiber. Specifically, the antibacterial performance decreased.

[0063] Furthermore, the bio-nylon fibers containing the plant active ingredients of Examples 1 to 3 and Comparative Examples 1 to 3 were purely spun into fabrics and then cut into stability samples of 20 cm * 20 cm. Each stability sample was placed in an environment of 42 °C and 75% relative humidity, and left standing for 960 h under continuous irradiation of a 100 W xenon lamp. Then, the antibacterial performance detection method described above was used to test the antibacterial performance of each stability sample. The specific test results are as follows: JPEG2025090009000003.jpg53170

[0064] As can be seen from the above table, in the bio-nylon fibers containing the plant active ingredients of the present invention, the plant active ingredients are firmly bound to the bio-nylon fibers, the stability of each plant active ingredient in the nylon fibers is good, and it is not easily lost due to the influence of external factors (such as washing, high temperature, high humidity, light, etc.), and the long-term effect is good. As can be seen from Comparative Example 1, after omitting the preparation of the second active ingredient, since the plant active ingredient is treated singly, various components cannot be blended to obtain an antibacterial effect, and there is a problem that the active ingredient is lost during the long-term standing process. As can be seen from Comparative Example 2, even if the treatment method of the plant active ingredient is changed, the influence on the stability of the bio-nylon fiber is small. As can be seen from Comparative Example 3, if the synergistic modification treatment of the amino group and sulfhydryl of the primary powder is omitted or the coating process of the second active ingredient is changed, it will affect the loading or coating effect of each plant active ingredient, and it is easily lost during the subsequent functional treatment process of the nylon fiber, and the loss of the active ingredient increases due to the influence of external factors (such as washing, high temperature, high humidity, light, etc.), and specifically the antibacterial performance decreases.

[0065] Furthermore, the breaking strength and elongation at break of the bio-nylon fibers containing the plant active ingredients prepared in Examples 1 to 3 and Comparative Examples 1 to 3 were detected. The specific detection results are as follows: JPEG2025090009000004.jpg23170

[0066] As can be seen from the above table, in the bio-nylon fiber containing the plant active ingredient of the present invention, the plant active ingredient is effectively bound to the bio-nylon fiber, realizing the functional modification of the nylon fiber. At the same time, it is possible to avoid the decrease in the physical properties of the modified nylon fiber and maintain the good physical properties of the nylon fiber. Here, the significant attenuation of the related physical properties of the nylon fiber in Comparative Example 3 is because, after omitting the synergistic modification treatment of the amino group and sulfhydryl of the primary powder, the dispersibility of the first active ingredient in the nylon fiber is poor, resulting in a decrease in the physical properties of the nylon fiber. At the same time, after omitting the preparation process of the second active ingredient, the decrease in the coating effect also affects the physical properties of the nylon fiber to a certain extent.

[0067] As can be seen from the above, the method for preparing bio-nylon fibers containing the plant active ingredients of the present invention comprises preparing a first component liquid containing the main plant active ingredients by extracting the first component of garden balsam, preparing a second component liquid containing the auxiliary plant active ingredients by extracting the second components of mugwort, spreading plant, and safflower, during the preparation process of the first active ingredient, preparing primary powder using aminosilane for amino modification, and then successively performing sulfhydryl modification treatment on the primary treated product using sodium thioglycolate, and then loading the first component liquid containing the main plant active ingredients, during the preparation process of the second active ingredient, performing a coating treatment on the second component emulsion containing the auxiliary plant active ingredients, preparing a functional masterbatch using the first active ingredient and the second active ingredient respectively, and then using it for the functional modification treatment of nylon fibers, during the functional modification process of nylon fibers, the problem that the addition amount of the main plant active ingredients (such as the king drug ingredients) is large and the influence on the small-dose auxiliary plant active ingredients (such as the minister drug ingredients) is significant, and the problem that the small-dose auxiliary plant active ingredients are likely to be lost during the functional treatment process of nylon fibers and cannot reach the effective amount, and the problem that each plant active ingredient cannot cooperate effectively can be effectively avoided. In the prepared bio-nylon fibers containing plant active ingredients, the main components and auxiliary components among the various plant active ingredients contained can cooperate effectively to achieve targeted improvement and relief of the corresponding symptoms. At the same time, the stability of the various plant active ingredients in the nylon fibers is good, they are not easily lost, the loss amount of each active ingredient can be controlled within the allowable range of efficacy, the various plant active ingredients in the nylon fibers can be formulated under the optimal formulation conditions for a long time, the effect of improving and relieving the corresponding symptoms is stable, and the long-term effect is good. Unless otherwise specified, all percentages employed in the present invention are by mass.

[0068] Finally, the above are only preferred embodiments of the present invention and are not intended to limit the present invention. Although the present invention is described in detail with reference to the above embodiments, those skilled in the art should note that it is still possible to modify the technical solutions described in each of the above embodiments or make equivalent substitutions for some technical features. Any modifications, equivalent substitutions, improvements, etc. made without departing from the spirit and principles of the present invention shall all be included within the protection scope of the present invention.

Claims

1. The method includes steps of extracting a first component, extracting a second component, preparing a first active component, preparing a second active component, preparing a functional master batch, and spinning. The step of extracting the first component is to crush the dried whole plant of garden balsam, then ultrasonically extract it twice with an aqueous ethanol solution, combine the extracts, and concentrate them to prepare a first component solution; The step of extracting the second component is to mix and grind the dried mugwort, elongated grass and safflower, then ultrasonically extract them twice with an aqueous ethanol solution, combine the extracts and concentrate them to prepare a second component solution; The steps of preparing the first active ingredient include the steps of primary treatment, secondary treatment, and loading, The primary treatment step is to uniformly mix nano-mesoporous silica and perlite to prepare a primary powder, then add the primary powder to toluene and disperse it uniformly by ultrasonic waves, add N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane and γ-aminopropyltrimethoxysilane under stirring conditions, stir for 30-40 minutes, heat to 80-90°C, keep warm and stir for 10-12 hours, separate the solid matter, wash the solid matter with anhydrous ethanol and dry it to prepare a primary treatment product; The secondary treatment step is to introduce the primary treatment product into a secondary treatment solution having a volume 13 to 15 times that of the primary treatment product, stir the solution for 10 to 12 hours, separate the solid matter, wash the solid matter with deionized water, and then dry the solid matter to prepare a secondary treatment product; In the secondary treatment step, the secondary treatment liquid is a deionized aqueous solution in which sodium thioglycolate is dissolved; The loading step is as follows: add the first component liquid, sodium dodecylbenzenesulfonate, to an ethanol solution, and stir uniformly; then add the secondary processed material and disperse uniformly; evacuate to a vacuum of 0.09-0.095 MPa; maintain the vacuum for 30-50 min; return to atmospheric pressure; heat to 35-40° C.; stir while keeping warm; filter and vacuum dry the solid matter to prepare the first active component; The step of preparing the second active ingredient is to add the second component liquid, sodium carboxymethylcellulose, and maltodextrin to deionized water, emulsify by ultrasonic wave, prepare a second component emulsion, add gum arabic and guar gum to deionized water, heat to 50-60°C, and stir uniformly to prepare a coating liquid, add the second component emulsion to the coating liquid, disperse uniformly by ultrasonic wave, cool to 4-6°C, leave to stand for 2-4 hours, filter the solid matter and vacuum dry to prepare the second active ingredient; The step of preparing the functional masterbatch is to prepare a first functional masterbatch using a first active ingredient, and to prepare a second functional masterbatch using a second active ingredient; The spinning step is to mix the first functional masterbatch, the second functional masterbatch and a nylon raw material, and spin the mixture to prepare a bio-nylon fiber containing plant active ingredients; A method for preparing bio-nylon fiber containing a plant active ingredient, comprising the steps of:

2. In the primary treatment step, the weight ratio of nano-mesoporous silica to perlite is 2-3:1; The volume ratio of the primary powder to toluene is 1:20-22; the weight ratio of the primary powder, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, and γ-aminopropyltrimethoxysilane is 8-10:1-2:0.8-1; The particle size of nano-mesoporous silica is 200-250 nm, and the specific surface area is 550-600 m ２ / g and the pore volume is 0.62-0.66 cm ２ 2. The method for preparing bio-nylon fiber containing plant active ingredients according to claim 1, characterized in that the fiber contains at least one botanical active ingredient, and the fiber contains at least one botanical active ingredient.

3. The method for preparing bio-nylon fiber containing plant active ingredients according to claim 1, characterized in that in the secondary treatment step, the content of sodium thioglycolate in the secondary treatment solution is 8 to 10 wt %.

4. In the supporting step, the weight ratio of the first component liquid, sodium dodecylbenzenesulfonate, the secondary product, and the ethanol solution is 16-18: 0.05-0.06: 7-8: 50-60; The method for preparing bio-nylon fiber containing plant active ingredients according to claim 1, characterized in that the volume concentration of ethanol in the aqueous ethanol solution is 50 to 60%.

5. In the step of preparing the second active ingredient, the volume ratio of the second ingredient emulsion to the coating liquid is 1:1.8-2.2; the weight ratio of the second component liquid, sodium carboxymethylcellulose, maltodextrin, and deionized water in the second component emulsion is 16-18:0.4-0.5:1-1.5:50-60; The method for preparing bio-nylon fiber containing plant active ingredients according to claim 1, characterized in that the weight ratio of gum arabic, guar gum and deionized water in the coating solution is 20-25:0.8-1:150-160.

6. The step of preparing the functional masterbatch is to uniformly mix nylon 66 slices, a first active ingredient, antioxidant 1790, and sodium stearate, and then control the temperature to 260-265°C, keep the mixture warm and melt, and extrude and granulate to prepare a first functional masterbatch; The weight ratio of nylon 66 slice, first active ingredient, antioxidant 1790, and sodium stearate in the first functional masterbatch is 80-90: 10-11: 1-1.2: 0.7-0.8; Nylon 66 slices, the second active ingredient, antioxidant 1790, and sodium stearate are mixed uniformly, and then the temperature is controlled to 260-265°C, and the mixture is melted by keeping the temperature, and extruded to granulate to prepare the second functional masterbatch; The method for preparing bio-nylon fiber containing plant active ingredients according to claim 1, characterized in that the weight ratio of nylon 66 slice, second active ingredient, antioxidant 1790, and sodium stearate in the second functional masterbatch is 80-90:20-22:1-1.2:0.7-0.

8.

7. The spinning step is to uniformly mix the nylon 66 slices, the first functional masterbatch, and the second functional masterbatch, control the melting temperature to 260-265°C, extrude and melt, control the spinning speed to 1600-1800m / min, spin the mixture to prepare fibers, and then stretch, oil and wind the fibers to prepare bio-nylon fibers containing plant active ingredients; The method for preparing bio-nylon fiber containing plant active ingredients according to claim 1, characterized in that in the spinning step, the weight ratio of nylon 66 slices, the first functional masterbatch, and the second functional masterbatch is 100:4-5:7-8.

8. the step of extracting the first component is as follows: after rinsing the garden balsam with deionized water and drying, it is pulverized to 1800-2000 mesh to obtain a first active ingredient fine powder; then the first active ingredient fine powder is put into 5-6 volumes of ethanol aqueous solution, stirred and heated to 40-50°C, kept warm and stirred, ultrasonically extracted for 20-30 minutes, heated to 55-65°C, kept warm and stirred, ultrasonically extracted for 10-20 minutes, filtered to obtain a first extract; the solid matter is put into 3-4 volumes of ethanol aqueous solution, stirred and heated to 55-65°C, kept warm and stirred, ultrasonically extracted for 10-20 minutes, filtered to obtain a second extract; the first extract and the second extract are combined and vacuum concentrated to 30-35% of the original volume to obtain a first component liquid; The volume concentration of ethanol in the ethanol aqueous solution is 65 to 75%; The method for preparing bio-nylon fiber containing plant active ingredients according to claim 1, characterized in that the ultrasonic frequency of ultrasonic extraction is 40-45 kHz and the ultrasonic power is 350-450 W.

9. The second component extraction step is to rinse the mugwort, the thornwort and the safflower with deionized water, dry them, and then crush them to 1800-2000 mesh to prepare a second active ingredient fine powder; then add the second active ingredient fine powder to 5-6 times the volume of an ethanol aqueous solution, stir and heat to 40-50°C, keep warm and stir, perform ultrasonic extraction for 20-30 minutes, continue to heat to 55-65°C, keep warm and stir, perform ultrasonic extraction for 10-20 minutes, filter the solid matter to obtain a first extract; add the solid matter to 3-4 times the volume of an ethanol aqueous solution, stir and heat to 55-65°C, keep warm and stir, perform ultrasonic extraction for 10-20 minutes, filter the solid matter to obtain a second extract; combine the first extract and the second extract, and vacuum concentrate to 30-35% of the original volume to prepare a second component liquid; The weight ratio of the mugwort, the elongated grass, and the safflower is 10-12:6-7:0.6-0.8; The volume concentration of ethanol in the ethanol aqueous solution is 65 to 75%; The method for preparing bio-nylon fiber containing plant active ingredients according to claim 1, characterized in that the ultrasonic frequency of ultrasonic extraction is 40-45 kHz and the ultrasonic power is 350-450 W.

10. A bio-nylon fiber containing a botanical active ingredient, characterized in that it is prepared by the method for preparing a bio-nylon fiber containing a botanical active ingredient according to any one of claims 1 to 9.

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