Patent Application
20250179693
The present disclosure claims priority to Chinese Patent Application No. 202311639241.6, filed on Dec. 4, 2023, the content of which is incorporated herein by reference in its entirety.
The present disclosure relates to the field of bio-nylon fibers, and more specifically, relates to a bio-nylon fiber containing plant active components and preparation method thereof.
Nylon fiber, English name Polyamide, scientific name polyamide, also known as Nylon, is the first synthetic fiber to be introduced globally. The most notable advantages of nylon fiber include its superior wear resistance compared to other fibers and its excellent elasticity. The elastic recovery rate of nylon fiber is even comparable to that of wool. Incorporating some nylon fiber into blended fabrics may significantly enhance the fabric's wear resistance. When nylon fibers are stretched to 103-106%, their elastic recovery rate may reach 100%. Moreover, nylon fibers may withstand thousands of flexes without breaking. Among the commercially available synthetic fibers in the prior art, the density of nylon fiber is second only to polypropylene fiber (PP). Therefore, nylon fibers may be processed into fine, soft, and smooth threads, which may be woven into aesthetically pleasing and durable fiber products. Like polyester fibers, nylon fibers are also corrosion-resistant, insect-resistant, and mildew-resistant. Nylon filaments may be used to make socks, underwear, shirts, sportswear, ski jackets, raincoats, etc.; Nylon short fibers may be blended with cotton, wool, and viscose fibers to produce fabrics with excellent wear resistance and strength. Additionally, nylon fibers may be used for making hook-and-loop fasteners, carpets, decorative fabrics, etc. Industrially, nylon fibers are primarily used in the manufacture of cord fabrics, conveyor belts, fishing nets, ropes, and more.
With the advancement of science and technology and the improvement of living standards, the functionality of nylon fibers may gradually fail to meet practical application requirements, leading to an increasing focus on the functional improvement of nylon fibers. In recent years, a plurality of functional nylon fibers with diverse properties has been developed both domestically and internationally, continuously innovating and offering broad application prospects. The prior art has already developed various functional nylon fibers with different characteristics, such as acid-resistant nylon fibers, antioxidant nylon fibers, antistatic elastic nylon fibers, antibacterial nylon fibers, skincare nylon fibers, radiation-resistant nylon fibers, etc. Therefore, it is significant to conduct research on the functionality of nylon fibers and to expand their application fields.
One aspect of the present disclosure provides a method for preparing a bio-nylon fiber including plant active components. The method includes extracting a first component, extracting a second component, preparing a first active component, preparing a second active component, preparing a functional masterbatch, and spinning. Extracting the first component includes: drying a whole herb of Speranskia tuberculata, pulverizing, performing an ultrasonic extraction twice using an ethanol aqueous solution to obtain a first extraction solution of the first component and a second extraction solution of the first component respectively, combining the first extraction solution of the first component and the second extraction solution of the first component, and concentrating to obtain a first component solution. Extracting the second component includes: drying Artemisia argyi, Lygodium japonicum and Carthamus tinctorius, mixing and pulverizing, performing an ultrasonic extraction twice using an ethanol aqueous solution to obtain a first extraction solution of the second component and a second extraction solution of the second component respectively, combining the first extraction solution of the second component and the second extraction solution of the second component, and concentrating to obtain a second component solution. Preparing the first active component includes first processing, second processing and loading. Where the first processing includes: mixing nano-mesoporous silica and perlite to obtain a primary powder, placing the primary powder into toluene and ultrasonically dispersing evenly; adding N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane and γ-aminopropyltrimethoxysilane while stirring, and stirring for 30-40 min; increasing the temperature to 80-90° C. while stirring, stirring the mixture for 10-12 hours at this temperature, and separating the mixture to obtain a solid material; and washing the solid material with anhydrous ethanol, and drying the solid material to obtain a first processed material. The second processing includes: placing the first processed material into 13-15 times the volume of a second processing solution to obtain a mixture, stirring the mixture for 10-12 hours, and separating the mixture to obtain a solid material; and washing the solid material with deionized water, drying the solid material to obtain a second processed material, where the second processing solution is a deionized aqueous solution of sodium mercaptoacetate. The loading includes: adding the first component solution and sodium dodecylbenzenesulfonate into an ethanol solution, and stirring evenly; adding the second processed material, and dispersing evenly to obtain a mixture; vacuuming until a vacuum degree reaches 0.09-0.095 MPa, maintaining at the vacuum degree of 0.09-0.095 MPa for 30-50 min; restoring to a normal pressure, and raising a temperature to 35-40° C.; and stirring the mixture at the temperature of 35-40° C. constantly, filtering the mixture to obtain a solid material, and vacuum drying the solid material to obtain the first active component. Preparing the second active component includes: adding the second component solution, sodium carboxymethyl cellulose, and maltodextrin to deionized water, and ultrasonically emulsifying to obtain a second component emulsion for later use; adding Arabic gum and guar gum to deionized water, heating to 50-60° C. while stirring evenly, to obtain a coating solution; adding the second component emulsion to the coating solution to obtain a mixture, ultrasonically dispersing evenly, and cooling to 4-6° C.; and keeping the mixture at this temperature for 2-4 hours, filtering the mixture to obtain a solid material, and vacuum drying the solid material to obtain the second active component. Preparing the functional masterbatch includes using the first active component to prepare a first functional masterbatch and using the second active component to prepare a second functional masterbatch. The spinning includes: mixing the first functional masterbatch, the second functional masterbatch and nylon raw material, and spinning to obtain the bio-nylon fiber including the plant active component.
Another aspect of the present disclosure provides a bio-nylon fiber including nylon 66 and a plurality of plant active components, wherein the plurality of plant active components are extracted from Speranskia tuberculata, Artemisia argyi, Lygodium japonicum and Carthamus tinctorius.
To have a clearer understanding of the technical features, objectives, and effects of the present disclosure, the following specific embodiments of the present disclosure are now described.
To enhance the performance and application range of nylon fibers, the inventors develop bio-nylon (e.g., big-bio-nylon) fiber containing plant active components. This functional modification may be achieved by incorporating plant active components that can synergistically realize the functions of dispelling wind, relieving pain, and anti-inflammation into the nylon fibers. This modification may enable the effective and sustained release of the plant active components on the bio-nylon (e.g., big-bio-nylon) fiber. Additionally, the functionally modified bio-nylon (e.g., big-bio-nylon) fibers may be used to produce bandages, joint supports, shoulder supports, waist supports, and even vests and other downstream innerwear products. The plant active components released by the bio-nylon (e.g., big-bio-nylon) fibers may be absorbed through the skin, effectively improving and alleviating corresponding symptoms, and avoiding the direct stimulation of the gastrointestinal tract by orally administered plant active components.
During the process of modifying nylon fibers using a combination of plant active components, the inventors discovered the following issues. First, after completing the functional modification of nylon fibers using a plurality of plant active components, the main components and auxiliary components of these active components may not effectively synergize, failing to achieve the desired effects of dispelling wind, relieving pain, and anti-inflammation, resulting in suboptimal improvement and relief of rheumatic pain. Second, the stability of the plurality of plant active components in the nylon fibers may vary, leading to different rates of loss of these components within the nylon fibers. When subjected to external factors (such as washing, high temperature, high humidity, light exposure, etc.), the amount of loss may differ, causing the plant active components within the nylon fibers to fail to cooperate under optimal ratio conditions, thereby affecting the stability and long-term effectiveness of the bio-nylon (e.g., big-bio-nylon) fibers in relieving rheumatic pain. Third, during the functional modification of nylon fibers using a combination of plant active components, due to the large amount of main plant active components (such as sovereign herbs) added, there may be a significant impact on the small amounts of auxiliary plant active components (such as ministerial herbs). Furthermore, the small amounts of auxiliary plant active components may easily be lost during the functional processing of nylon fibers, failing to reach an effective dosage, which may result in the failure of effective cooperation among the plant active components and, consequently, in suboptimal improvement and relief of rheumatic pain.
A method for preparing bio-nylon (e.g., big-bio-nylon) fibers containing plant active components, specifically as follows.
After washing a whole herb of Speranskia tuberculata with 4 times the volume of deionized water, the whole herb is placed in a vacuum drying oven, where the vacuum is maintained at 0.01 MPa, and the vacuum drying temperature is controlled at 60° C. until the moisture content of the whole herb of Speranskia tuberculata is 4 wt %. The dried herb is then transferred to an ultrafine pulverizer, where the pulverizing temperature is controlled at 38° C., and it is pulverized to 1800 mesh, resulting in a micro-powder of a first active component. The micro-powder is then added to five times the volume of an ethanol aqueous solution, stirred, and heated to 40° C. After maintaining the temperature and stirring for 5 hours, ultrasonic extraction is performed for 20 minutes. The temperature is then increased to 55° C., and after maintaining the temperature and stirring for 20 minutes, ultrasonic extraction is performed for 10 minutes. The solid material is filtered out, and the first extraction solution is obtained. The solid material is then added to three times the volume of an ethanol aqueous solution, stirred, and heated to 55° C. After maintaining the temperature and stirring for 20 minutes, ultrasonic extraction is performed for 10 minutes, and the solid material is filtered out to obtain the second extraction solution. The first and second extraction solutions are combined, and vacuum concentrated at 65° C. under a vacuum degree of 0.04 MPa until the volume is reduced to 30% of the original volume, resulting in the first component solution.
In this process, the ethanol aqueous solution has a volume concentration of 65%.
The ultrasonic extraction is performed at an ultrasonic frequency of 40 kHz and an ultrasonic power of 350 W.
After respectively washing Artemisia argyi, Lygodium japonicum and Carthamus tinctorius with 4 times the volume of deionized water, the herbs are placed in a vacuum drying oven, where the vacuum is maintained at 0.01 MPa, and the vacuum drying temperature is controlled at 60° C. until the moisture content is 4 wt %. The dried herbs are then transferred to a jet mill, where they are mixed and pulverized to 100 mesh. The mixture is then placed in an ultrafine pulverizer, where the pulverizing temperature is controlled at 38° C., and the mixture is pulverized to 1800 mesh, resulting in a micro-powder of the second active component. The micro-powder of the second active component is then added to 5 times the volume of an ethanol aqueous solution, stirred, and heated to 40° C. After maintaining the temperature and stirring for 5 hours, ultrasonic extraction is performed for 20 minutes. The temperature is then increased to 55° C., and after maintaining the temperature and stirring for 20 minutes, ultrasonic extraction is performed for 10 minutes. A solid material is filtered out, and a first extraction solution is obtained. The solid material is then added to 3 times the volume of an ethanol aqueous solution, stirred, and heated to 55° C. After maintaining the temperature and stirring for 20 minutes, ultrasonic extraction is performed for 10 minutes, and the solid material is filtered out to obtain a second extraction solution. The first and second extraction solutions are combined and vacuum concentrated at 65° C. under a vacuum degree of 0.04 MPa until the volume is reduced to 30% of the original volume, resulting in the second component solution.
The Artemisia argyi, the Lygodium japonicum and the Carthamus tinctorius are in a weight ratio of 10:6:0.6.
The ethanol aqueous solution has a volume concentration of 65%.
The ultrasonic extraction is performed at an ultrasonic frequency of 40 kHz and an ultrasonic power of 350 W.
According to a weight ratio of 2:1, nano-mesoporous silica and perlite are added to a high-speed mixer, where the mixing speed is controlled at 700 rpm, and mixed for 5 minutes to obtain a primary powder. The primary powder is then added to 20 times the volume of toluene and ultrasonically dispersed evenly. Under stirring conditions, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane and γ-aminopropyltrimethoxysilane are added, stirred for 30 minutes, then heated to 80° C. under stirring. After maintaining the temperature and stirring for 10 hours, the solid material is separated, washed twice with 4 times the volume of anhydrous ethanol, and dried at 60° C. for 8 hours to obtain a first processed material.
The nano-mesoporous silica has a particle size of 200 nm, a specific surface area of 550 m2/g, and a pore volume of 0.62 cm3/g.
The primary powder, the N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, and the γ-aminopropyltrimethoxysilane are in a weight ratio of 8:1:0.8.
The first processed material is added to 13 times the volume of a second processing solution, stirred for 10 hours, and the solid material is separated. After washing with 8 times the volume of deionized water, the solid material is dried to a constant weight in a constant-temperature drying oven to obtain a second processed material.
The second processing solution is an aqueous solution of deionized water in which sodium mercaptoacetate is dissolved. The content of sodium mercaptoacetate in the second processing solution is 8 wt %.
The first component solution and sodium dodecylbenzenesulfonate are added to an ethanol solution, stirred for 10 minutes, and then the second processed material is added and evenly dispersed. After vacuuming to a vacuum degree of 0.09 MPa and maintaining the vacuum for 30 minutes, the pressure is restored to normal, and the temperature is increased to 35° C. After maintaining the temperature and stirring for 20 hours, the solid material is filtered out and placed in a vacuum drying oven. The vacuum is controlled at 0.02 MPa, the vacuum drying temperature is 70° C., and vacuum drying is performed until the moisture content is 1 wt %, resulting in a first active component.
The first component solution, the sodium dodecylbenzenesulfonate, the second processed material, and the ethanol solution are in a weight ratio of 16:0.05:7:50. The ethanol aqueous solution has a volume concentration of 50%.
The second component solution, sodium carboxymethyl cellulose, and maltodextrin are added into deionized water, heated to 40° C., and emulsified ultrasonically to uniformly form a second component emulsion, which is set aside for later use. Arabic gum and guar gum are added into deionized water, heated to 50° C., and stirred to form a coating solution. The second component emulsion is then added to 1.8 times the volume of the coating solution, ultrasonically dispersed for 1.5 hours, cooled to 4° C., and allowed to stand for 2 hours. The solid material is then filtered and placed in a vacuum drying oven, where the vacuum is maintained at 0.05 MPa and the drying temperature is controlled at 70° C. Vacuum drying is performed until the moisture content is 1 wt %, yielding a second active component.
In the second component emulsion, the second component solution, the sodium carboxymethyl cellulose, the maltodextrin, and the deionized water are in a weight ratio of 16:0.4:1:50.
In the coating solution, the Arabic gum, the guar gum, and the deionized water are in a weight ratio of 20:0.8:150.
Nylon 66 chips, the first active component, antioxidant 1790, and sodium stearate are mixed uniformly and then added to a screw extruder, while temperature is controlled at 260° C., and after being in a molten state, extruding and granulating are performed to obtain a first functional masterbatch. Simultaneously, nylon 66 chips, the second active component, antioxidant 1790, and sodium stearate are mixed uniformly and added to a screw extruder, while the temperature is controlled at 260° C., and after being in a molten state, extruding and granulating are performed to obtain a second functional masterbatch.
As used herein, the term Nylon 66 refers to a type of polyamide or nylon. Nylon 66 is made of two monomers each containing 6 carbon atoms, hexamethylenediamine and adipic acid. Nylon 66 (or “Poly[imino(1,6-dioxohexamethylene)iminohexamethylene]”) has a chemical formula of (C12H22N2O2)n.
As used herein, the term antioxidant 1790 refers to 1,3,5-tris[(4-tert-butyl-3-hydroxy-2,6-dimethylphenyl)methyl]-1,3,5-triazinane-2,4,6-trione with a chemical formula of C42H57N3O6.
In the first functional masterbatch, the nylon 66 chips, the first active component, the antioxidant 1790, and the sodium stearate are in a weight ratio of 80:10:1:0.7.
In the second functional masterbatch, the nylon 66 chips, the second active component, the antioxidant 1790, and the sodium stearate are in a weight ratio of 80:20:1:0.7.
Nylon 66 chips, the first functional masterbatch, and the second functional masterbatch are mixed uniformly. The temperature is controlled at the melting temperature of 260° C.; and after extrusion melting, a screw spinning machine is used, and the spinning speed is controlled at 1600 m/min for producing fibers. The fibers are then drawn, oiled, and wound to produce bio-nylon fibers containing plant active components.
The nylon 66 chips, the first functional masterbatch, and the second functional masterbatch are in a weight ratio of 100:4:7.
As disclosed herein, the bio-nylon fibers containing plant active components are prepared using the aforementioned preparation method.
A method for preparing bio-nylon fibers containing plant active components, specifically as follows:
After washing a whole herb of Speranskia tuberculata with 6 times the volume of deionized water, the whole herb is placed in a vacuum drying oven, where the vacuum is maintained at 0.015 MPa and the drying temperature is controlled at 65° C. until the moisture content of the whole herb of Speranskia tuberculata is 5 wt %. The dried herb is then transferred to an ultrafine pulverizer, where the pulverizing temperature is controlled at 40° C., and the dried herb is pulverized to 1900 mesh, resulting in a micro-powder of a first active component. The micro-powder is then added to an ethanol aqueous solution at 5.5 times its volume, stirred, and heated to 45° C. After maintaining the temperature and stirring for 5.5 hours, ultrasonic extraction is performed for 25 minutes. The temperature is then increased to 60° C., and after maintaining the temperature and stirring for 25 minutes, ultrasonic extraction is performed for 15 minutes. A solid material is filtered out, and a first extraction solution is obtained. The solid material is then added to 3.5 times the volume of an ethanol aqueous solution, stirred, and heated to 60° C. After maintaining the temperature and stirring for 25 minutes, ultrasonic extraction is performed for 15 minutes. A solid material is filtered out to obtain a second extraction solution. The first extraction solution and the second extraction solution are combined, and vacuum concentrated at 70° C. under a vacuum degree of 0.045 MPa until the volume is reduced to 32% of the original volume, resulting in a first component solution.
In this process, the ethanol aqueous solution has an ethanol concentration of 70%.
The ultrasonic extraction has an ultrasonic frequency of 42 kHz and an ultrasonic power of 400 W.
After respectively washing Artemisia argyi, Lygodium japonicum and Carthamus tinctorius with 6 times the volume of deionized water, the herbs are placed in a vacuum drying oven, where the vacuum is maintained at 0.015 MPa and the drying temperature is controlled at 65° C. until the moisture content is 5 wt %. The dried herbs are then transferred to a jet mill, where they are mixed and pulverized to 120 mesh. The mixture is then placed in an ultrafine pulverizer, where the pulverizing temperature is controlled at 40° C., and it is pulverized to 1900 mesh, resulting in a micro-powder of a second active component. The micro-powder is then added 5.5 times the volume of an ethanol aqueous solution, stirred, and heated to 45° C. After maintaining the temperature and stirring for 5.5 hours, ultrasonic extraction is performed for 25 minutes. The temperature is then increased to 60° C., and after maintaining the temperature and stirring for 25 minutes, ultrasonic extraction is performed for 15 minutes. A solid material is filtered out, and a first extraction solution is obtained. The solid material is then added to 3.5 times the volume of an ethanol aqueous solution, stirred, and heated to 60° C. After maintaining the temperature and stirring for 25 minutes, ultrasonic extraction is performed for 15 minutes. A solid material is filtered out to obtain a second extraction solution. The first extraction solution and the second extraction solution are combined and vacuum concentrated at 70° C. under a vacuum degree of 0.045 MPa until the volume is reduced to 32% of the original volume, resulting in a second component solution.
The Artemisia argyi, the Lygodium japonicum and the Carthamus tinctorius are in a weight ratio of 11:6.5:0.7.
The ethanol aqueous solution has an ethanol concentration of 70%.
The ultrasonic extraction is performed at an ultrasonic frequency of 42 kHz, and an ultrasonic power of 400 W.
According to a weight ratio of 2.5:1, nano-mesoporous silica and perlite are added to a high-speed mixer, where the mixing speed is controlled at 750 rpm, and mixed for 8 minutes to obtain a primary powder. The primary powder is then added to 21 times the volume of toluene and ultrasonically dispersed evenly. Under stirring conditions, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane and γ-aminopropyltrimethoxysilane are added, stirred for 35 minutes, then heated to 85° C. while stirring. After maintaining the temperature and stirring for 11 hours, a solid material is separated. The solid material is washed 3 times with 5 times the volume of anhydrous ethanol and dried at 65° C. for 9 hours to obtain a first processed material.
The nano-mesoporous silica has a particle size of 220 nm, a specific surface area of 590 m2/g, and a pore volume of 0.65 cm3/g.
The primary powder, the N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, and the γ-aminopropyltrimethoxysilane are in a weight ratio of 9:1.5:0.9.
The first processed material is added to 14 times the volume of a second processing solution, stirred for 11 hours, and a solid material is separated. After washing with deionized water at 9 times its volume, the solid material is dried to constant weight in a constant-temperature drying oven to obtain a second processed material.
The second processing solution is an aqueous solution of deionized water in which sodium mercaptoacetate is dissolved. In the second processing solution, the sodium mercaptoacetate has a content of 9 wt %.
The first component solution and sodium dodecylbenzene sulfonate are added to an ethanol solution, stirred for 15 minutes, and then the second processed material is added and evenly dispersed. After vacuuming to a vacuum degree of 0.092 MPa and maintaining the vacuum for 40 minutes, the pressure is restored to normal, and the temperature is increased to 38° C. After maintaining the temperature and stirring for 22 hours, the solid material is filtered out and placed in a vacuum drying oven. The vacuum is controlled at 0.025 MPa, the vacuum drying temperature is 75° C., and vacuum drying is performed until the moisture content is 1.2 wt %, yielding the first active component.
The first component solution, the sodium dodecylbenzene sulfonate, the second processed material, and the ethanol solution are in a weight ratio of 17:0.055:7.5:55.
The ethanol solution has a volume concentration of 55%.
The second component solution, sodium carboxymethyl cellulose, and maltodextrin are added into deionized water, heated to 45° C., and ultrasonically emulsified to uniformly form a second component emulsion, which is set aside for later use. Arabic gum and guar gum are added into deionized water, heated to 55° C., and stirred to form a coating solution. The second component emulsion is then added to 2 times the volume of the coating solution, ultrasonically dispersed for 2 hours, cooled to 5° C., and allowed to stand for 3 hours, resulting in a solid material. The solid material is then filtered and placed in a vacuum drying oven, where the vacuum is maintained at 0.055 MPa and the drying temperature is controlled at 75° C. Vacuum drying is performed until the moisture content is 1.2 wt %, yielding the second active component.
In the second component emulsion, the second component solution, the sodium carboxymethyl cellulose, the maltodextrin, and the deionized water are in a weight ratio of 17:0.45:1.3:55.
In the coating solution, the Arabic gum, the guar gum, and the deionized water are in a weight ratio of 22:0.9:155.
Nylon 66 chips, the first active component, antioxidant 1790, and sodium stearate are mixed uniformly and then added to a screw extruder, while temperature is controlled at 263° C., and after being in a molten state, extrusion and granulating are performed to obtain a first functional masterbatch. Simultaneously, nylon 66 chips, the second active component, antioxidant 1790, and sodium stearate are mixed uniformly and added to a screw extruder, while the temperature is controlled at 263° C., and after being in a molten state, extruding and granulating are performed to obtain a second functional masterbatch.
In the first functional masterbatch, the nylon 66 chips, the first active component, the antioxidant 1790, and the sodium stearate are in a weight ratio of 85:10.5:1.1:0.75.
In the second functional masterbatch, the nylon 66 chips, the second active component, the antioxidant 1790, and the sodium stearate are in a weight ratio of 85:21:1.1:0.75.
Nylon 66 chips, the first functional masterbatch, and the second functional masterbatch are mixed uniformly. The temperature is controlled at the melting temperature of 263° C. After extrusion melting, a screw spinning machine is used, and the spinning speed is controlled at 1700 m/min for producing fibers. The fibers are then drawn, oiled, and wound to obtain bio-nylon fibers containing plant active components.
The nylon 66 chips, the first functional masterbatch, and the second functional masterbatch are in a weight ratio of 100:4.7:7.5.
As disclosed herein, the bio-nylon fibers containing plant active components are prepared using the aforementioned preparation method.
A method for preparing bio-nylon fibers containing plant active components, specifically as follows:
After washing a whole herb of Speranskia tuberculata with 8 times the volume of deionized water, the whole herb is placed in a vacuum drying oven, where the vacuum is maintained at 0.02 MPa and the drying temperature is controlled at 70° C. until the moisture content of the whole herb of Speranskia tuberculata is 6 wt %, resulting in a dried herb. The dried herb is then transferred to an ultrafine pulverizer, where the pulverizing temperature is controlled at 42° C., and the dried herb is pulverized to 2000 mesh, resulting in a micro-powder of a first active component. The micro-powder is then added to 6 times the volume of an ethanol aqueous solution, stirred, and heated to 50° C. After maintaining the temperature and stirring for 6 hours, ultrasonic extraction is performed for 30 minutes. The temperature is then increased to 65° C., and after maintaining the temperature and stirring for 30 minutes, ultrasonic extraction is performed for 20 minutes. A solid material is filtered out, and a first extraction solution is obtained. The solid material is then added to 4 times the volume of an ethanol aqueous solution, stirred, and heated to 65° C. After maintaining the temperature and stirring for 30 minutes, ultrasonic extraction is performed for 20 minutes, and a solid material is filtered out to obtain a second extraction solution. The first extraction solution and the second extraction solution are combined and vacuum concentrated at 75° C. under a vacuum degree of 0.05 MPa until the volume is reduced to 35% of the original volume, resulting in a first component solution.
In this process, the ethanol aqueous solution has an ethanol concentration of 75%.
The ultrasonic extraction has an ultrasonic frequency of 45 kHz, and an ultrasonic power of 450 W.
After respectively washing Artemisia argyi, Lygodium japonicum and Carthamus tinctorius with 8 times the volume of deionized water, the herbs are placed in a vacuum drying oven, where the vacuum is maintained at 0.02 MPa and the drying temperature is controlled at 70° C. until the moisture content is 6 wt %, resulting in dried herbs. The dried herbs are then transferred to a jet mill, then mixed and pulverized to 150 mesh, resulting in a mixture. The mixture is then placed in an ultrafine pulverizer, where the pulverizing temperature is controlled at 42° C., and the mixture is pulverized to 2000 mesh, resulting in a micro-powder of a second active component. The micro-powder is then added to 6 times the volume of an ethanol aqueous solution, stirred, and heated to 50° C. After maintaining the temperature and stirring for 6 hours, ultrasonic extraction is performed for 30 minutes. The temperature is then increased to 65° C., and after maintaining the temperature and stirring for 30 minutes, ultrasonic extraction is performed for 20 minutes. A solid material is filtered out, and a first extraction solution is obtained. The solid material is then added to 4 times the volume of an ethanol aqueous solution, stirred, and heated to 65° C. After maintaining the temperature and stirring for 30 minutes, ultrasonic extraction is performed for 20 minutes. The solid material is filtered out to obtain a second extraction solution. The first extraction solution and the second extraction solution are combined and vacuum concentrated at 75° C. under a vacuum degree of 0.05 MPa until the volume is reduced to 35% of the original volume, resulting in a second component solution.
The Artemisia argyi, the Lygodium japonicum and the Carthamus tinctorius are in a weight ratio of 12:7:0.8.
The ethanol aqueous solution has an ethanol concentration of 75%.
The ultrasonic extraction has an ultrasonic frequency of 45 kHz, and an ultrasonic power of 450 W.
According to a weight ratio of 3:1, nano-mesoporous silica and perlite are added to a high-speed mixer, where the mixing speed is controlled at 800 rpm, and mixed for 10 minutes to obtain a primary powder. The primary powder is then added to 22 times the volume of toluene and ultrasonically dispersed evenly. Under stirring conditions, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane and γ-aminopropyltrimethoxysilane are added, stirred for 40 minutes, then heated to 90° C. under stirring. After maintaining the temperature and stirring for 12 hours, a solid material is separated, washed 3 times with 6 times the volume of anhydrous ethanol, and dried at 70° C. for 10 hours to obtain a first processed material.
The nano-mesoporous silica has a particle size of 200-250 nm, a specific surface area of 550-600 m2/g, and a pore volume of 0.62-0.66 cm3/g.
The primary powder, the N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, and the γ-aminopropyltrimethoxysilane are in a weight ratio of 10:2:1.
The first processed material is added to 15 times the volume of a second processing solution, stirred for 12 hours, and a solid material is separated. After washing with 10 times the volume of deionized water, the solid material is dried to constant weight in a constant-temperature drying oven to obtain a second processed material.
The second processing solution is an aqueous solution of deionized water in which sodium mercaptoacetate is dissolved. In the second processing solution, the sodium mercaptoacetate has a content of 10 wt %.
The first component solution and sodium dodecylbenzenesulfonate are added to an ethanol solution, stirred for 20 minutes, and then the second processed material is added and evenly dispersed. After vacuuming to a vacuum degree of 0.095 MPa and maintaining the vacuum for 50 minutes, the pressure is restored to normal, and the temperature is increased to 40° C. After maintaining the temperature and stirring for 24 hours, the solid material is filtered out and placed in a vacuum drying oven. The vacuum is controlled at 0.03 MPa, the vacuum drying temperature is 80° C., and vacuum drying is performed until the moisture content is 1.5 wt %, yielding the first active component.
The first component solution, the sodium dodecylbenzenesulfonate, the second processed material, and the ethanol solution are in a weight ratio of 18:0.06:8:60.
The ethanol solution has an ethanol concentration of 60%.
The second component solution, sodium carboxymethyl cellulose, and maltodextrin are added into deionized water, heated to 50° C., and ultrasonically emulsified to form a uniform second component emulsion, which is set aside for later use. Arabic gum and guar gum are added into deionized water, heated to 60° C., and stirred to form a coating solution. The second component emulsion is then added to 2.2 times the volume of the coating solution, ultrasonically dispersed for 2.5 hours, cooled to 6° C., and allowed to stand for 4 hours. The solid material is then filtered and placed in a vacuum drying oven, where the vacuum is maintained at 0.06 MPa and the drying temperature is controlled at 80° C. Vacuum drying is performed until the moisture content is 1.5 wt %, yielding the second active component.
In the second component emulsion, the second component solution, the sodium carboxymethyl cellulose, the maltodextrin, and the deionized water are in a weight ratio of 18:0.5:1.5:60.
In the coating solution, the Arabic gum, the guar gum, and the deionized water are in a weight ratio of 25:1:160.
Nylon 66 chips, the first active component, antioxidant 1790, and sodium stearate are mixed uniformly and then added to a screw extruder, while the temperature is controlled at 265° C., and after being in a molten state, extruding and granulating are performed to obtain a first functional masterbatch. Simultaneously, nylon 66 chips, the second active component, antioxidant 1790, and sodium stearate are mixed uniformly and added to a screw extruder, while the temperature is controlled at 265° C., and after being in a molten state, extruding and granulating are performed to obtain a second functional masterbatch.
In the first functional masterbatch, the nylon 66 chips, the first active component, the antioxidant 1790, and the sodium stearate are in a weight ratio of 90:11:1.2:0.8.
In the second functional masterbatch, the nylon 66 chips, the second active component, the antioxidant 1790, and the sodium stearate are in a weight ratio of 90:22:1.2:0.8.
Nylon 66 chips, the first functional masterbatch, and the second functional masterbatch are mixed uniformly. The temperature is controlled at the melting temperature of 265° C., and after extrusion melting, a screw spinning machine is used, and the spinning speed is controlled at 1800 m/min for producing fibers. The fibers are then drawn, oiled, and wound to obtain bio-nylon fibers containing plant active components.
The nylon 66 chips, the first functional masterbatch, and the second functional masterbatch are in a weight ratio of 100:5:8.
As disclosed herein, the bio-nylon fibers containing plant active components are prepared using the aforementioned preparation method.
The preparation method of bio-nylon fiber containing plant active components in Embodiment 2 is adopted, where the differences are: (1) omitting the step of extracting a first component, and in the step of extracting a second component, the subsequent extracting steps are performed with Speranskia tuberculata, Artemisia argyi, Lygodium japonicum and Carthamus tinctorius together to obtain a total component solution, where Speranskia tuberculata, Artemisia argyi, Lygodium japonicum and Carthamus tinctorius are in a weight ratio of 30:11:6.5:0.7; and (2) omitting the step of preparing a second active component, and in the step of loading, the aforementioned total component solution is used for preparing a first active component.
The preparation method of bio-nylon fiber containing plant active components in Embodiment 2 is adopted, where the differences are: (1) in the step of preparing a second active component, the first component solution is used for preparing the second active component, followed by the step of preparing a first functional masterbatch; (2) in the step of preparing a first active component, the second component solution is used for preparing the first active component, followed by the step of preparing a second functional masterbatch; and (3) in the step of spinning, nylon 66 chips, the first functional masterbatch, and the second functional masterbatch are in a weight ratio of 100:6:6.5.
The preparation method of bio-nylon fiber containing plant active components in Embodiment 2 is adopted, where the differences are: (1) in the step of preparing a first active component, a primary powder obtained from the first processing is used instead of a second processed material in the step of loading; and (2) in the step of preparing a second active component, a second component emulsion is added into a coating solution, dispersed by ultrasound, and then spray-dried to obtain the second active component.
The bio-nylon fiber containing plant active components from Embodiments 1-3 and Comparative Example 1 is blended with spandex to make experimental bandages, where the content of bio-nylon fiber containing plant active components in each experimental bandage is controlled at 94 wt %, and the content of spandex is 6 wt %.
A total of 120 volunteers aged 30-50 years suffering from rheumatic pain (such as rheumatic low back pain, rheumatic joint pain, rheumatic neck and shoulder pain, etc.) are selected, and the number of male and female volunteers is controlled to be equal. The 120 volunteers are randomly divided into 6 groups, where the number of males and females in each group is also controlled to be equal.
Groups 1-3 correspond to the application of the experimental bandages of Embodiments 1-3, and groups 4-6 correspond to the application of the experimental bandages of Comparative Examples 1-3. The specific method of application is: after cleaning the skin in the rheumatic pain area daily, the experimental bandage is fixed to the rheumatic pain area, where the experimental bandage is kept fixed for at least 12 hours every day, and applied continuously for 42 days. At the same time, during the continuous application period, the experimental bandage undergoes regular washing once every two days. The effectiveness of each experimental bandage is investigated (significantly effective, effective, ineffective), and the corresponding number of volunteers is counted; in addition, the number of volunteers with recurrence or aggravation of rheumatic pain among those who experienced significantly effective and effective relief during the application period and within 7 days after stopping the application is also counted.
A significantly effective result is defined as the effective elimination of rheumatic pain in the fixed area of the experimental bandage, with no recurrence during the application period.
An effective result is defined as significant alleviation of rheumatic pain in the fixed area of the experimental bandage, with no aggravation during the application period.
An ineffective result is defined as no significant difference in rheumatic pain in the fixed area of the experimental bandage compared to the absence of the experimental bandage.
The specific test results are as follows:
It may be seen that in the bio-nylon fiber containing plant active components of the present disclosure, the first active component containing the sovereign herb Speranskia tuberculata is combined with the second active component containing the ministerial herb Artemisia argyi, the adjuvant herb Lygodium japonicum, and the guiding herb Carthamus tinctorius, where the effective controlled release of each plant active component in the first and second active components is achieved through different processing methods. This allows the active components to remain within the effective dosage ratio range for a long period, resulting in improved and alleviated rheumatic pain. Furthermore, during the test process, the experimental bandages underwent multiple routine washings and were still able to achieve the aforementioned effect. This also demonstrates that the plant active components in the bio-nylon fiber of the present disclosure combine well with the nylon fiber and maintain good long-term effectiveness.
It may be seen from Comparative Example 1 that when using the process method where all the plant active components are mixed and then loaded, on the one hand, the cooperation effect of the plant active components is not ideal; on the other hand, due to the large addition of the sovereign herb, the smaller amounts of the adjuvant herb and the guiding herb are greatly affected, hindering the efficacy of the adjuvant herb and the guiding herb, which also leads to poor cooperation of the plant active components. This is specifically manifested as a reduction in the number of people with significant effects, an increase in the inefficacy rate, and an increase in the number of people whose rheumatic pain recurred or worsened after stopping the use of the experimental bandage.
It may be seen from Comparative Example 2 that using the preparation method of the second active component to treat the first component solution containing the sovereign herb Speranskia tuberculata and prepare the first functional masterbatch, and using the preparation method of the first active component to treat the second component solution containing the ministerial herb Artemisia argyi, the adjuvant herb Lygodium japonicum, and the guiding herb Carthamus tinctorius to prepare the second functional masterbatch, due to the change in the processing methods for different components, the release amount of each component in the bio-nylon fiber could not be effectively and stably controlled. This resulted in the inability of the active components to cooperate within the effective dosage ratio range, leading to an inability to effectively improve and alleviate rheumatic pain. This was specifically manifested as a reduction in the number of people with significant effects, an increase in the inefficacy rate, and an increase in the number of people whose rheumatic pain recurred or worsened after stopping the use of the experimental bandage.
It may be seen from Comparative Example 3 that in the preparation process of the first active component of the present disclosure, after modifying the primary powder with amino silane for amino modification and further modifying the first processed material with sodium mercaptoacetate for mercapto modification, the sovereign herb Speranskia tuberculata in the first active component may be effectively loaded and controlled for release. At the same time, combined with the coating in preparing the second active component, the coating and controlled release effects of the ministerial herb Artemisia argyi, the adjuvant herb Lygodium japonicum, and the guiding herb Carthamus tinctorius in the second active component may be improved, thereby allowing the active components to cooperate within the effective dosage ratio range. After omitting the relevant technical means in Comparative Example 3, the effect of improving and alleviating rheumatic pain showed a certain degree of decline.
Further, according to the antibacterial content specified in GB/T 20944.3-2008 “Textiles—Evaluation of Antibacterial Performance—Part 3: Oscillation Method,” antibacterial performance tests were performed on the bio-nylon fiber containing plant active components of Embodiments 1-3 and Comparative Examples 1-3, where the specific test results are as follows:
Staphylococcus
aureus, %
Escherichia
coli, %
Klebsiella
pneumoniae, %
Candida
albicans, %
It may be seen that the bio-nylon fiber containing plant active components of the present disclosure, in addition to the aforementioned ability to specifically improve and alleviate rheumatic pain, also includes good antibacterial functionality. It may be seen from Comparative Example 1 and Comparative Example 2 that changing the processing method of the plant active components has a minimal impact on the antibacterial performance of the bio-nylon fiber. It may be seen from Comparative Example 3 that omitting the amino and mercapto synergistic modification processing of the primary powder, as well as changing the coating process of the second active component, affects the loading or coating effect of the plant active components. In the subsequent functional processing of the nylon fiber, the plant active components are prone to loss, specifically manifesting as a decrease in antibacterial performance.
Further, the bio-nylon fiber containing plant active components of Embodiments 1-3 and Comparative Examples 1-3 is each spun into fabric and then cut into stability samples measuring 20 cm*20 cm. Each stability sample is placed in an environment with a temperature of 42° C. and a relative humidity of 75%, and after being exposed to continuous irradiation of a 100 W xenon lamp for 960 hours, antibacterial performance tests are conducted on each stability sample using the aforementioned antibacterial performance detection method.
The specific test results are as follows:
Staphylococcus
aureus, %
Escherichia
coli, %
Klebsiella
pneumoniae, %
Candida
albicans, %
It may be seen that in the bio-nylon fiber containing plant active components of the present disclosure, the plant active components are firmly combined with the bio-nylon fiber, and the plant active components exhibit good stability in the nylon fiber. The plant active components are not easily lost when subjected to external factors (such as washing, high temperature, high humidity, light, etc.), and maintain good long-term effectiveness. It may be seen from Comparative Example 1 that after omitting the preparation of the second active component, due to the singular processing method of the plant active components, the various components are unable to cooperate to achieve an antibacterial effect, and during long-term static placement, there is a problem of loss of active components. It may be seen from Comparative Example 2 that changing the processing method of the plant active components has a minimal impact on the stability of the bio-nylon fiber. It may be seen from Comparative Example 3 that omitting the amino and mercapto synergistic modification processing of the primary powder and changing the coating process of the second active component, affects the loading or coating effect of the plant active components. In the subsequent functional processing of the nylon fiber, the plant active components are easily lost, and when subjected to external factors (such as washing, high temperature, high humidity, light, etc.), the loss of active components is significant, specifically manifesting as a reduction in antibacterial performance.
Further, the breaking strength and breaking elongation rate of the bio-nylon fiber containing plant active components, prepared in Embodiments 1-3 and Comparative Examples 1-3, were tested. The specific test results are as follows:
It may be seen that in the bio-nylon fiber containing plant active component of the present disclosure, the plant active component may effectively bind with the bio-nylon fiber. This enables functional modification of the nylon fiber while avoiding a reduction in the physical properties of the modified nylon fiber, effectively maintaining the good physical performance of the nylon fiber. The significant deterioration in the physical properties of the nylon fiber in Comparative Example 3 is due to the omission of the amino and mercapto synergistic modification processing of the primary powder, resulting in poor dispersion of the first active component in the nylon fiber, which leads to a reduction in the physical properties of the nylon fiber. Additionally, the change in the preparation process of the second active component further reduces the coating effect, which also affects the physical properties of the nylon fiber to a certain extent.
In summary, it may be seen that the preparation method of the bio-nylon fiber containing plant active component in the present disclosure involves extracting the first component from Speranskia tuberculata to obtain a first component solution containing the main plant active component. The second component is extracted from Artemisia argyi, Lygodium japonicum and Carthamus tinctorius to obtain a second component solution containing auxiliary plant active components. During the preparation of the first active component, amino modification of the primary powder is performed using amino silane, followed by mercapto modification processing of the first processed material using sodium mercaptoacetate, and then loading the first component solution containing the main plant active component. During the preparation of the second active component, the second component emulsion containing auxiliary plant active component is subjected to coating. Functional masterbatches are prepared separately from the first and second active components, which are then used in the functional modification process of the nylon fiber. This method effectively avoids the problem during the functional modification process of the nylon fiber, where the large amount of the main plant active component (such as the sovereign herb component) significantly affects the smaller doses of auxiliary plant active component (such as the guiding herb component). Additionally, it prevents the issue where the small doses of auxiliary plant active components are easily lost during the functional processing of the nylon fiber, failing to reach an effective dose, which prevents the plant active component from effectively cooperating. The resulting bio-nylon fiber containing plant active components includes various plant active components, with the main and auxiliary components effectively cooperating to specifically improve and alleviate corresponding symptoms. Furthermore, the various plant active components exhibit good stability in the nylon fiber, with minimal loss. The loss of active components may be controlled within the permissible range of efficacy, allowing the multiple plant active components in the nylon fiber to cooperate under optimal ratio conditions for an extended period, providing stable and long-lasting improvement and alleviation of the corresponding symptoms.
Unless otherwise specified, all percentages used in the present disclosure are mass percentages.
Compared to the prior art, the beneficial effects of the disclosure are as follows:
Finally, it should be noted that the above descriptions are merely preferred embodiments of the present disclosure and are not intended to limit the present disclosure. Although the present disclosure has been described in detail with reference to the aforementioned embodiments, those skilled in the art may still modify the technical solutions described in the aforementioned embodiments or make equivalent replacements for certain technical features. Any modifications, equivalent replacements, improvements, etc., made within the spirit and principle of the present disclosure should be included in the protection scope of the present disclosure.
| Number | Date | Country | Kind |
|---|---|---|---|
| 202311639241.6 | Dec 2023 | CN | national |
