CN112725923A - Chinlon macrobio-fiber containing ginkgo, rose, camellia, pomegranate and radix puerariae and preparation method thereof - Google Patents
Chinlon macrobio-fiber containing ginkgo, rose, camellia, pomegranate and radix puerariae and preparation method thereof Download PDFInfo
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- CN112725923A CN112725923A CN202011639410.2A CN202011639410A CN112725923A CN 112725923 A CN112725923 A CN 112725923A CN 202011639410 A CN202011639410 A CN 202011639410A CN 112725923 A CN112725923 A CN 112725923A
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Classifications
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- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
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- D01F6/90—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
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- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
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- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
Abstract
The invention discloses a chinlon macrobiotic fiber containing ginkgo, rose, camellia, pomegranate and kudzu root and a preparation method thereof, belonging to the technical field of fiber materials. The chinlon macrobiotic fiber is prepared from the following raw materials in parts by weight: 100-150 parts of chinlon chips, 5-10 parts of biological modifier, 3-10 parts of Gd/CaZrO nano particles and 1-3 parts of polyamide chain extender. The prepared chinlon macrobiotic fiber containing ginkgo, rose, camellia, red pomegranate and radix puerariae has high shielding efficiency within a wide range of 10MHz-40GHz and tensile strength of more than or equal to 180MPa, and can reach more than 99.99 percent of shielding efficiency, and meanwhile, the chinlon macrobiotic fiber still has excellent antibacterial performance after being washed for many times.
Description
Technical Field
The invention belongs to the technical field of fiber materials, and particularly relates to a chinlon macrobio-fiber containing gingko, rose, camellia, pomegranate and radix puerariae and a preparation method thereof.
Background
With the progress of science and technology and the development of industry, the petrochemical industry gradually extends the branch of synthetic fibers, thereby enriching the types of textile fibers. Chinlon is the trade name of polyamide fiber in China, which has become a synthetic fiber second to the amount of terylene, and the common nylon fibers in the textile industry include nylon 66 and nylon 6.
The nylon has a series of excellent performances, wear resistance is the first of textile fibers, breaking strength is high, elasticity is good, extension is large, moisture absorption in synthetic fibers is good, and the nylon is second to vinylon. Nylon is therefore often used to make athletic suits, undergarments, swimwear, outdoor tents, and the like. Gradually, the functionalization and differentiation of fabric products has become a trend of social development.
Along with the improvement of living standard of people, people put forward higher requirements on living quality, and the development and the application of multifunctional textile fabrics are more and more extensive. In recent years, the expression "cosmetic on body" has prevailed. Specifically, green pure natural nuisanceless plant extracts with special biological activity are arranged on fabrics (especially underwear) so as to gradually exert the effect through contact friction with the skin in the daily wearing process.
The invention patent CN201810699619.4 discloses a herbal mixed nylon fiber and a preparation method thereof, in the preparation process of the nylon fiber, herbal plant source components are added, so that the prepared herbal mixed nylon fiber has the functionality of a plant extract, and has the functions of moisture absorption and static electricity resistance, and also has the characteristics of oxidation resistance, light resistance, heat resistance and long service life. However, in the preparation process, the loss of effective components of plants is serious, the fibers are easy to age, the service life of the product is short, the function is single, the cost is extremely high, and the market popularization and application are difficult.
Disclosure of Invention
Aiming at the characteristics of poor strength, short service life and single function of the polyamide fiber in the prior art, the invention develops the active fiber with biological function prepared by adding the bioactive substance into the polyamide fiber and modifying the polyamide fiber, and the obtained fiber has good strength, washing resistance, antibiosis, radiation protection, easy degradation, environmental protection and simple preparation process, and is suitable for large-scale popularization and application.
In order to achieve the technical purpose, the technical scheme adopted by the invention is as follows:
the chinlon macrobiotic fiber containing ginkgo, rose, camellia, pomegranate and kudzu root is prepared from the following raw materials in parts by weight: 100-150 parts of chinlon chips, 5-10 parts of biological modifier, 3-10 parts of Gd/CaZrO nano particles and 1-3 parts of polyamide chain extender.
Preferably, the preparation method of the biological modifier comprises the following steps: weighing 15-20 parts of ginkgo leaf, 3-5 parts of rose petal, 3-10 parts of camellia petal, 1-5 parts of pomegranate and 1-3 parts of kudzu root, mixing, drying in a drying oven until the water content is 10-20%, crushing, sieving with a 100-mesh sieve for later use, adding 60% ethanol solution according to the material-liquid ratio of 1:50 (g/mL), performing ultrasonic wave assisted extraction at the ultrasonic frequency of 40kHz and the power of 500W at the temperature of 50 ℃ for 60min, centrifuging at 2000r/min for 30min, taking supernatant, and performing vacuum rotary evaporation and concentration at 50 ℃ to obtain the biological modifier.
Preferably, the preparation method of the Gd/CaZrO nanoparticles comprises the following steps: 3g Gd2O3Fully and uniformly mixing the powder and 5g of urea in distilled water to obtain a solution A; 20g of ZrO were weighed2And 10g of CaO are mixed into the solution A, the mixture is uniformly mixed and transferred into a rotary evaporator to be rotated and evaporated for 1h, the solvent is completely removed to obtain a solid precursor, then the solid precursor is heated at the speed of 4 ℃/min, N2Roasting at 1300 ℃ for 2h under protection, cooling to room temperature, and performing ball milling to obtain Gd/CaZrO nano particles.
Preferably, the particle size of the Gd/CaZrO nanoparticles is 200-400 nm.
Preferably, the polyamide chain extender is polymethyl methacrylate.
A preparation method of chinlon macrobiological fiber containing gingko, rose, camellia, pomegranate and radix puerariae comprises the following steps:
1) preparing a biological modifier: weighing 15-20 parts of ginkgo leaves, 3-5 parts of rose petals, 3-10 parts of camellia petals, 1-5 parts of pomegranate and 1-3 parts of kudzu roots, mixing, drying in a drying oven until the water content is 10-20%, crushing, sieving with a 100-mesh sieve for later use, adding 60% ethanol solution according to the material-liquid ratio of 1:50 (g/mL), performing ultrasonic wave assisted extraction at the ultrasonic frequency of 40kHz and the power of 500W at the temperature of 50 ℃ for 60min, centrifuging at 2000r/min for 30min, taking supernatant, and performing vacuum rotary evaporation and concentration at 50 ℃ to obtain the biological modifier; (ii) a
2) Preparing Gd/CaZrO nano particles: the preparation method of the Gd/CaZrO nano particles comprises the following steps: 3g Gd2O3Fully and uniformly mixing the powder and 5g of urea in distilled water to obtain a solution A; 20g of ZrO were weighed2And 10g of CaO are mixed into the solution A, the mixture is uniformly mixed and transferred into a rotary evaporator to be rotated and evaporated for 1h, the solvent is completely removed to obtain a solid precursor, then the solid precursor is heated at the speed of 4 ℃/min, N2Roasting at 1300 ℃ for 2h under protection, cooling to room temperature, and performing ball milling to obtain Gd/CaZrO nano particles;
3) mixing and melting nylon chips, a biological modifier, Gd/CaZrO nano particles and a polyamide chain extender, extruding the mixture into a melt by using a double-screw device, and conveying the melt to a melt pipeline; and then the mixture is input into a spinning box body through a metering pump, and is subjected to melt spinning and cooling through a spinneret plate to obtain fiber tows.
Preferably, the mixing melting temperature of the twin screw in the step (3) is 235 ℃, and the extrusion pressure is 12 MPa.
Each of the raw materials of the present invention is commercially available.
Semen Ginkgo is leaf of Ginkgo of Ginkgoaceae. The flavone component contained in folium Ginkgo can inhibit the formation and deposition of pigment in dermis layer, and has effects of whitening skin and preventing and treating pigment plaque. Besides flavone, trace elements such as zinc, manganese, molybdenum and the like in the ginkgo leaves can also eliminate oxygen free radicals and inhibit the growth of melanin. The flavonoid glycoside and flavonol in folium Ginkgo are free radical scavenger, and can protect dermal layer cells, improve blood circulation, and prevent cells from being oxidized to generate wrinkles.
The rose is native to China and has a long cultivation history, and is a shrub of rosa in rosaceae in plant taxonomy. The rose contains a small amount of volatile oil, yellow crystalline extract, rubbing agent, gallic acid, pigment, etc. The main component of the rose oil is alcohol compounds. The food herbal term means that the food has the effects of benefiting lung and spleen, benefiting liver and gallbladder, and is fragrant, sweet and beautiful in taste and refreshing. The long-term taking of the product has good beautifying effect, can effectively remove free radicals, eliminate pigmentation and arouse the vitality of hair and spring.
Camellia, also known as: camellia japonica, Camellia sinensis, Theaceae, Camellia genus evergreen shrub and small arbor. Ancient name is sea pomegranate. Yuming Hua, Dong-enduring winter or Datura stramonium, and is also classified into Huadong camellia, Chuan camellia and late camellia. The camellia contains rich catechin, vitamin C, tannic acid and amino acid components, has excellent moisturizing and anti-wrinkle effects, has soothing and antioxidant activities, can effectively prevent melanin from precipitating, keeps the skin bright, and maintains the health and freshness of the skin.
Pomegranate is a variety of pomegranate and is named because the pericarp of the ripe pomegranate is pink. The red pomegranate contains a large amount of pomegranate polyphenols, anthocyanin and isoflavone, the oxidation resistance of the red pomegranate is 3 times higher than that of green tea, and more 20 times higher than that of vitamin C, free radicals which induce diseases and aging in a human body can be effectively neutralized, metabolism is promoted, toxins are discharged, the health and regeneration functions of cells are guaranteed, and the effects of whitening and resisting aging are achieved.
Pueraria lobata (Willd.) Ohwi is dry root of Pueraria lobata (Willd.) Ohwi of Leguminosae, commonly known as Pueraria lobata (Willd.) Ohwi. Isoflavone components (puerarin, daidzin, daidzein, genistein, genistin, etc.) in radix Puerariae can remarkably inhibit the catalytic activity of tyrosinase, interrupt the oxidation process of melanin, and inhibit the generation and formation of melanin, thereby preventing pigment deposition such as chloasma and sunburn, and whitening and resisting aging.
In the prior art, a common means is to add silver ions or chemical antioxidants to improve the antibacterial performance and the antioxidant performance of the fabric, and in practical application, the additives have single functions and poor adhesive force, and the efficacy is greatly reduced after multiple times of washing. The fabric is endowed with antibacterial and antioxidant performance by adding ginkgo leaf, rose petal, camellia petal, pomegranate and kudzu root powder. The rose oil in the rose can promote the full dissolution of flavonoid bactericidal substances in ginkgo and kudzuvine root and antioxidant active substances in camellia pomegranate, and the five purely natural substances are added into the nylon fiber, so that the comprehensive performance of the nylon fiber is greatly improved.
Meanwhile, Gd/CaZrO nano particles are added, Gd is fixed in a perovskite structure formed by high-temperature reaction of ZrO and CaO through solid-phase reaction, the radiation resistance of the nylon fiber can be improved due to the existence of rare earth particles, uniform dispersion of bioactive mixtures such as ginkgo leaves and the like can be promoted due to the existence of the nano particles, bioactive substances are fixed, and loss of the active substances is reduced. Meanwhile, the strength performance of the fiber is greatly improved.
Has the advantages that: the prepared chinlon macrobiotic fiber containing gingko, rose, camellia, red pomegranate and radix puerariae has high shielding efficiency within a wide range of 10MHz-40GHz and tensile strength of more than or equal to 180MPa, and the shielding efficiency can reach more than 99.99 percent, and meanwhile, the chinlon macrobiotic fiber still has excellent antioxidant and antibacterial properties after being washed for many times.
Detailed Description
The technical solution of the present invention is further described below with reference to specific embodiments, but is not limited thereto.
Example 1
The chinlon macrobiotic fiber containing ginkgo, rose, camellia, pomegranate and kudzu root is prepared from the following raw materials in parts by weight: 100 parts of nylon chips, 5 parts of biological modifier, 3 parts of Gd/CaZrO nano particles and 1 part of polyamide chain extender.
Preferably, the preparation method of the biological modifier comprises the following steps: weighing 15-20 parts of ginkgo leaf, 3-5 parts of rose petal, 3-10 parts of camellia petal, 1-5 parts of pomegranate and 1-3 parts of kudzu root, mixing, drying in a drying oven until the water content is 10-20%, crushing, sieving with a 100-mesh sieve for later use, adding 60% ethanol solution according to the material-liquid ratio of 1:50 (g/mL), performing ultrasonic wave assisted extraction at the ultrasonic frequency of 40kHz and the power of 500W at the temperature of 50 ℃ for 60min, centrifuging at 2000r/min for 30min, taking supernatant, and performing vacuum rotary evaporation and concentration at 50 ℃ to obtain the biological modifier.
The preparation method of the Gd/CaZrO nano particles comprises the following steps: 3g Gd2O3Fully and uniformly mixing the powder and 5g of urea in distilled water to obtain a solution A; 20g of ZrO were weighed2And 10g of CaO are mixed into the solution A, the mixture is uniformly mixed and transferred into a rotary evaporator to be rotated and evaporated for 1h, the solvent is completely removed to obtain a solid precursor, then the solid precursor is heated at the speed of 4 ℃/min, N2Roasting at 1300 ℃ for 2h under protection, cooling to room temperature, and performing ball milling to obtain Gd/CaZrO nano particles.
The particle size of the Gd/CaZrO nano particles is 200-400 nm.
The polyamide chain extender is polymethyl methacrylate.
A preparation method of chinlon macrobiological fiber containing gingko, rose, camellia, pomegranate and radix puerariae comprises the following steps:
1) preparing a biological modifier: weighing 15-20 parts of ginkgo leaves, 3-5 parts of rose petals, 3-10 parts of camellia petals, 1-5 parts of pomegranate and 1-3 parts of kudzu roots, mixing, drying in a drying oven until the water content is 10-20%, crushing, sieving with a 100-mesh sieve for later use, adding 60% ethanol solution according to the material-liquid ratio of 1:50 (g/mL), performing ultrasonic wave assisted extraction at the ultrasonic frequency of 40kHz and the power of 500W at the temperature of 50 ℃ for 60min, centrifuging at 2000r/min for 30min, taking supernatant, and performing vacuum rotary evaporation and concentration at 50 ℃ to obtain the biological modifier;
2) preparing Gd/CaZrO nano particles: the preparation method of the Gd/CaZrO nano particles comprises the following steps: 3g Gd2O3Fully and uniformly mixing the powder and 5g of urea in distilled water to obtain a solution A; 20g of ZrO were weighed2And 10g of CaO are mixed into the solution A, the mixture is uniformly mixed and transferred into a rotary evaporator to be rotated and evaporated for 1h, the solvent is completely removed to obtain a solid precursor, then the solid precursor is heated at the speed of 4 ℃/min, N2Roasting at 1300 ℃ for 2h under protection, cooling to room temperature, and performing ball milling to obtain Gd/CaZrO nano particles;
3) mixing and melting nylon chips, a biological modifier, Gd/CaZrO nano particles and a polyamide chain extender, extruding the mixture into a melt by using a double-screw device, and conveying the melt to a melt pipeline; and then the mixture is input into a spinning box body through a metering pump, and is subjected to melt spinning and cooling through a spinneret plate to obtain fiber tows.
The mixing and melting temperature in the twin-screw in the step (3) is 235 ℃, and the extrusion pressure is 12 MPa.
Example 2
The chinlon macrobiotic fiber containing ginkgo, rose, camellia, pomegranate and kudzu root is prepared from the following raw materials in parts by weight: 120 parts of nylon chips, 8 parts of biological modifier, 7 parts of Gd/CaZrO nano particles and 2 parts of polyamide chain extender.
The preparation method of the biological modifier comprises the following steps: weighing 15-20 parts of ginkgo leaf, 3-5 parts of rose petal, 3-10 parts of camellia petal, 1-5 parts of pomegranate and 1-3 parts of kudzu root, mixing, drying in a drying oven until the water content is 10-20%, crushing, sieving with a 100-mesh sieve for later use, adding 60% ethanol solution according to the material-liquid ratio of 1:50 (g/mL), performing ultrasonic wave assisted extraction at the ultrasonic frequency of 40kHz and the power of 500W at the temperature of 50 ℃ for 60min, centrifuging at 2000r/min for 30min, taking supernatant, and performing vacuum rotary evaporation and concentration at 50 ℃ to obtain the biological modifier.
The preparation method of the Gd/CaZrO nano particles comprises the following steps: 3g Gd2O3Fully and uniformly mixing the powder and 5g of urea in distilled water to obtain a solution A; 20g of ZrO were weighed2And 10g of CaO are mixed into the solution A, the mixture is uniformly mixed and transferred into a rotary evaporator to be rotated and evaporated for 1h, the solvent is completely removed to obtain a solid precursor, then the solid precursor is heated at the speed of 4 ℃/min, N2Roasting at 1300 ℃ for 2h under protection, cooling to room temperature, and performing ball milling to obtain Gd/CaZrO nano particles.
The particle size of the Gd/CaZrO nano particles is 200-400 nm.
The polyamide chain extender is polymethyl methacrylate.
A preparation method of chinlon macrobiological fiber containing gingko, rose, camellia, pomegranate and radix puerariae comprises the following steps:
1) preparing a biological modifier: the preparation method of the biological modifier comprises the following steps: weighing 15-20 parts of ginkgo leaves, 3-5 parts of rose petals, 3-10 parts of camellia petals, 1-5 parts of pomegranate and 1-3 parts of kudzu roots, mixing, drying in a drying oven until the water content is 10-20%, crushing, sieving with a 100-mesh sieve for later use, adding 60% ethanol solution according to the material-liquid ratio of 1:50 (g/mL), performing ultrasonic wave assisted extraction at the ultrasonic frequency of 40kHz and the power of 500W at the temperature of 50 ℃ for 60min, centrifuging at 2000r/min for 30min, taking supernatant, and performing vacuum rotary evaporation and concentration at 50 ℃ to obtain the biological modifier;
2) preparing Gd/CaZrO nano particles: the preparation method of the Gd/CaZrO nano particles comprises the following steps: 3g Gd2O3Fully and uniformly mixing the powder and 5g of urea in distilled water to obtain a solution A; 20g of ZrO were weighed2And 10g of CaO are mixed into the solution A, the mixture is uniformly mixed and transferred into a rotary evaporator to be rotated and evaporated for 1h, the solvent is completely removed to obtain a solid precursor, then the solid precursor is heated at the speed of 4 ℃/min, N2Roasting at 1300 ℃ for 2h under protection, cooling to room temperature, and performing ball milling to obtain Gd/CaZrO nano particles;
3) mixing and melting nylon chips, a biological modifier, Gd/CaZrO nano particles and a polyamide chain extender, extruding the mixture into a melt by using a double-screw device, and conveying the melt to a melt pipeline; and then the mixture is input into a spinning box body through a metering pump, and is subjected to melt spinning and cooling through a spinneret plate to obtain fiber tows.
The mixing and melting temperature in the twin-screw in the step (3) is 235 ℃, and the extrusion pressure is 12 MPa.
Example 3
The chinlon macrobiotic fiber containing ginkgo, rose, camellia, pomegranate and kudzu root is prepared from the following raw materials in parts by weight: 150 parts of nylon chips, 10 parts of biological modifier, 10 parts of Gd/CaZrO nano particles and 3 parts of polyamide chain extender.
The preparation method of the biological modifier comprises the following steps: weighing 15-20 parts of ginkgo leaf, 3-5 parts of rose petal, 3-10 parts of camellia petal, 1-5 parts of pomegranate and 1-3 parts of kudzu root, mixing, drying in a drying oven until the water content is 10-20%, crushing, sieving with a 100-mesh sieve for later use, adding 60% ethanol solution according to the material-liquid ratio of 1:50 (g/mL), performing ultrasonic wave assisted extraction at the ultrasonic frequency of 40kHz and the power of 500W at the temperature of 50 ℃ for 60min, centrifuging at 2000r/min for 30min, taking supernatant, and performing vacuum rotary evaporation and concentration at 50 ℃ to obtain the biological modifier.
The preparation method of the Gd/CaZrO nano particles comprises the following steps: 3g Gd2O3Fully and uniformly mixing the powder and 5g of urea in distilled water to obtain a solution A; 20g of ZrO were weighed2And 10g of CaO are mixed into the solution A, the mixture is uniformly mixed and transferred into a rotary evaporator to be rotated and evaporated for 1h, the solvent is completely removed to obtain a solid precursor, then the solid precursor is heated at the speed of 4 ℃/min, N2Roasting at 1300 ℃ for 2h under protection, cooling to room temperature, and performing ball milling to obtain Gd/CaZrO nano particles.
The particle size of the Gd/CaZrO nano particles is 200-400 nm.
The polyamide chain extender is polymethyl methacrylate.
A preparation method of chinlon macrobiological fiber containing gingko, rose, camellia, pomegranate and radix puerariae comprises the following steps:
1) preparing a biological modifier: weighing 15-20 parts of ginkgo leaves, 3-5 parts of rose petals, 3-10 parts of camellia petals, 1-5 parts of pomegranate and 1-3 parts of kudzu roots, mixing, drying in a drying oven until the water content is 10-20%, crushing, sieving with a 100-mesh sieve for later use, adding 60% ethanol solution according to the material-liquid ratio of 1:50 (g/mL), performing ultrasonic wave assisted extraction at the ultrasonic frequency of 40kHz and the power of 500W at the temperature of 50 ℃ for 60min, centrifuging at 2000r/min for 30min, taking supernatant, and performing vacuum rotary evaporation and concentration at 50 ℃ to obtain the biological modifier;
2) preparing Gd/CaZrO nano particles: the preparation method of the Gd/CaZrO nano particles comprises the following steps: 3g Gd2O3Fully and uniformly mixing the powder and 5g of urea in distilled water to obtain a solution A; 20g of ZrO were weighed2And 10g of CaO are mixed into the solution A, the mixture is uniformly mixed and transferred into a rotary evaporator to be rotated and evaporated for 1h, the solvent is completely removed to obtain a solid precursor, then the solid precursor is heated at the speed of 4 ℃/min, N2Roasting at 1300 ℃ for 2h under protection, cooling to room temperature, and performing ball milling to obtain Gd/CaZrO nano particles;
3) mixing and melting nylon chips, a biological modifier, Gd/CaZrO nano particles and a polyamide chain extender, extruding the mixture into a melt by using a double-screw device, and conveying the melt to a melt pipeline; and then the mixture is input into a spinning box body through a metering pump, and is subjected to melt spinning and cooling through a spinneret plate to obtain fiber tows.
The mixing and melting temperature in the twin-screw in the step (3) is 235 ℃, and the extrusion pressure is 12 MPa.
Comparative example 1
The chinlon macrobiotic fiber containing ginkgo, rose, camellia, pomegranate and kudzu root is prepared from the following raw materials in parts by weight: 150 parts of nylon chips, 10 parts of biological modifier, 10 parts of Gd/CaZrO nano particles and 3 parts of polyamide chain extender.
The preparation method of the biological modifier comprises the following steps: weighing 15-20 parts of ginkgo leaf, 3-5 parts of rose petal, 3-10 parts of camellia petal, 1-5 parts of pomegranate and 1-3 parts of kudzu root, mixing, drying in a drying oven until the water content is 10-20%, crushing, sieving with a 100-mesh sieve for later use, adding 60% ethanol solution according to the material-liquid ratio of 1:50 (g/mL), performing ultrasonic wave assisted extraction at the ultrasonic frequency of 40kHz and the power of 500W at the temperature of 50 ℃ for 60min, centrifuging at 2000r/min for 30min, taking supernatant, and performing vacuum rotary evaporation and concentration at 50 ℃ to obtain the biological modifier.
The preparation method of the CaZrO nano particles comprises the following steps: fully and uniformly mixing 5g of urea in distilled water to obtain a solution A; 20g of ZrO were weighed2And 10g of CaO are mixed into the solution A, the mixture is uniformly mixed and transferred into a rotary evaporator to be rotated and evaporated for 1h, the solvent is completely removed to obtain a solid precursor, then the solid precursor is heated at the speed of 4 ℃/min, N2Roasting at 1300 ℃ for 2h under protection, cooling to room temperature, and performing ball milling to obtain CaZrO nanoparticles.
The particle size of the CaZrO nano particles is 200-400 nm.
The polyamide chain extender is polymethyl methacrylate.
A preparation method of chinlon macrobiological fiber containing gingko, rose, camellia, pomegranate and radix puerariae comprises the following steps:
1) preparing a biological modifier: weighing 15-20 parts of ginkgo leaves, 3-5 parts of rose petals, 3-10 parts of camellia petals, 1-5 parts of pomegranate and 1-3 parts of kudzu roots, mixing, drying in a drying oven until the water content is 10-20%, crushing, sieving with a 100-mesh sieve for later use, adding 60% ethanol solution according to the material-liquid ratio of 1:50 (g/mL), performing ultrasonic wave assisted extraction at the ultrasonic frequency of 40kHz and the power of 500W at the temperature of 50 ℃ for 60min, centrifuging at 2000r/min for 30min, taking supernatant, and performing vacuum rotary evaporation and concentration at 50 ℃ to obtain the biological modifier;
2) preparation of CaZrO nanoparticles: the preparation method of the CaZrO nano particles comprises the following steps: 5g of urea is fully and uniformly mixed in distilled water to obtain a solution A; 20g of ZrO were weighed2And 10g of CaO are mixed into the solution A, the mixture is uniformly mixed and transferred into a rotary evaporator to be rotated and evaporated for 1h, the solvent is completely removed to obtain a solid precursor, then the solid precursor is heated at the speed of 4 ℃/min, N2Roasting at 1300 ℃ for 2h under protection, cooling to room temperature, and performing ball milling to obtain CaZrO nanoparticles;
3) mixing and melting the nylon chips, the biological modifier, the CaZrO nano particles and the polyamide chain extender, extruding the mixture into a melt by using a double-screw device, and conveying the melt to a melt pipeline; and then the mixture is input into a spinning box body through a metering pump, and is subjected to melt spinning and cooling through a spinneret plate to obtain fiber tows.
The mixing and melting temperature in the twin-screw in the step (3) is 235 ℃, and the extrusion pressure is 12 MPa.
This comparative example is the same as example 3 except that CaZrO nanoparticles which have not been modified with Gd are used.
Comparative example 2
The chinlon macrobiotic fiber containing ginkgo, rose, camellia, pomegranate and kudzu root is prepared from the following raw materials in parts by weight: 150 parts of nylon chips, 10 parts of biological modifier, 10 parts of Gd/CaZrO nano particles and 3 parts of polyamide chain extender.
The preparation method of the biological modifier comprises the following steps: 3-5 parts of rose petals, 3-10 parts of camellia petals, 1-5 parts of pomegranate and 1-3 parts of kudzu roots, mixing, drying in a drying oven until the water content is 10-20%, crushing, sieving with a 100-mesh sieve for later use, adding 60% ethanol solution according to the material-liquid ratio of 1:50 (g/mL), performing ultrasonic wave assisted extraction for 60min under the conditions of ultrasonic frequency of 40kHz, power of 500W and 50 ℃, centrifuging at 2000r/min for 30min, taking supernatant, and performing vacuum rotary evaporation and concentration at 50 ℃ to obtain the biological modifier.
This comparative example is the same as example 3 except that no ginkgo biloba leaves are added to the biological modifier.
Comparative example 3
The chinlon macrobiotic fiber containing ginkgo, rose, camellia, pomegranate and kudzu root is prepared from the following raw materials in parts by weight: 150 parts of nylon chips, 10 parts of biological modifier, 10 parts of Gd/CaZrO nano particles and 3 parts of polyamide chain extender.
The preparation method of the biological modifier comprises the following steps: weighing 15-20 parts of ginkgo leaves, 3-10 parts of camellia petals, 1-5 parts of pomegranate and 1-3 parts of kudzu roots, mixing, drying in a drying oven until the water content is 10-20%, crushing, sieving with a 100-mesh sieve for later use, adding 60% ethanol solution according to the material-liquid ratio of 1:50 (g/mL), performing ultrasonic wave assisted extraction for 60min under the conditions of ultrasonic frequency of 40kHz, power of 500W and 50 ℃, centrifuging for 30min at 2000r/min, taking supernatant, and performing vacuum rotary evaporation and concentration at 50 ℃ to obtain the biological modifier.
This comparative example is the same as example 3 except that no rose petals are added to the biological modifier.
Comparative example 4
The chinlon macrobiotic fiber is prepared from the following raw materials in parts by weight: 150 parts of nylon chips, 10 parts of Gd/CaZrO nano particles and 3 parts of polyamide chain extender.
The preparation method of the Gd/CaZrO nano particles comprises the following steps: 3g Gd2O3Fully and uniformly mixing the powder and 5g of urea in distilled water to obtain a solution A; 20g of ZrO were weighed2And 10g of CaO are mixed into the solution A, the mixture is uniformly mixed and transferred into a rotary evaporator to be rotated and evaporated for 1h, the solvent is completely removed to obtain a solid precursor, then the solid precursor is heated at the speed of 4 ℃/min, N2Roasting at 1300 ℃ for 2h under protection, cooling to room temperature, and performing ball milling to obtain Gd/CaZrO nano particles.
The particle size of the Gd/CaZrO nano particles is 200-400 nm.
The polyamide chain extender is polymethyl methacrylate.
A preparation method of chinlon macrobiotic fiber comprises the following steps:
1) preparing Gd/CaZrO nano particles: the preparation method of the Gd/CaZrO nano particles comprises the following steps: 3g Gd2O3Fully and uniformly mixing the powder and 5g of urea in distilled water to obtain a solution A; 20g of ZrO were weighed2And 10g of CaO are mixed into the solution A, the mixture is uniformly mixed and transferred into a rotary evaporator to be rotated and evaporated for 1h, the solvent is completely removed to obtain a solid precursor, then the solid precursor is heated at the speed of 4 ℃/min, N2Roasting at 1300 ℃ for 2h under protection, cooling to room temperature, and performing ball milling to obtain Gd/CaZrO nano particles;
2) mixing and melting the nylon chips, the Gd/CaZrO nano particles and the polyamide chain extender, extruding the mixture into a melt by using a double-screw device, and conveying the melt to a melt pipeline; and then the mixture is input into a spinning box body through a metering pump, and is subjected to melt spinning and cooling through a spinneret plate to obtain fiber tows.
The mixing and melting temperature in the twin-screw in the step (3) is 235 ℃, and the extrusion pressure is 12 MPa.
The comparative example is the same as example 3 except that the biological modifier prepared from ginkgo leaves, rose petals, camellia petals, pomegranate and kudzu roots is not added.
Performance testing
The fibers obtained in examples 1 to 3 of the present invention and comparative examples 1 to 4 were subjected to performance tests, respectively
Antioxidant property
The ABTS free radical decolorization method is adopted for the oxidation resistance test. ABTS was first dissolved in water and made up into a 7mM solution, and the prepared ABTS solution was then mixed with potassium persulfate (K) at a final concentration of 2.45mM2S2O8) The solution is reacted to give ABTS free radical cations (ABTS +), after which the mixed solution is left to stand in the dark for 12-16 h. The free radicals remain stable in the dark for more than two days at room temperature. Prior to use, the ABTS + solution was diluted with phosphate buffer solution (0.1M, pH 7.4) to an absorbance value at 734nm in the range 0.700. + -. 0.025 and 10mg of sample was added to 10mL of ABTS + solution. After 30min, the ABTS + absorbance values were again tested and the antioxidant properties of the samples were calculated using the formula.
Wherein A isctrlTo initial ABTS + absorbance value, AsplIs the ABTS + absorbance value of the sample after 30min immersion.
Antibacterial property
The antibacterial performance test selects gram-positive bacteria staphylococcus aureus and escherichia coli as test strains, and the antibacterial performance is quantitatively tested according to the standard GB/T20944.3-2008. The specific method comprises the following steps: placing a sample (0.75g) and the prepared bacterial liquid in a water bath kettle to oscillate for 24 hours; the temperature of Escherichia coli and Staphylococcus aureus was set to 30 ℃ and 24 ℃ respectively while shaking. Then, the bacterial solution was diluted 1000 times with a sterilized phosphate buffer solution to prepare a test bacterial solution. After dilution, the bacterial liquid was inoculated on an agar medium and cultured at 37 ℃ for 24 hours and 48 hours for Escherichia coli and Staphylococcus aureus, respectively. Finally, the number of colonies on agar medium was counted. And calculating the bacteriostasis rate by using a formula.
Wherein N isctrlAnd NsplThe number of colonies cultured from the standard cotton and the test sample, respectively.
Water washing Performance test
The water Wash test was performed in a Wash Tec-P water washer. The washing conditions were as follows: 2g/L commercial detergent, bath ratio 1:50, temperature maintained at 40. + -. 2 ℃ and 10min per wash was recorded as one time. After washing, the test specimens were rinsed clean with tap water and air dried naturally. Samples were washed at different times and tested for both antioxidant and antibacterial properties as described above.
Mechanical Property test
The samples were characterized using a universal prototype at room temperature, a fiber holding length of 25.4mm and a draw rate of 20mm/min, and the average was taken for 10 groups of samples. The weight m is weighed, the density ρ of the sample is measured, and the cross-sectional area is calculated using the formula m ═ ρ ls.
Test of radiation protection Property
The test is carried out according to the national standard of GB/T22583-2009 radiation-proof knitwear.
TABLE 1 test results of antioxidant and antibacterial properties
| Antioxidant Property (%) | Antibacterial Property (%) | |
| Example 1 | 60.5 | 99.8 |
| Example 2 | 65.9 | 99.9 |
| Example 3 | 69.5 | 99.9 |
| Comparative example 1 | 50.1 | 95.2 |
| Comparative example 2 | 44.3 | 91.6 |
| Comparative example 3 | 45.1 | 93.5 |
| Comparative example 4 | 35.9 | 40.3 |
TABLE 2 Wash Performance test
TABLE 3 mechanical Property testing
TABLE 4 radiation resistance test
| Shielding effectiveness% | |
| Example 1 | 99.999915 |
| Example 2 | 99.999918 |
| Example 3 | 99.999250 |
| Comparative example 1 | 70.999260 |
| Comparative example 2 | 99.995351 |
| Comparative example 3 | 99.994123 |
| Comparative example 4 | 99.993010 |
As can be seen from the above table, the fibers of the examples of the present invention have better antioxidant and antibacterial properties than the comparative examples, and after 30 times of water washing, the performance is reduced by only 2.9%, while the comparative examples without modified particles and part of bioactive components have obviously reduced comprehensive properties. This is probably due to the fact that the nanoparticles and the bioactive components of the present invention have a synergistic interaction, and the lack of the components is weak. The formula and the preparation method of each component of the composite fiber ensure the comprehensive performance of the composite fiber.
It should be noted that the above-mentioned embodiments are only some of the preferred modes for implementing the invention, and not all of them. Obviously, all other embodiments obtained by persons of ordinary skill in the art based on the above-mentioned embodiments of the present invention without any creative effort shall fall within the protection scope of the present invention.
Claims (7)
1. The chinlon macrobiotic fiber containing ginkgo, rose, camellia, pomegranate and kudzu root is characterized by being prepared from the following raw materials in parts by weight: 100-150 parts of chinlon chips, 5-10 parts of biological modifier, 3-10 parts of Gd/CaZrO nano particles and 1-3 parts of polyamide chain extender.
2. The chinlon macrobiotic fiber containing gingko, rose, camellia, pomegranate and kudzu root as claimed in claim 1, wherein the preparation method of the biological modifier is as follows: weighing 15-20 parts of ginkgo leaf, 3-5 parts of rose petal, 3-10 parts of camellia petal, 1-5 parts of pomegranate and 1-3 parts of kudzu root, mixing, drying in a drying oven until the water content is 10-20%, crushing, sieving with a 100-mesh sieve for later use, adding 60% ethanol solution according to the material-liquid ratio of 1:50 (g/mL), performing ultrasonic wave assisted extraction at the ultrasonic frequency of 40kHz and the power of 500W at the temperature of 50 ℃ for 60min, centrifuging at 2000r/min for 30min, taking supernatant, and performing vacuum rotary evaporation concentration at 50 ℃ to obtain the biological modifier.
3. The chinlon macrobio-fiber containing gingko, rose, camellia, pomegranate and radix puerariae according to claim 1, wherein the preparation method of the Gd/CaZrO nanoparticles comprises the following steps: 3g Gd2O3Fully and uniformly mixing the powder and 5g of urea in distilled water to obtain a solution A; 20g of ZrO were weighed2And 10g of CaO are mixed into the solution A, the mixture is uniformly mixed and transferred into a rotary evaporator to be rotated and evaporated for 1h, the solvent is completely removed to obtain a solid precursor, then the solid precursor is heated at the speed of 4 ℃/min, N2Roasting at 1300 ℃ for 2h under protection, cooling to room temperature, and performing ball milling to obtain Gd/CaZrO nano particles.
4. The chinlon macrobio-fiber containing gingko, rose, camellia, pomegranate and kudzu root as claimed in claim 3, wherein the particle size of Gd/CaZrO nanoparticles is 200-400 nm.
5. The chinlon macrobio-fiber containing gingko, rose, camellia, pomegranate and kudzu root as claimed in claim 1, wherein the polyamide chain extender is polymethyl methacrylate.
6. A method for preparing the chinlon macrobio-fiber containing gingko, rose, camellia, pomegranate and kudzu root according to any one of claims 1 to 5, which is characterized by comprising the following steps:
1) preparing a biological modifier; weighing 15-20 parts of ginkgo leaves, 3-5 parts of rose petals, 3-10 parts of camellia petals, 1-5 parts of pomegranate and 1-3 parts of kudzu roots, mixing, drying in a drying oven until the water content is 10-20%, crushing, sieving with a 100-mesh sieve for later use, adding 60% ethanol solution according to the material-liquid ratio of 1:50 (g/mL), performing ultrasonic wave assisted extraction at the ultrasonic frequency of 40kHz and the power of 500W at the temperature of 50 ℃ for 60min, centrifuging at 2000r/min for 30min, taking supernatant, and performing vacuum rotary evaporation and concentration at 50 ℃ to obtain a biological modifier;
2) preparing Gd/CaZrO nano particles: the preparation method of the Gd/CaZrO nano particles comprises the following steps: 3g Gd2O3Fully and uniformly mixing the powder and 5g of urea in distilled water to obtain a solution A; 20g of ZrO were weighed2And 10g of CaO are mixed into the solution A, the mixture is uniformly mixed and transferred into a rotary evaporator to be rotated and evaporated for 1h, the solvent is completely removed to obtain a solid precursor, then the solid precursor is heated at the speed of 4 ℃/min, N2Roasting at 1300 ℃ for 2h under protection, cooling to room temperature, and performing ball milling to obtain Gd/CaZrO nano particles;
3) mixing and melting nylon chips, a biological modifier, Gd/CaZrO nano particles and a polyamide chain extender, extruding the mixture into a melt by using a double-screw device, and conveying the melt to a melt pipeline; and then the mixture is input into a spinning box body through a metering pump, and is subjected to melt spinning and cooling through a spinneret plate to obtain fiber tows.
7. The method for preparing chinlon macrobio-fiber containing gingko, rose, camellia, pomegranate and kudzu root according to claim 6, wherein the mixing and melting temperature in the twin-screw of step (3) is 235 ℃, and the extrusion pressure is 12 MPa.
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| CN202011639410.2A CN112725923A (en) | 2020-12-31 | 2020-12-31 | Chinlon macrobio-fiber containing ginkgo, rose, camellia, pomegranate and radix puerariae and preparation method thereof |
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| CN202011639410.2A CN112725923A (en) | 2020-12-31 | 2020-12-31 | Chinlon macrobio-fiber containing ginkgo, rose, camellia, pomegranate and radix puerariae and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011155807A2 (en) * | 2010-06-11 | 2011-12-15 | Seok Myung-Ho | Antibacterial synthetic fiber and method for producing same |
| CN102677215A (en) * | 2012-06-05 | 2012-09-19 | 太仓市宏亿化纤有限公司 | Antibacterial moisture-transfer chinlon 6 and preparation method thereof |
| US20140048738A1 (en) * | 2010-12-28 | 2014-02-20 | Shanghai Genius Advanced Material(Group) Co., Ltd. | Nano particle/polyamide composite material, preparation method therefor, and use thereof |
| CN103620097A (en) * | 2010-06-11 | 2014-03-05 | 柳寅植 | Antibacterial synthetic fiber, and method for manufacturing same |
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2020
- 2020-12-31 CN CN202011639410.2A patent/CN112725923A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011155807A2 (en) * | 2010-06-11 | 2011-12-15 | Seok Myung-Ho | Antibacterial synthetic fiber and method for producing same |
| CN103620097A (en) * | 2010-06-11 | 2014-03-05 | 柳寅植 | Antibacterial synthetic fiber, and method for manufacturing same |
| US20140048738A1 (en) * | 2010-12-28 | 2014-02-20 | Shanghai Genius Advanced Material(Group) Co., Ltd. | Nano particle/polyamide composite material, preparation method therefor, and use thereof |
| CN102677215A (en) * | 2012-06-05 | 2012-09-19 | 太仓市宏亿化纤有限公司 | Antibacterial moisture-transfer chinlon 6 and preparation method thereof |
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