CN112030258A - Dandelion-containing nylon fiber and preparation method thereof - Google Patents
Dandelion-containing nylon fiber and preparation method thereof Download PDFInfo
- Publication number
- CN112030258A CN112030258A CN202011015655.8A CN202011015655A CN112030258A CN 112030258 A CN112030258 A CN 112030258A CN 202011015655 A CN202011015655 A CN 202011015655A CN 112030258 A CN112030258 A CN 112030258A
- Authority
- CN
- China
- Prior art keywords
- dandelion
- particles
- preparation
- preparing
- sio
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—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
- 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
-
- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention provides a nylon fiber containing dandelion and a preparation method thereof, wherein the preparation method comprises the following steps: preparing dandelion extract, preparing modified particles, preparing modified liquid, preparing functional master batches, mixing, spinning, primary drafting, dipping, shaping, oiling, secondary drafting and winding. The preparation of the modified particles comprises the preparation of SiO2Particle, loading and coating. The breaking strength of the nylon fiber is 6.1-6.7 g/d, and the wet breaking strength is 5.4-6.2 g/d; the elongation at break is 21-27%, and the wet elongation at break is 27-31%; the bacteriostatic rate of the antibacterial agent on staphylococcus aureus, escherichia coli, candida albicans and other bacteria reaches 95.2-97.1%.
Description
Technical Field
The invention relates to the field of nylon fibers, in particular to a nylon fiber containing dandelion and a preparation method thereof.
Background
Chinlon, also known as Nylon (Nylon), is known as Polyamide and is called Polyamide (PA) in english, and is the first synthetic fiber appearing in the world. Polyamide density 1.15g/cm3On the left and right sides, the main chain of the molecule contains repeated amide groups [ NHCO ]]The thermoplastic resins include aliphatic PA, aliphatic-aromatic PA and aromatic PA. The aliphatic PA has many varieties, large yield and wide application, and the name is determined by the specific carbon atom number of the synthetic monomer.
The nylon fiber has the most outstanding advantages of better wear resistance and elasticity than other fibers, and the elastic recovery rate of the nylon fiber can be comparable to that of wool. Among the commercialized synthetic fibers, those having a specific gravity inferior to that of polypropylene (specific gravity of 1) are lighter than those of polyester fibers (specific gravity of 1.38). Therefore, the nylon fiber can be processed into a fine, even, soft and smooth silk thread for weaving into attractive and durable fiber products. Meanwhile, the molding sand has the same corrosion resistance as polyester fiber, is not afraid of being damaged by worms, and is not easy to mildew.
With the progress of science and technology and the improvement of living standard of people, both the functionality and the yield of the fiber are far from meeting the actual demand, and people are more and more paying attention to the functional improvement of the textile. Therefore, the functional research on the nylon fiber becomes particularly important.
Dandelion, herb of common alias, herba violae, herb of veronicastrum, and HUALANG. Perennial herb of Compositae. The head-shaped inflorescence, the seeds are provided with pompon formed by white crown hairs, and the pompon floats to a new place along with wind after the flowers bloom to inoculate new life. The dandelion contains a plurality of chemical components, has good effects of promoting lactation, resisting bacteria, benefiting gallbladder and resisting tumors, and is a health-care plant used as both medicine and food. The plant plants have the effects of cooling, reducing internal heat and sterilizing, and provide a new angle and resource for the development and utilization of multifunctional fibers. From the development and utilization perspective, the dandelion-containing nylon fiber is also a novel fiber material which is not completely developed and utilized, and still has great potential and value for the research, development and innovation and performance perfection of the nylon fiber.
The existing nylon fiber product containing plant active ingredients is usually prepared by loading the active ingredients on a carrier in a carrier loading mode to prepare a modifier, and then mixing the modifier with fiber raw materials for spinning. The applicant finds that in the spinning process by mixing the modifying agent containing the dandelion active ingredient with the fiber raw material and the auxiliary agent, the dandelion active ingredient is easily influenced by other raw materials and high temperature, the loss is high, and the modification effect is unstable. The applicant also finds that the active ingredients of the nylon fiber product containing the dandelion are not tightly combined with the fiber, and the long-term stability is not good when the polyamide fiber product containing the dandelion is researched and developed by the applicant.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides a nylon fiber containing dandelion and a preparation method thereof, so as to realize the following purposes:
(1) the problems that the active ingredients of the dandelion are easily affected by other raw materials and high temperature, the loss is high and the modification effect is unstable in the process of mixing the modifying agent containing the dandelion active ingredients with the fiber raw materials and the auxiliary agents for spinning are solved;
(2) overcomes the problems of insufficient tight combination of the modifier containing the dandelion active ingredient and the fiber and poor long-term stability.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of nylon fiber containing dandelion comprises the following steps: preparing dandelion extract, preparing modified particles, preparing modified liquid, preparing functional master batches, mixing, spinning, primary drafting, dipping, shaping, oiling, secondary drafting and winding;
the preparation of the modified particles comprises the preparation of SiO2Particle, loading and coating;
the modified particle is the SiO prepared by the method2The particles are used as a core after loading the active ingredients of the dandelion extract, and a polymethyl methacrylate shell used as a protective shell is coated on the outer layer;
the particle size of the modified particles is 0.25-0.35 μm.
Further, the dandelion extract is prepared by cleaning fresh dandelion leaves, draining, and stirring into paste; adding 6-7 times of the volume of the extracting solution, and uniformly dispersing by ultrasonic; then carrying out ultrasonic extraction to prepare the dandelion extract; the extracting solution is glycerol.
Further, the method comprisesPreparation of SiO2Mixing ethyl orthosilicate, ethanol, citric acid betaine, hydroxylamine hydrochloride, ammonia water and deionized water, and stirring for 12-16 h at the temperature of 35-40 ℃; then adding triethoxysilane and a silane coupling agent MPS; continuously stirring for 6-8 h; after centrifugal separation to obtain solid matter, calcining to obtain the SiO2Particles.
Further, the loading step comprises mixing the dandelion extract with the SiO2Mixing the particles, putting into 3 times volume of ethanol, and performing ultrasonic dispersion uniformly; centrifuging to obtain a solid; drying the solid at 70-75 ℃ to prepare the SiO loaded with the dandelion active ingredient2Particles.
Further, the coating is to coat the SiO after the loading2Mixing the particles with ethanol and NaHCO3Mixing monoglyceride fatty acid glyceride and sodium dodecyl benzene sulfonate, and stirring; adding methyl methacrylate and potassium persulfate; and heating to 70-90 ℃, and preserving the heat for 5-6 hours to obtain the modified particles.
Further, preparing the functional master batch, namely mixing nylon 66 slices, modified particles, polyvinylpyrrolidone, phosphite antioxidant and sodium stearate, heating and melting for 30min at 280 ℃, and granulating to prepare the functional master batch;
the nylon 66 slices are as follows: modified particles: polyvinylpyrrolidone: phosphite ester: the ratio of the sodium stearate to the sodium stearate is 150-200: 20-25: 3-5: 1-2 by weight.
Further, in the spinning, common chinlon 66 chips and the functional mother particles are mixed, extruded and melted at 260 ℃, and spun after metering to prepare fibers;
the common chinlon 66 slices: the weight ratio of the functional master batch is 100: (3-5).
Preferably, the weight ratio of ethyl orthosilicate: ethanol: citric acid betaine: and (3) hydroxylamine hydrochloride: ammonia water: deionized water: triethoxy silane: the silane coupling agent MPS has a weight ratio of 10-15: 200-300: 2-5: 1-3: 5-6: 30-35: 2-3.
Preferably, the SiO2 particles: ethanol: NaHCO 3: monoglyceride fatty acid glyceride: sodium dodecylbenzenesulfonate: methyl methacrylate: the ratio of the parts by weight of the potassium persulfate is 20-40: 200-300: 2-5: 1-3: 80-90: 2-3.
A nylon fiber containing dandelion is prepared by the preparation method.
According to the dandelion-containing polyamide fiber, the modified particles can enable active ingredients of dandelion extracts to be combined with the fiber more tightly. The protective shell of the modified particles shrinks, and the fiber macromolecules and the modified particle micromolecules are spliced to form a tightly connected net structure.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the preparation method of the dandelion-containing polyamide fiber, in the spinning processing process, the influence of the active ingredients of the dandelion extract by other raw materials and process conditions can be ignored, the loss rate of the active ingredients is low, and the modification effect is stable;
(2) the preparation method of the dandelion-containing nylon fiber can ensure that the dandelion modified components are tightly combined with the fiber, and the long-term stability is good;
(3) the nylon fiber containing dandelion has the breaking strength of 6.1-6.7 g/d and the wet breaking strength of 5.4-6.2 g/d;
(4) the nylon fiber containing dandelion has the elongation at break of 21-27% and the wet elongation at break of 27-31%;
(5) the dandelion-containing nylon fiber has the bacteriostasis rate of 95.2-97.1% on staphylococcus aureus, escherichia coli, candida albicans and other bacteria; after 50 times of standard washing, the antibacterial performance reduction rate is less than 5.3%;
(6) the dandelion-containing polyamide fiber disclosed by the invention is good in mite prevention effect, and the mite prevention rate reaches 93.3-94.5%.
Detailed Description
In order to more clearly understand the technical features, objects, and effects of the present invention, specific embodiments of the present invention will now be described.
Example 1
A preparation method of nylon fiber containing dandelion comprises the steps of preparation of dandelion extract, preparation of modified particles, preparation of functional master batches, spinning, oiling and winding forming.
The preparation method of the dandelion extract comprises the steps of cleaning fresh dandelion leaves, draining, stirring at 300RPM into paste, adding 6 times of the volume of the extracting solution, heating to 40 ℃, and uniformly dispersing by ultrasonic; heating to 50 deg.C, and performing ultrasonic extraction for 30 min; filtering to remove solid substances, and retaining the extractive solution to obtain the herba Taraxaci extract.
The extracting solution is glycerol.
The ultrasonic extraction power is 250W.
The preparation of the modified particles comprises the preparation of SiO2Particle, loading and coating.
The preparation of SiO2Mixing ethyl orthosilicate, ethanol, citric acid betaine, hydroxylamine hydrochloride, ammonia water and deionized water, and stirring at 200RPM for 12h at 35 ℃; then adding triethoxysilane and a silane coupling agent MPS; stirring at 150RPM for 6 h; centrifuging to obtain solid substance; heating to 500 ℃ by adopting a heating mode with the speed of 2 ℃/min, calcining the solid matter, and keeping the temperature for 2 hours to prepare the SiO2Particles.
The ethyl orthosilicate: ethanol: citric acid betaine: and (3) hydroxylamine hydrochloride: ammonia water: deionized water: triethoxy silane: the ratio of the silane coupling agent MPS in parts by weight is 10:300:2:1:6:35:2: 2.
The particle size of the SiO2 particles is 0.05-0.1 μm.
Loading, mixing the dandelion extract with SiO2Mixing the particles, putting into 3 times volume of ethanol, and performing ultrasonic dispersion for 10min under the ultrasonic frequency condition of 30 KHz; then centrifugally separating at 6000RPM to obtain solid; drying the solid at 70 deg.C to obtain SiO loaded with herba Taraxaci active ingredient2Particles.
Coating, the loaded SiO2Mixing the particles with ethanol and NaHCO3Mixing monoglyceride fatty acid glyceride and sodium dodecyl benzene sulfonate, and stirring at 200RPM for 10min; adding methyl methacrylate and potassium persulfate; heating to 70 ℃, and preserving the heat for 5 hours to obtain the modified particles.
The SiO2Particle: ethanol: NaHCO 23: monoglyceride fatty acid glyceride: sodium dodecylbenzenesulfonate: methyl methacrylate: the ratio of the potassium persulfate to the potassium persulfate is 20:300:2:1:1:80:2 in parts by weight.
The modified particles are SiO2The particles are loaded with dandelion active ingredients and used as core bodies, and polymethyl methacrylate shells used as protective shells are coated on the outer layers.
The particle size of the modified particles is 0.25-0.35 μm.
The preparation method of the functional master batch comprises the steps of mixing nylon 66 slices, modified particles, polyvinylpyrrolidone, phosphite antioxidant and sodium stearate, heating and melting for 30min at 280 ℃ by adopting a double-screw extruder, and granulating to obtain the functional master batch.
The nylon 66 slices are as follows: modified particles: polyvinylpyrrolidone: phosphite ester: the weight ratio of sodium stearate is 200:20:3:1: 1.
And in the spinning step, common chinlon 66 chips and the functional mother particles are mixed, extruded and melted at 260 ℃, and spun after metering to prepare the fiber.
The common chinlon 66 slices: the weight ratio of the functional master batch is 100: 3.
the spinning is carried out by adopting a single-screw spinning machine, the diameter of a screw is 20mm, the length/diameter ratio is 25, the rotating speed of the screw is 10rpm, a spinneret plate is 120 holes, and the length/diameter ratio of the spinneret hole is 3.0.
And oiling, namely oiling the shaped fiber.
And winding, namely winding the oiled fiber to obtain the dandelion-containing polyamide fiber of the embodiment.
The winding speed is 600 m/min.
Through detection, the breaking strength of the nylon fiber containing dandelion in the embodiment is 6.1g/d, and the wet breaking strength is 5.4 g/d; elongation at break of 22% and wet elongation at break of 27%; the bacteriostasis rate to staphylococcus aureus, colibacillus, candida albicans and other bacteria is 95.2 percent; after 50 times of standard washing, the antibacterial performance reduction rate is 5.2%; the anti-mite rate is 93.5%.
Example 2
A preparation method of nylon fiber containing dandelion comprises the steps of preparation of dandelion extract, preparation of modified particles, preparation of functional master batches, spinning, oiling and winding forming.
The preparation of the dandelion extract comprises the steps of cleaning fresh dandelion leaves, draining, stirring at 400RPM into paste, adding 7 times of the volume of the extracting solution, heating to 45 ℃, and uniformly dispersing by ultrasonic; heating to 55 deg.C, and performing ultrasonic extraction for 35 min; filtering to remove solid substances, and retaining the extractive solution to obtain the herba Taraxaci extract.
The extracting solution is glycerol.
The ultrasonic extraction power is 300W.
The preparation of the modified particles comprises the preparation of SiO2Particle, loading and coating.
The preparation of SiO2Mixing ethyl orthosilicate, ethanol, citric acid betaine, hydroxylamine hydrochloride, ammonia water and deionized water, and stirring at 250RPM for 14h at 40 ℃; then adding triethoxysilane and a silane coupling agent MPS; stirring at 200RPM for 7 h; centrifuging to obtain solid substance; heating to 500 ℃ by adopting a heating mode with the speed of 2 ℃/min, calcining the solid matter, and keeping the temperature for 2 hours to prepare the SiO2Particles.
The ethyl orthosilicate: ethanol: citric acid betaine: and (3) hydroxylamine hydrochloride: ammonia water: deionized water: triethoxy silane: the ratio of the silane coupling agent MPS in parts by weight is 10:200:2:1:5:30:2: 2.
The particle size of the SiO2 particles is 0.05-0.1 μm.
Loading, mixing the dandelion extract with SiO2Mixing the particles, putting into 3 times volume of ethanol, and ultrasonically dispersing for 15min under the condition of 35KHz ultrasonic frequency; then centrifugally separating at 6500RPM to obtain solid; drying the solid at a temperature of 75 ℃Preparing SiO loaded with dandelion active ingredient2Particles.
Coating, the loaded SiO2Mixing the particles with ethanol and NaHCO3Mixing monoglyceride fatty acid glyceride and sodium dodecyl benzene sulfonate, and stirring at 250RPM for 12 min; adding methyl methacrylate and potassium persulfate; heating to 80 ℃, and preserving heat for 6 hours to obtain the modified particles.
The SiO2Particle: ethanol: NaHCO 23: monoglyceride fatty acid glyceride: sodium dodecylbenzenesulfonate: methyl methacrylate: the ratio of the potassium persulfate to the potassium persulfate is 20:200:2:1:1:80:2 in parts by weight.
The modified particles are SiO2The particles are loaded with dandelion active ingredients and used as core bodies, and polymethyl methacrylate shells used as protective shells are coated on the outer layers.
The particle size of the modified particles is 0.25-0.35 μm.
The preparation method of the functional master batch comprises the steps of mixing nylon 66 slices, modified particles, polyvinylpyrrolidone, phosphite antioxidant and sodium stearate, heating and melting for 30min at 280 ℃ by adopting a double-screw extruder, and granulating to obtain the functional master batch.
The nylon 66 slices are as follows: modified particles: polyvinylpyrrolidone: phosphite ester: the weight ratio of sodium stearate is 180:25:3:2: 1.
And in the spinning step, common chinlon 66 chips and the functional mother particles are mixed, extruded and melted at 260 ℃, and spun after metering to prepare the fiber.
The common chinlon 66 slices: the weight ratio of the functional master batch is 100: 5.
the spinning is carried out by adopting a single-screw spinning machine, the diameter of a screw is 22mm, the length/diameter ratio is 28, the rotating speed of the screw is 12rpm, a spinneret plate is 120 holes, and the length/diameter ratio of the spinneret hole is 3.2.
And oiling, namely oiling the shaped fiber.
And winding, namely winding the oiled fiber to obtain the dandelion-containing polyamide fiber of the embodiment.
The winding speed was 700 m/min.
Through detection, the breaking strength of the nylon fiber containing dandelion in the embodiment is 6.7g/d, and the wet breaking strength is 6.2 g/d; elongation at break of 26% and elongation at wet break of 30%; the bacteriostasis rate to staphylococcus aureus, colibacillus, candida albicans and other bacteria is 97.0 percent; after 50 times of standard washing, the antibacterial performance reduction rate is 4.7%; the anti-mite rate is 94.5%.
Example 3
A preparation method of nylon fiber containing dandelion comprises the steps of preparation of dandelion extract, preparation of modified particles, preparation of functional master batches, spinning, oiling and winding forming.
The preparation of the dandelion extract comprises the steps of cleaning fresh dandelion leaves, draining, stirring at 400RPM into paste, adding 7 times of the volume of the extracting solution, heating to 45 ℃, and uniformly dispersing by ultrasonic; heating to 55 deg.C, and performing ultrasonic extraction for 40 min; filtering to remove solid substances, and retaining the extractive solution to obtain the herba Taraxaci extract.
The extracting solution is glycerol.
The ultrasonic extraction power is 350W.
The preparation of the modified particles comprises the preparation of SiO2Particle, loading and coating.
The preparation of SiO2Mixing ethyl orthosilicate, ethanol, citric acid betaine, hydroxylamine hydrochloride, ammonia water and deionized water, and stirring at 300RPM for 16h at 40 ℃; then adding triethoxysilane and a silane coupling agent MPS; stirring at 200RPM for 8 h; centrifuging to obtain solid substance; heating to 500 ℃ by adopting a heating mode with the speed of 2 ℃/min, calcining the solid matter, and keeping the temperature for 2 hours to prepare the SiO2Particles.
The ethyl orthosilicate: ethanol: citric acid betaine: and (3) hydroxylamine hydrochloride: ammonia water: deionized water: triethoxy silane: the ratio of the silane coupling agent MPS in parts by weight is 15: 300:2:1:6:35:2: 2.
The particle size of the SiO2 particles is 0.05-0.1 μm.
Loading, mixing the dandelion extract with SiO2Mixing the particles, adding into 3 times volume of ethanol, and ultrasonically dispersing for 15min under 40KHz ultrasonic frequency; then centrifugally separating at 7000RPM to obtain solid; drying the solid at 75 deg.C to obtain SiO loaded with herba Taraxaci active ingredient2Particles.
Coating, the loaded SiO2Mixing the particles with ethanol and NaHCO3Mixing monoglyceride fatty acid glyceride and sodium dodecyl benzene sulfonate, and stirring at 300RPM for 12 min; adding methyl methacrylate and potassium persulfate; heating to 90 ℃, and preserving heat for 6 hours to obtain the modified particles.
The SiO2Particle: ethanol: NaHCO 23: monoglyceride fatty acid glyceride: sodium dodecylbenzenesulfonate: methyl methacrylate: the ratio of the potassium persulfate to the potassium persulfate is 40:300:5:3:3:90:3 in parts by weight.
The modified particles are SiO2The particles are loaded with dandelion active ingredients and used as core bodies, and polymethyl methacrylate shells used as protective shells are coated on the outer layers.
The particle size of the modified particles is 0.25-0.35 μm.
The preparation method of the functional master batch comprises the steps of mixing nylon 66 slices, modified particles, polyvinylpyrrolidone, phosphite antioxidant and sodium stearate, heating and melting for 30min at 280 ℃ by adopting a double-screw extruder, and granulating to obtain the functional master batch.
The nylon 66 slices are as follows: modified particles: polyvinylpyrrolidone: phosphite ester: the weight ratio of sodium stearate is 200:25:5:2: 2.
And in the spinning step, common chinlon 66 chips and the functional mother particles are mixed, extruded and melted at 260 ℃, and spun after metering to prepare the fiber.
The common chinlon 66 slices: the weight ratio of the functional master batch is 100: 3.
the spinning is carried out by adopting a single-screw spinning machine, the diameter of a screw is 22mm, the length/diameter ratio is 26, the rotating speed of the screw is 10rpm, a spinneret plate is 160 holes, and the length/diameter ratio of the spinneret hole is 3.2.
And oiling, namely oiling the shaped fiber.
And winding, namely winding the oiled fiber to obtain the dandelion-containing polyamide fiber of the embodiment.
The winding speed was 700 m/min.
Through detection, the rupture strength of the nylon fiber containing dandelion in the embodiment is 6.4g/d, and the wet rupture strength is 6.0 g/d; elongation at break of 25% and wet elongation at break of 29%; the bacteriostasis rate to staphylococcus aureus, colibacillus, candida albicans and other bacteria is 96.6 percent; after 50 times of standard washing, the antibacterial performance reduction rate is 5.0 percent; the anti-mite rate is 93.9%.
Example 4
A preparation method of polyamide fiber containing dandelion comprises the steps of preparation of dandelion extract, preparation of modified particles, preparation of modified liquid, preparation of functional master batch, spinning, dipping, sizing, oiling, winding and forming.
The preparation of the dandelion extract comprises the steps of cleaning fresh dandelion leaves, draining, stirring at 400RPM into paste, adding 7 times of the volume of the extracting solution, heating to 45 ℃, and uniformly dispersing by ultrasonic; heating to 55 deg.C, and performing ultrasonic extraction for 35 min; filtering to remove solid substances, and retaining the extractive solution to obtain the herba Taraxaci extract.
The extracting solution is glycerol.
The ultrasonic extraction power is 300W.
The preparation of the modified particles comprises the preparation of SiO2Particle, loading and coating.
The preparation of SiO2Mixing ethyl orthosilicate, ethanol, citric acid betaine, hydroxylamine hydrochloride, ammonia water and deionized water, and stirring at 250RPM for 14h at 40 ℃; then adding triethoxysilane and a silane coupling agent MPS; stirring at 200RPM for 7 h; centrifuging to obtain solid substance; heating to 500 ℃ by adopting a heating mode with the speed of 2 ℃/min, calcining the solid matter, and keeping the temperature for 2 hours to prepare the SiO2Particles.
The ethyl orthosilicate: ethanol: citric acid betaine: and (3) hydroxylamine hydrochloride: ammonia water: deionized water: triethoxy silane: the ratio of the silane coupling agent MPS in parts by weight is 10:200:2:1:5:30:2: 2.
The particle size of the SiO2 particles is 0.05-0.1 μm.
Loading, mixing the dandelion extract with SiO2Mixing the particles, putting into 3 times volume of ethanol, and ultrasonically dispersing for 15min under the condition of 35KHz ultrasonic frequency; then centrifugally separating at 6500RPM to obtain solid; drying the solid at 75 deg.C to obtain SiO loaded with herba Taraxaci active ingredient2Particles.
Coating, the loaded SiO2Mixing the particles with ethanol and NaHCO3Mixing monoglyceride fatty acid glyceride and sodium dodecyl benzene sulfonate, and stirring at 250RPM for 12 min; adding methyl methacrylate and potassium persulfate; heating to 80 ℃, and preserving heat for 6 hours to obtain the modified particles.
The SiO2Particle: ethanol: NaHCO 23: monoglyceride fatty acid glyceride: sodium dodecylbenzenesulfonate: methyl methacrylate: the ratio of the potassium persulfate to the potassium persulfate is 20:200:2:1:1:80:2 in parts by weight.
The modified particles are SiO2The particles are loaded with dandelion active ingredients and used as core bodies, and polymethyl methacrylate shells used as protective shells are coated on the outer layers.
The particle size of the modified particles is 0.25-0.35 μm.
Preparing the modified liquid, namely mixing a chinlon FDY oiling agent with the modified particles, adding polyethylene glycol monooleate and polyethylene glycol 200, and performing ultrasonic dispersion for 15min to obtain a mixed solution with the modified particle concentration of 6 wt%; adding the herba Taraxaci extract into the mixture, heating to 70 deg.C, stirring at 150RPM for 10min to obtain the modified solution.
The addition amount of the polyethylene glycol monooleate and the polyethylene glycol 200 accounts for 0.3 wt% of the mixed solution.
The polyethylene glycol monooleate: the polyethylene glycol 200 has a weight ratio of 1: 2.
The dandelion extract: the weight ratio of the mixed solution is 1: 25.
The preparation method of the functional master batch comprises the steps of mixing nylon 66 slices, modified particles, polyvinylpyrrolidone, phosphite antioxidant and sodium stearate, heating and melting for 30min at 280 ℃ by adopting a double-screw extruder, and granulating to obtain the functional master batch.
The nylon 66 slices are as follows: modified particles: polyvinylpyrrolidone: phosphite ester: the weight ratio of sodium stearate is 180:25:3:2: 1.
And in the spinning step, common chinlon 66 chips and the functional mother particles are mixed, extruded and melted at 260 ℃, and spun after metering to prepare the fiber.
The common chinlon 66 slices: the weight ratio of the functional master batch is 100: 5.
the spinning is carried out by adopting a single-screw spinning machine, the diameter of a screw is 22mm, the length/diameter ratio is 28, the rotating speed of the screw is 12rpm, a spinneret plate is 120 holes, and the length/diameter ratio of the spinneret hole is 3.2.
And (3) the impregnation is to completely immerse the fiber into the modification solution with 5 times of volume and at 50 ℃, and to stand for 4 hours.
And (4) sizing, draining the modified liquid on the surface of the dipped fiber, and then carrying out sizing treatment by adopting a heat-setting fan. The shaping is carried out by blowing hot air at 45 ℃ for 90 min; then standing for 50min at normal temperature.
The impregnation and sizing can ensure that the dandelion extract and the modified particles are tightly arranged on the surface of the fiber. The protective shell of the modified particles shrinks, and the fiber macromolecules and the modified particle micromolecules are spliced to form a tightly connected net structure. Meanwhile, the core body of the modified particles, the plurality of adjacent modified particles and the connecting rods of the dandelion extract further improve the bonding tightness of the active ingredients of the dandelion extract and the fibers.
And oiling, namely oiling the shaped fiber.
And winding, namely winding the oiled fiber to obtain the dandelion-containing polyamide fiber of the embodiment.
The winding speed was 700 m/min.
Through detection, the breaking strength of the nylon fiber containing dandelion in the embodiment is 6.7g/d, and the wet breaking strength is 6.2 g/d; elongation at break of 26% and elongation at wet break of 30%; the bacteriostasis rate to staphylococcus aureus, colibacillus, candida albicans and other bacteria is 97.3 percent; after 50 times of standard washing, the antibacterial performance reduction rate is 3.9%; the anti-mite rate is 94.8%.
Comparative example 1
The technical scheme of the embodiment 2 is adopted, and the difference is that common commercial nano SiO with the particle size range of 0.05-0.1 μm is adopted2And (3) adding the particles into the prepared dandelion extract for loading, and preparing modified particles loaded with the dandelion active ingredient without a coating step. And the modifier is used in the nylon fiber preparation process.
Through detection, the breaking strength of the nylon fiber containing dandelion prepared in the comparative example 1 is 5.6g/d, and the wet breaking strength is 5.3 g/d; elongation at break of 19% and elongation at wet break of 24%; the bacteriostasis rate to staphylococcus aureus, colibacillus, candida albicans and other bacteria is 88.5 percent; after 50 times of standard washing, the antibacterial performance reduction rate is 15.3%; the anti-mite rate is 81.6%.
It can be seen that the modified particles loaded with the dandelion active ingredient in the comparative example 1, in the process of mixing the fiber raw material and the auxiliary agent for spinning, the active ingredient of the modified particles may be affected by other raw materials and high temperature, the loss rate is high, and the modification effect is not satisfactory; moreover, the active ingredients are not tightly bound to the fibers, and the long-term stability is not good.
All percentages used in the present invention are mass percentages unless otherwise indicated.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of polyamide fiber containing dandelion is characterized by comprising the following steps: preparing dandelion extract, preparing modified particles, preparing modified liquid, preparing functional master batches, mixing, spinning, primary drafting, dipping, shaping, oiling, secondary drafting and winding;
the preparation of the modified particles comprises the preparation of SiO2Particle, loading and coating;
the modified particle is the SiO prepared by the method2The particles are used as a core after loading the active ingredients of the dandelion extract, and a polymethyl methacrylate shell used as a protective shell is coated on the outer layer;
the particle size range of the modified particles is 0.25-0.35 mu m;
the functional master batch is prepared from the modified particles, nylon 66 slices, polyvinylpyrrolidone, phosphite antioxidant and sodium stearate.
2. The method for preparing dandelion-containing nylon fiber according to claim 1, wherein the dandelion extract is prepared by washing fresh dandelion leaves, draining, and mashing into paste; adding 6-7 times of the volume of the extracting solution, and uniformly dispersing by ultrasonic; then carrying out ultrasonic extraction to prepare the dandelion extract; the extracting solution is glycerol.
3. The method for preparing nylon fiber containing dandelion according to claim 1, wherein the SiO is prepared2Mixing ethyl orthosilicate, ethanol, citric acid betaine, hydroxylamine hydrochloride, ammonia water and deionized water, and stirring for 12-16 h at the temperature of 35-40 ℃; then adding triethoxysilane and a silane coupling agent MPS; continuously stirring for 6-8 h; after centrifugal separation to obtain solid matter, calcining to obtain the SiO2Particles.
4. The method for preparing dandelion-containing polyamide fiber according to claim 1, wherein the loading comprises mixing the dandelion extract with the SiO2Mixing the particles, putting into 3 times volume of ethanol, and performing ultrasonic dispersion uniformly; centrifuging to obtain a solid; drying the solid at 70-75 ℃ to prepare the SiO loaded with the dandelion active ingredient2Particles.
5. The method for preparing dandelion-containing nylon fiber according to claim 1, wherein the coating is performed by loading SiO2Mixing the particles with ethanol and NaHCO3Mixing monoglyceride fatty acid glyceride and sodium dodecyl benzene sulfonate, and stirring; adding methyl methacrylate and potassium persulfate; and heating to 70-90 ℃, and preserving the heat for 5-6 hours to obtain the modified particles.
6. The method for preparing polyamide fiber containing dandelion according to claim 1, wherein the preparation of the functional masterbatch is carried out by mixing nylon 66 slices, modified particles, polyvinylpyrrolidone, phosphite antioxidant and sodium stearate, heating and melting for 30min at 280 ℃, and granulating to obtain the functional masterbatch;
the nylon 66 slices are as follows: modified particles: polyvinylpyrrolidone: phosphite ester: the ratio of the sodium stearate to the sodium stearate is 150-200: 20-25: 3-5: 1-2 by weight.
7. The method for preparing nylon fiber containing dandelion according to claim 1, wherein the spinning comprises mixing common nylon 66 chips with the functional mother particles, extruding and melting at 260 ℃, metering, and spinning to obtain fiber;
the common chinlon 66 slices: the weight ratio of the functional master batch is 100: (3-5).
8. The preparation method of dandelion-containing nylon fiber according to claim 3, wherein the weight ratio of ethyl orthosilicate: ethanol: citric acid betaine: and (3) hydroxylamine hydrochloride: ammonia water: deionized water: triethoxy silane: the silane coupling agent MPS has a weight ratio of 10-15: 200-300: 2-5: 1-3: 5-6: 30-35: 2-3.
9. The method for preparing dandelion-containing nylon fiber according to claim 5, wherein the SiO2 particles: ethanol: NaHCO 3: monoglyceride fatty acid glyceride: sodium dodecylbenzenesulfonate: methyl methacrylate: the ratio of the parts by weight of the potassium persulfate is 20-40: 200-300: 2-5: 1-3: 80-90: 2-3.
10. A nylon fiber containing dandelion, which is characterized by being prepared by the preparation method of claims 1 to 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011015655.8A CN112030258A (en) | 2020-09-24 | 2020-09-24 | Dandelion-containing nylon fiber and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011015655.8A CN112030258A (en) | 2020-09-24 | 2020-09-24 | Dandelion-containing nylon fiber and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112030258A true CN112030258A (en) | 2020-12-04 |
Family
ID=73574379
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011015655.8A Pending CN112030258A (en) | 2020-09-24 | 2020-09-24 | Dandelion-containing nylon fiber and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112030258A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116145275A (en) * | 2023-04-20 | 2023-05-23 | 山东天纤新材料有限公司 | Diclofenac sodium modified viscose large biological fiber and preparation method thereof |
| CN117344398A (en) * | 2023-12-04 | 2024-01-05 | 潍坊瑞银纺织科技有限公司 | Large biological nylon fiber containing plant active ingredients and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040259973A1 (en) * | 2001-10-17 | 2004-12-23 | Shuji Sakuma | Anti-bacterial composite particles and anti-bacterial resin composition |
| CN104695043A (en) * | 2015-02-12 | 2015-06-10 | 浙江理工大学 | Preparation method of grafted SiO2 particle cluster orientation reinforced polyester fiber |
| CN109605608A (en) * | 2018-11-30 | 2019-04-12 | 中科纺织研究院（青岛）有限公司 | A kind of plant source chinlon master batch and preparation method thereof |
| CN110863252A (en) * | 2019-11-06 | 2020-03-06 | 百事基材料（青岛）股份有限公司 | Plant functional polyester filament and preparation method thereof |
| CN111235672A (en) * | 2020-03-27 | 2020-06-05 | 百事基材料（青岛）股份有限公司 | Artemisia argyi or mint extract modified polyamide fiber and preparation method thereof |
| CN111621871A (en) * | 2020-07-02 | 2020-09-04 | 中科纺织研究院（青岛）有限公司 | Radix isatidis extract modified polyamide fiber and preparation method thereof |
-
2020
- 2020-09-24 CN CN202011015655.8A patent/CN112030258A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040259973A1 (en) * | 2001-10-17 | 2004-12-23 | Shuji Sakuma | Anti-bacterial composite particles and anti-bacterial resin composition |
| CN104695043A (en) * | 2015-02-12 | 2015-06-10 | 浙江理工大学 | Preparation method of grafted SiO2 particle cluster orientation reinforced polyester fiber |
| CN109605608A (en) * | 2018-11-30 | 2019-04-12 | 中科纺织研究院（青岛）有限公司 | A kind of plant source chinlon master batch and preparation method thereof |
| CN110863252A (en) * | 2019-11-06 | 2020-03-06 | 百事基材料（青岛）股份有限公司 | Plant functional polyester filament and preparation method thereof |
| CN111235672A (en) * | 2020-03-27 | 2020-06-05 | 百事基材料（青岛）股份有限公司 | Artemisia argyi or mint extract modified polyamide fiber and preparation method thereof |
| CN111621871A (en) * | 2020-07-02 | 2020-09-04 | 中科纺织研究院（青岛）有限公司 | Radix isatidis extract modified polyamide fiber and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116145275A (en) * | 2023-04-20 | 2023-05-23 | 山东天纤新材料有限公司 | Diclofenac sodium modified viscose large biological fiber and preparation method thereof |
| CN117344398A (en) * | 2023-12-04 | 2024-01-05 | 潍坊瑞银纺织科技有限公司 | Large biological nylon fiber containing plant active ingredients and preparation method thereof |
| CN117344398B (en) * | 2023-12-04 | 2024-03-19 | 潍坊瑞银纺织科技有限公司 | Large biological nylon fiber containing plant active ingredients and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112030258A (en) | Dandelion-containing nylon fiber and preparation method thereof | |
| CN105105328B (en) | A kind of loud and clear solid spice pearl and preparation method thereof for cigarette filter rod | |
| CN106929931B (en) | Viscose fiber containing isatis root extract and preparation method thereof | |
| EP3819410A2 (en) | Plant-based functional polyester filament and preparation method thereof | |
| CN112011847A (en) | Lotus leaf, isatis root or aloe modified polyester fiber and preparation method thereof | |
| CN107158447A (en) | A kind of antibacterial zeins dressing with controllable orientation and preparation method thereof | |
| CN112779627A (en) | ES macrobio fiber containing active ingredients of tangerine peel, orange and pomelo and preparation method thereof | |
| CN112030261A (en) | Dacron fiber containing dandelion and preparation method thereof | |
| CN110656400B (en) | Sheath-core polylactic acid cigarette tow, preparation method and application thereof | |
| CN112323171A (en) | Lavender-containing nylon fiber and preparation method thereof | |
| CN113150488A (en) | Clothes hanger with mosquito repelling effect and preparation method thereof | |
| CN111041887A (en) | Antibacterial, mildew-proof and moth-proof rice paper raw pulp, prepared rice paper and preparation method | |
| CN110714238A (en) | Preparation method of skin-core structure antibacterial polyester | |
| CN108716028A (en) | A kind of long-acting antiseptic and antiviral Chloranthus glaber cellulose fibre and preparation method thereof | |
| CN112359487A (en) | Olive-containing polypropylene spun-bonded non-woven fabric and preparation method thereof | |
| CN112064131A (en) | Viscose containing dandelion and preparation method thereof | |
| CN111088695A (en) | Agilawood-flavor finishing fabric and preparation method thereof | |
| CN111411407A (en) | Production process of regenerated super-dull elastic composite yarn | |
| CN106637474A (en) | Antibacterial nylon stretch yarn | |
| CN106400173A (en) | Preparation method of Chinese herbal medicine fragrant polyarmide fiber | |
| CN109537101A (en) | A kind of antibacterial emulation wig silk and its manufacturing method | |
| CN112323165A (en) | Preparation method of hemp tea fiber | |
| CN112251835A (en) | Olive-containing polyamide fiber and preparation method thereof | |
| CN111979592A (en) | Lotus leaf, isatis root or aloe modified polyamide fiber and preparation method thereof | |
| CN112981589B (en) | Chinlon 6 filament and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20201204 |
|
| RJ01 | Rejection of invention patent application after publication |