CN116288787A - Preparation method of chinlon large biological fiber containing bioactive components - Google Patents
Preparation method of chinlon large biological fiber containing bioactive components Download PDFInfo
- Publication number
- CN116288787A CN116288787A CN202310053690.6A CN202310053690A CN116288787A CN 116288787 A CN116288787 A CN 116288787A CN 202310053690 A CN202310053690 A CN 202310053690A CN 116288787 A CN116288787 A CN 116288787A
- Authority
- CN
- China
- Prior art keywords
- bioactive
- polyvinyl alcohol
- nylon
- preparation
- stirring
- 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.)
- Granted
Links
- 230000000975 bioactive effect Effects 0.000 title claims abstract description 116
- 239000000835 fiber Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 229920006052 Chinlon® Polymers 0.000 title claims abstract description 21
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 56
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 56
- 229920001778 nylon Polymers 0.000 claims abstract description 42
- 150000001875 compounds Chemical class 0.000 claims abstract description 33
- 239000004677 Nylon Substances 0.000 claims abstract description 32
- 238000005406 washing Methods 0.000 claims abstract description 21
- 239000003607 modifier Substances 0.000 claims abstract description 17
- 239000012867 bioactive agent Substances 0.000 claims abstract description 16
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000004132 cross linking Methods 0.000 claims abstract description 12
- 238000009987 spinning Methods 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000005469 granulation Methods 0.000 claims abstract description 6
- 230000003179 granulation Effects 0.000 claims abstract description 6
- 238000004945 emulsification Methods 0.000 claims abstract 3
- 230000006641 stabilisation Effects 0.000 claims abstract 2
- 238000011105 stabilization Methods 0.000 claims abstract 2
- 238000003756 stirring Methods 0.000 claims description 47
- 239000000243 solution Substances 0.000 claims description 36
- 239000004615 ingredient Substances 0.000 claims description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 238000001816 cooling Methods 0.000 claims description 23
- 229920000858 Cyclodextrin Polymers 0.000 claims description 18
- 239000001116 FEMA 4028 Substances 0.000 claims description 18
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims description 18
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims description 18
- 229960004853 betadex Drugs 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 18
- 239000003381 stabilizer Substances 0.000 claims description 18
- 239000003995 emulsifying agent Substances 0.000 claims description 16
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 16
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 229920000642 polymer Polymers 0.000 claims description 15
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 13
- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical compound FC(F)(F)CCCBr DBCAQXHNJOFNGC-UHFFFAOYSA-N 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- YIVJZNGAASQVEM-UHFFFAOYSA-N Lauroyl peroxide Chemical compound CCCCCCCCCCCC(=O)OOC(=O)CCCCCCCCCCC YIVJZNGAASQVEM-UHFFFAOYSA-N 0.000 claims description 10
- 229930195725 Mannitol Natural products 0.000 claims description 10
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 10
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims description 10
- 239000002202 Polyethylene glycol Substances 0.000 claims description 10
- 229920001214 Polysorbate 60 Polymers 0.000 claims description 10
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 10
- 229920002472 Starch Polymers 0.000 claims description 10
- 125000002091 cationic group Chemical group 0.000 claims description 10
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Substances CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 claims description 10
- 229910021389 graphene Inorganic materials 0.000 claims description 10
- 239000000594 mannitol Substances 0.000 claims description 10
- 235000010355 mannitol Nutrition 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- 229920001223 polyethylene glycol Polymers 0.000 claims description 10
- 239000002244 precipitate Substances 0.000 claims description 10
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 10
- 239000008107 starch Substances 0.000 claims description 10
- 235000019698 starch Nutrition 0.000 claims description 10
- 238000009210 therapy by ultrasound Methods 0.000 claims description 10
- ODLHGICHYURWBS-LKONHMLTSA-N trappsol cyclo Chemical compound CC(O)COC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](COCC(C)O)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](COCC(C)O)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](COCC(C)O)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](COCC(C)O)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)COCC(O)C)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1COCC(C)O ODLHGICHYURWBS-LKONHMLTSA-N 0.000 claims description 10
- 230000001804 emulsifying effect Effects 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 6
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 5
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000002074 melt spinning Methods 0.000 claims description 5
- 238000007493 shaping process Methods 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 claims 1
- 230000008025 crystallization Effects 0.000 claims 1
- 239000006185 dispersion Substances 0.000 claims 1
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 33
- 238000002844 melting Methods 0.000 abstract description 7
- 230000008018 melting Effects 0.000 abstract description 7
- 230000002045 lasting effect Effects 0.000 abstract description 6
- 241000222122 Candida albicans Species 0.000 abstract description 5
- 241000588724 Escherichia coli Species 0.000 abstract description 5
- 241000191967 Staphylococcus aureus Species 0.000 abstract description 5
- 229940095731 candida albicans Drugs 0.000 abstract description 5
- 230000004048 modification Effects 0.000 abstract description 3
- 238000012986 modification Methods 0.000 abstract description 3
- 239000012670 alkaline solution Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 8
- 230000000694 effects Effects 0.000 description 6
- 230000002209 hydrophobic effect Effects 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 238000004108 freeze drying Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000006116 polymerization reaction Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 241001474374 Blennius Species 0.000 description 3
- 239000000022 bacteriostatic agent Substances 0.000 description 3
- 238000007909 melt granulation Methods 0.000 description 3
- 241000205585 Aquilegia canadensis Species 0.000 description 2
- 241000222336 Ganoderma Species 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 244000269722 Thea sinensis Species 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000004005 microsphere Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 235000003261 Artemisia vulgaris Nutrition 0.000 description 1
- 240000006891 Artemisia vulgaris Species 0.000 description 1
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 241000167854 Bourreria succulenta Species 0.000 description 1
- 241000628997 Flos Species 0.000 description 1
- 240000008397 Ganoderma lucidum Species 0.000 description 1
- 235000001637 Ganoderma lucidum Nutrition 0.000 description 1
- 244000082204 Phyllostachys viridis Species 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 241000195474 Sargassum Species 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 239000001522 artemisia absinthium l. herb extract Substances 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 230000003385 bacteriostatic effect Effects 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000019693 cherries Nutrition 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000001726 jatropha manihot extract Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000008093 supporting effect Effects 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229940092665 tea leaf extract Drugs 0.000 description 1
- 229940119569 wormwood extract Drugs 0.000 description 1
- 229940106668 yucca extract Drugs 0.000 description 1
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)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention provides a preparation method of chinlon large biological fiber containing bioactive components, which is characterized by comprising the steps of inclusion, stabilization, preparation of modified polyvinyl alcohol, crosslinking, emulsification, blending, granulation and spinning. The chinlon large biological fiber prepared by the invention has good antibacterial effect, lasting antibacterial performance, natural and pollution-free performance, the antibacterial rate of staphylococcus aureus after washing for 50 times is 99-99.6%, the antibacterial rate of candida albicans is 97.9-98.5%, and the antibacterial rate of escherichia coli is 99.2-99.7%. According to the invention, the polyvinyl alcohol is subjected to grafting modification, and after the modifier is added for grafting, the thermal stability is stronger; the bioactive component inclusion compound is activated in alkaline solution, and then is crosslinked and polymerized with modified polyvinyl alcohol and epichlorohydrin to form a network structure, so that the antibacterial effect is more durable. The bioactive components are prepared into the bioactive agent, so that not only is a great loss of a high-temperature melting environment avoided, but also the bioactive agent has good compatibility with nylon slices, and the mechanical property of the fiber is prevented from being reduced.
Description
Technical Field
The invention belongs to the technical field of fibers, and particularly relates to a preparation method of nylon large biological fibers containing bioactive components.
Background
Nylon, also known as nylon fiber, polyamide fiber, is the first synthetic fiber in the world, known as its excellent wear resistance, and can be blended or pure spun into various medical and textile products, such as various wear-resistant nylon socks, nylon garments, etc. or blended into various wear-resistant clothing materials. With the enhancement of health care consciousness of people, antibacterial demands are also put forward on textiles, and the adhesion of germs on human bodies is reduced. Therefore, people often add a bacteriostatic agent into the fiber to obtain a PP product with a bacteriostatic function, and most of the added bacteriostatic agents at present are mainly inorganic bacteriostatic agents, for example, the patent number of CN201810145868.9 is named as a preparation method of a color-change-resistant antibacterial nylon fiber, and the antibacterial nylon fiber is provided with nano silver as the antibacterial agent, but the nano silver is harmful to human bodies and causes certain environmental pollution.
The bioactive components with antibacterial function are added into the nylon fiber, so that the natural antibacterial property of the nylon fiber can be endowed, and the nylon fiber is safe and environment-friendly and is beneficial to the human body. The bioactive components are added to the nylon fibers by adopting an after-finishing method, the antibacterial components only exist on the surfaces of the fibers, the antibacterial effect is greatly reduced after washing or friction, and the antibacterial property is not durable; the bioactive components are added in the fiber preparation process, so that the preparation environment temperature of the nylon fiber is high, a large amount of bioactive components are easy to run off, meanwhile, the bioactive components are easy to agglomerate, and the mechanical properties of the fiber are also affected to a certain extent.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation method of a nylon large biological fiber containing bioactive components, which realizes the aims of reducing the loss of a large amount of bioactive components in the preparation process of the nylon large biological fiber and avoiding the decline of the mechanical properties of the fiber.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of nylon large biological fiber containing bioactive components comprises the following steps:
s1, inclusion
Adding the bioactive components into 10-15 times deionized water, stirring for 10-15min, adding beta-cyclodextrin, performing ultrasonic treatment at 50-60deg.C for 1-2 hr at ultrasonic frequency of 120-150KHz, wherein the beta-cyclodextrin has slightly conical hollow cylindrical solid ring structure, and the cavity is shielded by C-H bond to form a hydrophobic region, so that bioactive components can be embedded into the cavity to form clathrate; concentrating under reduced pressure at 80-90deg.C after reaction, cooling to room temperature, and placing into cooling chamber to separate out crystal to obtain precipitate; washing the precipitate for 3-5 times, and drying in 70-80deg.C drying oven for 2-3 hr to obtain clathrate of bioactive components.
Preferably, the mass ratio of the bioactive component to the beta-cyclodextrin is 1:2-4.
Preferably, the bioactive component is one or more of tea extract, seaweed extract, ganoderma extract, folium Artemisiae Argyi extract, flos Lonicerae extract, orange extract, herba Menthae extract, bamboo extract, cherry extract, and Yucca extract.
Preferably, the cooling chamber temperature is 5-10 ℃.
S2, stability
Adding stabilizer into the bioactive ingredient clathrate, stirring for 20-25min, and lyophilizing with lyophilizing machine to obtain stable bioactive ingredient clathrate.
Preferably, the freeze-drying is carried out by treating for 16-20h at-50 to-60 ℃ and then vacuum drying for 20-24h at 30-35 ℃.
Preferably, the stabilizer is added in an amount of 3-6wt% of the bioactive ingredient clathrate; the stabilizer comprises hydroxypropyl-beta-cyclodextrin, polyethylene glycol, mannitol and cationic starch, wherein the mass ratio of the hydroxypropyl-beta-cyclodextrin to the polyethylene glycol to the mannitol to the cationic starch is 5-8:10-12:1-3:0.5-1.
S3, preparation of modified polyvinyl alcohol
Adding polyvinyl alcohol into deionized water, stirring at 85-90 ℃ for 60-70min, and obtaining polyvinyl alcohol solution after the solution is uniform and stable; adding 1-3mol/L hydrochloric acid to adjust pH to 4-5, adding modifier, performing ultrasonic treatment at 70-80deg.C for 40-50min at ultrasonic frequency of 220-260kHz, adding glutaraldehyde and lauroyl peroxide, stirring at 70-80deg.C for 30-40min, suction filtering, washing for 3-5 times, and drying to obtain modified polyvinyl alcohol with better thermal stability.
Preferably, the mass fraction of the polyvinyl alcohol solution is 5-10%.
Preferably, the modifier is acrylic acid, N-vinyl pyrrolidone, methyl methacrylate or ethylene glycol dimethacrylate, and the mass ratio of the acrylic acid to the N-vinyl pyrrolidone to the methyl methacrylate to the ethylene glycol dimethacrylate is 5-10:3-6:10-15:2-5; the addition amount of the modifier is 10-15wt% of the polyvinyl alcohol.
Preferably, the glutaraldehyde is added in an amount of 5-7wt% of the polyvinyl alcohol, and the lauroyl peroxide is added in an amount of 1-2wt% of the glutaraldehyde.
S4, cross-linking
Adding the stable bioactive component clathrate into NaOH solution, and stirring at 40-45deg.C for 8-12min to obtain mixed solution;
adding modified polyvinyl alcohol into the mixed solution, adding graphene, stirring for 15-25min at 40-50 ℃, cooling to room temperature, then adding epichlorohydrin dropwise, stirring for 60-80min, wherein the stirring speed is 500-600r/min, thus obtaining polymer solution, and crosslinking polymerization forms a network structure on the surface of the inclusion compound, so that the inclusion effect of beta-cyclodextrin is maintained, and meanwhile, the performance and the structure are more stable.
Preferably, the addition amount of the modified polyvinyl alcohol is 20-30wt% of the stable bioactive ingredient inclusion compound; the addition amount of the epichlorohydrin is 10-15wt% of the stable bioactive ingredient inclusion compound, and the dripping rate is 1-3ml/min; the addition amount of the graphene is 0.5-1.5wt% of the stable bioactive ingredient inclusion compound.
S5, emulsifying
Adding methyl silicone oil and an emulsifier into the polymer solution, stirring for 18-25min, emulsifying and dispersing, and stirring at a speed of 300-400r/min; heating to 55-65deg.C in water bath, sealing, reacting for 3-4 hr, concentrating at 60-80deg.C under reduced pressure, repeatedly washing with acetone and deionized water for 3-4 times, and vacuum drying at 70-80deg.C for 2-4 hr to obtain bioactive agent.
The bioactive agent is microsphere, uniform in particle size, round in shape, and 90-100 μm in particle size, and has good thermal stability.
Preferably, the mass ratio of the methyl silicone oil to the polymer solution is 5-6:1-2.
Further, the addition amount of the emulsifier is 4-6wt% of the methyl silicone oil; the components of the emulsifier are sodium laurylsulfate and Tween 60, and the mass ratio of the sodium laurylsulfate to the Tween 60 is 1:5-6.
S6, blending
8-10 parts of bioactive agent, 90-100 parts of chinlon slices, 0.3-0.5 part of tris (2, 4-di-tert-butylphenyl) phosphite ester and 0.4-0.6 part of EBS are added into a high-speed mixer for blending for 5-10min to obtain a blend.
S7, granulating
The blend was fed into a twin screw extruder and the temperature of the various zones of the host set to: melting and granulating at 290-300 deg.C, 285-295 deg.C, 295-305 deg.C, 300-310 deg.C, 295-305 deg.C, 285-295 deg.C and host rotation speed of 240-360rpm to obtain bioactive master batch.
S8, spinning
Placing the bioactive master batch and the nylon slices into a spinning machine for melt spinning to obtain fiber tows; and cooling, oiling, stretching and shaping the fiber tows to obtain the nylon large biological fibers.
Preferably, the mass ratio of the bioactive master batch to the chinlon slices is 5-7:93-95.
By adopting the technical scheme, the invention has the following technical effects:
1. the chinlon large biological fiber prepared by the invention has lasting antibacterial effect, the antibacterial rate of the chinlon large biological fiber to staphylococcus aureus is 99-99.6% after 50 times of water washing, the antibacterial rate of candida albicans is 97.9-98.5%, and the antibacterial rate of escherichia coli is 99.2-99.7% (measured according to GB/T20944.3-2007).
2. The invention modifies bioactive components, which not only avoids a great deal of loss in high-temperature fusion environment, but also has good compatibility with nylon slices, thereby avoiding the decrease of mechanical properties of fibers. Through detection, the loss rate of the bioactive components is 2.3-3.1% in the process of melting granulation; the breaking strength of the nylon large biological fiber is 4.2-4.6cN/dtex, the breaking elongation is 47-51%, and the mechanical property is excellent.
3. The stabilizing agent is added into the inclusion compound of the bioactive components, so that the inclusion supporting effect of the beta-cyclodextrin is ensured, meanwhile, the dispersibility of the inclusion compound is improved, and the phenomenon of agglomeration is avoided to influence the performance of the fiber.
4. The polyvinyl alcohol is grafted and modified, and the thermal stability is stronger after the modifier is added for grafting; activating the inclusion compound of the bioactive component in an alkaline solution, and then cross-linking and polymerizing the inclusion compound of the bioactive component with modified polyvinyl alcohol and epichlorohydrin to form a network structure, so that the inclusion compound of the bioactive component has a certain slow-release effect on the bioactive component, and the antibacterial effect is more durable; adding methyl silicone oil and an emulsifier to form composite microspheres, namely a bioactive agent; the bioactive agent has uniform particle diameter, round shape, and particle diameter of 90-100 μm, and has high stability under high temperature environment, and can prevent the damage to bioactive components due to high temperature during extrusion granulation.
5. The nylon large biological fiber prepared by the invention has good antibacterial effect, lasting antibacterial performance, natural and pollution-free performance, no harm to human body and a certain development prospect in the fiber field.
Detailed Description
The invention will be further illustrated with reference to specific examples.
Example 1 a preparation method of a chinlon macrobiological fiber containing bioactive components, comprising the following steps:
s1, inclusion
Adding the bioactive component into deionized water with a volume of 12 times, stirring for 15min, adding beta-cyclodextrin, performing ultrasonic treatment at 55deg.C for 1.5H at an ultrasonic frequency of 130KHz, wherein the beta-cyclodextrin has a slightly conical hollow cylindrical solid ring structure, and the cavity is shielded by C-H bond to form a hydrophobic region, so that bioactive component can be embedded into the hydrophobic region to form clathrate; concentrating under reduced pressure at 80deg.C after the reaction is finished, cooling to room temperature, and placing into a cooling chamber to precipitate crystals to obtain precipitate; washing the precipitate for 5 times, and drying in a drying oven at 80deg.C for 2 hr to obtain bioactive component clathrate.
The mass ratio of the bioactive component to the beta-cyclodextrin is 1:3.
the bioactive components comprise tea extract, seaweed extract, mugwort extract and honeysuckle extract in a mass ratio of 1:1:1:1; the cooling chamber temperature was 8 ℃.
S2, stability
Adding stabilizer into the bioactive ingredient clathrate, stirring for 25min, and lyophilizing with a lyophilizer to obtain stable bioactive ingredient clathrate.
The freeze-drying is carried out for 18 hours at the temperature of minus 55 ℃ and then is carried out for 22 hours under the vacuum drying at the temperature of 35 ℃.
The addition amount of the stabilizer is 5wt% of the bioactive ingredient inclusion compound; the stabilizer comprises hydroxypropyl-beta-cyclodextrin, polyethylene glycol, mannitol and cationic starch, wherein the mass ratio of the hydroxypropyl-beta-cyclodextrin to the polyethylene glycol to the mannitol to the cationic starch is 6:11:2:0.7.
s3, preparation of modified polyvinyl alcohol
Adding polyvinyl alcohol into deionized water, stirring for 65min at 85 ℃ until the solution is uniform and stable to obtain a polyvinyl alcohol solution; adding 2mol/L hydrochloric acid to adjust pH to 4.5, adding modifier, performing ultrasonic treatment at 75deg.C for 45min, performing ultrasonic frequency of 240kHz, adding glutaraldehyde and lauroyl peroxide, stirring at 75deg.C for 35min, vacuum filtering, washing for 5 times, and drying to obtain modified polyvinyl alcohol with better thermal stability.
The mass fraction of the polyvinyl alcohol solution is 8%.
The modifier is acrylic acid, N-vinyl pyrrolidone, methyl methacrylate and ethylene glycol dimethacrylate, and the mass ratio of the acrylic acid to the N-vinyl pyrrolidone to the methyl methacrylate to the ethylene glycol dimethacrylate is 7:5:12:3; the addition amount of the modifier is 13wt% of the polyvinyl alcohol.
The addition amount of glutaraldehyde is 6wt% of the polyvinyl alcohol, and the addition amount of lauroyl peroxide is 1.5wt% of glutaraldehyde.
S4, cross-linking
Adding the stable bioactive component clathrate into NaOH solution, and stirring at 45deg.C for 10min to obtain mixed solution;
adding modified polyvinyl alcohol into the mixed solution, adding graphene, stirring for 20min at 45 ℃, cooling to room temperature, dropwise adding epichlorohydrin, stirring for 70min at the stirring rate of 500r/min to obtain a polymer solution, and performing cross-linking polymerization on the surface of an inclusion compound to form a network structure, so that the inclusion effect of beta-cyclodextrin is reserved, and meanwhile, the performance and the structure are more stable.
The addition amount of the modified polyvinyl alcohol is 25wt% of the stable bioactive ingredient inclusion compound; the addition amount of the epichlorohydrin is 13wt% of the stable bioactive ingredient inclusion compound, and the dripping rate is 2ml/min; the addition amount of the graphene is 1wt% of the stable bioactive ingredient inclusion compound.
S5, emulsifying
Adding methyl silicone oil and an emulsifier into the polymer solution, stirring for 20min, emulsifying and dispersing, and stirring at the speed of 350r/min; heating to 60 ℃ in water bath, hermetically reacting for 3.5h, concentrating at 70 ℃ under reduced pressure after the reaction is finished, repeatedly washing for 4 times by using acetone and deionized water, and drying at 80 ℃ in vacuum for 3h to obtain the bioactive agent.
The mass ratio of the methyl silicone oil to the polymer solution is 5:1.
The addition amount of the emulsifier is 5wt% of the methyl silicone oil; the components of the emulsifier are sodium laurylsulfate and Tween 60, and the mass ratio of the sodium laurylsulfate to the Tween 60 is 1:5.
S6, blending
9 parts of a bioactive agent, 95 parts of chinlon slices, 0.4 part of tris (2, 4-di-tert-butylphenyl) phosphite ester and 0.5 part of EBS are added into a high-speed mixer to blend for 8 minutes according to parts by weight, so as to obtain a blend.
S7, granulating
The blend was fed into a twin screw extruder and the temperature of the various zones of the host set to: 295 ℃, 290 ℃, 300 ℃, 305 ℃, 300 ℃, 290 ℃ and the rotation speed of a host machine of 300rpm, and obtaining bioactive master batch.
S8, spinning
Placing the bioactive master batch and the nylon slices into a spinning machine for melt spinning to obtain fiber tows; and cooling, oiling, stretching and shaping the fiber tows to obtain the nylon large biological fibers.
The mass ratio of the bioactive master batch to the chinlon slices is 6:94.
The chinlon large biological fiber prepared in the embodiment 1 has lasting antibacterial effect, the antibacterial rate of staphylococcus aureus is 99.5% after 50 times of water washing, the antibacterial rate of candida albicans is 98.2%, and the antibacterial rate of escherichia coli is 99.5%; the breaking strength is 4.6cN/dtex, the breaking elongation is 47%, and the mechanical property is excellent; in the melt granulation process, the loss rate of the bioactive ingredient was 2.3%.
Example 2 a preparation method of a chinlon macrobiological fiber containing bioactive components, comprising the following steps:
s1, inclusion
Adding the bioactive components into 10 times deionized water, stirring for 10min, adding beta-cyclodextrin, performing ultrasonic treatment at 50deg.C for 1 hr at ultrasonic frequency of 120KHz, wherein the beta-cyclodextrin has slightly conical hollow cylindrical solid ring structure, and the cavity is shielded by C-H bond to form a hydrophobic region, so that bioactive components can be embedded into the cavity to form clathrate; concentrating under reduced pressure at 80deg.C after the reaction is finished, cooling to room temperature, and placing into a cooling chamber to precipitate crystals to obtain precipitate; washing the precipitate for 3 times, and drying in a 70 ℃ drying oven for 3 hours to obtain the bioactive ingredient clathrate.
The mass ratio of the bioactive component to the beta-cyclodextrin is 1:2.
the bioactive components comprise folium Camelliae sinensis extract, sargassum extract, ganoderma extract, and folium Artemisiae Argyi extract at a mass ratio of 1:1:1:1.
The cooling chamber temperature was 5 ℃.
S2, stability
Adding stabilizer into the bioactive ingredient clathrate, stirring for 20min, and lyophilizing with a lyophilizer to obtain stable bioactive ingredient clathrate.
The freeze-drying is carried out by treating for 16 hours at-50 ℃ and then vacuum drying for 20 hours at 30 ℃.
The addition amount of the stabilizer is 3wt% of the bioactive ingredient inclusion compound; the stabilizer comprises hydroxypropyl-beta-cyclodextrin, polyethylene glycol, mannitol and cationic starch, wherein the mass ratio of the hydroxypropyl-beta-cyclodextrin to the polyethylene glycol to the mannitol to the cationic starch is 5:10:1:0.5.
s3, preparation of modified polyvinyl alcohol
Adding polyvinyl alcohol into deionized water, stirring for 60min at 85 ℃ until the solution is uniform and stable to obtain a polyvinyl alcohol solution; adding 1mol/L hydrochloric acid to adjust pH to 4, adding modifier, performing ultrasonic treatment at 70deg.C for 40min at ultrasonic frequency of 220kHz, adding glutaraldehyde and lauroyl peroxide, stirring at 70deg.C for 30min, vacuum filtering, washing for 3 times, and drying to obtain modified polyvinyl alcohol with better thermal stability.
The mass fraction of the polyvinyl alcohol solution is 5%.
The modifier is acrylic acid, N-vinyl pyrrolidone, methyl methacrylate and ethylene glycol dimethacrylate, and the mass ratio of the acrylic acid to the N-vinyl pyrrolidone to the methyl methacrylate to the ethylene glycol dimethacrylate is 5:3:10:2; the addition amount of the modifier is 10wt% of the polyvinyl alcohol.
The addition amount of glutaraldehyde is 5wt% of the polyvinyl alcohol, and the addition amount of lauroyl peroxide is 1wt% of glutaraldehyde.
S4, cross-linking
Adding the stable bioactive component clathrate into NaOH solution, and stirring at 40deg.C for 8min to obtain mixed solution;
adding modified polyvinyl alcohol into the mixed solution, adding graphene, stirring for 15min at 40 ℃, cooling to room temperature, dropwise adding epichlorohydrin, stirring for 60min at the stirring rate of 500r/min to obtain a polymer solution, and performing cross-linking polymerization on the surface of an inclusion compound to form a network structure, so that the inclusion effect of beta-cyclodextrin is reserved, and meanwhile, the performance and the structure are more stable.
The addition amount of the modified polyvinyl alcohol is 20wt% of the stable bioactive ingredient inclusion compound; the addition amount of the epichlorohydrin is 10wt% of the stable bioactive ingredient inclusion compound, and the dripping rate is 1ml/min; the addition amount of the graphene is 0.5wt% of the stable bioactive ingredient inclusion compound.
S5, emulsifying
Adding methyl silicone oil and an emulsifier into the polymer solution, stirring for 18min, emulsifying and dispersing, and stirring at the speed of 300r/min; heating to 55 ℃ in water bath, hermetically reacting for 3 hours, concentrating under reduced pressure at 60 ℃ after the reaction is finished, repeatedly washing with acetone and deionized water for 3-4 times, and drying in vacuum at 70 ℃ for 4 hours to obtain the bioactive agent.
The mass ratio of the methyl silicone oil to the polymer solution is 6:1.
The addition amount of the emulsifier is 4wt% of the methyl silicone oil; the components of the emulsifier are sodium laurylsulfate and Tween 60, and the mass ratio of the sodium laurylsulfate to the Tween 60 is 1:5.
S6, blending
8 parts of a bioactive agent, 100 parts of chinlon slices, 0.3 part of tris (2, 4-di-tert-butylphenyl) phosphite ester and 0.4 part of EBS are added into a high-speed mixer for blending for 5min to obtain a blend.
S7, granulating
The blend was fed into a twin screw extruder and the temperature of the various zones of the host set to: melting and granulating at 290 ℃, 285 ℃, 295 ℃, 300 ℃, 295 ℃, 285 ℃ and a host rotation speed of 240rpm to obtain bioactive master batch.
S8, spinning
Placing the bioactive master batch and the nylon slices into a spinning machine for melt spinning to obtain fiber tows; and cooling, oiling, stretching and shaping the fiber tows to obtain the nylon large biological fibers.
The mass ratio of the bioactive master batch to the chinlon slices is 5:95.
The chinlon large biological fiber prepared in the example 2 has lasting antibacterial effect, the antibacterial rate of staphylococcus aureus is 99% after 50 times of water washing, the antibacterial rate of candida albicans is 97.9%, and the antibacterial rate of escherichia coli is 99.2%; the breaking strength is 4.45cN/dtex, the breaking elongation is 50%, and the mechanical property is excellent; in the melt granulation process, the loss rate of the bioactive ingredient was 3.1%.
Example 3 a preparation method of a chinlon macrobiose containing bioactive components, comprising the following steps:
s1, inclusion
Adding the bioactive components into 15 times deionized water, stirring for 15min, adding beta-cyclodextrin, performing ultrasonic treatment at 60deg.C for 2H at ultrasonic frequency of 150KHz, wherein the beta-cyclodextrin has slightly conical hollow cylindrical solid ring structure, and the cavity is shielded by C-H bond to form a hydrophobic region, so that bioactive components can be embedded into the hydrophobic region to form clathrate; concentrating at 85deg.C under reduced pressure after reaction, cooling to room temperature, and placing into a cooling chamber to separate out crystals to obtain precipitate; washing the precipitate for 5 times, and drying in a drying oven at 80deg.C for 3 hr to obtain bioactive component clathrate.
The mass ratio of the bioactive component to the beta-cyclodextrin is 1:4.
the bioactive components comprise tea leaf extract, seaweed extract, ganoderma lucidum extract, wormwood extract and honeysuckle extract in a mass ratio of 1:1:1:1.
The cooling chamber temperature was 10 ℃.
S2, stability
Adding stabilizer into the bioactive ingredient clathrate, stirring for 25min, and lyophilizing with a lyophilizer to obtain stable bioactive ingredient clathrate.
The freeze-drying is carried out by treating for 20 hours at-60 ℃ and then vacuum drying for 24 hours at 35 ℃.
The addition amount of the stabilizer is 6wt% of the bioactive ingredient inclusion compound; the stabilizer comprises hydroxypropyl-beta-cyclodextrin, polyethylene glycol, mannitol and cationic starch, wherein the mass ratio of the hydroxypropyl-beta-cyclodextrin to the polyethylene glycol to the mannitol to the cationic starch is 8:12:3:1.
s3, preparation of modified polyvinyl alcohol
Adding polyvinyl alcohol into deionized water, stirring for 70min at 90 ℃ until the solution is uniform and stable to obtain a polyvinyl alcohol solution; adding 3mol/L hydrochloric acid to adjust pH to 5, adding modifier, performing ultrasonic treatment at 80deg.C for 50min at ultrasonic frequency of 260kHz, adding glutaraldehyde and lauroyl peroxide, stirring at 80deg.C for 40min, vacuum filtering, washing for 5 times, and drying to obtain modified polyvinyl alcohol with better thermal stability.
The mass fraction of the polyvinyl alcohol solution is 10%.
The modifier is acrylic acid, N-vinyl pyrrolidone, methyl methacrylate and ethylene glycol dimethacrylate, and the mass ratio of the acrylic acid to the N-vinyl pyrrolidone to the methyl methacrylate to the ethylene glycol dimethacrylate is 10:6:15:5; the addition amount of the modifier is 15wt% of the polyvinyl alcohol.
The addition amount of glutaraldehyde is 7wt% of the polyvinyl alcohol, and the addition amount of lauroyl peroxide is 2wt% of glutaraldehyde.
S4, cross-linking
Adding the stable bioactive component clathrate into NaOH solution, and stirring at 45deg.C for 12min to obtain mixed solution;
adding modified polyvinyl alcohol into the mixed solution, adding graphene, stirring for 25min at 50 ℃, cooling to room temperature, dropwise adding epichlorohydrin, stirring for 80min at the stirring rate of 600r/min to obtain a polymer solution, and performing cross-linking polymerization on the surface of an inclusion compound to form a network structure, so that the inclusion effect of beta-cyclodextrin is reserved, and meanwhile, the performance and the structure are more stable.
The addition amount of the modified polyvinyl alcohol is 30wt% of the stable bioactive ingredient inclusion compound; the addition amount of the epichlorohydrin is 15wt% of the stable bioactive ingredient inclusion compound, and the dripping rate is 3ml/min; the addition amount of the graphene is 1.5wt% of the stable bioactive ingredient inclusion compound.
S5, emulsifying
Adding methyl silicone oil and an emulsifier into the polymer solution, stirring for 25min, emulsifying and dispersing at a stirring speed of 400r/min; heating to 65 ℃ in water bath, hermetically reacting for 4 hours, concentrating at 80 ℃ under reduced pressure after the reaction is finished, repeatedly washing for 4 times by using acetone and deionized water, and drying for 4 hours at 80 ℃ in vacuum to obtain the bioactive agent.
The mass ratio of the methyl silicone oil to the polymer solution is 5.5:1.3.
The addition amount of the emulsifier is 5wt% of the methyl silicone oil; the components of the emulsifier are sodium laurylsulfate and Tween 60, and the mass ratio of the sodium laurylsulfate to the Tween 60 is 1:5.
S6, blending
10 parts of a bioactive agent, 90 parts of chinlon slices, 0.5 part of tris (2, 4-di-tert-butylphenyl) phosphite ester and 0.6 part of EBS are added into a high-speed mixer for blending for 10 minutes to obtain a blend.
S7, granulating
The blend was fed into a twin screw extruder and the temperature of the various zones of the host set to: melting and granulating at 300 ℃, 295 ℃, 305 ℃, 310 ℃, 305 ℃ and 295 ℃ with the rotation speed of a host machine of 360rpm to obtain bioactive master batch.
S8, spinning
Placing the bioactive master batch and the nylon slices into a spinning machine for melt spinning to obtain fiber tows; and cooling, oiling, stretching and shaping the fiber tows to obtain the nylon large biological fibers.
The mass ratio of the bioactive master batch to the chinlon slices is 7:93.
The chinlon large biological fiber prepared in the embodiment 1 has lasting antibacterial effect, the antibacterial rate of staphylococcus aureus is 99.6 percent after 50 times of water washing, the antibacterial rate of candida albicans is 98.5 percent, and the antibacterial rate of escherichia coli is 99.7 percent; the breaking strength is 4.2cN/dtex, the breaking elongation is 51%, and the mechanical property is excellent; the loss rate of the bioactive component during the melt granulation process was 2.6%.
Comparative example 1
Representative example 1 was selected, the bioactive agent was removed, an equal proportion of the bioactive ingredient was directly added, and the rest was identical to example 1, as comparative example 1, since the bioactive ingredient was lost in a large amount by pyrolysis due to the high temperature environment of granulation, the loss rate was 80% or more, and the mechanical properties of the fiber were greatly lowered, the breaking strength was 2.1cN/dtex, and the elongation at break was 20%.
Comparative example 2
Representative example 1 is selected, modified polyvinyl alcohol is removed, equal proportion of polyvinyl alcohol is directly added in the step S4, the rest is the same as the example 1, as comparative example 2, the nylon fiber prepared in comparative example 2 has breaking strength of 3.2cN/dtex and elongation at break of 37 percent, the loss rate of bioactive components in the melting granulation process is 34 percent, the mechanical property is reduced compared with the example 1, the bioactive components are easier to lose, the thermal stability of the modified polyvinyl alcohol is better, and the modified polyvinyl alcohol is more resistant to high temperature and is not easy to decompose in a melting environment.
Comparative example 3
The representative example 1 is selected, the stabilizer is removed, the bioactive component inclusion compound is directly reacted with the modified polyvinyl alcohol, the rest is the same as the example 1, as comparative example 3, the loss rate of the bioactive component of the nylon fiber prepared in comparative example 3 is 2.7%, compared with the example 1, the fiber is basically unchanged, but the breaking strength of the fiber is 2.9cN/dtex, the breaking elongation is 30%, the mechanical property is greatly reduced, the addition of the stabilizer is proved to improve the dispersibility of the inclusion compound, and the phenomenon of agglomeration is avoided to influence the mechanical property of the fiber.
The proportions are mass proportions, and the percentages are mass percentages, unless otherwise specified; the raw materials are all commercially available.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, but 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 modifications may be made to the technical solutions described in the foregoing embodiments, or equivalents may be substituted for some of the technical features thereof. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the nylon large biological fiber containing the bioactive components is characterized by comprising the steps of inclusion, stabilization, preparation of modified polyvinyl alcohol, crosslinking, emulsification, blending, granulation and spinning.
2. The preparation method of the nylon macrobiological fiber containing the bioactive components, which is characterized in that the inclusion is carried out, the bioactive components are added into deionized water which is 10 to 15 times of the bioactive components, the mixture is stirred for 10 to 15 minutes, then beta-cyclodextrin is added, the ultrasonic treatment is carried out for 1 to 2 hours at 50 to 60 ℃, the ultrasonic frequency is 120 to 150KHz, the concentration is carried out at 80 to 90 ℃ under reduced pressure after the reaction is finished, the mixture is cooled to room temperature, and the mixture is placed into a cooling chamber to be separated out for crystallization, thus obtaining precipitate; washing the precipitate for 3-5 times, and drying in 70-80deg.C drying oven for 2-3 hr to obtain clathrate of bioactive components.
3. The preparation method of the nylon macrobiological fiber containing the bioactive components, as claimed in claim 1, wherein the stabilizing agent is added into the bioactive component inclusion compound, stirred for 20-25min, and freeze-dried by a freeze dryer to obtain the stabilized bioactive component inclusion compound.
4. The method for preparing nylon macrobiological fiber containing bioactive ingredient according to claim 3, wherein the stabilizer is added in an amount of 3-6wt% of the bioactive ingredient clathrate; the stabilizer comprises hydroxypropyl-beta-cyclodextrin, polyethylene glycol, mannitol and cationic starch, wherein the mass ratio of the hydroxypropyl-beta-cyclodextrin to the polyethylene glycol to the mannitol to the cationic starch is 5-8:10-12:1-3:0.5-1.
5. The preparation method of the nylon macrobiological fiber containing the bioactive components, as claimed in claim 1, is characterized in that the preparation of the modified polyvinyl alcohol comprises the steps of adding the polyvinyl alcohol into deionized water, stirring for 60-70min at 85-90 ℃ until the solution is uniform and stable, and obtaining a polyvinyl alcohol solution; adding 1-3mol/L hydrochloric acid to adjust pH to 4-5, adding modifier, performing ultrasonic treatment at 70-80deg.C for 40-50min, performing ultrasonic frequency of 220-260kHz, adding glutaraldehyde and lauroyl peroxide, stirring at 70-80deg.C for 30-40min, suction filtering, washing for 3-5 times, and drying to obtain modified polyvinyl alcohol.
6. The preparation method of the nylon macrobiological fiber containing the bioactive component as claimed in claim 5, wherein the mass fraction of the polyvinyl alcohol solution is 5-10%;
the modifier is acrylic acid, N-vinyl pyrrolidone, methyl methacrylate and ethylene glycol dimethacrylate, and the mass ratio of the acrylic acid to the N-vinyl pyrrolidone to the methyl methacrylate to the ethylene glycol dimethacrylate is 5-10:3-6:10-15:2-5; the addition amount of the modifier is 10-15wt% of the polyvinyl alcohol;
the addition amount of glutaraldehyde is 5-7wt% of polyvinyl alcohol, and the addition amount of lauroyl peroxide is 1-2wt% of glutaraldehyde.
7. The preparation method of the nylon macrobiological fiber containing the bioactive components, as claimed in claim 1, is characterized in that the crosslinking is carried out, the stable bioactive component inclusion compound is added into NaOH solution, and the mixture is stirred for 8-12min at 40-45 ℃ to obtain mixed solution;
adding modified polyvinyl alcohol into the mixed solution, adding graphene, stirring for 15-25min at 40-50 ℃, cooling to room temperature, adding epichlorohydrin dropwise, stirring for 60-80min, and stirring at a speed of 500-600r/min to obtain a polymer solution;
the addition amount of the modified polyvinyl alcohol is 20-30wt% of the stable bioactive ingredient inclusion compound; the addition amount of the epichlorohydrin is 10-15wt% of the stable bioactive ingredient inclusion compound, and the dripping rate is 1-3ml/min; the addition amount of the graphene is 0.5-1.5wt% of the stable bioactive ingredient inclusion compound.
8. The preparation method of the nylon macrobiological fiber containing the bioactive components, which is characterized in that the emulsifying is carried out, the methyl silicone oil and the emulsifying agent are added into the polymer solution for stirring for 18-25min for emulsification and dispersion, and the stirring speed is 300-400r/min; heating to 55-65deg.C in water bath, sealing, reacting for 3-4 hr, concentrating at 60-80deg.C under reduced pressure, repeatedly washing with acetone and deionized water for 3-4 times, and vacuum drying at 70-80deg.C for 2-4 hr to obtain bioactive agent;
the mass ratio of the methyl silicone oil to the polymer solution is 5-6:1-2;
the addition amount of the emulsifier is 4-6wt% of methyl silicone oil; the components of the emulsifier are sodium laurylsulfate and Tween 60, and the mass ratio of the sodium laurylsulfate to the Tween 60 is 1:5-6.
9. The preparation method of the nylon macrobiological fiber containing the bioactive component, according to the claim 1, is characterized in that 8-10 parts of the bioactive agent, 90-100 parts of nylon slices, 0.3-0.5 part of tris (2, 4-di-tert-butylphenyl) phosphite ester and 0.4-0.6 part of EBS are added into a high-speed mixer for 5-10min to obtain the blend.
10. The preparation method of the nylon large biological fiber containing the bioactive components, which is characterized in that the spinning is carried out by placing bioactive master batch and nylon slices into a spinning machine for melt spinning to obtain fiber tows; cooling, oiling, stretching and shaping fiber tows to obtain nylon large biological fibers;
the mass ratio of the bioactive master batch to the chinlon slices is 5-7:93-95.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310053690.6A CN116288787B (en) | 2023-02-03 | 2023-02-03 | Preparation method of chinlon large biological fiber containing bioactive components |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310053690.6A CN116288787B (en) | 2023-02-03 | 2023-02-03 | Preparation method of chinlon large biological fiber containing bioactive components |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116288787A true CN116288787A (en) | 2023-06-23 |
| CN116288787B CN116288787B (en) | 2024-06-14 |
Family
ID=86833152
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310053690.6A Active CN116288787B (en) | 2023-02-03 | 2023-02-03 | Preparation method of chinlon large biological fiber containing bioactive components |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116288787B (en) |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63314201A (en) * | 1987-06-17 | 1988-12-22 | Japan Organo Co Ltd | Method for immobilizing cyclodextrin |
| CN101402029A (en) * | 2008-10-21 | 2009-04-08 | 浙江大学 | Homogeneous crosslinking beta-cyclodextrin/wolfram carbine composite microsphere and method of producing the same |
| CN104357952A (en) * | 2014-11-21 | 2015-02-18 | 浙江和也健康科技有限公司 | Bamboo leaf flavonoid mint core-sheath compound fiber |
| US20150051168A1 (en) * | 2012-03-09 | 2015-02-19 | Dong-A St Co.,Ltd | Stable liquid pharmaceutical composition containing piroxicam or its pharmaceutically acceptable salt and hyaluronic acid or its pharmaceutically acceptable salt and the manufacturing method thereof |
| CN104475749A (en) * | 2014-09-04 | 2015-04-01 | 河南城建学院 | Preparation method of beta-cyclodextrin stabilized embedded nanoscale zero-valent iron |
| CN108796655A (en) * | 2018-07-02 | 2018-11-13 | 宁波蒙曼生物科技有限公司 | A kind of medical terylene of modification and preparation method thereof |
| CN112481730A (en) * | 2020-11-22 | 2021-03-12 | 张志明 | Flame-retardant antiviral antibacterial colored fiber and production method thereof |
| CN115028968A (en) * | 2022-05-30 | 2022-09-09 | 福建华峰新材料有限公司 | Antibacterial functional master batch, preparation method thereof, antibacterial polyester fiber and fabric |
| CN115181821A (en) * | 2022-07-12 | 2022-10-14 | 百草边大生物科技(青岛)有限公司 | Preparation method of antiviral cow leather containing tea active ingredients |
-
2023
- 2023-02-03 CN CN202310053690.6A patent/CN116288787B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63314201A (en) * | 1987-06-17 | 1988-12-22 | Japan Organo Co Ltd | Method for immobilizing cyclodextrin |
| CN101402029A (en) * | 2008-10-21 | 2009-04-08 | 浙江大学 | Homogeneous crosslinking beta-cyclodextrin/wolfram carbine composite microsphere and method of producing the same |
| US20150051168A1 (en) * | 2012-03-09 | 2015-02-19 | Dong-A St Co.,Ltd | Stable liquid pharmaceutical composition containing piroxicam or its pharmaceutically acceptable salt and hyaluronic acid or its pharmaceutically acceptable salt and the manufacturing method thereof |
| CN104475749A (en) * | 2014-09-04 | 2015-04-01 | 河南城建学院 | Preparation method of beta-cyclodextrin stabilized embedded nanoscale zero-valent iron |
| CN104357952A (en) * | 2014-11-21 | 2015-02-18 | 浙江和也健康科技有限公司 | Bamboo leaf flavonoid mint core-sheath compound fiber |
| CN108796655A (en) * | 2018-07-02 | 2018-11-13 | 宁波蒙曼生物科技有限公司 | A kind of medical terylene of modification and preparation method thereof |
| CN112481730A (en) * | 2020-11-22 | 2021-03-12 | 张志明 | Flame-retardant antiviral antibacterial colored fiber and production method thereof |
| CN115028968A (en) * | 2022-05-30 | 2022-09-09 | 福建华峰新材料有限公司 | Antibacterial functional master batch, preparation method thereof, antibacterial polyester fiber and fabric |
| CN115181821A (en) * | 2022-07-12 | 2022-10-14 | 百草边大生物科技(青岛)有限公司 | Preparation method of antiviral cow leather containing tea active ingredients |
Non-Patent Citations (2)
| Title |
|---|
| 常桂霞;: "香型锦纶的研制", 合成纤维, no. 09, 25 September 2007 (2007-09-25), pages 30 - 32 * |
| 李伟;杨丰宇;吴思雨;赵君霞;贺君钰;石军;尉震;: "β-环糊精修饰聚乙烯醇纳米纤维的制备及其吸附性质研究", 天津农学院学报, no. 04, 31 December 2013 (2013-12-31), pages 21 - 24 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116288787B (en) | 2024-06-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Kian et al. | A review on processing techniques of bast fibers nanocellulose and its polylactic acid (PLA) nanocomposites | |
| US11566348B2 (en) | Method of preparing plant-based functional polyester filament | |
| CN111155186B (en) | Graphene multifunctional viscose fiber and preparation method thereof | |
| CN106048892A (en) | Preparation method of GO/SA/PVA composite nanofiber membrane carrying nano silver particles | |
| CN105040142A (en) | Antibacterial polyester fibers and preparation method thereof | |
| CN113638069B (en) | Long-carbon-prepared composite modified nano platinum bamboo pulp fiber for mask base cloth and preparation method thereof | |
| CN108359229B (en) | Enhanced polylactic acid-based composite material and preparation method thereof | |
| CN111019288A (en) | Preparation method of ABS (acrylonitrile-butadiene-styrene) composite plastic product capable of reducing loss of plant extract | |
| CN109267168B (en) | Composite antibacterial polyester staple fiber and preparation method thereof | |
| CN112522802B (en) | Anti-ultraviolet antibacterial polypropylene filament and preparation method thereof | |
| CN116288787B (en) | Preparation method of chinlon large biological fiber containing bioactive components | |
| CN115262019A (en) | Manufacturing method of antibacterial anti-yellowing ZnO antimony-free polyester fiber | |
| CN1425704A (en) | Process for preparing antibiotic polyester | |
| CN112160155B (en) | Flame-retardant antibacterial fabric | |
| CN110760943A (en) | Preparation and application of fresh flower fiber filament for spinning | |
| CN106978642A (en) | The preparation method of sun-proof anti-bacterial fibre precursor | |
| CN112048797B (en) | Flame-retardant yarn and production process thereof | |
| CN110144650B (en) | Multifunctional pearl polylactic acid blended yarn and preparation method thereof | |
| CN115928237B (en) | Probiotic healthy fiber and preparation method thereof | |
| CN115058787B (en) | Preparation method of antibacterial and antiviral cool feeling fiber | |
| CN102345186A (en) | Novel soybean protein synthetic fiber and preparation method | |
| CN109537162B (en) | Preparation method of tough non-woven fabric for packaging | |
| CN112457570A (en) | Preparation method of halogen-free environment-friendly flame-retardant master batch for long glass fiber reinforced polypropylene composite material | |
| CN111088602A (en) | High-flexibility biodegradable non-woven fabric | |
| KR100454571B1 (en) | Polysaccharides fiber containing nano size metal particles and method of manufacturing 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 | ||
| GR01 | Patent grant |