CN114875521B - Preparation method of efficient antibacterial and antiviral fiber - Google Patents
Preparation method of efficient antibacterial and antiviral fiber Download PDFInfo
- Publication number
- CN114875521B CN114875521B CN202210625731.XA CN202210625731A CN114875521B CN 114875521 B CN114875521 B CN 114875521B CN 202210625731 A CN202210625731 A CN 202210625731A CN 114875521 B CN114875521 B CN 114875521B
- Authority
- CN
- China
- Prior art keywords
- antibacterial
- antiviral
- tio
- polyamide
- parts
- 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.)
- Active
Links
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 112
- 230000000840 anti-viral effect Effects 0.000 title claims abstract description 109
- 239000000835 fiber Substances 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229920002292 Nylon 6 Polymers 0.000 claims abstract description 87
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 82
- 239000002131 composite material Substances 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000009987 spinning Methods 0.000 claims abstract description 16
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 12
- 239000012792 core layer Substances 0.000 claims abstract description 10
- 239000010410 layer Substances 0.000 claims abstract description 10
- 239000010949 copper Substances 0.000 claims description 81
- 239000007864 aqueous solution Substances 0.000 claims description 39
- 229910052802 copper Inorganic materials 0.000 claims description 38
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 239000003242 anti bacterial agent Substances 0.000 claims description 30
- 239000008367 deionised water Substances 0.000 claims description 28
- 229910021641 deionized water Inorganic materials 0.000 claims description 28
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 claims description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 23
- 238000001035 drying Methods 0.000 claims description 21
- 239000002002 slurry Substances 0.000 claims description 20
- 150000001735 carboxylic acids Chemical class 0.000 claims description 18
- 241000222122 Candida albicans Species 0.000 claims description 14
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims description 14
- 241000588724 Escherichia coli Species 0.000 claims description 14
- 241000191967 Staphylococcus aureus Species 0.000 claims description 14
- 229940095731 candida albicans Drugs 0.000 claims description 14
- 229910001431 copper ion Inorganic materials 0.000 claims description 14
- 238000010992 reflux Methods 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 12
- 208000037797 influenza A Diseases 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 238000006068 polycondensation reaction Methods 0.000 claims description 9
- 238000007142 ring opening reaction Methods 0.000 claims description 9
- 239000004952 Polyamide Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 229920002647 polyamide Polymers 0.000 claims description 8
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 claims description 8
- 238000005119 centrifugation Methods 0.000 claims description 7
- 238000000605 extraction Methods 0.000 claims description 7
- 239000000047 product Substances 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- 239000006228 supernatant Substances 0.000 claims description 7
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 6
- 239000011668 ascorbic acid Substances 0.000 claims description 6
- 229960005070 ascorbic acid Drugs 0.000 claims description 6
- 235000010323 ascorbic acid Nutrition 0.000 claims description 6
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 6
- TYFQFVWCELRYAO-UHFFFAOYSA-N suberic acid Chemical compound OC(=O)CCCCCCC(O)=O TYFQFVWCELRYAO-UHFFFAOYSA-N 0.000 claims description 6
- 239000013049 sediment Substances 0.000 claims description 5
- 238000010345 tape casting Methods 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- 125000001931 aliphatic group Chemical group 0.000 claims description 4
- 239000003638 chemical reducing agent Substances 0.000 claims description 4
- 150000001879 copper Chemical class 0.000 claims description 4
- TVIDDXQYHWJXFK-UHFFFAOYSA-N dodecanedioic acid Chemical compound OC(=O)CCCCCCCCCCC(O)=O TVIDDXQYHWJXFK-UHFFFAOYSA-N 0.000 claims description 4
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 claims description 4
- WLJVNTCWHIRURA-UHFFFAOYSA-N pimelic acid Chemical compound OC(=O)CCCCCC(O)=O WLJVNTCWHIRURA-UHFFFAOYSA-N 0.000 claims description 4
- 239000001361 adipic acid Substances 0.000 claims description 3
- 235000011037 adipic acid Nutrition 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 3
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 3
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 2
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 2
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 2
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 2
- 239000012279 sodium borohydride Substances 0.000 claims description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 2
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 2
- DZLFLBLQUQXARW-UHFFFAOYSA-N tetrabutylammonium Chemical compound CCCC[N+](CCCC)(CCCC)CCCC DZLFLBLQUQXARW-UHFFFAOYSA-N 0.000 claims description 2
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 2
- 235000019441 ethanol Nutrition 0.000 claims 1
- 230000003115 biocidal effect Effects 0.000 abstract description 5
- 238000011065 in-situ storage Methods 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 5
- 230000006378 damage Effects 0.000 abstract description 3
- 238000011068 loading method Methods 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 230000009467 reduction Effects 0.000 abstract description 3
- 230000002155 anti-virotic effect Effects 0.000 abstract description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 abstract 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 9
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 6
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000012752 auxiliary agent Substances 0.000 description 5
- 238000009833 condensation Methods 0.000 description 5
- 230000005494 condensation Effects 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 238000001125 extrusion Methods 0.000 description 4
- 239000004744 fabric Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000003642 reactive oxygen metabolite Substances 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 206010069767 H1N1 influenza Diseases 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 241000712431 Influenza A virus Species 0.000 description 2
- 239000004594 Masterbatch (MB) Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- 239000003094 microcapsule Substances 0.000 description 2
- 125000000864 peroxy group Chemical group O(O*)* 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 201000010740 swine influenza Diseases 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- QFGCFKJIPBRJGM-UHFFFAOYSA-N 12-[(2-methylpropan-2-yl)oxy]-12-oxododecanoic acid Chemical compound CC(C)(C)OC(=O)CCCCCCCCCCC(O)=O QFGCFKJIPBRJGM-UHFFFAOYSA-N 0.000 description 1
- 206010059866 Drug resistance Diseases 0.000 description 1
- 241000784732 Lycaena phlaeas Species 0.000 description 1
- 230000010718 Oxidation Activity Effects 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 230000019522 cellular metabolic process Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002074 melt spinning Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000012815 thermoplastic material Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/12—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyamide as constituent
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
- D01D5/34—Core-skin structure; Spinnerette packs therefor
-
- 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)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Artificial Filaments (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to a preparation method of an efficient antibacterial and antiviral fiber, in particular to a preparation method of an antibacterial and antiviral polyamide 6 composite fiber prepared by loading nano Cu with TiO 2. The invention is characterized in that nano simple substance Cu is generated on the surface of TiO 2 by an in-situ reduction method, then TiO 2 carboxylic acid which is used for generating nano simple substance Cu on the surface is modified, polyamide 6 is introduced by in-situ polymerization to obtain the high-efficiency antibacterial and antiviral polyamide 6, and the antibacterial and antiviral polyamide 6 composite fiber is obtained by taking the antibacterial and antiviral polyamide 6 as a skin layer and taking the conventional polyamide 6 as a core layer and carrying out composite spinning. The polyamide 6 fiber prepared by the invention does not harm the environment in the use process, and has the characteristics of high efficiency, durability, antibiosis and antivirus.
Description
Technical Field
The invention belongs to the field of antibacterial and antiviral fiber synthesis, relates to a preparation method of antibacterial and antiviral polyamide 6 fibers, and in particular relates to a preparation method of antibacterial and antiviral polyamide 6 composite fibers with higher mechanical properties by loading nano copper with TiO 2.
Background
Polyamide 6 (PA 6) is a thermoplastic material which is generally white and semitransparent, has strong crystallinity, enables intermolecular hydrogen bonds to be formed by amide bonds on a molecular main chain, has strong intermolecular acting force, has higher mechanical strength, wear resistance and corrosion resistance, and is widely applied to the fields of textiles, industrial filaments, packaging industry and the like. The health risk caused by pathogenic bacteria brings a secondary serious test to people who cannot prevent sudden diseases, and if the antibacterial and antiviral functions of the PA6 can be improved, the comprehensive performance of the PA6 can be further improved, and the PA6 can be more applied to scenes needing antibacterial and antiviral.
The antibacterial modification of the PA6 is mainly realized by adding an antibacterial agent, and comprises the steps of fabric after-finishing and melt blending extrusion. The after-finishing of the fabric is a method for performing antibacterial modification by attaching an antibacterial agent to the formed fibers, and comprises the steps of dipping, smearing, spraying the antibacterial agent and the like, and the after-finishing method of the fabric is simple and convenient, has less loss and less influence by other fiber forming links, but has poor washing fastness of the fibers and is not environment-friendly. The blending extrusion is to disperse the antibacterial auxiliary agent into the PA6 by utilizing the shearing effect of the screw, and then obtain the PA6 antibacterial fiber through melt spinning, and the blending extrusion can intermittently produce master batch and continuously adjust the auxiliary agent dosage to carry out differential production, but the antibacterial agent is difficult to disperse the auxiliary agent uniformly only by the screw extrusion, and the auxiliary agent needs to be added to avoid agglomeration, poor spinnability and obvious decrease of the mechanical property of the fiber.
The antibacterial agents are mainly classified into organic and inorganic antibacterial agents. Organic antibacterial agents are primarily antibacterial by affecting the activity of biological proteins. The organic antibacterial agent has the advantages of wide and efficient sources, low cost and simple process, but the organic antibacterial agent has larger toxicity and poorer durability, and can cause microorganisms to generate drug resistance. The inorganic antibacterial agent is mainly divided into a metal ion antibacterial agent and a photocatalytic antibacterial agent. The metal ion antibacterial agent kills bacteria by breaking cell metabolism through dissolving out heavy metal ions, but the heavy metal ions can generate toxicity to human bodies after long-time dissolution and accumulation. The photocatalytic antibacterial agent generates hydroxyl free radicals and peroxy free radicals under the illumination condition, and the two free radicals have strong oxidation activity and can be combined with organic matters in microorganisms for sterilization.
The nano copper is a non-leaching antibacterial agent, and compared with the common copper antibacterial agent, the nano copper has the characteristics of large specific surface area, no toxicity and stability, and the nano copper particles directly react with water and oxygen in the air to generate active oxygen free radicals to play an antibacterial and antiviral role. The patent CN202110324666.2 is prepared by mixing and hybridizing graphene, nano copper, microporous silicon dioxide and nano microcapsules to obtain a composite antibacterial material of the nano copper microcapsules coated with the graphene, and then melting, mixing, extruding and granulating the material and polypropylene slices to obtain the nano copper antibacterial and antiviral master batch.
Because of the size, the nano copper is easy to agglomerate, the application of the nano copper in the aspect of fiber antibiosis is less in the prior art, the TiO 2 has better antibiosis performance, but the antibiosis performance can only be exerted under the condition of ultraviolet rays, the dispersibility in a polymer matrix is poor, and the method has important significance in developing the efficient antibiosis and antivirus fiber.
Disclosure of Invention
The invention aims to provide a preparation method of an efficient antibacterial and antiviral fiber, in particular to a preparation method for preparing an antibacterial and antiviral polyamide 6 fiber by loading nano copper with TiO 2. According to the invention, firstly, nano simple substance copper (Cu-TiO 2) with the size of 2-10nm is generated on the surface of TiO 2 by an in-situ reduction method, then Cu is loaded with TiO 2 carboxylic acid to be modified to obtain carboxylic acid modified Cu-TiO 2(CM-Cu-TiO2, CM-Cu-TiO 2 is introduced in situ in the synthesis process of polyamide 6 to obtain antibacterial and antiviral polyamide 6, and finally, the antibacterial and antiviral polyamide 6 composite fiber is obtained by taking the antibacterial and antiviral polyamide 6 as a skin layer and the conventional polyamide 6 as a core layer through composite spinning.
The nano simple substance copper obtained by the method has the size of 2-10nm, the nano simple substance copper with the size has higher catalytic reaction antibacterial and antiviral activity, the nano copper can activate oxygen in water and air to generate Reactive Oxygen Species (ROS), and the ROS (hydroxyl radicals, superoxide radicals and hydrogen peroxide) have strong oxidizing property, can directly or indirectly damage the structure and function of cells, and lead to cell membrane rupture to cause bacterial death. Furthermore, the CM-Cu-TiO 2 obtained by modifying carboxylic acid has better compatibility with polyamide 6, can be uniformly and stably dispersed in polyamide 6 melt in-situ polymerization of polyamide monomers, avoids the problem of agglomeration of nano-scale Cu-loaded TiO 2, can be better complexed with nano-copper to maintain the nano-copper of Cu-TiO 2 in a reduction state all the time, continuously releases active oxygen free radicals to play a role in resisting bacteria and viruses, and the complexed carboxyl can promote the nano-copper to generate the active oxygen free radicals, so that the antibacterial and antiviral effects are further improved. Besides, the nano copper can make up the defect that titanium dioxide is difficult to play an antibacterial role when not irradiated by ultraviolet light, and plays a role in cooperating with efficient antibacterial and antiviral effects. The invention adopts the skin-core structure to spin, the high-efficiency antibacterial and antiviral polyamide 6 component of the skin layer plays an antibacterial and antiviral role, and the conventional polyamide 6 component of the core layer plays a role of supporting mechanical properties. Therefore, the fiber obtained by the invention has high-efficiency durable antibacterial and antiviral effects, has higher mechanical properties, and can be used in the field with higher requirements on the antibacterial and antiviral properties of the fiber.
The invention relates to a preparation method of efficient antibacterial and antiviral fibers, which comprises the following specific steps:
(1) According to the mass portion, 2 to 5 portions of nano titanium dioxide are dispersed in 50 portions of deionized water under certain conditions in an ultrasonic manner to prepare a TiO 2 aqueous solution, and 0.2 to 1.0 portion of copper salt is dissolved in 50 portions of deionized water to prepare a copper ion aqueous solution. Mixing TiO 2 aqueous solution and copper ion aqueous solution in a flask, condensing and refluxing, stirring, adding 50 parts of reducer aqueous solution dropwise into the flask, and stirring at 60-90 ℃ for 3-24 h to obtain dark solution. And centrifugally separating the obtained product by deionized water and absolute ethyl alcohol, and finally drying to obtain the nano TiO 2 -loaded nano copper composite antibacterial agent. The size of the generated nano elemental copper is 2-10nm;
(2) Adding 100 parts of absolute ethyl alcohol into 1-3 parts of aliphatic dibasic acid, 15-20 parts of nano TiO 2 loaded nano copper composite antibacterial agent (TiO 2 -Cu) and 0.5-2 parts of caprolactam, condensing, refluxing and stirring for 0.5-5 hours to obtain carboxylic acid modified nano TiO 2 loaded nano copper composite antibacterial agent slurry (CM-TiO 2 -Cu slurry), then putting the modified CM-TiO 2 -Cu slurry into a centrifuge tube for centrifugation, removing sediment obtained by supernatant, washing for 3-5 times by using ethyl alcohol and water, and drying to obtain carboxylic acid modified CM-TiO 2-Cu(CM-TiO2 -Cu.
(3) Adding 1-3 parts by mass of CM-TiO 2 -Cu, 100 parts by mass of caprolactam and 2-5 parts by mass of deionized water into a polymerization reaction kettle, carrying out ring-opening prepolymerization, carrying out polycondensation, and finally carrying out tape casting, granulating and extraction to obtain the composite antibacterial and antiviral polyamide 6 slice.
(4) And drying the high-efficiency antibacterial and antiviral polyamide 6 slices and the conventional polyamide 6 slices at 90-120 ℃ for 24-36 hours, taking the antibacterial and antiviral polyamide 6 as a skin layer and the conventional polyamide 6 as a core layer, and adding the antibacterial and antiviral polyamide 6 and the conventional polyamide into a composite spinning machine according to a certain proportion for spinning to obtain the high-efficiency antibacterial and antiviral polyamide 6 composite fiber.
In the step (1), the certain condition of ultrasonic dispersion of TiO 2 under certain conditions means that the time is 20-60 min and the ultrasonic frequency is 30-60 kHz;
in the step (1), the copper salt refers to one of copper chloride, copper sulfate and copper nitrate;
In the step (1), the aqueous solution of the reducing agent is one of 0.1-0.5 mol/L of aqueous solution of citric acid, hydrazine hydrate, sodium borohydride, ascorbic acid, sodium hypophosphite and tetrabutylammonium borohydride;
In the step (2), the aliphatic dibasic acid refers to one of adipic acid, pimelic acid, suberic acid, azelaic acid, sebacic acid and dodecanedioic acid;
in the step (3), the reaction condition of ring-opening pre-polymerization is that the temperature is 200-260 ℃, the pressure is 0.1-1.0 MPa, and the time is 2-5 h;
In the step (3), the polycondensation reaction condition is that the temperature is 240-260 ℃, the pressure is-0.02-0.10 MPa, and the time is 2-5 h;
In the step (4), the antibacterial and antiviral polyamide 6 and the conventional polyamide are in a mass ratio of (1-3): 2.
According to the preparation method of the efficient antibacterial and antiviral fiber, in the step (4), the breaking strength of the antibacterial and antiviral polyamide 6 composite fiber is 3.0-4.5 cN/dtex, the breaking elongation is 15-30%, the antibacterial and antiviral effects on staphylococcus aureus, escherichia coli, candida albicans and H1N1 influenza A virus are more than 99%, and after the fiber is washed for 50 times, the antibacterial and antiviral effects on staphylococcus aureus, escherichia coli, candida albicans and H1N1 influenza A virus are still more than 97%, so that the antibacterial and antiviral fiber has good water-washing resistance and efficient antibacterial and antiviral properties.
The invention has the beneficial effects that:
(1) Safety: the invention is a non-dissolution type antibacterial and antiviral auxiliary agent, which does not harm human body and environment, and is safer and more environment-friendly;
(2) Stability: the nano copper is always in a reduced state, and continuously releases peroxy free radicals, so that the nano copper has lasting antibacterial and antiviral effects;
(3) High-efficiency antibacterial: the nano copper can still play an antibacterial and antiviral effect when no ultraviolet radiation is generated, and the nano copper is combined with TiO 2 to realize higher antibacterial and antiviral effects;
(4) High strength: the antibacterial and antiviral polyamide 6 composite fiber has better spinnability and higher mechanical property.
Detailed Description
The application is further described below in conjunction with the detailed description. It is to be understood that these examples are illustrative of the present application and are not intended to limit the scope of the present application. Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the teachings of the present application, and such equivalents are intended to fall within the scope of the application as defined in the appended claims.
Example 1, a preparation method of a high-efficiency antibacterial and antiviral fiber comprises the following specific steps:
(1) According to the parts by mass, 2 parts of nano titanium dioxide is ultrasonically dispersed in 50 parts of deionized water at the frequency of 60kHz for 20min to prepare a TiO 2 aqueous solution, and 0.2 part of anhydrous copper sulfate is dissolved in 50 parts of deionized water to prepare a copper ion aqueous solution. The aqueous solution of TiO 2 and the aqueous solution of copper ions were mixed in a flask and then subjected to condensation reflux at 80℃and then stirred while 50 parts of 0.1mol/L aqueous solution of citric acid were added dropwise to the flask and stirred at 60℃for 3 hours to obtain a dark solution. And (3) centrifugally separating the obtained product by deionized water and absolute ethyl alcohol, and finally drying to obtain the nano TiO 2 -loaded nano copper composite antibacterial agent (TiO 2 -Cu).
(2) Adding 100 parts of absolute ethyl alcohol into 1 part of adipic acid, 15 parts of TiO 2 -Cu and 0.5 part of caprolactam, condensing and refluxing at 80 ℃, stirring for 0.5h to obtain carboxylic acid modified nano TiO 2 loaded nano copper composite antibacterial agent slurry (CM-TiO 2 -Cu slurry), then putting the CM-TiO 2 -Cu slurry into a centrifuge tube for centrifugation, removing a precipitate obtained by supernatant, washing with ethyl alcohol and water for 3 times, and drying to obtain carboxylic acid modified TiO 2-Cu(CM-TiO2 -Cu.
(3) Adding 1 part of CM-TiO 2 -Cu, 100 parts of caprolactam and 2 parts of deionized water into a polymerization reaction kettle, firstly carrying out ring-opening prepolymerization at 200 ℃ and 0.1Mpa for 2 hours, then carrying out polycondensation at 240 ℃ and 0.02Mpa for 2 hours, and finally carrying out belt casting, granulating and extraction to obtain the high-efficiency antibacterial and antiviral polyamide 6 slice.
(4) And drying the high-efficiency antibacterial and antiviral polyamide 6 slices and the conventional polyamide 6 slices at 100 ℃ for 24 hours, taking the antibacterial and antiviral polyamide 6 as a skin layer and the conventional polyamide 6 as a core layer, and adding the antibacterial and antiviral polyamide 6 and the conventional polyamide 6 into a composite spinning machine according to the mass ratio of 1:2 for spinning to obtain the high-efficiency antibacterial and antiviral polyamide 6 composite fiber.
The breaking strength of the high-efficiency antiviral polyamide 6 fiber prepared by the invention is 4.5cN/dtex, the breaking elongation is 30%, the antibacterial and antiviral effects on staphylococcus aureus, escherichia coli, candida albicans and influenza A H1N1 virus are up to 99.1%, and after the fiber is washed for 50 times, the antibacterial and antiviral effects on staphylococcus aureus, escherichia coli, candida albicans and influenza A H1N1 virus are still up to more than 97%, so that the fiber has better water-washing resistance and high-efficiency antibacterial and antiviral properties.
Example 2, a preparation method of a high-efficiency antibacterial and antiviral fiber, comprises the following specific steps:
(1) According to the parts by mass, 5 parts of nano titanium dioxide is ultrasonically dispersed in 50 parts of deionized water at the frequency of 30kHz for 60min to prepare a TiO 2 aqueous solution, and 1 part of copper chloride is dissolved in 50 parts of deionized water to prepare a copper ion aqueous solution. The aqueous solution of TiO 2 and the aqueous solution of copper ions were mixed in a flask and then subjected to condensation reflux at 80℃and then stirred while 50 parts of 0.5mol/L aqueous solution of ascorbic acid was added dropwise to the flask and stirred at 90℃for 24 hours to obtain a dark solution. And (3) centrifugally separating the obtained product by deionized water and absolute ethyl alcohol, and finally drying to obtain the nano TiO 2 -loaded nano copper composite antibacterial agent (TiO 2 -Cu).
(2) Adding 100 parts of absolute ethyl alcohol into 3 parts of suberic acid, 20 parts of TiO 2 -Cu and 2 parts of caprolactam, condensing and refluxing at 80 ℃ and stirring for 5 hours to obtain carboxylic acid modified nano TiO 2 loaded nano copper composite antibacterial agent slurry (CM-TiO 2 -Cu slurry), then putting the CM-TiO 2 -Cu slurry into a centrifuge tube for centrifugation, removing sediment obtained by supernatant, washing with ethyl alcohol and water for 5 times, and drying to obtain carboxylic acid modified TiO 2-Cu(CM-TiO2 -Cu.
(3) Adding 3 parts of CM-TiO 2 -Cu, 100 parts of caprolactam and 5 parts of deionized water into a polymerization reaction kettle, carrying out ring-opening prepolymerization at 260 ℃ and 1.0Mpa for 5 hours, carrying out polycondensation at 260 ℃ and-0.10 MPa for 5 hours, and finally carrying out tape casting, granulating and extraction to obtain the high-efficiency antibacterial and antiviral polyamide 6 slice.
(4) And drying the high-efficiency antibacterial and antiviral polyamide 6 slices and the conventional polyamide 6 slices at 100 ℃ for 36 hours, taking the antibacterial and antiviral polyamide 6 as a skin layer and the conventional polyamide 6 as a core layer, and adding the antibacterial and antiviral polyamide 6 and the conventional polyamide 6 into a composite spinning machine according to the mass ratio of 3:2 for spinning to obtain the high-efficiency antibacterial and antiviral polyamide 6 composite fiber.
The breaking strength of the high-efficiency antiviral polyamide 6 fiber prepared by the invention is 3.0cN/dtex, the breaking elongation is 27%, the antibacterial and antiviral effects on staphylococcus aureus, escherichia coli, candida albicans and influenza A H1N1 virus reach 99.9%, and after the fiber is washed for 50 times, the antibacterial and antiviral effects on staphylococcus aureus, escherichia coli, candida albicans and influenza A H1N1 virus still reach more than 97%, so that the fiber has better water-washing resistance and high-efficiency antibacterial and antiviral properties.
Example 3, a preparation method of a high-efficiency antibacterial and antiviral fiber, comprises the following specific steps:
(1) According to the parts by mass, 3 parts of nano titanium dioxide is ultrasonically dispersed in 50 parts of deionized water at the frequency of 40kHz for 40min to prepare a TiO 2 aqueous solution, and 0.5 part of copper chloride is dissolved in 50 parts of deionized water to prepare a copper ion aqueous solution. The aqueous solution of TiO 2 and the aqueous solution of copper ions were mixed in a flask and then subjected to condensation reflux at 80℃and then stirred while 50 parts of 0.3mol/L aqueous solution of ascorbic acid was added dropwise to the flask and stirred at 70℃for 20 hours to obtain a dark solution. And (3) centrifugally separating the obtained product by deionized water and absolute ethyl alcohol, and finally drying to obtain the nano TiO 2 -loaded nano copper composite antibacterial agent (TiO 2 -Cu).
(2) Adding 100 parts of absolute ethyl alcohol into 2 parts of dodecanedioic acid, 15 parts of TiO 2 -Cu and 1 part of caprolactam, condensing and refluxing at 80 ℃ and stirring for 2 hours to obtain carboxylic acid modified nano TiO 2 loaded nano copper composite antibacterial agent slurry (CM-TiO 2 -Cu slurry), then putting the CM-TiO 2 -Cu slurry into a centrifuge tube for centrifugation, removing a precipitate obtained by supernatant, washing with ethyl alcohol and water for 5 times, and drying to obtain carboxylic acid modified TiO 2-Cu(CM-TiO2 -Cu.
(3) 2 Parts of CM-TiO 2 -Cu, 100 parts of caprolactam and 3 parts of deionized water are added into a polymerization reaction kettle, ring-opening pre-polymerization is carried out for 4 hours at 230 ℃ and 0.6Mpa, polycondensation is carried out for 4 hours at 250 ℃ and 0.05Mpa, and finally high-efficiency antibacterial and antiviral polyamide 6 slices are obtained through belt casting, granulating and extraction.
(4) And drying the high-efficiency antibacterial and antiviral polyamide 6 slices and the conventional polyamide 6 slices at 110 ℃ for 36 hours, taking the antibacterial and antiviral polyamide 6 as a skin layer and the conventional polyamide 6 as a core layer, and adding the antibacterial and antiviral polyamide 6 and the conventional polyamide into a composite spinning machine according to the mass ratio of 1:1 for spinning to obtain the high-efficiency antibacterial and antiviral polyamide 6 composite fiber.
The breaking strength of the high-efficiency antiviral polyamide 6 fiber prepared by the invention is 4.0cN/dtex, the breaking elongation is 15%, the antibacterial and antiviral effects on staphylococcus aureus, escherichia coli, candida albicans and influenza A H1N1 virus are 99.5%, and after the fiber is washed for 50 times, the antibacterial and antiviral effects on staphylococcus aureus, escherichia coli, candida albicans and influenza A H1N1 virus are still more than 97%, so that the fiber has good water-washing resistance and high-efficiency antibacterial and antiviral properties.
Example 4, a method for preparing a high-efficiency antibacterial and antiviral fiber, comprises the following specific steps:
(1) According to the parts by mass, 4 parts of nano titanium dioxide is ultrasonically dispersed in 50 parts of deionized water at the frequency of 30kHz for 50min to prepare a TiO 2 aqueous solution, and 0.7 part of copper chloride is dissolved in 50 parts of deionized water to prepare a copper ion aqueous solution. The aqueous solution of TiO 2 and the aqueous solution of copper ions were mixed in a flask and then subjected to condensation reflux at 80℃and then stirred while 50 parts of 0.4mol/L aqueous solution of ascorbic acid was added dropwise to the flask and stirred at 80℃for 20 hours to obtain a dark solution. And (3) centrifugally separating the obtained product by deionized water and absolute ethyl alcohol, and finally drying to obtain the nano TiO 2 -loaded nano copper composite antibacterial agent (TiO 2 -Cu).
(2) Adding 100 parts of absolute ethyl alcohol into 3 parts of sebacic acid, 16 parts of TiO 2 -Cu and 2 parts of caprolactam, condensing and refluxing at 80 ℃ and stirring for 3 hours to obtain carboxylic acid modified nano TiO 2 loaded nano copper composite antibacterial agent slurry (CM-TiO 2 -Cu slurry), then putting the CM-TiO 2 -Cu slurry into a centrifuge tube for centrifugation, removing sediment obtained by supernatant, washing with ethyl alcohol and water for 5 times, and drying to obtain carboxylic acid modified TiO 2-Cu(CM-TiO2 -Cu.
(3) Adding 3 parts of CM-TiO 2 -Cu, 100 parts of caprolactam and 4 parts of deionized water into a polymerization reaction kettle, firstly carrying out ring-opening prepolymerization at 250 ℃ and 0.5Mpa for 4 hours, then carrying out polycondensation at 240 ℃ and 0.06Mpa for 3 hours, and finally carrying out tape casting, granulating and extraction to obtain the high-efficiency antibacterial and antiviral polyamide 6 slice.
(4) And drying the high-efficiency antibacterial and antiviral polyamide 6 slices and the conventional polyamide 6 slices at 120 ℃ for 24 hours, taking the antibacterial and antiviral polyamide 6 as a skin layer and the conventional polyamide 6 as a core layer, and adding the antibacterial and antiviral polyamide 6 and the conventional polyamide into a composite spinning machine according to the mass ratio of 1:2 for spinning to obtain the high-efficiency antibacterial and antiviral polyamide 6 composite fiber.
The breaking strength of the high-efficiency antiviral polyamide 6 fiber prepared by the invention is 3.5cN/dtex, the breaking elongation is 18%, the antibacterial and antiviral effects on staphylococcus aureus, escherichia coli, candida albicans and influenza A H1N1 virus reach 99.9%, and after the fiber is washed for 50 times, the antibacterial and antiviral effects on staphylococcus aureus, escherichia coli, candida albicans and influenza A H1N1 virus still reach more than 97%, so that the fiber has better water-washing resistance and high-efficiency antibacterial and antiviral properties.
Example 5, a method for preparing a high-efficiency antibacterial and antiviral fiber, comprises the following specific steps:
(1) According to the parts by mass, 3 parts of nano titanium dioxide is ultrasonically dispersed in 50 parts of deionized water at 50kHz for 30min to prepare a TiO 2 aqueous solution, and 0.6 part of copper chloride is dissolved in 50 parts of deionized water to prepare a copper ion aqueous solution. The aqueous solution of TiO 2 and the aqueous solution of copper ions were mixed in a flask and then subjected to condensation reflux at 80℃and then stirred while 50 parts of 0.3mol/L aqueous solution of ascorbic acid was added dropwise to the flask and stirred at 80℃for 22 hours to obtain a dark solution. And (3) centrifugally separating the obtained product by deionized water and absolute ethyl alcohol, and finally drying to obtain the nano TiO 2 -loaded nano copper composite antibacterial agent (TiO 2 -Cu).
(2) Adding 100 parts of absolute ethyl alcohol into 3 parts of sebacic acid, 16 parts of TiO 2 -Cu and 0.5 part of caprolactam, condensing and refluxing at 80 ℃ and stirring for 3 hours to obtain carboxylic acid modified nano TiO 2 loaded nano copper composite antibacterial agent slurry (CM-TiO 2 -Cu slurry), then putting the CM-TiO 2 -Cu slurry into a centrifuge tube for centrifugation, removing sediment obtained by supernatant, washing with ethyl alcohol and water for 5 times, and drying to obtain carboxylic acid modified TiO 2-Cu(CM-TiO2 -Cu.
(3) Adding 1 part of CM-TiO 2 -Cu, 100 parts of caprolactam and 2 parts of deionized water into a polymerization reaction kettle, firstly carrying out ring-opening prepolymerization at 240 ℃ and 0.8Mpa for 5 hours, then carrying out polycondensation at 250 ℃ and-0.09 Mpa for 2 hours, and finally carrying out tape casting, granulating and extraction to obtain the high-efficiency antibacterial and antiviral polyamide 6 slice.
(4) And drying the high-efficiency antibacterial and antiviral polyamide 6 slices and the conventional polyamide 6 slices at 90 ℃ for 36 hours, taking the antibacterial and antiviral polyamide 6 as a skin layer and the conventional polyamide 6 as a core layer, and adding the antibacterial and antiviral polyamide 6 and the conventional polyamide into a composite spinning machine according to the mass ratio of 1:1 for spinning to obtain the high-efficiency antibacterial and antiviral polyamide 6 composite fiber.
The breaking strength of the high-efficiency antiviral polyamide 6 fiber prepared by the invention is 4.5cN/dtex, the breaking elongation is 18%, the antibacterial and antiviral effects on staphylococcus aureus, escherichia coli, candida albicans and influenza A H1N1 virus are 99.2%, and after the fiber is washed for 50 times, the antibacterial and antiviral effects on staphylococcus aureus, escherichia coli, candida albicans and influenza A H1N1 virus are still more than 97%, so that the fiber has good water-washing resistance and high-efficiency antibacterial and antiviral properties.
Claims (6)
1. A method for preparing an efficient antibacterial and antiviral fiber, which is characterized by comprising the following steps:
(1) According to the mass parts, 2-5 parts of TiO 2 are ultrasonically dispersed in 50 parts of deionized water under certain conditions to prepare a TiO 2 aqueous solution, and 0.2-1.0 part of copper salt is dissolved in 50 parts of deionized water to prepare a copper ion aqueous solution; mixing the TiO 2 aqueous solution and the copper ion aqueous solution in a flask, condensing and refluxing after mixing, then stirring, adding 50 parts of reducing agent aqueous solution dropwise into the flask at the same time, and stirring at 60-90 ℃ for 3-24 hours to obtain a dark solution; centrifugally separating the obtained product by deionized water and absolute ethyl alcohol, and finally drying to obtain Cu-TiO 2, wherein Cu-TiO 2 is a TiO 2 efficient antibacterial agent with nano elemental copper generated on the surface, and the size of the generated nano elemental copper is 2-10nm;
(2) Adding 100 parts of absolute ethyl alcohol into 1-3 parts of aliphatic dibasic acid, 15-20 parts of Cu-TiO 2 and 0.5-2 parts of caprolactam, condensing, refluxing and stirring for 0.5-5 hours to obtain carboxylic acid modified Cu-TiO 2 slurry, then placing the CM-Cu-TiO 2 slurry into a centrifuge tube for centrifugation, removing sediment obtained by supernatant, washing with ethanol and water for 3-5 times, and drying to obtain carboxylic acid modified Cu-TiO 2;
(3) Adding 1-3 parts of carboxylic acid modified Cu-TiO 2, 100 parts of caprolactam and 2-5 parts of deionized water into a polymerization reaction kettle, carrying out ring opening prepolymerization, then carrying out polycondensation, and finally carrying out tape casting, granulating and extraction to obtain high-efficiency antibacterial and antiviral polyamide 6 slices;
(4) And drying the high-efficiency antibacterial and antiviral polyamide 6 slices and the conventional polyamide 6 slices at 90-120 ℃ for 24-36 hours, taking the antibacterial and antiviral polyamide 6 as a skin layer and the conventional polyamide 6 as a core layer, adding the antibacterial and antiviral polyamide 6 and the conventional polyamide into a composite spinning machine according to a proportion for spinning, and then drawing to obtain the high-efficiency antibacterial and antiviral polyamide 6 composite fiber.
2. The method for preparing the efficient antibacterial and antiviral fiber according to claim 1, wherein in the step (1), the certain condition of ultrasonic dispersion of TiO 2 under certain conditions means that the time is 20-60 min and the ultrasonic frequency is 30-60 kHz; the copper salt refers to one of copper chloride, copper sulfate and copper nitrate; the aqueous solution of the reducing agent is one of 0.1-0.5 mol/L of aqueous solution of citric acid, hydrazine hydrate, sodium borohydride, ascorbic acid, sodium hypophosphite and tetrabutylammonium borohydride.
3. The method for preparing high-efficiency antibacterial and antiviral fibers according to claim 1, wherein in the step (2), the aliphatic dibasic acid is one of adipic acid, pimelic acid, suberic acid, azelaic acid, sebacic acid and dodecanedioic acid.
4. The method for preparing the efficient antibacterial and antiviral fiber according to claim 1, wherein in the step (3), the reaction condition of ring-opening pre-polymerization is that the temperature is 200-260 ℃, the pressure is 0.1-1.0 MPa, and the time is 2-5 h; the reaction condition of polycondensation is that the temperature is 240-260 ℃, the pressure is-0.02 to-0.10 MPa, and the time is 2-5 h.
5. The method for preparing the efficient antibacterial and antiviral fiber according to claim 1, wherein in the step (4), the mass ratio of the antibacterial and antiviral polyamide 6 to the conventional polyamide is (1-3): 2.
6. The preparation method of the efficient antibacterial and antiviral fiber according to claim 1, wherein the breaking strength of the antibacterial and antiviral polyamide 6 fiber is 3.0-4.5 cN/dtex, the elongation at break is 15-30%, the antibacterial and antiviral effects on staphylococcus aureus, escherichia coli, candida albicans and influenza A H1N1 viruses are more than 99%, and the antibacterial and antiviral effects on staphylococcus aureus, escherichia coli, candida albicans and influenza A H1N1 viruses are still more than 97% after the fiber is washed for 50 times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210625731.XA CN114875521B (en) | 2022-06-02 | 2022-06-02 | Preparation method of efficient antibacterial and antiviral fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210625731.XA CN114875521B (en) | 2022-06-02 | 2022-06-02 | Preparation method of efficient antibacterial and antiviral fiber |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114875521A CN114875521A (en) | 2022-08-09 |
| CN114875521B true CN114875521B (en) | 2024-05-28 |
Family
ID=82679589
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210625731.XA Active CN114875521B (en) | 2022-06-02 | 2022-06-02 | Preparation method of efficient antibacterial and antiviral fiber |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114875521B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115323522B (en) * | 2022-09-20 | 2023-08-18 | 江苏集萃先进纤维材料研究所有限公司 | Antibacterial polyamide fiber and preparation method thereof |
| CN117107388B (en) * | 2023-09-27 | 2024-03-26 | 东莞信鸿工程塑料有限公司 | Antibacterial flame-retardant polyamide fiber material and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001064981A1 (en) * | 2000-02-28 | 2001-09-07 | Unitika Fibers Ltd. | Antibacterial polyamide fiber and method for producing the same |
| CN103388191A (en) * | 2013-07-05 | 2013-11-13 | 江苏中杰澳新材料有限公司 | Skin-core type polyamide antibacterial fiber and preparation method thereof |
| CN105332083A (en) * | 2015-12-01 | 2016-02-17 | 东华大学 | Preparation method for nano copper oxide-loaded mesoporous zirconium phosphate antibacterial polyamide fiber |
| CN109762162A (en) * | 2018-12-25 | 2019-05-17 | 中国纺织科学研究院有限公司 | Functionality polyamide and its continuous producing method |
| CN111184026A (en) * | 2020-03-05 | 2020-05-22 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of nano-copper/bismuth vanadate composite antibacterial agent |
-
2022
- 2022-06-02 CN CN202210625731.XA patent/CN114875521B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001064981A1 (en) * | 2000-02-28 | 2001-09-07 | Unitika Fibers Ltd. | Antibacterial polyamide fiber and method for producing the same |
| CN103388191A (en) * | 2013-07-05 | 2013-11-13 | 江苏中杰澳新材料有限公司 | Skin-core type polyamide antibacterial fiber and preparation method thereof |
| CN105332083A (en) * | 2015-12-01 | 2016-02-17 | 东华大学 | Preparation method for nano copper oxide-loaded mesoporous zirconium phosphate antibacterial polyamide fiber |
| CN109762162A (en) * | 2018-12-25 | 2019-05-17 | 中国纺织科学研究院有限公司 | Functionality polyamide and its continuous producing method |
| CN111184026A (en) * | 2020-03-05 | 2020-05-22 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of nano-copper/bismuth vanadate composite antibacterial agent |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114875521A (en) | 2022-08-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN114875521B (en) | Preparation method of efficient antibacterial and antiviral fiber | |
| Yue et al. | Highly recyclable and super-tough hydrogel mediated by dual-functional TiO2 nanoparticles toward efficient photodegradation of organic water pollutants | |
| CN115044073A (en) | Preparation method and application of nano-copper master batch with antibacterial and antiviral functions | |
| CN103588886B (en) | A kind of Easily-water dispersible nanocrystalline cellulose and preparation method thereof | |
| WO2017036221A1 (en) | Preparation and use of silver-modified spiral titanium dioxide nanofibre photocatalyst | |
| CN103361885A (en) | Preparation method of antibacterial silk fibroin fibrous membrane | |
| CN101993527A (en) | Preparation method and application of silver-containing PET based composite resin material | |
| CN112472818B (en) | Nano material using modified natural melanin as carrier, and preparation method and application thereof | |
| CN107385562A (en) | A kind of alginic acid/Nano Silver composite nano fiber and preparation method thereof | |
| CN114989577B (en) | Preparation method and application of antibacterial and antiviral master batch | |
| CN102190825A (en) | Preparation methods for antibacterial plastic master batches and product | |
| CN112795098A (en) | Antibacterial plastic and preparation method thereof | |
| CN114875513B (en) | Preparation method of nano-copper antibacterial antiviral black fiber | |
| CN103835025A (en) | Preparation method of permanently-antibacterial poly guanidine alginate fibers | |
| CN107698754A (en) | A kind of preparation method of graphene oxide modified polyamide 6 | |
| Yang et al. | Nanofibrous materials | |
| CN115058787B (en) | Preparation method of antibacterial and antiviral cool feeling fiber | |
| CN111995799B (en) | Preparation method of nano-silver/cellulose composite antibacterial material | |
| CN110871099A (en) | Ag-containing material3PO4And carboxylated g-C3N4Preparation method of photocatalytic degradation nano-fiber | |
| CN112226848A (en) | Chitosan-graphene oxide composite fiber and preparation method and application thereof | |
| CN112143025A (en) | Compound antibacterial agent and preparation method and application thereof | |
| CN117626472A (en) | Preparation method of efficient antibacterial antiviral colored fiber | |
| CN114892300B (en) | Preparation method of antibacterial antiviral thermal fiber | |
| CN116446066A (en) | Preparation method of synergistic antibacterial antiviral deodorizing fiber | |
| CN116479544A (en) | Preparation method of efficient antibacterial and antiviral functional fiber |
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 | ||
| GR01 | Patent grant |