CN114892300A - Preparation method of antibacterial antiviral thermal fiber - Google Patents
Preparation method of antibacterial antiviral thermal fiber Download PDFInfo
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- CN114892300A CN114892300A CN202210625721.6A CN202210625721A CN114892300A CN 114892300 A CN114892300 A CN 114892300A CN 202210625721 A CN202210625721 A CN 202210625721A CN 114892300 A CN114892300 A CN 114892300A
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- antibacterial
- antiviral
- parts
- coffee carbon
- warm
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- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 117
- 230000000840 anti-viral effect Effects 0.000 title claims abstract description 97
- 239000000835 fiber Substances 0.000 title claims abstract description 75
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 86
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 83
- 229920002292 Nylon 6 Polymers 0.000 claims abstract description 49
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000010949 copper Substances 0.000 claims abstract description 29
- 229910052802 copper Inorganic materials 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000002074 melt spinning Methods 0.000 claims abstract description 12
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 41
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 35
- 239000000243 solution Substances 0.000 claims description 31
- 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
- 238000001035 drying Methods 0.000 claims description 22
- 239000002002 slurry Substances 0.000 claims description 20
- 150000001735 carboxylic acids Chemical class 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 16
- 239000007864 aqueous solution Substances 0.000 claims description 15
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- 241000588724 Escherichia coli Species 0.000 claims description 14
- 241000191967 Staphylococcus aureus Species 0.000 claims description 14
- 239000002244 precipitate Substances 0.000 claims description 14
- 238000010992 reflux Methods 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- 239000003443 antiviral agent Substances 0.000 claims description 12
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 11
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 11
- 238000004321 preservation Methods 0.000 claims description 9
- 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 8
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 8
- 238000006068 polycondensation reaction Methods 0.000 claims description 8
- 239000000047 product Substances 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
- 238000009987 spinning Methods 0.000 claims description 8
- 241000222122 Candida albicans Species 0.000 claims description 7
- 229940095731 candida albicans Drugs 0.000 claims description 7
- 150000001720 carbohydrates Chemical class 0.000 claims description 7
- 238000005266 casting Methods 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 7
- 238000005520 cutting process Methods 0.000 claims description 7
- 238000000605 extraction Methods 0.000 claims description 7
- 239000004744 fabric Substances 0.000 claims description 7
- 238000007142 ring opening reaction Methods 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
- 238000006243 chemical reaction Methods 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
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims description 5
- 229910001431 copper ion Inorganic materials 0.000 claims description 5
- 206010069767 H1N1 influenza Diseases 0.000 claims description 4
- 241000712431 Influenza A virus Species 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 125000001931 aliphatic group Chemical group 0.000 claims description 4
- 239000011668 ascorbic acid Substances 0.000 claims description 4
- 229960005070 ascorbic acid Drugs 0.000 claims description 4
- 235000010323 ascorbic acid Nutrition 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
- 238000002156 mixing Methods 0.000 claims description 4
- 201000010740 swine influenza Diseases 0.000 claims description 4
- 239000001361 adipic acid Substances 0.000 claims description 3
- 235000011037 adipic acid Nutrition 0.000 claims description 3
- 238000001132 ultrasonic dispersion Methods 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
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-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
- 239000008103 glucose Substances 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
- 230000002045 lasting effect Effects 0.000 abstract description 6
- 238000011065 in-situ storage Methods 0.000 abstract description 5
- 238000011068 loading method Methods 0.000 abstract description 4
- 230000009467 reduction Effects 0.000 abstract description 4
- 230000003115 biocidal effect Effects 0.000 abstract description 3
- -1 carbon carboxylic acid Chemical class 0.000 abstract description 2
- 230000002155 anti-virotic effect Effects 0.000 abstract 2
- 230000014759 maintenance of location Effects 0.000 abstract 1
- 239000003242 anti bacterial agent Substances 0.000 description 10
- 208000037797 influenza A Diseases 0.000 description 10
- 241000894006 Bacteria Species 0.000 description 8
- 241000700605 Viruses Species 0.000 description 6
- 238000009833 condensation Methods 0.000 description 6
- 230000005494 condensation Effects 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 238000005338 heat storage Methods 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 239000003642 reactive oxygen metabolite Substances 0.000 description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000004753 textile Substances 0.000 description 4
- 230000006378 damage Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 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
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 206010011409 Cross infection Diseases 0.000 description 1
- 239000004594 Masterbatch (MB) Substances 0.000 description 1
- 206010029803 Nosocomial infection Diseases 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 238000004332 deodorization Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000012510 hollow fiber Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 244000000010 microbial pathogen Species 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 238000012643 polycondensation polymerization Methods 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 239000000126 substance 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
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
- C08G69/16—Preparatory processes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
-
- 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
- D01D5/08—Melt spinning methods
-
- 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
- D01D5/24—Formation of filaments, threads, or the like with a hollow 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/085—Copper
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Textile Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Artificial Filaments (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention relates to a preparation method of antibacterial antiviral warm polyamide 6 fibers, and particularly relates to a preparation method of antibacterial antiviral warm polyamide 6 fibers with a hollow structure, wherein the antibacterial antiviral warm polyamide 6 fibers are prepared by loading nano copper on coffee carbon. The invention is characterized in that nano elemental copper is generated on the surface of coffee carbon by an in-situ reduction method, then the coffee carbon carboxylic acid with the nano elemental copper generated on the surface is modified and then is subjected to in-situ polymerization to introduce polyamide 6 to obtain antibacterial antiviral warm polyamide 6, and finally the antibacterial antiviral warm polyamide 6 fiber is obtained by melt spinning. The polyamide 6 fiber prepared by the invention has the characteristics of high efficiency, lasting antibiosis and antivirus, comfort and warmth retention, and still has better antibiosis and antivirus performances after the fiber is washed for 50 times.
Description
Technical Field
The invention belongs to the field of synthesis of antibacterial and antiviral fibers, relates to a preparation method of antibacterial and antiviral polyamide 6 fibers, and particularly relates to a preparation method of antibacterial, antiviral and warm-keeping polyamide 6 fibers with a hollow structure, wherein the antibacterial and antiviral polyamide 6 fibers are obtained by loading nano copper on coffee carbon.
Background
Viruses and bacteria bring great influence on human life, many diseases are caused by the viruses and the bacteria, pillows and mattresses in bedrooms and in the day and night, and even clothes and shoes which are not cleaned in time can hide the shadow of pathogenic microorganisms. Among the transmission paths of a plurality of bacteria and viruses, the textile is one of the main carriers, and is porous and loose, so that various impurities are easily adsorbed, and the textile becomes a carrier for breeding and parasitizing the bacteria and the viruses, and the cross infection rate of the public environment is greatly improved. In the post epidemic era, the awareness of consumers on cleanness and sanitation is greatly improved, and people also show great desire and demand for healthy and durable antibacterial and antiviral products.
Most of the existing antibacterial and antiviral materials have single functions, and people need to endow fiber textiles with special functions through a post-treatment process. Patent CN202010189222.8 discloses a method for preparing fiber and fabric with antibacterial and warm-keeping functions, which comprises mixing raw materials such as nano-silver antibacterial masterbatch and carbon fiber, melting and extruding, spinning, boiling in boiling water, and drying to obtain the antibacterial and warm-keeping fiber. The antibacterial and warm-keeping effects of the antibacterial and warm-keeping fibers prepared by the method are lasting, but the nano silver can enter a human body through the skin and the respiratory system and cause harm to the human body, and the antibacterial rate of the invention to various bacteria is not prominent, and the invention has no antiviral effect.
Antibacterial agents are generally classified into two major classes, inorganic and organic. The former uses silver, zinc, copper and the like as main raw materials, and inorganic filler as a carrier to prepare the inorganic antibacterial agent, and has good high-temperature resistance. The latter uses esters, alcohols and phenols as main raw materials, and has low high temperature resistance. The common inorganic antibacterial agents such as silver-loaded inorganic antibacterial agents and zinc-loaded inorganic antibacterial agents have the defects of insufficient safety of heavy metals to human bodies, non-lasting antibacterial effect and the like. Therefore, there is a need to develop a healthy, durable, multifunctional antibacterial and antiviral textile.
Disclosure of Invention
The invention aims to provide an antibacterial antiviral warm-keeping fiber, and particularly relates to a preparation method of an antibacterial antiviral warm-keeping polyamide 6 fiber with a hollow structure, wherein the antibacterial antiviral warm-keeping polyamide 6 fiber is obtained by loading nano copper on coffee carbon. The preparation method comprises the steps of firstly generating nano elemental copper (Cu @ coffee carbon) on the surface of coffee carbon by an in-situ reduction method, then modifying Cu @ coffee carbon carboxylic acid to obtain carboxylic acid modified Cu @ coffee carbon, obtaining antibacterial and antiviral polyamide 6 by introducing the carboxylic acid modified Cu @ coffee carbon in situ in the synthesis process of polyamide 6, and finally obtaining the antibacterial, antiviral and warm-keeping polyamide 6 fiber with a hollow structure by melt spinning.
Different from the dissolution type antibacterial mechanism of copper ions, the elemental copper is catalytic reaction antibacterial, plays an antibacterial and antiviral role by releasing Reactive Oxygen Species (ROS), and does not pollute the environment during antibacterial and antiviral. The size of the nano elemental copper obtained by the invention is 2-10nm, the nano elemental copper has higher catalytic reaction antibacterial and antiviral activity, the nano copper can activate oxygen in water and air to generate ROS (reactive oxygen species), and the ROS (hydroxyl free radicals, superoxide free radicals and hydrogen peroxide) have strong oxidability and can directly or indirectly damage the structure and the function of cells, so that cell membranes are ruptured to cause the death of bacteria. Furthermore, coffee carbon and nano copper are compounded, so that the antibacterial and antiviral fiber has the functions of comfort, warm keeping, anion emission and the like. The carboxylic acid modified Cu @ coffee carbon has good compatibility with polyamide 6, and can be uniformly and stably dispersed in polyamide in-situ polymerization of polyamide 6 monomers, so that the agglomeration problem of the nanoscale Cu @ coffee carbon is avoided. In addition, the nano copper with the size of 2-10nm has more exposed surface defects, carboxyl can be better complexed with the nano copper to maintain the nano copper of the Cu @ coffee carbon to be in a reduction state all the time, active oxygen free radicals are continuously released to play the role of 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.
The coffee carbon has good compatibility with polyamide 6 after being modified by loading elemental copper and carboxylic acid, can be uniformly dispersed in a polyamide 6 matrix, and has good spinnability and heat storage and warm keeping effects. In addition, the invention combines the advantages of the hollow fiber structure, the antibacterial, antiviral and warm-keeping polyamide 6 slice is subjected to melt spinning and passes through the C-shaped spinneret holes to obtain the antibacterial, antiviral and warm-keeping polyamide 6 fiber with the hollow structure, the prepared fiber not only can play a role in heat storage and warm keeping by means of coffee carbon, but also the hollow structure is combined with countless holes of the coffee carbon to form a honeycomb-shaped heat storage structure, and the fiber prepared by the structure can better lock the human body heat. Therefore, the fiber obtained by the invention has high-efficiency and lasting antibacterial and antiviral effects and heat storage and warm keeping effects, and can be applied to the fields of children clothes, military cold wear and the like with higher requirements on antibacterial, antiviral and warm keeping performances of the fiber.
The invention relates to a preparation method of an antibacterial antiviral warm-keeping fiber, which comprises the following specific steps:
(1) according to the mass parts, 2-5 parts of coffee carbon are ultrasonically dispersed in 50 parts of deionized water under certain conditions to prepare a coffee carbon water solution, and 0.2-1.0 part of copper salt is dissolved in 50 parts of deionized water to prepare a copper ion water solution. Mixing coffee carbohydrate solution and copper ion aqueous solution in a flask, condensing and refluxing, then stirring, dropwise adding 50 parts of reducing agent aqueous solution into the flask, and stirring at 60-90 ℃ for 3-24 hours to obtain dark solution. And centrifugally separating the obtained product by using deionized water and absolute ethyl alcohol, and finally drying to obtain the coffee carbon (Cu @ coffee carbon) antibacterial and antiviral agent with the surface generating nano elemental copper. The size of the generated nano simple substance copper is 2-10 nm;
(2) adding 1-3 parts of aliphatic dibasic acid, 15-20 parts of Cu @ coffee carbon and 0.5-2 parts of caprolactam into 100 parts of absolute ethyl alcohol, carrying out condensation reflux, stirring for 0.5-5 h to obtain carboxylic acid modified coffee carbon slurry (CM-Cu @ coffee carbon slurry) with a surface generating nano elemental copper, then placing the CM-Cu @ coffee carbon slurry into a centrifuge tube for centrifugation, removing supernatant to obtain precipitate, washing the precipitate with ethanol and water for 3-5 times, and drying to obtain carboxylic acid modified coffee carbon (CM-Cu @ coffee carbon) with a surface generating nano elemental copper.
(3) Adding 1-3 parts of CM-Cu @ coffee carbon, 100 parts of caprolactam and 2-5 parts of deionized water into a polymerization reaction kettle, opening a ring, performing prepolymerization, performing polycondensation, and finally performing belt casting, grain cutting and extraction to obtain the antibacterial, antiviral and warm-keeping polyamide 6 slice.
(4) Drying the antibacterial antiviral warm polyamide 6 slices at 90-120 ℃ for a period of time, adding the slices into a melt spinning machine for spinning, and then drawing to obtain the antibacterial antiviral warm polyamide 6 fiber.
According to the preparation method of the antibacterial antiviral thermal fiber, in the step (1), the ultrasonic dispersion condition of the coffee carbon is that the time is 20-60 min, and the ultrasonic frequency is 30-60 kHz;
in the above method for preparing the antibacterial antiviral thermal fiber, in the step (1), the copper salt is one of copper chloride, copper sulfate and copper nitrate;
according to the preparation method of the antibacterial antiviral thermal fiber, in the step (1), the reducing agent aqueous solution is one of 0.1-0.5 mol/L citric acid, hydrazine hydrate, sodium borohydride, ascorbic acid, sodium hypophosphite, tetrabutylammonium borohydride and glucose aqueous solution;
the preparation method of the antibacterial antiviral warm-keeping fiber comprises the following specific reaction in the step (2): the aliphatic dibasic acid is one of adipic acid, suberic acid, sebacic acid and dodecanedioic acid;
according to the preparation method of the antibacterial antiviral thermal fiber, in the step (3), the ring-opening prepolymerization reaction conditions are that the temperature is 200-260 ℃, the pressure is 0.1-1.0 MPa, and the time is 2-5 h;
according to the preparation method of the antibacterial antiviral warm-keeping fiber, in the step (3), the condensation polymerization reaction conditions are that the temperature is 240-260 ℃, the pressure is-0.02-0.10 MPa, and the time is 2-5 h;
in the preparation method of the antibacterial antiviral warm-keeping fiber, in the step (4), a spinneret plate selected during melt spinning is a C-shaped spinneret hole, and the obtained fiber is of a hollow structure;
according to the preparation method of the antibacterial, antiviral and warm-keeping fiber, in the step (4), the breaking strength of the antibacterial, antiviral and warm-keeping polyamide 6 fiber is 2.5-3.5 cN/dtex, the breaking elongation is 15-30%, the antibacterial effect on staphylococcus aureus, escherichia coli and candida albicans can reach more than 99%, the antiviral effect on H1N1 influenza A virus can reach more than 99%, the antibacterial rate on escherichia coli and staphylococcus aureus can still reach more than 97% after the fiber is washed for 50 times, the antiviral effect on H1N1 influenza A virus can reach more than 97%, and the heat-keeping rate of the fabric prepared from the fiber can reach more than 55%, so that the fabric has good resistance to water washing, high-efficiency antibacterial and antiviral and warm-keeping performances.
By adopting the technical scheme of the invention, the following beneficial effects can be achieved:
(1) safety: the Cu @ coffee carbon prepared by the invention is a non-dissoluble antibacterial antiviral auxiliary agent, does not harm human health, and does not pollute the environment in a long-term use process;
(2) and (3) lasting antibiosis: the nano copper in the antibacterial antiviral thermal fiber is always in a reduction state, plays a role in resisting bacteria and viruses by continuously releasing active oxygen free radicals, has high-efficiency and lasting antibacterial and antiviral effects, and can be realized under the condition of dark reaction without depending on light source excitation in the process of releasing the active oxygen free radicals by the nano copper;
(3) the warm-keeping function: the coffee carbon is added, so that the fiber not only has the antibacterial and antiviral functions, but also has the functions of heat storage, warm keeping, bacteriostasis, deodorization, negative ion emission and the like.
Detailed Description
The invention will be further illustrated with reference to specific embodiments. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Embodiment 1, a method for preparing an antibacterial antiviral thermal fiber, comprising the following steps:
(1) 2 parts of coffee carbon powder was ultrasonically dispersed (ultrasonic time 20min, frequency 30kHz) in 50 parts of deionized water to obtain a coffee carbon solution, and 0.2 part of copper sulfate was dissolved in 50 parts of deionized water to prepare a copper sulfate aqueous solution. A flask containing an aqueous copper sulfate solution and a coffee carbohydrate solution was condensed under reflux at 80 ℃ and 50 parts of a 0.1mol/L aqueous citric acid solution was dropwise added to the flask while stirring. The mixed solution was stirred at 60 ℃ for 15h until a dark solution was obtained. Washing and centrifuging the obtained product by absolute ethyl alcohol and deionized water, and finally drying to obtain the Cu @ coffee carbon antibacterial antiviral agent.
(2) Adding 1 part of adipic acid, 15 parts of Cu @ coffee carbon antibacterial and antiviral agent and 0.5 part of caprolactam into 100 parts of absolute ethyl alcohol, carrying out condensation reflux at 80 ℃, stirring for 0.5h to obtain carboxylic acid modified Cu @ coffee carbon slurry (CM-Cu @ coffee carbon slurry), then placing the modified CM-Cu @ coffee carbon slurry into a centrifuge tube for centrifugation, removing supernatant to obtain precipitate, washing the precipitate with ethanol and water for 3 times, and drying to obtain carboxylic acid modified Cu @ coffee carbon (CM-Cu @ coffee carbon).
(3) Adding 1 part of CM-Cu @ coffee carbon, 100 parts of caprolactam and 2 parts of deionized water into a polymerization reaction kettle, carrying out ring-opening prepolymerization, and reacting for 2 hours at the temperature of 200 ℃ and the pressure of 0.1 MPa; and then, raising the temperature to 240 ℃, carrying out polycondensation reaction for 2h under the pressure of-0.02 MPa, and finally carrying out belt casting, grain cutting and extraction to obtain the antibacterial and antiviral polyamide 6 slice with the heat preservation function.
(4) Drying the antibacterial antiviral warm polyamide 6 chips at 100 ℃ for 24h, and adding the chips into a melt spinning machine for spinning to obtain the antibacterial antiviral warm polyamide 6 fiber with a hollow structure.
The breaking strength of the antibacterial antiviral warm-keeping polyamide 6 fiber prepared by the invention is 3.5cN/dtex, the breaking elongation is 15%, the antibacterial effect on staphylococcus aureus, escherichia coli and candida albicans can reach 99.2%, the antiviral effect on influenza A H1N1 virus can reach 99.1%, after the fiber is washed for 50 times, the antibacterial rate on escherichia coli and staphylococcus aureus can still reach more than 97%, the antiviral effect on influenza A H1N1 virus can reach 97.8%, and the heat-keeping rate of the fabric prepared by the fiber can reach 55.8%.
Embodiment 2, a method for preparing an antibacterial antiviral thermal fiber, comprising the following steps:
(1) ultrasonic dispersing 5 parts of coffee carbon powder in 50 parts of deionized water (ultrasonic time 60min, frequency 30kHz) to obtain coffee carbon water solution, and dissolving 1 part of copper sulfate in 50 parts of deionized water to prepare copper sulfate water solution. A flask containing an aqueous copper sulfate solution and a coffee carbohydrate solution was condensed under reflux at 80 ℃ and 50 parts of a 0.5mol/L aqueous ascorbic acid solution was added dropwise to the flask while stirring. The mixed solution was stirred at 90 ℃ for 24h until a dark solution was obtained. Washing and centrifuging the obtained product by absolute ethyl alcohol and deionized water, and finally drying to obtain the Cu @ coffee carbon antibacterial antiviral agent.
(2) Adding 3 parts of suberic acid, 20 parts of Cu @ coffee carbon antibacterial and antiviral agent and 2 parts of caprolactam into 100 parts of absolute ethyl alcohol, carrying out condensation reflux at 80 ℃, stirring for 5 hours to obtain carboxylic acid modified Cu @ coffee carbon slurry (CM-Cu @ coffee carbon slurry), then putting the modified CM-Cu @ coffee carbon slurry into a centrifuge tube for centrifugation, removing supernatant to obtain precipitate, washing the precipitate with ethanol and water for 5 times, and drying to obtain carboxylic acid modified Cu @ coffee carbon (CM-Cu @ coffee carbon).
(3) Adding 3 parts of CM-Cu @ coffee carbon, 100 parts of caprolactam and 5 parts of deionized water into a polymerization reaction kettle, carrying out ring-opening prepolymerization, and reacting for 5 hours at the temperature of 260 ℃ and the pressure of 1.0 MPa; and then, keeping the temperature at 260 ℃ and the pressure at-0.10 MPa for polycondensation reaction for 5h, and finally carrying out belt casting, grain cutting and extraction to obtain the antibacterial and antiviral polyamide 6 slice with the heat preservation function.
(4) Drying the antibacterial antiviral warm polyamide 6 chips at 100 ℃ for 36h, and adding the chips into a melt spinning machine for spinning to obtain the antibacterial antiviral warm polyamide 6 fiber with a hollow structure.
The breaking strength of the antibacterial antiviral warm-keeping polyamide 6 fiber prepared by the invention is 2.5cN/dtex, the breaking elongation is 30%, the antibacterial effect on staphylococcus aureus, escherichia coli and candida albicans can reach more than 99.8%, the antiviral effect on influenza A H1N1 virus can reach 99.7%, after the fiber is washed for 50 times, the antibacterial rate on escherichia coli and staphylococcus aureus can still reach more than 97%, the antiviral effect on influenza A H1N1 virus can reach 97.3%, and the heat preservation rate of the fabric prepared by the fiber can reach 59.2%.
Embodiment 3, a method for preparing an antibacterial antiviral thermal fiber, comprising the following steps:
(1) 3 parts of coffee carbon powder is ultrasonically dispersed in 50 parts of deionized water (ultrasonic time is 40min, frequency is 40kHz) to obtain coffee carbon solution, and 0.5 part of copper chloride is dissolved in 50 parts of deionized water to prepare copper chloride aqueous solution. A flask containing an aqueous copper chloride solution and a coffee carbohydrate solution was condensed under reflux at 80 ℃ and 50 parts of a 0.3mol/L aqueous citric acid solution was dropwise added to the flask while stirring. The mixed solution was stirred at 90 ℃ for 8h until a dark solution was obtained. Washing and centrifuging the obtained product by absolute ethyl alcohol and deionized water, and finally drying to obtain the Cu @ coffee carbon antibacterial antiviral agent.
(2) Adding 2 parts of dodecanedioic acid, 15 parts of Cu @ coffee carbon antibacterial antiviral agent and 1 part of caprolactam into 100 parts of absolute ethyl alcohol, carrying out condensation reflux at 80 ℃, stirring for 2 hours to obtain carboxylic acid modified Cu @ coffee carbon slurry (CM-Cu @ coffee carbon slurry), then putting the modified CM-Cu @ coffee carbon slurry into a centrifugal tube for centrifugation, removing supernatant to obtain precipitate, washing the precipitate with ethanol and water for 5 times, and drying to obtain carboxylic acid modified Cu @ coffee carbon (CM-Cu @ coffee carbon).
(3) Adding 2 parts of CM-Cu @ coffee carbon, 100 parts of caprolactam and 3 parts of deionized water into a polymerization reaction kettle, carrying out ring-opening prepolymerization, and reacting for 4 hours at the temperature of 230 ℃ and the pressure of 0.6 MPa; and then, the temperature is increased to 250 ℃, the polycondensation reaction is carried out for 4h under the pressure of minus 0.05MPa, and finally, the antibacterial and antiviral polyamide 6 slice with the function of keeping warm is obtained through belt casting, grain cutting and extraction.
(4) Drying the antibacterial antiviral warm polyamide 6 chips at 100 ℃ for 36h, and adding the chips into a melt spinning machine for spinning to obtain the antibacterial antiviral warm polyamide 6 fiber with a hollow structure.
The breaking strength of the antibacterial antiviral warm-keeping polyamide 6 fiber prepared by the invention is 3.0cN/dtex, the elongation at break is 15%, the antibacterial effect on staphylococcus aureus, escherichia coli and candida albicans can reach 99.5%, the antiviral effect on influenza A H1N1 virus can reach 99.6%, after the fiber is washed for 50 times, the antibacterial rate on escherichia coli and staphylococcus aureus can still reach more than 97%, the antiviral effect on influenza A H1N1 virus can reach 97.3%, and the heat preservation rate can reach 57.6%.
Embodiment 4, a method for preparing an antibacterial antiviral thermal fiber, comprising the following steps:
(1) ultrasonic dispersion (ultrasonic time 50min, frequency 30kHz) of 4 parts of coffee carbon powder in 50 parts of deionized water to obtain a coffee carbon solution, and dissolving 0.7 part of copper chloride in 50 parts of deionized water to prepare a copper chloride aqueous solution. A flask containing an aqueous copper chloride solution and a coffee carbohydrate solution was condensed under reflux at 80 ℃ and 50 parts of an aqueous ascorbic acid solution of 0.4mol/L was added dropwise to the flask while stirring. The mixed solution was stirred at 80 ℃ for 12h until a dark solution was obtained. Washing and centrifuging the obtained product through absolute ethyl alcohol and deionized water, and finally drying to obtain the Cu @ coffee carbon antibacterial antiviral agent.
(2) Adding 3 parts of sebacic acid, 15 parts of Cu @ coffee carbon antibacterial and antiviral agent and 2 parts of caprolactam into 100 parts of absolute ethyl alcohol, carrying out condensation reflux at 80 ℃, stirring for 3 hours to obtain carboxylic acid modified Cu @ coffee carbon slurry (CM-Cu @ coffee carbon slurry), then putting the modified CM-Cu @ coffee carbon slurry into a centrifuge tube for centrifugation, removing supernatant to obtain precipitate, washing the precipitate with ethanol and water for 5 times, and drying to obtain carboxylic acid modified Cu @ coffee carbon (CM-Cu @ coffee carbon).
(3) Adding 3 parts of CM-Cu @ coffee carbon, 100 parts of caprolactam and 4 parts of deionized water into a polymerization reaction kettle, carrying out ring-opening prepolymerization, and reacting for 4 hours at the temperature of 250 ℃ and the pressure of 0.5 MPa; and then, reducing the temperature to 240 ℃, carrying out polycondensation reaction for 3h under the pressure of-0.06 MPa, and finally carrying out belt casting, grain cutting and extraction to obtain the antibacterial and antiviral polyamide 6 slice with the heat preservation function.
(4) Drying the antibacterial antiviral warm polyamide 6 chips at 100 ℃ for 24h, and adding the chips into a melt spinning machine for spinning to obtain the antibacterial antiviral warm polyamide 6 fiber with a hollow structure.
The breaking strength of the antibacterial antiviral warm-keeping polyamide 6 fiber prepared by the invention is 2.6cN/dtex, the breaking elongation is 17%, the antibacterial effect on staphylococcus aureus, escherichia coli and candida albicans can reach 99.9%, the antiviral effect on influenza A H1N1 virus can reach 99.9%, after the fiber is washed for 50 times, the antibacterial rate on escherichia coli and staphylococcus aureus can still reach more than 97%, the antiviral effect on influenza A H1N1 virus can reach 98.6%, and the heat preservation rate can reach 61.3%.
Embodiment 5, a method for preparing an antibacterial antiviral thermal fiber, comprising the following steps:
(1) 3 parts of coffee carbon powder was ultrasonically dispersed (ultrasonic time 30min, frequency 50kHz) in 50 parts of deionized water to obtain a coffee carbon aqueous solution, and 0.2 part of copper sulfate was dissolved in 50 parts of deionized water to prepare a copper sulfate aqueous solution. A flask containing an aqueous copper sulfate solution and a coffee carbohydrate solution was condensed under reflux at 80 ℃ and 50 parts of a 0.3mol/L aqueous citric acid solution was dropwise added to the flask while stirring. The mixed solution was stirred at 80 ℃ for 18h until a dark solution was obtained. Washing and centrifuging the obtained product by absolute ethyl alcohol and deionized water, and finally drying to obtain the Cu @ coffee carbon antibacterial antiviral agent.
(2) Adding 3 parts of sebacic acid, 15 parts of Cu @ coffee carbon antibacterial and antiviral agent and 1 part of caprolactam into 100 parts of absolute ethyl alcohol, carrying out condensation reflux at 80 ℃, stirring for 2 hours to obtain carboxylic acid modified Cu @ coffee carbon slurry (CM-Cu @ coffee carbon slurry), then putting the modified CM-Cu @ coffee carbon slurry into a centrifuge tube for centrifugation, removing supernatant to obtain precipitate, washing the precipitate with ethanol and water for 5 times, and drying to obtain carboxylic acid modified Cu @ coffee carbon (CM-Cu @ coffee carbon).
(3) Adding 2 parts of CM-Cu @ coffee carbon, 100 parts of caprolactam and 2 parts of deionized water into a polymerization reaction kettle, carrying out ring-opening prepolymerization, and reacting for 5 hours at the temperature of 240 ℃ and the pressure of 0.8 MPa; and then, raising the temperature to 250 ℃, carrying out polycondensation reaction for 2h under the pressure of-0.09 MPa, and finally carrying out belt casting, grain cutting and extraction to obtain the antibacterial and antiviral polyamide 6 slice with the heat preservation function.
(4) Drying the antibacterial antiviral warm polyamide 6 chips at 100 ℃ for 24h, and adding the chips into a melt spinning machine for spinning to obtain the antibacterial antiviral warm polyamide 6 fiber with a hollow structure.
The breaking strength of the antibacterial antiviral warm-keeping polyamide 6 fiber prepared by the invention is 2.7cN/dtex, the breaking elongation is 16%, the antibacterial effect on staphylococcus aureus, escherichia coli and candida albicans can reach 99.5%, the antiviral effect on influenza A H1N1 virus can reach 99.5%, after the fiber is washed for 50 times, the antibacterial rate on escherichia coli and staphylococcus aureus can still reach more than 97%, the antiviral effect on influenza A H1N1 virus can reach 97.8%, and the heat preservation rate can reach 57.7%.
Claims (6)
1. A preparation method of antibacterial antiviral thermal fiber is characterized by comprising the following steps: the preparation method comprises the following steps:
(1) ultrasonically dispersing 2-5 parts of coffee carbon in 50 parts of deionized water to prepare a coffee carbon aqueous solution, and dissolving 0.2-1.0 part of copper salt in 50 parts of deionized water to prepare a copper ion aqueous solution; mixing a coffee carbohydrate solution and a copper ion aqueous solution in a flask, condensing and refluxing after mixing, dropwise adding 50 parts of a reducing agent aqueous solution into the flask while stirring, and stirring for 3-24 hours at 60-90 ℃ to obtain a dark solution; centrifugally separating the obtained product by using deionized water and absolute ethyl alcohol, and finally drying to obtain the coffee carbon antibacterial antiviral agent with the surface generating nano elemental copper;
(2) adding 1-3 parts of aliphatic dibasic acid, 15-20 parts of coffee carbon with nano elemental copper generated on the surface and 0.5-2 parts of caprolactam into 100 parts of absolute ethyl alcohol, condensing, refluxing and stirring for 0.5-5 hours to obtain coffee carbon slurry with carboxylic acid modified with nano elemental copper generated on the surface, then placing the coffee carbon slurry with nano elemental copper generated on the modified surface into a centrifugal tube for centrifugation, removing supernatant to obtain precipitate, washing the precipitate with ethanol and water for 3-5 times, and drying to obtain coffee carbon with nano elemental copper generated on the carboxylic acid modified surface;
(3) adding 1-3 parts of carboxylic acid modified coffee carbon with nano elemental copper generated on the surface, 100 parts of caprolactam and 2-5 parts of deionized water into a polymerization reaction kettle, opening a ring, performing prepolymerization, performing polycondensation, and finally performing belt casting, grain cutting and extraction to obtain antibacterial, antiviral and warm-keeping polyamide 6 slices;
(4) drying the antibacterial antiviral warm polyamide 6 slices at 90-120 ℃ for a period of time, and adding the slices into a melt spinning machine for spinning to obtain the antibacterial antiviral warm polyamide 6 fiber with a hollow structure.
2. The preparation method of the antibacterial antiviral thermal fiber according to claim 1, wherein in the step (1), the ultrasonic dispersion condition of the coffee carbon is that the time is 20-60 min, and the ultrasonic frequency is 30-60 kHz; the copper salt is one of copper chloride, copper sulfate and copper nitrate; the reducing agent aqueous solution is one of 0.1-0.5 mol/L citric acid, hydrazine hydrate, sodium borohydride, ascorbic acid, sodium hypophosphite, tetrabutylammonium borohydride and glucose aqueous solution.
3. The method for preparing antibacterial antiviral thermal fiber as claimed in claim 1, wherein in step (2), the aliphatic dibasic acid is one of adipic acid, suberic acid, sebacic acid, and dodecanedioic acid.
4. The preparation method of the antibacterial antiviral thermal fiber according to claim 1, wherein in the step (3), the ring-opening prepolymerization reaction conditions are that the temperature is 200-260 ℃, the pressure is 0.1-1.0 MPa, and the time is 2-5 h; the reaction conditions of polycondensation are 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 antibacterial antiviral thermal fiber according to claim 1, wherein in the step (4), the spinneret plate used in the melt spinning is a C-shaped spinneret hole, and the obtained fiber has a hollow structure.
6. The preparation method of the antibacterial, antiviral and warm-keeping fiber according to claim 1, characterized in that the breaking strength of the prepared antibacterial, antiviral and warm-keeping polyamide 6 fiber with the hollow structure is 2.5-3.5 cN/dtex, the elongation at break is 15-30%, the antibacterial effect on staphylococcus aureus, escherichia coli and candida albicans can reach more than 99%, the antiviral effect on H1N1 influenza A virus can reach more than 99%, the antibacterial rate on escherichia coli and staphylococcus aureus can still reach more than 97% after the fiber is washed for 50 times, the antiviral effect on H1N1 influenza A virus can reach more than 97%, and the heat preservation rate of the fabric prepared by the fiber can reach more than 55%, so that the fabric has good water washing resistance, high-efficiency antibacterial, antiviral and warm-keeping performance.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107498068A (en) * | 2017-09-22 | 2017-12-22 | 大连理工大学 | A kind of preparation method of flower-like nanometer copper |
| CN108659525A (en) * | 2018-06-04 | 2018-10-16 | 东华大学 | A method of PA6/ meso-porous nano material@Ag composite antibacterial fibres are prepared based on situ aggregation method |
| CN109122720A (en) * | 2018-09-20 | 2019-01-04 | 安徽江淮汽车集团股份有限公司 | A kind of antibacterial agent and preparation method thereof |
| 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 |
| CN112296346A (en) * | 2019-07-25 | 2021-02-02 | 上海沪正实业有限公司 | Nano copper powder and application thereof in preparation of copper-fiber-containing antibacterial and deodorant socks |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107498068A (en) * | 2017-09-22 | 2017-12-22 | 大连理工大学 | A kind of preparation method of flower-like nanometer copper |
| CN108659525A (en) * | 2018-06-04 | 2018-10-16 | 东华大学 | A method of PA6/ meso-porous nano material@Ag composite antibacterial fibres are prepared based on situ aggregation method |
| CN109122720A (en) * | 2018-09-20 | 2019-01-04 | 安徽江淮汽车集团股份有限公司 | A kind of antibacterial agent and preparation method thereof |
| 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 |
| CN112296346A (en) * | 2019-07-25 | 2021-02-02 | 上海沪正实业有限公司 | Nano copper powder and application thereof in preparation of copper-fiber-containing antibacterial and deodorant socks |
| 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 |
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