CN105544189A - Preparation method of antibacterial conductive cotton fiber - Google Patents
Preparation method of antibacterial conductive cotton fiber Download PDFInfo
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- CN105544189A CN105544189A CN201610056257.8A CN201610056257A CN105544189A CN 105544189 A CN105544189 A CN 105544189A CN 201610056257 A CN201610056257 A CN 201610056257A CN 105544189 A CN105544189 A CN 105544189A
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- cotton fiber
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- cotton
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- 229920000742 Cotton Polymers 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 230000000844 anti-bacterial effect Effects 0.000 title abstract description 9
- 239000000835 fiber Substances 0.000 claims abstract description 67
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000000126 substance Substances 0.000 claims abstract description 15
- 206010070834 Sensitisation Diseases 0.000 claims abstract description 13
- 238000007747 plating Methods 0.000 claims abstract description 13
- 230000008313 sensitization Effects 0.000 claims abstract description 13
- 230000004913 activation Effects 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 10
- 239000003446 ligand Substances 0.000 claims abstract description 9
- XNRABACJWNCNEQ-UHFFFAOYSA-N silver;azane;nitrate Chemical compound N.[Ag+].[O-][N+]([O-])=O XNRABACJWNCNEQ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 20
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 16
- 230000003115 biocidal effect Effects 0.000 claims description 15
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 11
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 10
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 10
- 239000001119 stannous chloride Substances 0.000 claims description 10
- 235000011150 stannous chloride Nutrition 0.000 claims description 10
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 8
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 8
- 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 6
- 239000008103 glucose Substances 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000002203 pretreatment Methods 0.000 claims description 4
- 238000007788 roughening Methods 0.000 claims description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims description 2
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 claims description 2
- 235000011180 diphosphates Nutrition 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims description 2
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical class OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 239000003242 anti bacterial agent Substances 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 33
- 239000004753 textile Substances 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 210000002268 wool Anatomy 0.000 abstract 1
- 239000008367 deionised water Substances 0.000 description 32
- 229910021641 deionized water Inorganic materials 0.000 description 32
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 25
- 229910052709 silver Inorganic materials 0.000 description 23
- 239000004332 silver Substances 0.000 description 23
- 238000003756 stirring Methods 0.000 description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 12
- 238000000576 coating method Methods 0.000 description 10
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 9
- 239000011159 matrix material Substances 0.000 description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 8
- 239000004677 Nylon Substances 0.000 description 8
- 238000001994 activation Methods 0.000 description 8
- 239000011248 coating agent Substances 0.000 description 8
- 229920001778 nylon Polymers 0.000 description 8
- 238000005406 washing Methods 0.000 description 8
- 238000000151 deposition Methods 0.000 description 5
- 230000008021 deposition Effects 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 238000005352 clarification Methods 0.000 description 4
- 238000002242 deionisation method Methods 0.000 description 4
- 239000003995 emulsifying agent Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 230000000845 anti-microbial effect Effects 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- WKVMOQXBMPYPGK-UHFFFAOYSA-N 2-[bis(carboxymethyl)amino]acetic acid;sodium Chemical compound [Na].OC(=O)CN(CC(O)=O)CC(O)=O WKVMOQXBMPYPGK-UHFFFAOYSA-N 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 239000004952 Polyamide Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920002647 polyamide Polymers 0.000 description 2
- 238000006424 Flood reaction Methods 0.000 description 1
- 101100062772 Neurospora crassa (strain ATCC 24698 / 74-OR23-1A / CBS 708.71 / DSM 1257 / FGSC 987) dcl-2 gene Proteins 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229920004933 Terylene® Polymers 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- -1 before silver-plated Substances 0.000 description 1
- 230000036760 body temperature Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- CEYULKASIQJZGP-UHFFFAOYSA-L disodium;2-(carboxymethyl)-2-hydroxybutanedioate Chemical compound [Na+].[Na+].[O-]C(=O)CC(O)(C(=O)O)CC([O-])=O CEYULKASIQJZGP-UHFFFAOYSA-L 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- VZOPRCCTKLAGPN-ZFJVMAEJSA-L potassium;sodium;(2r,3r)-2,3-dihydroxybutanedioate;tetrahydrate Chemical compound O.O.O.O.[Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O VZOPRCCTKLAGPN-ZFJVMAEJSA-L 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 229940048084 pyrophosphate Drugs 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 1
- 229940074446 sodium potassium tartrate tetrahydrate Drugs 0.000 description 1
- 229940048086 sodium pyrophosphate Drugs 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 235000019818 tetrasodium diphosphate Nutrition 0.000 description 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/11—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
- D06M11/20—Halides of elements of Groups 4 or 14 of the Periodic Table, e.g. zirconyl chloride
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/58—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides
- D06M11/59—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides with ammonia; with complexes of organic amines with inorganic substances
- D06M11/60—Ammonia as a gas or in solution
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/58—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides
- D06M11/64—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides with nitrogen oxides; with oxyacids of nitrogen or their salts
- D06M11/65—Salts of oxyacids of nitrogen
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/34—Polyamides
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention relates to a preparation method of antibacterial conductive cotton fiber. Cotton fiber short fiber loose wool is used as a raw material. The method comprises the following steps that the cotton short fiber is deoiled, coarsened and subjected to sensitization pretreatment, a low concentration silver nitrate-ammonia water solution is added for activation, then chemical silvering is carried out, a chelating ligand agent is added during chemical silvering to replace some ammonia water, and high-temperature solidifying treatment is carried out after chemical silvering. The operation is simple, the technological performance is stable, energy consumption is small, and industrial production is easy. By the adoption of the antibacterial conductive cotton fiber, the plating layer combining firmness degree is high, the conductivity is good, the specific surface area resistance reaches 10-100 ohm/cm, the properties of common cotton fiber are reserved, and the cotton fiber can be used as the antibacterial and conductive cotton fiber, and can be made into antibacterial conductive cotton yarn after being matched with different proportions of common cotton short fiber to be used for various textiles.
Description
Technical field
The present invention relates to a kind of preparation method of antibiotic conductive cotton fiber, the method, by making matrix have good electric conductivity at matrix surface plating layer of metal silverskin, belongs to new textile material field.
Background technology
Silver plated fiber is a kind of high performance functional fibre, and the function such as the antibacterial and deodouring of its uniqueness, anti-electromagnetic radiation, antistatic, regulate body temperature is attracted attention by people.The outer plating technology of fiber mainly contains chemical plating, plating and Vacuum Deposition three class.Adopt Electroless Silver Plating have technique simple, be applicable to the advantages such as irregular matrix material, cost are lower, but it is difficult to there is reaction in current Electroless Silver Plating, control bath stability is poor, and silver-plated price is more expensive, the conductive fiber coating problem that not evenly binding strength is not high of preparation.
Before making the present invention, Chinese invention patent, CNl311369A, disclose a kind of chemical silver plating method of organic fiber, take silver ammino solution as silver plating liquid, before silver-plated, raw material is cleaned in acetone soln, then surface activation process is carried out, catalyst P dCl2 catalysis with salpeter solution and hydrochloric acid solution.The method use this organic solvent of acetone, have employed again precious metal palladium as catalyst, cost compare is high.Chinese invention patent CN100570047C discloses a kind of preparation method of high-performance conductive fiber, using sodium potassium tartrate tetrahydrate as reductant, adopts oxalic acid solution to soak solidification.Have employed organic solvent 2-dichloroethanes or dimethylbenzene equally as alligatoring agent, cost compare is high.Chinese invention patent CN101012552A discloses a kind of stable fibre chemistry silver-coating method that can repeatedly supplement, and using formaldehyde as reductant, has reacted rear interpolation ammoniacal liquor and formaldehyde, continues chemical silvering.Formaldehyde toxic and volatile, adopts formaldehyde to pollute.
The base material more than invented is all the chemical fibres such as terylene, nylon, has no precedent the cotton silver-coating method as base material.Appearance of the present invention, has filled up national blank.
Summary of the invention
Problem to be solved by this invention is the deficiency overcoming prior art existence, and provides a kind of preparation method of cotton antibiotic conductive fiber.
The technical solution adopted in the present invention is:
A kind of preparation method of antibiotic conductive cotton fiber, fall apart hair for raw material with cotton fiber short fiber, comprise the steps: to deoil to cotton short fiber, alligatoring, sensitization pre-treatment, adds low concentration silver nitrate-ammonia spirit activation, then carries out chemical silvering, add chelating ligands agent when chemical silvering and replace partial ammonia water, after silver-plated, carry out hot setting process.
Preferably, described cotton short fiber roughening process adopts alkali treatment, and temperature is 50 DEG C ± 5 DEG C, and dip time is 30 ~ 40min.
Preferably, described alkali is NaOH, and the concentration of NaOH is 30 ~ 60ml/l.
Preferably, described sensitization pre-treatment, floods 15 ~ 18min under adopting the stannous chloride solution normal temperature of 5 ~ 16g/L, and the cotton fiber after then adopting the sodium bicarbonate solution of 1g/L to rinse stannous chloride dipping, clarifies to cleaning solution.
Preferably, after described silver nitrate-ammonia spirit activation, the formula carrying out chemical plating liquid is composed as follows:
Reducing solution is filled a prescription: glucose 10 ~ 15g/L;
Oxidation solution is filled a prescription: silver nitrate 10 ~ 20g/L;
Ammoniacal liquor: appropriate;
Chelating ligands agent 0.1 ~ 1.5g/L.
Preferably, the chelating ligands agent added in described chemical silvering is nitrilotriacetic acid salt, citrate or pyrophosphate.
Preferably, described silver-plated after carry out hot setting process, hot setting is temperature is 80 ~ 100 DEG C, time 5 ~ 7min.
The principle of foundation of the present invention is:
1, cotton short fiber roughening treatment can adopt acid or alkali treatment, but base extraction affects the mechanical property of fiber, and the easy etching apparatus of hydrochloric acid, nitric acid is more expensive, relatively good with NaOH.
2, when carrying out sensitized treatment with stannous chloride, not very even, easily being washed, the present invention adds sodium bicarbonate solution cleaning, and solution ph is raised, and stannous chloride forms nanogel and is deposited on cotton fiber surface, formed relatively more firm, more uniform sedimentary deposit.Thereafter adopt the activation of low concentration silver ammino solution, strengthen the adhesion of matrix and silver, make silver-plated after be not easy to fall down.
3, chemistry crosses in formula of liquid and adds chelating ligands agent, for stable plating solution, reduces surface porosity factor and roughness, makes coating surface even.The Ag particle of separating out is less, forms nano-Ag particles, can anti-oxidation, reduces the impurity that coating is separated out, and increases the uniformity that Argent grain is separated out.
Compared with prior art, the present invention has following obvious advantage:
NaOH corrosivity is lower, low price, may be used for the alligatoring of fiber, the nano-colloid of tin ash is formed during sodium bicarbonate cleaning stannous chloride, Nano silver deposition can be helped even, add chelating ligands agent in plating solution, the uniformity of coating and the binding strength between itself and matrix fiber can be significantly improved.The present invention is simple to operate, processing performance is stablized, cost is low, and power consumption is few, is easy to suitability for industrialized production, adopt antibiotic conductive fiber prepared by the present invention, coating binding strength is high, and electric conductivity is good, and specific area resistance reaches 10-100 Ω/cm, and retain the characteristic of original fiber, can use in multiple textile material.
Accompanying drawing explanation
The schematic surface of the silver-plated rear conductive fiber that Fig. 1 provides for the embodiment of the present invention.
Detailed description of the invention
Below in conjunction with drawings and Examples, technical solution of the present invention and effect are further described.
Embodiment one:
The present embodiment adopts the cotton short fiber of 1g to do matrix fiber.
The first step: oil removing.By 0.1g NaOH, 0.1gOP emulsifying agent, the profound washing powder of 0.1g joins in the deionized water of 50mL and dissolves, and bath temperature is 50 DEG C, stirs, and then adds load weighted cotton short fiber (1g) and stirs 30min, then fully wash.
Second step: alligatoring.Joined in 50mL deionized water by 7mL NaOH, then add the cotton short fiber that previous step handles well, bath temperature is 50 DEG C, stirs 30min, then fully washes.
3rd step: sensitization.Weighing 0.5g stannous chloride is dissolved in 0.5mL hydrochloric acid, join until completely dissolved in 50mL deionized water, the cotton short fiber finally adding previous step process fully stirs 10min again, and temperature is 30 DEG C, the complete rear 1g/L sodium bicarbonate solution of sensitization embathes 3min, more fully washes.
Tetra-Walk: activation.Take 0.05g silver nitrate to be dissolved in a small amount of deionized water, then drip ammoniacal liquor in solution, during beginning, in solution, occur reddish brown precipitation, continue to drip ammoniacal liquor to solution clarification; Then add deionized water to 50mL, the cotton short fiber finally adding previous step process fully stirs 3min, and bath temperature is 30 DEG C. and fully washing is clean afterwards.
5th step: deposition of silver.
1,113mL reducing solution is prepared: weigh 0.9g glucose and be fully dissolved in 113mL deionized water;
2,38mL silver liquid ammonia is prepared. weigh 0.4875g silver nitrate and be dissolved in a small amount of deionized water, in solution, drip ammoniacal liquor again, during beginning, occur precipitation, continue to drip ammoniacal liquor and clarify to solution, add deionized water again to 37.5mL, finally add 0.0075g nitrilotriacetic acid sodium and be dissolved in wherein.
3, pour in reducing solution by the silver liquid ammonia prepared, shake up, add rapidly the cotton short fiber that the 4th step activates, 30 DEG C are fully stirred 30min.
6th step: take out fiber, deionization is washed, 80 DEG C of dry 2h, namely obtains the cotton short fiber of antibiotic conductive, as shown in Figure 1, its schematic surface.
Test shows, the cotton conductive fiber anti-microbial property of preparation is good, reaches FZ/T73023-2006AAA level antibacterial standard; Electric conductivity is good, and sheet resistance is 10-100 Ω/cm, and coating is fine and closely woven evenly and remain the characteristic of original fiber, and soft, color is silver gray.
Embodiment two:
The present embodiment adopts the cotton short fiber of 1g to do matrix fiber.
The first step: oil removing.By 0.1g NaOH, 0.1gOP emulsifying agent, 0.1g washing powder joins in the deionized water of 50mL and dissolves, and bath temperature is 50 DEG C, stirs, and then adds 1 gram of cotton short fiber and stirs 30min.Then fully wash.
Second step: alligatoring.Joined in 50mL deionized water by 5mL NaOH, then add the cotton short fiber that previous step handles well, bath temperature is 55 DEG C, stirs 30min, then fully washes.
3rd step: sensitization.Weighing 0.4g stannous chloride is dissolved in 0.5mL hydrochloric acid, join until completely dissolved in 50mL deionized water, the nylon fibre finally adding previous step process fully stirs 10min again, and temperature is 30 DEG C, the complete rear 1g/L sodium bicarbonate solution of sensitization embathes 3min, more fully washes.
Tetra-Walk: activation.Taking 0.04g silver nitrate is dissolved in a small amount of deionized water, in solution, drip ammoniacal liquor again to solution clarification, then add deionized water to 50mL, the cotton short fiber finally adding previous step process fully stirs 3min, bath temperature is 28 DEG C, and fully washing is clean afterwards.
5th step: deposition of silver.
1,112mL reducing solution is prepared: weigh 0.9g glucose and be fully dissolved in 112mL deionized water;
2,38mL silver liquid ammonia is prepared. weigh 0.5g silver nitrate and be dissolved in a small amount of deionized water, then drip ammoniacal liquor in solution, during beginning, occur precipitation, continue to drip ammoniacal liquor and clarify to solution.Add deionized water again to 38mL, finally add 0.006g nitrilotriacetic acid sodium and be dissolved in wherein.
3, pour in reducing solution by the silver liquid ammonia prepared, shake up, add rapidly the cotton short fiber that the 4th step activates, 30 DEG C are fully stirred 30min.
6th step: take out fiber, deionization is washed, 85 DEG C of dry 2h, namely obtains the cotton short fiber of antibiotic conductive, as shown in Figure 1, its schematic surface.
Test shows, the cotton conductive fiber electric conductivity of preparation is good, and sheet resistance is 7-9 Ω/cm.
Embodiment three:
The present embodiment adopts 1g polyamide fibre to do matrix fiber.
The first step: oil removing.By 0.1gOP emulsifying agent, 0.1g washing powder joins in the deionized water of 60mL and dissolves, and bath temperature is 50 DEG C, stirs, and then adds 1 gram of nylon fibre and stirs 30min, then fully wash.
Second step: alligatoring.Joined in 50mL deionized water by 6mL NaOH, then add the nylon fibre that previous step handles well, bath temperature is 55 DEG C, stirs 30min, fully washes.
3rd step: sensitization.Weighing 0.6g stannous chloride is dissolved in 0.5mL hydrochloric acid, join until completely dissolved in 50mL deionized water, the nylon fibre finally adding previous step process fully stirs 10min again, and temperature is 30 DEG C, the complete rear 1g/L sodium bicarbonate solution of sensitization embathes 3min, more fully washes.
Tetra-Walk: activation.Taking 0.06g silver nitrate is dissolved in a small amount of deionized water, in solution, drip ammoniacal liquor again to solution clarification, then add deionized water to 50mL, the nylon fibre finally adding previous step process fully stirs 3min, bath temperature is 35 DEG C, and fully washing is clean afterwards.
5th step: deposition of silver.
1,112.5mL reducing solution is prepared: weigh 0.9g glucose and be fully dissolved in 112.5mL deionized water;
2,37.5mL silver liquid ammonia is prepared. weigh 0.6g silver nitrate and be dissolved in a small amount of deionized water, in solution, drip ammoniacal liquor again, during beginning, occur precipitation, continue to drip ammoniacal liquor and clarify to solution, add deionized water again to 37.5mL, finally add 0.01g sodium pyrophosphate and be dissolved in wherein.
3, pour in reducing solution by the silver liquid ammonia prepared, shake up, add rapidly the nylon fibre that the 4th step activates, 30 DEG C are fully stirred 30min.
6th step: take out fiber, deionization is washed, 90 DEG C of dry 2h, namely obtains conduction nylon fibre, as shown in Figure 1, its schematic surface.
Test shows, the polyamide fibre conductive fiber anti-microbial property of preparation is good, reaches FZ/T73023-2006AAA level antibacterial standard; Electric conductivity is good, and sheet resistance is 10-100 Ω/cm, and coating is fine and closely woven evenly and remain the characteristic of original fiber, and soft, color is silver gray.
Embodiment four:
The present embodiment adopts 1g cotton to do matrix fiber.
The first step: oil removing.By 0.1gOP emulsifying agent, 0.1g washing powder joins in the deionized water of 60mL and dissolves, and bath temperature is 55 DEG C, stirs, and then adds 1 gram of cotton short fiber and stirs 30min, then fully wash.
Second step: alligatoring.Joined in 50mL deionized water by 6mL NaOH, then add the cotton short fiber that previous step handles well, bath temperature is 55 DEG C, stirs 30min, fully washes.
3rd step: sensitization.Weighing 0.6g stannous chloride is dissolved in 0.5mL hydrochloric acid, join until completely dissolved in 50mL deionized water, the cotton short fiber finally adding previous step process fully stirs 10min again, and temperature is 35 DEG C, the complete rear 1g/L sodium bicarbonate solution of sensitization embathes 3min, more fully washes.
Tetra-Walk: activation.Taking 0.05g silver nitrate is dissolved in a small amount of deionized water, in solution, drip ammoniacal liquor again to solution clarification, then add deionized water to 50mL, the cotton short fiber finally adding previous step process fully stirs 3min, bath temperature is 35 DEG C, and fully washing is clean afterwards.
5th step: deposition of silver.
1,112.5mL reducing solution is prepared: weigh 0.9g glucose and be fully dissolved in 112.5mL deionized water;
2,37.5mL silver liquid ammonia is prepared. weigh 0.7g silver nitrate and be dissolved in a small amount of deionized water, in solution, drip ammoniacal liquor again, during beginning, occur precipitation, continue to drip ammoniacal liquor and clarify to solution, add deionized water again to 37.5mL, finally add 0.009g natrium citricum and be dissolved in wherein.
3, the silver liquid ammonia prepared is poured in reducing solution, shake up.Add rapidly the cotton short fiber that the 4th step activates, 35 DEG C are fully stirred 30min.
6th step: take out fiber, deionization is washed, 100 DEG C of dry 2h, namely obtains the cotton short fiber of antibiotic conductive, as shown in Figure 1, its schematic surface.
Test shows, the cotton conductive fiber anti-microbial property of preparation is good, reaches FZ/T73023-2006AAA level antibacterial standard; Electric conductivity is good, and sheet resistance is 10-100 Ω/cm, and coating is fine and closely woven evenly and remain the characteristic of original fiber, and soft, color is silver gray.
Claims (7)
1. the preparation method of an antibiotic conductive cotton fiber, fall apart hair for raw material with cotton fiber short fiber, it is characterized in that, comprise the steps: to deoil to cotton short fiber, alligatoring, sensitization pre-treatment, add low concentration silver nitrate-ammonia spirit activation, then carry out chemical silvering, add chelating ligands agent when chemical silvering and replace partial ammonia water, after silver-plated, carry out hot setting process.
2. the preparation method of a kind of antibiotic conductive cotton fiber according to claim 1, is characterized in that, described cotton short fiber roughening process adopts alkali treatment, and temperature is 50 DEG C ± 5 DEG C, and dip time is 30 ~ 40min.
3. the preparation method of a kind of antibiotic conductive cotton fiber according to claim 2, is characterized in that, described alkali is NaOH, and the concentration of NaOH is 30 ~ 60ml/l.
4. the preparation method of a kind of antibiotic conductive cotton fiber according to claim 1, it is characterized in that, described sensitization pre-treatment, 15 ~ 18min is flooded under adopting the stannous chloride solution normal temperature of 5 ~ 16g/L, then the cotton fiber after adopting the sodium bicarbonate solution of 1g/L to rinse stannous chloride dipping, clarifies to cleaning solution.
5. the preparation method of a kind of antibiotic conductive cotton fiber according to claim 1, is characterized in that, after described silver nitrate-ammonia spirit activation, the formula carrying out chemical plating liquid is composed as follows:
Reducing solution is filled a prescription: glucose 10 ~ 15g/L;
Oxidation solution is filled a prescription: silver nitrate 10 ~ 20g/L;
Ammoniacal liquor: appropriate;
Chelating ligands agent 0.1 ~ 1.5g/L.
6. the preparation method of a kind of antibiotic conductive cotton fiber according to claim 1, is characterized in that, the chelating ligands agent added in described chemical silvering is nitrilotriacetic acid salt, citrate or pyrophosphate.
7. the preparation method of a kind of antibiotic conductive cotton fiber according to claim 1, is characterized in that, described silver-plated after carry out hot setting process, hot setting is temperature is 80 ~ 100 DEG C, time 5 ~ 7min.
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CN109576989A (en) * | 2018-11-06 | 2019-04-05 | 杭州旭富康科技有限公司 | A kind of preparation method of antibiotic cotton fiber |
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CN106498585A (en) * | 2016-11-29 | 2017-03-15 | 潍坊百禾工艺品有限公司 | A kind of sterilization anti-static fabric, its manufacture method and application |
CN107558051A (en) * | 2017-10-23 | 2018-01-09 | 苏州泰克银纤维科技有限公司 | A kind of Preparation equipment of efficient polyamide fibre conductive fiber |
CN109576989A (en) * | 2018-11-06 | 2019-04-05 | 杭州旭富康科技有限公司 | A kind of preparation method of antibiotic cotton fiber |
CN114774895A (en) * | 2022-03-31 | 2022-07-22 | 莫纶(珠海)新材料科技有限公司 | Al2O3Composite functional fiber and its prepn |
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CN115584627A (en) * | 2022-11-04 | 2023-01-10 | 杭州卡彤服饰有限公司 | Antibacterial socks and preparation method thereof |
CN115584627B (en) * | 2022-11-04 | 2024-01-19 | 炫银纺织技术(杭州)有限公司 | Antibacterial sock and preparation method thereof |
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