WO2008131720A1 - Verfahren zur herstellung einer bioaktiven cellulosefaser mit hohem weissgrad - Google Patents
Verfahren zur herstellung einer bioaktiven cellulosefaser mit hohem weissgrad Download PDFInfo
- Publication number
- WO2008131720A1 WO2008131720A1 PCT/DE2008/000642 DE2008000642W WO2008131720A1 WO 2008131720 A1 WO2008131720 A1 WO 2008131720A1 DE 2008000642 W DE2008000642 W DE 2008000642W WO 2008131720 A1 WO2008131720 A1 WO 2008131720A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- fibers
- nanosilver
- silver
- fiber
- cellulose
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- 230000000975 bioactive effect Effects 0.000 title claims abstract description 12
- 229920003043 Cellulose fiber Polymers 0.000 title claims description 4
- 230000000844 anti-bacterial effect Effects 0.000 claims abstract description 21
- 229920002678 cellulose Polymers 0.000 claims abstract description 12
- 239000001913 cellulose Substances 0.000 claims abstract description 12
- 239000004753 textile Substances 0.000 claims abstract description 9
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 72
- 239000000835 fiber Substances 0.000 claims description 63
- 239000002245 particle Substances 0.000 claims description 14
- 230000008569 process Effects 0.000 claims description 14
- 239000003381 stabilizer Substances 0.000 claims description 13
- 239000000725 suspension Substances 0.000 claims description 12
- -1 wool Polymers 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000000465 moulding Methods 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- 238000009987 spinning Methods 0.000 claims description 9
- ZTHYODDOHIVTJV-UHFFFAOYSA-N Propyl gallate Chemical compound CCCOC(=O)C1=CC(O)=C(O)C(O)=C1 ZTHYODDOHIVTJV-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000004952 Polyamide Substances 0.000 claims description 4
- 229920002647 polyamide Polymers 0.000 claims description 4
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 claims description 3
- 235000010388 propyl gallate Nutrition 0.000 claims description 3
- 150000003512 tertiary amines Chemical class 0.000 claims description 3
- 229920000742 Cotton Polymers 0.000 claims description 2
- 239000004743 Polypropylene Substances 0.000 claims description 2
- 239000004744 fabric Substances 0.000 claims description 2
- 239000002608 ionic liquid Substances 0.000 claims description 2
- 229920001155 polypropylene Polymers 0.000 claims description 2
- XIYUIMLQTKODPS-UHFFFAOYSA-M 1-ethyl-3-methylimidazol-3-ium;acetate Chemical compound CC([O-])=O.CC[N+]=1C=CN(C)C=1 XIYUIMLQTKODPS-UHFFFAOYSA-M 0.000 claims 1
- LFTLOKWAGJYHHR-UHFFFAOYSA-N N-methylmorpholine N-oxide Chemical compound CN1(=O)CCOCC1 LFTLOKWAGJYHHR-UHFFFAOYSA-N 0.000 claims 1
- 238000001891 gel spinning Methods 0.000 claims 1
- 229920000728 polyester Polymers 0.000 claims 1
- 210000002268 wool Anatomy 0.000 claims 1
- 229910052709 silver Inorganic materials 0.000 abstract description 52
- 239000004332 silver Substances 0.000 abstract description 52
- 230000000845 anti-microbial effect Effects 0.000 abstract description 13
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 238000001125 extrusion Methods 0.000 abstract description 3
- 238000004806 packaging method and process Methods 0.000 abstract description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 10
- 229910001385 heavy metal Inorganic materials 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 239000002105 nanoparticle Substances 0.000 description 5
- 229910001961 silver nitrate Inorganic materials 0.000 description 5
- 241000195493 Cryptophyta Species 0.000 description 4
- SJRJJKPEHAURKC-UHFFFAOYSA-N N-Methylmorpholine Chemical compound CN1CCOCC1 SJRJJKPEHAURKC-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 244000005700 microbiome Species 0.000 description 4
- 229920002545 silicone oil Polymers 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 229910021536 Zeolite Inorganic materials 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000010457 zeolite Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 2
- 229920002101 Chitin Polymers 0.000 description 2
- 229920001661 Chitosan Polymers 0.000 description 2
- 229920000433 Lyocell Polymers 0.000 description 2
- 206010052428 Wound Diseases 0.000 description 2
- 208000027418 Wounds and injury Diseases 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000003242 anti bacterial agent Substances 0.000 description 2
- 229940088710 antibiotic agent Drugs 0.000 description 2
- 244000052616 bacterial pathogen Species 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000012496 blank sample Substances 0.000 description 2
- 239000007844 bleaching agent Substances 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002241 glass-ceramic Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000009940 knitting Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 239000000985 reactive dye Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- FHDQNOXQSTVAIC-UHFFFAOYSA-M 1-butyl-3-methylimidazol-3-ium;chloride Chemical compound [Cl-].CCCCN1C=C[N+](C)=C1 FHDQNOXQSTVAIC-UHFFFAOYSA-M 0.000 description 1
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 description 1
- 229920002972 Acrylic fiber Polymers 0.000 description 1
- 101710134784 Agnoprotein Proteins 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 241000199919 Phaeophyceae Species 0.000 description 1
- 241000218657 Picea Species 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- XEFQLINVKFYRCS-UHFFFAOYSA-N Triclosan Chemical compound OC1=CC(Cl)=CC=C1OC1=CC=C(Cl)C=C1Cl XEFQLINVKFYRCS-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229940072056 alginate Drugs 0.000 description 1
- 229920000615 alginic acid Polymers 0.000 description 1
- 235000010443 alginic acid Nutrition 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000002924 anti-infective effect Effects 0.000 description 1
- 239000004599 antimicrobial Substances 0.000 description 1
- 238000004380 ashing Methods 0.000 description 1
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 1
- 230000003385 bacteriostatic effect Effects 0.000 description 1
- 230000008275 binding mechanism Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000004113 cell culture Methods 0.000 description 1
- 230000032823 cell division Effects 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 230000004663 cell proliferation Effects 0.000 description 1
- 238000001516 cell proliferation assay Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000013270 controlled release Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 210000000805 cytoplasm Anatomy 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000368 destabilizing effect Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000000855 fungicidal effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 239000002674 ointment Substances 0.000 description 1
- 229920006149 polyester-amide block copolymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002516 radical scavenger Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229940100890 silver compound Drugs 0.000 description 1
- 150000003379 silver compounds Chemical class 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 239000000606 toothpaste Substances 0.000 description 1
- 230000002110 toxicologic effect Effects 0.000 description 1
- 231100000027 toxicology Toxicity 0.000 description 1
- 229960003500 triclosan Drugs 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 239000003357 wound healing promoting agent Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- 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
-
- 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
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
-
- 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
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/02—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from solutions of cellulose in acids, bases or salts
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
- Y10T442/20—Coated or impregnated woven, knit, or nonwoven fabric which is not [a] associated with another preformed layer or fiber layer or, [b] with respect to woven and knit, characterized, respectively, by a particular or differential weave or knit, wherein the coating or impregnation is neither a foamed material nor a free metal or alloy layer
- Y10T442/2525—Coating or impregnation functions biologically [e.g., insect repellent, antiseptic, insecticide, bactericide, etc.]
Definitions
- the invention relates to a process for the production of cellulosic moldings by the dry-wet extrusion process (Lyocellclar) with bioactive effect and high whiteness for use in the clothing sector and papermaking.
- bioactive denotes the antimicrobial activity which is based on the bactericidal effect of the element silver, which is used to increase its effectiveness as a nanoscale reagent. and used in casual wear and papers with high storage stability, uses in the medical field, for example for wound dressings, hospital textiles and in the filter and packaging industry are possible.
- silver is used more strongly today as a natural alternative to antibiotics.
- Contact with silver kills microorganisms such as bacteria, spores, mold and other fungi.
- the attack follows by destroying the enzymes that transport the nutrients for the cell, destabilizing the cell membrane and the cytoplasm, and finally disrupting cell division and proliferation [Hörn, Fraunhofer magazine 1, (2003)].
- the bactericidal concentration is the case of silver with 0.01 - given 1 mg / 1 [N Ullman's Encyclopedia of Industrial Chemischen mistry, 5th edition, Volume A, p.160, VCH (1993).].
- the effect of silver ions is used in a wide variety of applications. As is known, the silver can come into effect in gel-like suspensions or in or on fibers.
- WO2007 / 017901 a gel compound with nanoscale silver particles for direct wound treatment is described.
- nanosilver is used for ointments and toothpastes.
- Antimicrobial personal care products containing nanosilver on / in a polymer matrix are disclosed by DE60022344.
- US2002 / 0145132 describes the dispersion of nanoscale metal precursor particles in a polymer matrix (including cellulose) with subsequent evaporation of the solvent, reduction of the metal precursor particles and their fixation in the matrix by UV radiation.
- the molar ratio of metal to matrix is at least 1: 100.
- Cellulosic fibers with bacteriostatic or bactericidal properties are also used.
- a fiber having antimicrobial activity according to DE60119150 is obtained.
- nanoparticles are introduced into a cellulose fiber. These fibers show bactericidal properties, but concentrations in the range of 0.1-15 Ma.% Are necessary.
- the fiber shows a Nachfärbe capable from weak to strong brown and the mixing of the metal nanoparticles is a highly exothermic process, cooling to temperatures below 120 0 C absolutely necessary.
- the nanoparticles are preferably introduced in powder form, small agglomerations are accepted.
- the moldings are able to adsorb metals from heavy metal-containing media.
- the heavy metal loaded moldings can be used as a bactericidal and / or fungicidal material.
- the content of adsorbed heavy metals in these cellulosic shaped bodies is given as at least 70 mg / kg, based on the total weight. It is further stated that by dipping the fiber having a brown algae content of 11.39 mass%, based on the weight of the fiber, into a 0.05 M AgNO 3 solution, a silver content of 1855 mg / kg fiber was achieved. Since algae are natural products, the relatively limited binding capacities for heavy metals vary.
- the object of the invention is to develop a cellulosic molding and a process for the production of cellulosic moldings having an antibacterial effect and, at the same time, a high degree of whiteness for use in the clothing sector, papermaking, medicine and hygiene White goods and high-quality papers with high storage stability are to be used, and in order to ensure an even distribution of the particles silver suspensions should be used which show no agglomerate formation without further stabilizing agents.
- the object is achieved by using a highly active nanosilver in a chemically reduced form, for. B. according to EP1621217.
- a highly active nanosilver in a chemically reduced form, for. B. according to EP1621217.
- nanosilver with particle sizes of 5 - 20 nm as a suspension in non-aqueous liquids, it is possible to reduce the silver content to amounts of 0.0025%, based on the fiber, preferably 0.01%. These small amounts guarantee a low intrinsic color with a high degree of whiteness and at the same time still show an antibacterial effect.
- Integrating nanosilver into the fiber as metal offers the following advantages over the methods described above:
- Nanoparticles therefore often have significant differences in their mechanical, optical, electrical and magnetic properties compared to their coarse-grained counterparts.
- the atoms are in an elevated energetic state because they have a smaller number of nearest neighbors with which they interact. This leads to increased chemical or catalytic reactivity [Rössler, A. et al. , Chemistry in Our Time, 1, pp. 32-41 (2001)].
- Nanoscale silver therefore has a significantly higher antimicrobial effectiveness than conventional silver products with particle sizes of more than 500 nm because of the extremely large surface area.
- the formation of an oxide layer (Ag 2 O) is accelerated by the strong porosity. In this layer, the necessary for a bactericidal action silver ions (Ag + ) are present:
- the fibers Due to the high bactericidal effect of the nanosilver, it is not necessary to load the fiber with large silver concentrations. With concentrations below 0.01 Ma. -% of the fibers produced already reach an antimicrobial effect. Higher loaded fibers with concentrations of up to 5000 ppm can also be prepared by the process described without detrimental effects on the spinning safety, thermal stability and the textile-physical parameters. These fibers can be made by mixing with other fibers, such as. As cotton or synthetic fibers are brought to desired levels of silver in the yarn to be produced. This procedure allows a very economical production of bactericidal yarns. Likewise, the fibers can be processed into textile fabrics, expediently in admixture with other fibers, or into papers.
- bioactive fiber is done by the lyocell method.
- cellulose is dissolved in a solvent with the addition of stabilizers and spun by the dry-wet extrusion process to cellulosic fibers or warped into films.
- stabilizers for the spinning solution is required in order to maintain the thermal stability and to counteract the degradation of the cellulose and the solvent, which starts under technical conditions.
- Stabilizers used are pH-stabilizing and complexing substances and / or radical scavengers.
- the combination of gallic acid propyl ester, hydroxylamine and sodium hydroxide solution from WO1995 / 08010 is a stabilized stabilizer system which is well-recognized and has proven itself under industrial conditions.
- the solvent may be aqueous tertiary amine oxide, preferably A7 methylmorpholine ⁇ f-oxide (NMMO) or an ionic liquid, preferably 1-N-butyl-3-methylimidazolium chloride.
- the silver can be processed in the form of a suspension of nanosilver with particle sizes of 5 - 20 nm.
- liquids with low vapor pressure eg. As silicone oil, used without stabilizing agent.
- the addition takes place in the form of a nanosilver suspension in order to avoid agglomeration.
- the nanosilver suspension is applied directly to the pulp prior to the addition of solvent and stabilizer to later achieve a homogeneous distribution of the nanosilver particles in the spinning solution and later in the fiber.
- the invention is described in more detail in the following examples.
- the silver content in the fiber was determined by atomic absorption spectrometry after dry ashing.
- the antimicrobial activity was measured using a proliferation assay from Bio-Gate AG (NUMETRIKA TM, Bechert et al.). Nature Medicine 6, 1053-1056 (2000)).
- microorganisms are selectively applied to the specimens. After a complex but rapid, parallelized procedure, it is then tested whether adhering microorganisms can still multiply. If this growth is prevented by the special properties of the materials, the material is called antimicrobial.
- the so-called onset OD serves as a quantifiable parameter. This is the number of hours required for the remaining daughter cells to eventually grow to a cell culture of specific optical density (0.2 OD). Anti-microbial efficacy is always measured as the difference compared to a non-antimicrobial so-called blank.
- the degree of whiteness was determined according to DIN 5033 with the device datacolor SF600 (measuring conditions: with gloss, type of light D65 / 10 0 ) before and after 62 h exposure with a xenon radiator. A high value means a higher degree of whiteness.
- NMMO N-methylmorpholine W-oxide
- spruce pulp with a residual moisture content of 6.1 Ma. % and a degree of polymerization (DP) of about 500 and 3.375 g nanosilver (0.8% silver in silicone oil, NanoSilver BG TM, 5-20 nm).
- the nanosilver was applied directly to the pulp to guarantee a homogeneous distribution in the solution.
- the reactor was closed and the mash stirred for 15 minutes at room temperature and then applied vacuum of 30 mbar.
- the solution was homogenized in a kneader and the temperature increased in steps to 90 0 C. Subsequently, this spinning solution was spun at 9O 0 C through a spinneret with 480 holes and a nozzle hole diameter of 80 microns. The take-off speed was 30 m / min.
- the multifilament yarn was passed through several wash baths to wash out the NMMO. The fibers were cut to 60 mm and dried.
- Example 2 The fibers were prepared according to Example 1 and spun. 6.75 g of nano-silver (0.8% silver in silicone oil, NanoSilver BG TM, 5-20 nm) was added.
- Example 3 The fibers were prepared according to Example 1 and spun. 13.5 g of nano silver (0.8% silver in silicone oil, NanoSilver BG TM, 5-20 nm) was added. Table 1 .
- the concentrations were therefore set very low at 0.005-0.02% in order to determine the lower limit of the range of application. Due to the very low levels of silver, no influence on the textile-physical parameters can be seen. However, the recovery rate of silver is only about 50%.
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Nanotechnology (AREA)
- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Artificial Filaments (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
Description
Claims
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US12/451,113 US20100124861A1 (en) | 2007-04-25 | 2008-04-15 | Method for the production of a bioactive cellulose fiber with a high degree of whiteness |
GB0918682A GB2460993B (en) | 2007-04-25 | 2008-04-15 | Method for the production of a bioactive cellulose fiber with a high degree of brightness |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102007019768.5 | 2007-04-25 | ||
DE200710019768 DE102007019768A1 (de) | 2007-04-25 | 2007-04-25 | Verfahren zur Herstellung einer bioaktiven Cellulosefaser mit hohem Weißgrad |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2008131720A1 true WO2008131720A1 (de) | 2008-11-06 |
Family
ID=39685979
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/DE2008/000642 WO2008131720A1 (de) | 2007-04-25 | 2008-04-15 | Verfahren zur herstellung einer bioaktiven cellulosefaser mit hohem weissgrad |
Country Status (4)
Country | Link |
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US (1) | US20100124861A1 (de) |
DE (1) | DE102007019768A1 (de) |
GB (1) | GB2460993B (de) |
WO (1) | WO2008131720A1 (de) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2010025858A2 (de) * | 2008-09-02 | 2010-03-11 | Thüringisches Institut für Textil - und Kunststoff-Forschung e.V. | Funktionelle cellulosische formkörper |
CN101619501B (zh) * | 2009-08-14 | 2012-02-15 | 东华大学 | 一种直径可控的高分子超细纤维的制备方法 |
Families Citing this family (12)
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DE102009010968A1 (de) * | 2009-02-27 | 2010-09-02 | Flockfaser GmbH Thüringen | Antibakteriell aktive Flockfasern |
US20120094120A1 (en) | 2010-10-18 | 2012-04-19 | PurThread Technologies, Inc. | Enhancing and preserving anti-microbial performance in fibers with pigments |
CN102453968B (zh) * | 2010-11-03 | 2016-01-20 | 广东百合医疗科技股份有限公司 | 含纳米金属的抗菌性纤维、织物和伤口敷料及其制备方法 |
US20120164449A1 (en) * | 2010-12-23 | 2012-06-28 | Stephen Woodrow Foss | Fibers with improving anti-microbial performance |
GB2511528A (en) | 2013-03-06 | 2014-09-10 | Speciality Fibres And Materials Ltd | Absorbent materials |
WO2015023644A2 (en) | 2013-08-12 | 2015-02-19 | PurThread Technologies, Inc. | Antimicrobial and antifungal polymer fibers, fabrics, and methods of manufacture thereof |
US9878480B1 (en) | 2014-06-24 | 2018-01-30 | PurThread Technologies, Inc. | Method for making polymer feedstock usable for generation of fiber having anti-microbial properties |
TWI565853B (zh) | 2015-05-11 | 2017-01-11 | Acelon Chem & Fiber Corp | Preparation of nano - silver blended natural cellulose melt - blown non - woven |
TWI565852B (zh) | 2015-05-11 | 2017-01-11 | Acelon Chem & Fiber Corp | Preparation of Nano silver blended natural cellulose fibers method |
TWI551739B (zh) | 2015-05-11 | 2016-10-01 | Acelon Chem & Fiber Corp | 製備奈米銀掺混天然纖維素紡黏不織布的方法 |
CN113417168A (zh) * | 2021-07-06 | 2021-09-21 | 东莞市鼎丰印刷有限公司 | 一种具有银离子自动除菌纸功能的纸及其制造方法 |
EP4187004A1 (de) | 2021-11-25 | 2023-05-31 | AGXX Intellectual Property Holding GmbH | Fasermaterial mit antimikrobieller und geruchsneutralisierender wirkung |
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- 2008-04-15 WO PCT/DE2008/000642 patent/WO2008131720A1/de active Application Filing
- 2008-04-15 GB GB0918682A patent/GB2460993B/en not_active Expired - Fee Related
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Also Published As
Publication number | Publication date |
---|---|
US20100124861A1 (en) | 2010-05-20 |
DE102007019768A1 (de) | 2008-11-13 |
GB2460993A (en) | 2009-12-23 |
GB0918682D0 (en) | 2009-12-09 |
GB2460993B (en) | 2011-12-07 |
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