NO783459L - FILAMENTS OF REGENERATED CELLULOSE AND PROCEDURE FOR THEIR PREPARATION - Google Patents
FILAMENTS OF REGENERATED CELLULOSE AND PROCEDURE FOR THEIR PREPARATIONInfo
- Publication number
- NO783459L NO783459L NO783459A NO783459A NO783459L NO 783459 L NO783459 L NO 783459L NO 783459 A NO783459 A NO 783459A NO 783459 A NO783459 A NO 783459A NO 783459 L NO783459 L NO 783459L
- Authority
- NO
- Norway
- Prior art keywords
- viscose
- cellulose
- filaments
- emulsion
- weight
- Prior art date
Links
- 239000004627 regenerated cellulose Substances 0.000 title claims description 13
- 238000000034 method Methods 0.000 title claims description 11
- 229920000297 Rayon Polymers 0.000 claims description 57
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 40
- 229920000642 polymer Polymers 0.000 claims description 33
- 229920002678 cellulose Polymers 0.000 claims description 25
- 239000001913 cellulose Substances 0.000 claims description 25
- 239000000839 emulsion Substances 0.000 claims description 24
- 239000004793 Polystyrene Substances 0.000 claims description 22
- 229920002223 polystyrene Polymers 0.000 claims description 22
- 238000009987 spinning Methods 0.000 claims description 13
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 12
- 238000002347 injection Methods 0.000 claims description 12
- 239000007924 injection Substances 0.000 claims description 12
- 239000006224 matting agent Substances 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 8
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 6
- 238000001125 extrusion Methods 0.000 claims description 5
- 230000008929 regeneration Effects 0.000 claims description 4
- 238000011069 regeneration method Methods 0.000 claims description 4
- 239000000835 fiber Substances 0.000 description 31
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 27
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 16
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 13
- 235000011121 sodium hydroxide Nutrition 0.000 description 9
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 229910052938 sodium sulfate Inorganic materials 0.000 description 5
- 235000011152 sodium sulphate Nutrition 0.000 description 5
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 5
- 229960001763 zinc sulfate Drugs 0.000 description 5
- 229910000368 zinc sulfate Inorganic materials 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 2
- 239000005642 Oleic acid Substances 0.000 description 2
- 239000005708 Sodium hypochlorite Substances 0.000 description 2
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 239000003995 emulsifying agent Substances 0.000 description 2
- 238000007720 emulsion polymerization reaction Methods 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- 239000000344 soap Substances 0.000 description 2
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 2
- 229910052979 sodium sulfide Inorganic materials 0.000 description 2
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 2
- 125000003011 styrenyl group Chemical group [H]\C(*)=C(/[H])C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- QIVUCLWGARAQIO-OLIXTKCUSA-N (3s)-n-[(3s,5s,6r)-6-methyl-2-oxo-1-(2,2,2-trifluoroethyl)-5-(2,3,6-trifluorophenyl)piperidin-3-yl]-2-oxospiro[1h-pyrrolo[2,3-b]pyridine-3,6'-5,7-dihydrocyclopenta[b]pyridine]-3'-carboxamide Chemical compound C1([C@H]2[C@H](N(C(=O)[C@@H](NC(=O)C=3C=C4C[C@]5(CC4=NC=3)C3=CC=CN=C3NC5=O)C2)CC(F)(F)F)C)=C(F)C=CC(F)=C1F QIVUCLWGARAQIO-OLIXTKCUSA-N 0.000 description 1
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 201000004624 Dermatitis Diseases 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 description 1
- RSWGJHLUYNHPMX-ONCXSQPRSA-N abietic acid Chemical compound C([C@@H]12)CC(C(C)C)=CC1=CC[C@@H]1[C@]2(C)CCC[C@@]1(C)C(O)=O RSWGJHLUYNHPMX-ONCXSQPRSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 208000010668 atopic eczema Diseases 0.000 description 1
- JXLHNMVSKXFWAO-UHFFFAOYSA-N azane;7-fluoro-2,1,3-benzoxadiazole-4-sulfonic acid Chemical compound N.OS(=O)(=O)C1=CC=C(F)C2=NON=C12 JXLHNMVSKXFWAO-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000005108 dry cleaning Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012510 hollow fiber Substances 0.000 description 1
- 239000008240 homogeneous mixture Substances 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 231100000989 no adverse effect Toxicity 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 238000007383 open-end spinning Methods 0.000 description 1
- 150000001451 organic peroxides Chemical class 0.000 description 1
- 125000000864 peroxy group Chemical group O(O*)* 0.000 description 1
- JRKICGRDRMAZLK-UHFFFAOYSA-L persulfate group Chemical group S(=O)(=O)([O-])OOS(=O)(=O)[O-] JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000151 polyglycol Polymers 0.000 description 1
- 239000010695 polyglycol Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000012966 redox initiator Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 1
- 239000004289 sodium hydrogen sulphite Substances 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008961 swelling Effects 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
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
- D01F2/12—Addition of delustering agents to the spinning solution
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Artificial Filaments (AREA)
Description
Filamenter av regenerert cellulose og fremgangsmåte tilFilaments of regenerated cellulose and method thereof
deres fremstilling.their production.
Foreliggende oppfinnelse vedrører filamenter av regenerert cellulose og fremgangsmåte til deres fremstilling. The present invention relates to filaments of regenerated cellulose and a method for their production.
De fleste regenererte cellulosefilamenter fremstilles som fullstendig masse eller halvmatte filamenter inneholdende et matteringsmiddel. Titandioksyd er det mest vanlig benyttede matteringsmiddel for slike filamenter som for de fleste andre. Det har noen ulemper som motvirker dets utmerkede lysspredende egenskaper; det er en katalysator for fotonedbryt-ning av cellulose og noen fargestoffer, og er et slipemiddel slik at bruken av matte viskosefibre i open-erid spinning og i skåret luvstoff slik som cordfløyel, er begrenset. Et alterna-tivt matteringsmiddel som gir god matthet uten disse ulemper ville være ønskelig for mange formål. Most regenerated cellulose filaments are produced as fully pulped or semi-matted filaments containing a matting agent. Titanium dioxide is the most commonly used matting agent for such filaments as for most others. It has some drawbacks that counteract its excellent light diffusing properties; it is a catalyst for the photodecomposition of cellulose and some dyes, and is an abrasive so that the use of matte viscose fibers in open-erid spinning and in cut pile fabrics such as corduroy is limited. An alternative matting agent which gives good matting without these disadvantages would be desirable for many purposes.
Ifølge foreliggende oppfinnelse inneholder regenererte cellulosefilamenter som matteringsmiddel 0,5 - 5 vekt-%, basert på cellulose, av partikler av en styrenpolymer avledet fra en emulsjon av denne polymer. According to the present invention, regenerated cellulose filaments contain as matting agent 0.5 - 5% by weight, based on cellulose, of particles of a styrene polymer derived from an emulsion of this polymer.
Styrenpolymeren er en polymer omfattende minstThe styrene polymer is a polymer comprising at least
50 vekt-% styrenenheter. Den utgjøres fortrinnsvis av polystyren (styren-homopolymer) eller en kopolymer av styren inneholdende over 90 vek. t-% styrenenheter med små mengder av enheter av en eller flere andre vinylaromatiske monomerer, f.eks. divinyl-benzen. Polymerpartiklene i emulsjonen er fortrinnsvis mindre enn 5 micron, f.eks. 0,5 - 2,0 micron, i diameter. De er fortrinnsvis fremstilt ved emulsjonspolymerisasjon. 50% by weight styrene units. It preferably consists of polystyrene (styrene homopolymer) or a copolymer of styrene containing more than 90 wt. t-% styrene units with small amounts of units of one or more other vinylaromatic monomers, e.g. divinylbenzene. The polymer particles in the emulsion are preferably smaller than 5 microns, e.g. 0.5 - 2.0 micron, in diameter. They are preferably produced by emulsion polymerization.
S£y:Een-emuls j onspolymerisasj on kan oppnås under anvendelse av et konvensjonelt emulgeringsmiddel, f.eks. et alkyl-arensulfonat, en fettsyresåpe, en kolofoniumsyresåpe eller et kationisk emulgeringsmiddel, og en initiator, f.eks. et persul-fat, hydrogenperoksyd, et organisk peroksyd eller hydroperoksyd, eller et redoks-initiatorsystem, hvori en peroksy-initiator anvendes i forbindelse med et reduksjonsmiddel slik som et ferro-salt eller natriumbisulfitt. S£y:One-emulsion polymerization can be achieved using a conventional emulsifier, e.g. an alkyl arene sulphonate, a fatty acid soap, a rosin acid soap or a cationic emulsifier, and an initiator, e.g. a persulphate, hydrogen peroxide, an organic peroxide or hydroperoxide, or a redox initiator system, in which a peroxy initiator is used in conjunction with a reducing agent such as a ferrous salt or sodium bisulphite.
Ifølge foreliggende oppfinnelse er det også til-veiebrakt en fremgangsmåte til fremstilling av mattert regenerert cellulosefilamenter ved ekstrudering av viskose gjennom en spinndyse inn i en regenereringsoppløsning, idet en emulsjon av en styrenpolymer tilsettes til viskosen i en mengde på 0,5 - 5 vekt-% styrenpolymer basert på cellulose, før viskosen ekstruderes. According to the present invention, there is also a method for the production of mat regenerated cellulose filaments by extruding viscose through a spinning nozzle into a regeneration solution, an emulsion of a styrene polymer being added to the viscose in an amount of 0.5 - 5% by weight styrene polymer based on cellulose, before the viscose is extruded.
Viskosen inneholder vanligvis 6-10 vekt-% cellulose og 4,5 - 7»5vekt-% natriumhydroksyd. Regenereringsopp-løsningen inneholder vanligvis svovelsyre, f.eks. i en mengde på 6 - 12 vekt-%, natriumsulfat, f.eks< i en mengde på 10 - 26 vekt-%, og zinksulfat, f.eks. i en mengde på 0,5 - 6,0 vekt-%. The viscose usually contains 6-10% by weight cellulose and 4.5-7.5% by weight sodium hydroxide. The regeneration solution usually contains sulfuric acid, e.g. in an amount of 6 - 12% by weight, sodium sulfate, e.g. < in an amount of 10 - 26% by weight, and zinc sulfate, e.g. in an amount of 0.5 - 6.0% by weight.
Tilsetningen av polystyrenemulsjon til viskoseThe addition of polystyrene emulsion to viscose
for spinning av regenererte cellulosefibre er beskrevet i japansk patent nr. 40-9063-Polystyrenen anvendes i en mengde på 13 - 26% basert på cellulose, for dannelse av fibre med hult, flattrykt tverrsnitt. Man har funnet at de metoder som beskrives innevnte japanske patent i virkeligheten ikke leder til hule fibre; de fibre som dannes er meget svake, men er ikke hule. for spinning regenerated cellulose fibers is described in Japanese patent no. 40-9063-The polystyrene is used in an amount of 13 - 26% based on cellulose, for the formation of fibers with a hollow, flattened cross-section. It has been found that the methods described in the aforementioned Japanese patent do not in reality lead to hollow fibers; the fibers that are formed are very weak, but are not hollow.
Japansk patent nr. 47_32119 beskriver dannelseJapanese Patent No. 47_32119 describes formation
av fibre ved ekstrudering av en blanding av en styren-butadien-kopolymeremulsjon med viskose inn i en vandig oppløsning av svovelsyre og metanol. De dannede fibre er basert hovedsaklig på kopolymeren snarere enn regenerert cellulose, idet vektfor-holdet mellom kopolymer og cellulose er omkring 2,5:1. of fibers by extruding a mixture of a styrene-butadiene copolymer emulsion with viscose into an aqueous solution of sulfuric acid and methanol. The fibers formed are based mainly on the copolymer rather than regenerated cellulose, the weight ratio between copolymer and cellulose being around 2.5:1.
Polymeremulsjonen tilsettes fortrinnsvis til viskosen kort før ekstrudering for dannelse av filamenter. I en foretrukken fremgangsmåte blir en emulsjon av styrenpolymeren innsprøytet i en strøm av viskose kort før den ekstruderes. The polymer emulsion is preferably added to the viscose shortly before extrusion to form filaments. In a preferred method, an emulsion of the styrene polymer is injected into a stream of viscose card shortly before it is extruded.
Man anvender i dag enkelte ganger et innsprøytningsapparatAn injection device is sometimes used today
for innjisering av fargestoffer i viskose før ekstrudering og et slikt innsprøytningsapparat er regnet for innjisering av polymeremulsj onen. for injecting dyes into viscose before extrusion and such an injection device is designed for injecting the polymer emulsion.
Styrenpolymer-emulsjonen'kan alternativt blandesAlternatively, the styrene polymer emulsion can be mixed
med en liten mengde viskose, f.eks. ved 20 - 80 vekt-% styrenpolymer basert på cellulose, for dannelse av en innsprøytnings-emulsjon som innjiseres i hovedstrømmen av viskose kort før den ekstruderes. with a small amount of viscose, e.g. at 20 - 80% by weight of styrene polymer based on cellulose, to form an injection emulsion which is injected into the main stream of viscose card before it is extruded.
Mengden av polymeremulsjonen som tilsettes til viskosen er 0,5 - 5 vekt-% polymer, baserf på cellulose. The amount of the polymer emulsion added to the viscose is 0.5-5% by weight polymer, based on cellulose.
F.eks. kan ca. 1% polymer anvendes ved fremstilling av halvmatte filamenter og omkring 3% ved fremstilling av helt matte filamenter. Polymeren tilsettes fortrinnsvis til viskosen som en vandig emulsjon med konsentrasjon på 20 - 70 vekt-% polymer. Man har funnet at natriumhydroksydet i viskosen ikke ned-bryter polymeremulsjonen slik at polymerpartiklene forblir som adskilte partikler ved ekstruderingen, regenereringen, vaskingen og tørkingen. Polymerpartiklene fjernes ikke ved normal vasking av filamentene eller av fibre, garn og stoffer som er frem- E.g. can approx. 1% polymer is used in the production of semi-matte filaments and around 3% in the production of completely matte filaments. The polymer is preferably added to the viscose as an aqueous emulsion with a concentration of 20 - 70% polymer by weight. It has been found that the sodium hydroxide in the viscose does not break down the polymer emulsion so that the polymer particles remain as separate particles during extrusion, regeneration, washing and drying. The polymer particles are not removed by normal washing of the filaments or of fibres, yarns and substances that are
stilt fra disse.posed from these.
Forskjellige typer regenererte cellulosefilamenter, slik som høyvåtmodul-fibre og viskosefilamentgarn samt konven-sjonelle stabelfibre, kan fremstilles ifølge foreliggende oppfinnelse. Styrenpolymeren kan anvendes som et matteringsmiddel i hule filamenter fremstilt fra en viskose inneholdende 3 - 4 vekt-% natriumkarbonat, f.eks. som beskrevet i britisk patent nr. I.283.529. Det hule tverrsnitt oppstår fra bruk av natriumkarbonat og modifiseres ikke ved bruk av styrenpolymer-emulsjonen. Different types of regenerated cellulose filaments, such as high wet modulus fibers and viscose filament yarns as well as conventional staple fibers, can be produced according to the present invention. The styrene polymer can be used as a matting agent in hollow filaments produced from a viscose containing 3-4% by weight sodium carbonate, e.g. as described in British Patent No. I,283,529. The hollow cross-section arises from the use of sodium carbonate and is not modified by the use of the styrene polymer emulsion.
Polymerpartiklene, spesielt polystyren, er over-raskende effektive som matteringsmidler. Deres matterende effekt er større enn det man ville kunne forutsi fra forskjellen i brytningsindeks mellom regenerert cellulose og polystyren. The polymer particles, especially polystyrene, are surprisingly effective as matting agents. Their matting effect is greater than one would predict from the difference in refractive index between regenerated cellulose and polystyrene.
Fibre inneholdende styrenpolymer-matteringsmiddelet har et mykt grep og gir ikke opphav til slitasjeproblemer på apparater slik som open-end spinning-maskiner, garnføringer og cordfløyel-skjaSreredskaper. Fibrene er mindre foto-nedbrytbare enn fibre inneholdende titandioksyd. Styrenpolymeren har ingen uheldig innvirkning på farvbarheten og den blir ikke fjernet ved vasking ellert <b'ørr-rensning. Fibers containing the styrene polymer matting agent have a soft grip and do not give rise to wear problems on devices such as open-end spinning machines, yarn guides and corduroy cutting tools. The fibers are less photo-degradable than fibers containing titanium dioxide. The styrene polymer has no adverse effect on dyeability and it is not removed by washing or dry cleaning.
Oppfinnelsen illustreres ytterligere ved følgende eksempler, hvori delangivelsene og prosentangivelsene er ved vekt. The invention is further illustrated by the following examples, in which the parts and percentages are by weight.
Eksemgel_lEczema gel_l
Viskose ble fremstilt ved bløting av tremasse av opplysningskvalitet i 18% kaustisk soda, fulgt av pressing 2,8 ganger massevekten. Den ble for-eldet i 24 timer ved 20°C, deretter sulfidert med 33% karbondisulfid basert på cellulose i 2 timer og oppløst i en fortynnet vandig natriumhydroksyd oppløsning. Den fremstilte viskose omfattet 8,5% cellulose og 6, 0% natriumhydroksyd og hadde en viskositet på 60 poise. Viscose was produced by soaking wood pulp of lighting quality in 18% caustic soda, followed by pressing 2.8 times the pulp weight. It was pre-aged for 24 hours at 20°C, then sulphided with 33% carbon disulphide based on cellulose for 2 hours and dissolved in a dilute aqueous sodium hydroxide solution. The produced viscose comprised 8.5% cellulose and 6.0% sodium hydroxide and had a viscosity of 60 poise.
Viskosen ble modnet til et salt-tall på 6,0, deretter ble en 50% vandig polystyren-emulsjon ("Vinamul 7700") med en midlere partikkelstørrelse på 1 micron innjisert og umiddelbart godt blandet i en in-line-blandeinnretning. Mengden av innjisert polystyren var 3,0% basert på cellulose. The viscose was matured to a salt number of 6.0, then a 50% aqueous polystyrene emulsion ("Vinamul 7700") with an average particle size of 1 micron was injected and immediately well mixed in an in-line mixer. The amount of injected polystyrene was 3.0% based on cellulose.
Nesten umiddelbart etter blandingen og ved en saltverdi på 5, 9, ble viskosen ekstrudert gjennom 10.000 hull-stråledyser, hver med en diameter på 62 micron, inn i et spinnebad bestående av 10,0% svovelsyre, 23% natriumsulfat og 1,0% zinksulfat ved 50°C for dannelse av en fiberkabel av regenererte cellulosefilamenter. Fiberkabelen ble strukket 54%, oppdelt til 51 mm stabellengde og fiksert, vasket, avsvovlet og bleket på en måte som er vanlig ved behandling av regenererte cellulosefibre. Filamentene hadde et mål på Almost immediately after mixing and at a salt value of 5.9, the viscose was extruded through 10,000 hole jet nozzles, each 62 micron in diameter, into a spinning bath consisting of 10.0% sulfuric acid, 23% sodium sulfate and 1.0% zinc sulfate at 50°C to form a fiber cable of regenerated cellulose filaments. The fiber cable was stretched 54%, split into 51 mm stack length and fixed, washed, desulfurized and bleached in a manner common to the processing of regenerated cellulosic fibers. The filaments had a target on them
2,2 decitex. En myk finish av såpe-oljesyre ble påført etter den siste vasken i den siste operasjonskjeden. 2.2 decitex. A soft finish of soap-oleic acid was applied after the last wash in the last chain of operations.
De tørkede fibre hadde et godt, fullmatt utseende, dvs. matt, men ikke krittaktig. De fysikalske egenskaper til fibrene var de samme som for lignende fibre uten polystyren med den unntagelse at den spesifikke bruddspenning var noe lavere (2 - 3%)- Når fibrene ble tverrsnitt-undersøkt under et mikroskop, så man at fibrene var helt frie for oppsvulmet garn. Analyse viste at alt polystyren som var innsprøytet, var tilstede i fibrene, innen målemetodens nøyaktighetsgrenser. Polystyren var tilbake selv etter 50 kommersielle vaskinger. The dried fibers had a good fully matte appearance, i.e. matte but not chalky. The physical properties of the fibers were the same as for similar fibers without polystyrene with the exception that the specific breaking stress was somewhat lower (2 - 3%) - When the fibers were cross-sectionally examined under a microscope, it was seen that the fibers were completely free of swelling yarn. Analysis showed that all the polystyrene that had been injected was present in the fibres, within the measurement method's accuracy limits. The polystyrene was back even after 50 commercial washes.
Ekserngel_ 2Ex-Angel_ 2
Det ble fremstilt en viskosesammensetning inneholdende 8,6% cellulose, 6,0% natriumhydroksyd og 32% (basert på cellulose) karbondisulfid. Viskosen hadde et. kulefall på 40 sekunder. En 50% vandig emulsjon av polystyren ("Vinamul 7700") ble omrørt i viskosen i en mengde som ga 4 vekt-% polystyren beregnet på cellulose. Viskosen ble avluftet, filtrert og deretter bundet ved en saltverdi på 5,7, inn i et bad inneholdende 8,5% svovelsyre, 1,0% zinksulfat og 17,5 natriumsulfat ved 50°C under anvendelse av en 27 hull-jet, hulldiameter 127 micron. Spinnehastigheten var 65 m/min., og 20% luftstrekk ble påført. Garndenier-verdien var 330 decitex. Garnet ble vasket i kake-form, avsvovlet med natriumsulfidoppløsning, bleket med natrium-hypoklorittoppløsning, surgjort med fortynnet saltsyre, og etter vasking for oppnåelse av syrefritt materiale ble det gitt en mineralolje-finish før sentrifugering og tørking. Man fikk et ubetydelig tap av polystyren. Produktet var et viskosefilamentgarn med et godt, matt utseende. A viscose composition containing 8.6% cellulose, 6.0% sodium hydroxide and 32% (based on cellulose) carbon disulfide was prepared. Viscose had a. bullet drop in 40 seconds. A 50% aqueous emulsion of polystyrene ("Vinamul 7700") was stirred into the viscose in an amount giving 4% by weight of polystyrene based on cellulose. The viscose was deaerated, filtered and then bound at a salt value of 5.7, into a bath containing 8.5% sulfuric acid, 1.0% zinc sulfate and 17.5% sodium sulfate at 50°C using a 27 hole jet, hole diameter 127 micron. The spinning speed was 65 m/min, and 20% air stretch was applied. The yarn denier value was 330 decitex. The yarn was washed in cake form, desulfurized with sodium sulfide solution, bleached with sodium hypochlorite solution, acidified with dilute hydrochloric acid, and after washing to obtain acid-free material, given a mineral oil finish before centrifugation and drying. An insignificant loss of polystyrene was obtained. The product was a viscose filament yarn with a good matte appearance.
Eksemp_<e>l_2Example_<e>l_2
Det ble fremstilt en viskosesammensetning inneholdende 9,6% cellulose, 7,2% natriumhydroksyd og 33% (basert på cellulose) karbondisulfid. A viscose composition containing 9.6% cellulose, 7.2% sodium hydroxide and 33% (based on cellulose) carbon disulfide was prepared.
For tilsetning av polystyrenen ble det dannet en innsprøytningsviskose fra ovenstående viskose ved tilsetning av en 50% vandig polystyren-emulsjon i en mengde slik at når en del innsprøytningsviskose ble blandet med 19 deler viskose, inneholdt bindeviskose-produktet 2 vekt-% polystyren basert på cellulose. Innsprøytningsviskosen ble avluftet og filtrert før bruk. For the addition of the polystyrene, an injection viscose was formed from the above viscose by adding a 50% aqueous polystyrene emulsion in an amount such that when one part injection viscose was mixed with 19 parts viscose, the binder viscose product contained 2% by weight polystyrene based on cellulose . The injection viscose was deaerated and filtered before use.
Ekstra karbondisulfid ble innsprøytet og blandetAdditional carbon disulfide was injected and mixed
i viskosen for å heve saltverdien til 13,5 i viskoselinjen til spinnemaskinen. Like før spinning ble innsprøytningsviskosen utmålt i viskosen i de ovenfor angitte forhold, og samtidig ble en 20,6% vekt/volum natriumkarbonatoppløsning tilsatt til viskosen i en mengde slik at man fikk viskose inneholdende 4% natriumkarbonat, 7,3% cellulose, 5 , 5$ |~ jnatr iumhydr oksyd og " " T"~' 0,146% polystyren, med et kulefall på 55 sekunder. Denne vis- in the viscose to raise the salt value to 13.5 in the viscose line of the spinning machine. Just before spinning, the injection viscose was metered into the viscose in the conditions stated above, and at the same time a 20.6% weight/volume sodium carbonate solution was added to the viscose in an amount such that viscose containing 4% sodium carbonate, 7.3% cellulose, 5 , 5$ |~ jnatrium hydroxide oxide and " " T"~' 0.146% polystyrene, with a bullet drop of 55 seconds. This vis-
kosen ble spunnet gjennom 19 jets, hver omfattende 1.000 hull, hulldiameter 50 micron, inn i et bad inneholdende 10,5% svovelsyre, 2% zinksulfat og 23,5% natriumsulfat, ved 3535°C. the cotton was spun through 19 jets, each comprising 1,000 holes, hole diameter 50 micron, into a bath containing 10.5% sulfuric acid, 2% zinc sulfate and 23.5% sodium sulfate, at 3535°C.
Den således dannede fiberkabel ble ført gjennom et bad inneholdende 1,5 - 2% svovelsyre ved 93°C og strukket 70%. Fiberkabelen, med en total denier-verdi på 32.300 decitex, ble deretter oppskåret til en fiberlengde på 38 mm. Spinnehastigheten var 35 m/min. The thus formed fiber cable was passed through a bath containing 1.5 - 2% sulfuric acid at 93°C and stretched 70%. The fiber cable, with a total denier value of 32,300 decitex, was then cut to a fiber length of 38 mm. The spinning speed was 35 m/min.
Fibrene ble vasket, avsvovlet under anvendelse av 0,25% natrdiumsulfid og 0,13% natriumhydroksyd ved 70°C, bleket med natriumhypoklorittoppløsning og surgjort med fortynnet svovelsyre før påføring av en natriumoleat-olj esy.re-finish og tørking. The fibers were washed, desulfurized using 0.25% sodium sulfide and 0.13% sodium hydroxide at 70°C, bleached with sodium hypochlorite solution and acidified with dilute sulfuric acid before application of a sodium oleate oil finish and drying.
De fremstilte fibre var matte fibre med et hult tverrsnitt fra gassen utviklet fra natriumkarbonatet under spinningen. Fibre fremstilt ved samme prosess uten bruk av polystyren-emulsjon, hadde samme hule tverrsnitt, men manglet det ønskede matte utseende. The fibers produced were dull fibers with a hollow cross-section from the gas evolved from the sodium carbonate during spinning. Fibers produced by the same process without the use of polystyrene emulsion had the same hollow cross-section but lacked the desired matte appearance.
Eksempel_4Example_4
Det ble fremstilt viskose med følgende sammen-setning : Viscose was produced with the following composition:
6,5% cellulose, 6,5% natriumhydroksyd,6.5% cellulose, 6.5% sodium hydroxide,
30% karbondisulfid beregnet på cellulose, kulefall: 80 sekunder, 30% carbon disulphide calculated on cellulose, bullet drop: 80 seconds,
saltverdi ved spinning: 7«salt value when spinning: 7"
Det ble fremstilt en innsprøytningsviskose ved blanding av 6,5% av en 50% vandig polystyren-emulsjon med den ovenfor angitte viskose slik at innsprøytningsviskosen inneholdt 50% polystyren beregnet på cellulose. Etter at blandingen var ferdig, ble innsprøytningsviskosen filtrert og avluftet. Den ble tilsatt til hoved-viskosestrømmen i spinnemaskinen i et forhold som ga 3% polystyren basert på cellulose i viskosen. Etter føring gjennom en blandeinnretning for oppnåelse av homogen blanding, ble viskosen ekstrudert gjennom 19 jets, hver omfattende 1.000 hull med en diameter på 50 An injection viscose was produced by mixing 6.5% of a 50% aqueous polystyrene emulsion with the above-mentioned viscose so that the injection viscose contained 50% polystyrene based on cellulose. After the mixing was complete, the injection viscose was filtered and deaerated. It was added to the main viscose stream in the spinning machine in a ratio that gave 3% polystyrene based on cellulose in the viscose. After passing through a mixing device to obtain a homogeneous mixture, the viscose was extruded through 19 jets, each comprising 1,000 holes with a diameter of 50
micron, og inn i et bad inneholdende 6,8% svovelsyre, 4,5% zinksulfat og 11,8% natriumsulfat ved 40°C. Fiberkabelen ble micron, and into a bath containing 6.8% sulfuric acid, 4.5% zinc sulfate and 11.8% sodium sulfate at 40°C. The fiber cable was
ført gjennom et varmt syrebad og strukket 115%. Spinnehastigheten var 353 5 m/min. Fiberkabelen ble deretter oppskåret til fiber av 1,7 decitex og 38 mm lengde, og ble deretter vasket, avsvovlet, bleket og surgjort som beskrevet i eksempel 2. En finish bestående av natriumoleat, oljesyre og polyglykolstearat ble påført fibrene før de ble tørket. passed through a hot acid bath and stretched 115%. The spinning speed was 353 5 m/min. The fiber cable was then cut into fibers of 1.7 decitex and 38 mm length, and was then washed, desulfurized, bleached and acidified as described in Example 2. A finish consisting of sodium oleate, oleic acid and polyglycol stearate was applied to the fibers before they were dried.
De fremstilte fibre var høyvåtmodul-viskosefibre med et godt, matt utseende. The fibers produced were high wet modulus viscose fibers with a good matte appearance.
Claims (7)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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GB4262477 | 1977-10-13 |
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NO783459L true NO783459L (en) | 1979-04-18 |
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Application Number | Title | Priority Date | Filing Date |
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NO783459A NO783459L (en) | 1977-10-13 | 1978-10-12 | FILAMENTS OF REGENERATED CELLULOSE AND PROCEDURE FOR THEIR PREPARATION |
Country Status (9)
Country | Link |
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BE (1) | BE871210A (en) |
DE (1) | DE2843989A1 (en) |
ES (1) | ES474187A1 (en) |
FI (1) | FI783078A (en) |
FR (1) | FR2406011A1 (en) |
IT (1) | IT1160854B (en) |
NL (1) | NL7810311A (en) |
NO (1) | NO783459L (en) |
SE (1) | SE7810663L (en) |
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DE102011101321A1 (en) | 2011-05-12 | 2012-11-15 | Glanzstoff Bohemia S.R.O. | Flame-retardant cellulose regenerated filament fibers and process for its preparation |
ES2569859T3 (en) | 2012-05-14 | 2016-05-12 | Glanzstoff Bohemia S.R.O. | Regenerated cellulose fibers flame retardant and manufacturing process |
Family Cites Families (3)
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GB435948A (en) * | 1934-07-21 | 1935-10-02 | Glanzstoff Courtaulds Gmbh | Improvements in and relating to the manufacture of artificial silk and the like |
DE851997C (en) * | 1949-11-15 | 1952-10-09 | Chemische Werke Huels Ges Mit | Process for the production of shaped structures from cellulose hydrate |
FR1458612A (en) * | 1965-09-30 | 1966-03-04 | Cellophane Sa | Process for improving the surface properties of cellulosic film films |
-
1978
- 1978-10-09 DE DE19782843989 patent/DE2843989A1/en not_active Withdrawn
- 1978-10-10 FI FI783078A patent/FI783078A/en unknown
- 1978-10-12 BE BE78191078A patent/BE871210A/en unknown
- 1978-10-12 FR FR7829120A patent/FR2406011A1/en not_active Withdrawn
- 1978-10-12 SE SE7810663A patent/SE7810663L/en unknown
- 1978-10-12 NO NO783459A patent/NO783459L/en unknown
- 1978-10-13 ES ES474187A patent/ES474187A1/en not_active Expired
- 1978-10-13 NL NL7810311A patent/NL7810311A/en not_active Application Discontinuation
- 1978-10-13 IT IT69355/78A patent/IT1160854B/en active
Also Published As
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FI783078A (en) | 1979-04-14 |
DE2843989A1 (en) | 1979-04-19 |
NL7810311A (en) | 1979-04-18 |
BE871210A (en) | 1979-02-01 |
SE7810663L (en) | 1979-04-14 |
ES474187A1 (en) | 1979-05-16 |
IT1160854B (en) | 1987-03-11 |
FR2406011A1 (en) | 1979-05-11 |
IT7869355A0 (en) | 1978-10-13 |
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