US2536014A - Spinning of viscose - Google Patents

Spinning of viscose Download PDF

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US2536014A
US2536014A US716415A US71641546A US2536014A US 2536014 A US2536014 A US 2536014A US 716415 A US716415 A US 716415A US 71641546 A US71641546 A US 71641546A US 2536014 A US2536014 A US 2536014A
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viscose
bath
spinning
yarn
quaternary ammonium
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US716415A
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Cox Norman Louis
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EIDP Inc
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EI Du Pont de Nemours and Co
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Priority to FR957246D priority Critical patent/FR957246A/fr
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Priority to US716415A priority patent/US2536014A/en
Priority to GB31357/47A priority patent/GB652741A/en
Priority to DEP28793D priority patent/DE974548C/de
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    • 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
    • D01F2/10—Addition to the spinning solution or spinning bath of substances which exert their effect equally well in either
    • 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
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2913—Rod, strand, filament or fiber
    • Y10T428/2933—Coated or with bond, impregnation or core
    • Y10T428/2964—Artificial fiber or filament
    • Y10T428/2965—Cellulosic
    • 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
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2913—Rod, strand, filament or fiber
    • Y10T428/2973—Particular cross section
    • Y10T428/2978—Surface characteristic

Definitions

  • This invention relates to the regeneration of cellulose from viscose. More particularly, it relates to a new process for manufacturing regenerated cellulose articles such as filaments or films having improved properties.
  • An object of this invention is to provide a process of manufacturing regenerated cellulose filaments having gel swelling values lower than heretofore attainable and exhibiting considerably improved yarn properties. Another object is to provide a process whereby unripened viscose can be spun in conventional spinning equipment to give yarn of high quality. A further object is to provide a process of manufacturing regenerated cellulose yarn having entirely novel and desirable properties. Yet a further object is the provision of a high tenaci y. high fatigue resistant regenerated cellulose fiber having a noncrenulated surface and having improved soil and abrasion resistance. Other objects will appear hereinafter.
  • each of the four organic radicals attached to the nitrogen contains not more than four aliphatic carbons, at least three of these organic groups being completely aliphatic and the fourth one, when aromatic, containing only one benzene nucleus, said quaternary ammonium compound having no appreciable surface tension lowering properties.
  • Such quaternary ammonium compounds may contain four aliphatic groups attached to the nitrogen atom none of which groups are more than a carbon atoms in length or they may contain three of;
  • the anions in every instance are devoid of sur- 5 all determined according to the following pro-- cedure.
  • the gel thread was collected in a monolayer on a bobbin, by manually operating a traverse mechanism with the thread being stretched 80% in the hot dip bath.
  • the sample was centrifuged (1400 R. P. M.) for one minute, out off, and weighed in a closed bottle.
  • the sample was washed free of acid, dried in an oven a 1o5 6.
  • the ratio of the gel weight to cellulose weight (grams of gel per gram of cellulose) is referred to as the gel swelling. Variations may be introduced in the procedure, e. g., in the stretch, spinning speed, or length of bath travel, but these introduce only minor changes in the numerical values of gel swelling.
  • D value Another important indication of yarn quality is the factor referred to below as D value.
  • This factor relates to the rate of neutralization of the viscose filament in the coagulating and regenerating bath. It is determined by adding to the viscose a suitable indicator, in this case bromocresol purple (pH range 5.2 to 6.8), and observing the distance in inches from the spinneret at which point the purple color completely disappears in the traveling filament. This distance is the D value.
  • the selected quaternary ammonium compounds suitable for use in this invention reduce the rate of neutralization of the spinning filaments, hence increase the D value over that of unmodified viscose. It has been found that, in general, the greater the D value or the slower the rate of neutralization, the better the yarn properties. It is believed that the increased D value is an indication that the modifying agents of this invention permit greater dehydration of the viscose before the gel structure of the filament is permanently set.
  • the caustic content of 6% refers to the total alkalinity expressed as sodium hydroxide. It includesv the benzyltrimethylammonium hycombined in the form of sodium carbonate, sodium trithiocarbonate, and sodium cellulose xanthate.
  • the viscose is spun into 275 denier-100 filament yarn by extruding through a spinneret havlog holes of 0.0025-ipch diameter into primary coagulating and regenerating baths comprising (1) 6.0% H2504, 14% Nazsoi, and 15% 21180.4. and (2) 9% H2804, 22% NazSO4. 1% ZnSOr, and 5% W804.
  • the yarn is given a bath travel of 28 inches by using a roller guide.
  • the apparatus and general procedure used to lead viscose into the bath and to collect the formed thread are essentially the same as those used commercially in the so-called bobbin or spool process.
  • the specific conditions include a bath temperature of 58 C. and a first feed wheel speed of 485 inches per minute.
  • the filaments are carried through a water bath at 95 to 100 C. and wound up at such a speed as to give 80% stretch beyond the feed wheel.
  • the resulting regenerated gel yarn is washed free of acid and salt and then x processed.
  • the yarns which are dried on the bobbin or, alternately, partially relaxed before drying by rewinding on another bobbin, are twisted 4 turns per inch and tested after conditioning at 21 C. and 60% relative humidity for 48 hours.
  • modified viscose (the standard viscose of commercial operation), both controls being spun under conditions identical to those for the modified viscoses. It will be seen that the level of properties is lowest for the yarns from the unripened, unmodified viscoses. wet strengths of yarns from the unripened, modified viscoses of this invention are greater than those for ripened. control viscoses.
  • the yarn produced by this and the other examples has a number of remarkable properties which distinguish it sharply from other regenerated cellulose yarns.
  • the most readily apparent of these new features are the cross-section and the surface.
  • the cross sections of viacose yarn are observed and studied in the following manner. After imbedding the yarn in paraflln, cross sections are cut and affixed to a glass slide bya shellac cement. After removing the paraffin in xylene; the sections are swollen in water and photomicrographs are taken. For yarns prepared from unripened. unmodified viscose spun into zinc baths, a skin or outer shell which swells to a different extent from that of the core is visible.
  • the yarn from viscose spun in contact with the modifiers of this invention differs from regular viscose yarn in five other respects: 1) the density appears to be higher than that of normal viscose yarns of the same orientation; (2) the yarns of 0 this invention behave differently when :flbrillated eral order of less than 35, i. e., about 5 to about 35; a secondary swelling of less than 35%, i. e., about to about 85%; and less than about 40% core, the skin varying from about 60% to about 100%.
  • the amount of skin approaches 65 100%, the amount of core becomes negligible and the diffuse boundary is diflicult to bring out by the dyeing technique, the negligible-core yarns, obtained, for example, by Example III or X and described and claimed by this invention, still being characterized by lateral orders, secondary swellings, etc. which distinguish them from other yams as pointed out above.
  • Table 13 the physical characteristics of yarns from modified viscose in comparison with other known yarns are shown.
  • EXAWLE H A 7-6 viscose (7% cotton linter cellulose-6% total sodium hydroxide) modified with 1.5 milli and cord strength and fatigue resistance of the cord over warn produced from normally ripened viscose spun under identical conditions.
  • the dye absorption rate Table II refers to the time in minutes required for the absorption of of the dye by 5 gram y Yam Properties Unripened Ripcned from a bath consisting of 250 grams of water, 30 Modlfled Unmodified 0.1 gram of Pontamine Fast Green 5 BL and 1.5
  • EXAMPIE VI A cotton linter viscose containing 7% cellulose, 6% total sodium hydroxide, and 2.0 millimoles per 100 grams of tetramethylammonium chloride per 100 parts of viscose is prepared as described in Example I. The viscoseis spun in ,an unripened state in a sulfuric acid-sodium sulfate-zinc sulfate (8-14-15) bath and all conditions of Example I for spinning and processing are used with the exce tion that 100% in: stead of 80% stretch is employedin the secondary bath. The "table below shows the improvement in yarn properties and gel swellin obtained with this modifier.
  • the modifying agents suitable for the purpose of this invention are quaternary ammonium compounds having the gross formula wherein X is a hydroxyl group or an anion having-no surface activity, e. g., the chloride, bromide, iodide, sulfate, bisulfate, acetate, ctc., anions, and the radicals R1.
  • Ra. R: and R4. are organic groups having not more than four aliphatic carbons, at least three of these radicals being completely aliphatic and the fourth one. when aromatic, containing not more than one aromatic (benzene) nucleus. All R groups may be aliphatic and in that instance they may be alike or different. A chemical structure involving only short aliphatic chains or only one ammatic nucleus is intimately connected with the absence of surface-active properties in the ruodi-y.v
  • the first six mem. bers of the table are short-chain compounds, 1. e.. compounds having no aliphatic chain longer than four carbons or no aromatic chain longer than one benzene nucleus. It will be noted that they have substantially no surface tension-lowering effect. In comparison, it will be seen that surface activity becomes appreciable with a six to eight carbon chain, and is very high with compounds having twelve or more carbons in a chain.
  • Table XIII TSui-fiaco fliiflrwntre ens on, rom a r, Mqdmer d dynes per cm. per cm.
  • the preferred modifiers for use in this invention are those in which all four organic groups attached to the nitrogen atom are hydrocarbon groups or bywhich the radical X is hydroxyl or halogen of atomic weight above 19, i. e., chlorine. bromine,
  • the most useful modifiers are the" quaternary ammonium hydroxides having a total of. not more than ten carbon atoms in the molecule and in which all organic groups are hydrocarbon or hydroxyl-substituted hydrocarbon.
  • An obvious requirement of the modifying agents is that they be soluble in the viscose or in the coagulating bath, i. e., in alkaline or acidic media, to the extent of at lea t 0.5%. Furthermore, they must be substantially inert chemically toward'and unaffected by the components of the viscose and of the coagulating bath.
  • Suitable agents which may be mentioned in addition to those used in the examples are tetraethylammonium bromide, tetramethylammonium iodide, tetrapropylammonium hydroxide, tetrabutylammonium chloride, tributylpropylammonium hydroxide. tri(beta-hydroxyethyl) methylammo- 14 nium hydroxide. tributyl(beta-hydroxyethyl-am. monium iodide. etc.
  • the non-surface-active quaternary ammonium compounds may be used either in the viscose or in the coagulating-regenerating bath.
  • the agents may also be added to both the viscose and the bath in equal or different amounts, the total concentration being generally not more than about 10.0 millimoles per grams of total solvent.
  • the agent added to the bath may be the same as or different than the agent added to the viscose.
  • the viscose used in the process of the invention may be of a variety of types; for example, it may be from wood pulp, cotton linters, mixtures of the two, or even other types of cellulose.
  • the composition of the viscose may also be varied widely. For example, it may have a cellulose content of from 4 to 10% or even more and an alkali content of from 4 to 8% or more.
  • the standard viscoses of the industry i. e., those having between 5 and 7% cellulose and between 4-6% alkali, are preferably used.
  • the amount of carbon disulfide used in xanthation can be from 25-50% (based on the recoverable bone-dry cellulose).
  • a very useful embodiment of the invention is that illustrated in Example XII, wherein unripened viscose is modified with a combination of a non-surface-active quaternary ammonium compound and added alkali trithiocarbonate.
  • an unexpected synergistic effect is observed as regards the neutralization rate and the yarns are of remarkably high quality.
  • the quantity of alkali trithiocarbonate (e. g., sodium or potassium trithiocarbonate) to be added to the green viscose need only be sufiicient to bring the total trithiocarbonate content to between about 1% and about 3%, based on the viscose, which means in general that the amount added is between 0.2% and 2.25% of the weight of the viscose.
  • alkali trithiocarbonate e. g., sodium or potassium trithiocarbonate
  • the spinning baths suitable for use in the invention contain sulfuric acid, sodium sulfate, and zinc sulfate.
  • Zinc sulfate is an essential com-' ponent of the spinning bath since, in its absence,
  • the quaternary ammonium compounds have no effect on spinning and yarn properties.
  • additional salts of divalent metals known to reinforce or supplement the action of zinc sulfate may be used, such as ferrous sulfate, manganese sulfate, nickel sulfate, or chromic sulfate.
  • Ferrous sulfate is particularly useful.
  • the spinning bath contains from 4 to 12% of sulfuric acid, from 13 to 25% of sodium sulfate, and from 1 to 15% of zinc sulfate, optionally including between 0.8 and 6%, and preferably between 1% and 5%, of ferrous sulfate.
  • the optimum quantity of zinc sulfate from the standpoint of practical spinning speed appears to be 3 to 5%.
  • the filaments may be" given a long travel of 50 130-250 inches in the primary bath by means of a multiple roller setup which gradually applies tension to the traveling filaments and thereby orients them while they are still plastic.
  • the secondary bath may consist simply of water or of dilute (Ii-3%) sulfuric acid, or it may have the same composition as the coagulating bath but at a greater dilution, e. g., one-fourth of the concentration of the coagulating bath.
  • the temperature of the secondary bath is preferably between 50 and 100 C. Stretches of til-100% are'preferred for producing high tenacity yarn and 20-30% for tax,-
  • the bobbin process has been used in the examples, but it is immaterial whether spinning is by bobbin, bucket, or continuous processes.
  • the yarn cake is washed free of acid and salt and then dried under tension. If preferred, it may be twister or slasher-dried to enable the dry elongation of the finished product to be controlled.
  • the preferred procedure is to draw off the freshly coagulated gel yarn with a feed wheel speed equal to or less than the jet velocity and to apply all of the stretch between positively driven rollers traveling at different speeds.
  • the thread can be given a travel of 10-50 inches in the secondary bath of hot water or dilute bath. As mentioned above, the amount of stretch applied depends on the properties desired for the yarn.
  • novel and improved yarns obtainable through the process of this invention can, in general be used instead of regular regenerated cellulose fibers for anypurposes where the latter are finding applications, more particularly in the textile and tire cord industries.
  • a method of producing regenerated cellulosic 4.) structures which comprises the step of spinning a viscose solution in a spinning bath comprising an aqueous solution of sulfuric acid containing from 1% to 15% zinc sulfate, the said spinning being conducted in the presence of about 0.5 to about 10.0 millimoles per grams of one of said solutions of a water-soluble quaternary ammonium compound of the formula wherein R1, R2, R3, and R4 are organic groups which contain no more than four aliphatic carbon atoms, at least three of the said groups contain only aliphatic carbon atoms and the fourth of the said groups contains no more than one phenyl radical and where X- is an anion having substantially no surface activity.
  • a method of producing regenerated cellulosic structures which comprisesthe step of spinning viscose in an aqueous sulfuric acid spinning bath containing from 1% to 15% zinc sulfate together with, per 100 grams of bath, about 0.5 to about 10.0 millimoles of a water-soluble quaternary ammonium compound of the formula 17 wherein R1, Re, R: and R4 are aliphatic radicals. each of the said radicals containing no more "than 4 carbon atoms and xis an anion having substantially no surface activity.
  • a method of producing regenerated cellulosic structures which comprises the step of spinning viscose in an aqueous sulfuric acid spinning bath containing from 1% to zinc sulfate, the said viscose containing, Der 100 grams of viscose, about 0.5 to about 10.0 millimoles of a water-soluble monium compound of the formula quaternary ammonium compound of the formula [Rails] wherein R1, Ra, Re and R4 are aliphatic radicals ach of the said radicals containing nomore than 4 carbon atoms and X in an anion having substantially no surface activity.
  • R1, R2, and R3 are aliphatic radicals, each of the said radicals containing no more than 4 carbon atoms, the radical R4 containing no more than 4 aliphatic carbon atoms and no more than 1 phenyl radical, and X- is an anion having substantially no surface activity.
  • a method of producing regenerated cellulosic structures which comprises the step of spinning viscose in an aqueous sulfuric acid spinning bath containing from 1% to 15% zinc sulfate, the said viscose containing, per 100 grams of viscose, about 0.9 to about 3.0 millimoles of a water-soluble quaternary ammonium compound of the formula wherein R1, R2 and R3 are aliphatic radicals, each of the said radicals containing no more than 4 carbon atoms, the radical R4 contains no more than 4 aliphatic carbon atoms and no more than 1 phenyl radical, and X is an anion having substantially no surface activity.
  • a method of producing regenerated cellulosic structures which comprises the step of spinning viscose containing a water-soluble trithiocarbonate in addition to that formed during xanthation in an aqueous sulfuric acid bath con-- taining 1% to 15% zinc sulfate together with grams of bath, the said quaternary ammonium compound corresponding to the formula [RP-E m];- it
  • R1, Ra, Re and R4 are organic groups which contain no more than four aliphatic carbon atoms, at least three of the said groups containing only aliphatic carbon atoms, and the fourth of the said groups containing no more than one phenyl radical and whereas X- is an anion having substantially no surface-activity;
  • a process which comprises incorporating in viscose which contains a water-soluble trithiocarbonate in addition to that formed during xanthation about 0.9 to about 3.0 millimoles of a water-soluble, quaternary ammonium compound per 100 grams of viscose and extruding the resultant viscose into a coagulating bath comprising an aqueous solution of sulfuric acid and 1% to 15% zinc sulfate, the said quaternaryammonium compound corresponding to the formula [his]; l.
  • R1, R2, R3 and R4 are organic groups which contain no more than four aliphatic carbon atoms, at least three of the said groups contain ing only aliphatic carbon atoms, and the fourth of the said groups containing no more than one phenyl radical and where X"- is an anion having substantially no surface-activity.
  • a process which comprises. incorporating in viscose containing an alkali. metal trithiocarbonate in addition to that formed during xanthation about 0.9 toabout 3.0 millimoles of a water-soluble, quaternary ammonium compound per 100 grams of viscose, extruding the resultant viscose into a coagulating bath comprising an aqueous solution of 4% to 12% sulfuric acid, 13% to 25% sodium sulfate and 1% to 15% zinc sulfate, the said quaternary ammonium compound corresponding to the formula [ails];- i.
  • R1, R2, R3 and R4 are organic groups which contain no more than four aliphatic carbon phenyl radical and wherein X is an anion having substantially no surface-activity.
  • the coagulating bath contains about 0.9 to about 3.0 millimoles of a water-soluble, quaternary ammonium compound per 100 grams of bath, the said quaternary ammonium compound corresponding to the formula wherein R1, R2, R3 and R4 are organic groups which contain no more than four aliphatic carbon atoms, at least three of th said groups containing only aliphatic carbon atoms, and the fourth of the said groups containing no more than one phenyl radical and wherein X is an anion having substantially no surface-activity.
  • An aqueoussulfuric acid spinning bath for the spinning of regenerated cellulosic structures from viscose, said bath containing from 1% to 15% zinc sulfate together with about 0.5 to about 10.0 millimoles of a water-soluble, quaternary ammonium compound per 100 grams of bath, the said quaternary ammonium compound corresponding to the formula wherein R1, R2, R3 and R4 are organic groups which contain no more than four aliphatic carbon atoms, at least three of the said groups containing only aliphatic carbon atoms, and the fourth of thesaid groups containing no more than one phenyl radical and wherein X" is an anion having substantially no surface-activity.
  • An aqueous sulfuric acid bath for the spinning of regenerated cellulosic structures from viscose said bath containing from 4% to 12% sulfuric acid, 13% to 25% sodium sulfate, 1% to 15% zinc sulfate and about 0.9 to about 3.0 millimoles of a water-soluble, quaternary ammonium compound per 100 grams of bath, the said quaternary ammonium compound corresponding to the formula R: P [m-liLRJx- 4 wherein R1, R2, R3 and R4 are organic groups which contain no more than four aliphatic carbon" atoms, at least three of the said groups containing only aliphatic carbon atoms, and the fourth of the said groups containing no more than one phenyl radical and wherein X- is an anion having substantially no surface-activity.
  • An aqueous sulfuric bath for the spinning of regenerated cellulosic structures from viscose said bath containing from 4% to 12% sulfuric acid, 13% to 25% sodium sulfate, 1% to 15% zinc sulfate, 1% to ferrous sulfate and about 0.9 to about 3.0 millimoles of a water-soluble, quaternary ammonidm compound per 100 grams of bath, the said quaternary ammonium compound corresponding to the formula wherein R1, R2, R3 and R4 are organic groups which contain no more than four aliphatic carbon atoms, at least three of the said groups containing only aliphatic carbon atoms, and the fourth of the said groups containing no more than one phenyl radical and wherein X- is an anion having substantially no surface-activity.
  • a filament of regenerated cellulose having a smooth surface, showing no appreciable crenulation and having a core surrounded by a skin, the ratio of th cross-sectional area of the skin to the core eing greater than one and the boundary therebetween being diffuse.
  • a filament in accordance with claim 18 characterized by a lateral order of about 18.
  • a proczss is accordance with claim 1 in which the said quaternary ammonium compound is tetramethylammonium hydroxide.
  • Rcinthaler Artificial Silk, D. Van Nostrand Company, Incorporated, New York, 1928, page 138-147.

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  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Artificial Filaments (AREA)
US716415A 1946-12-14 1946-12-14 Spinning of viscose Expired - Lifetime US2536014A (en)

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FR957246D FR957246A (en, 2012) 1946-12-14
US716415A US2536014A (en) 1946-12-14 1946-12-14 Spinning of viscose
GB31357/47A GB652741A (en) 1946-12-14 1947-11-26 Spinning of viscose
DEP28793D DE974548C (de) 1946-12-14 1948-12-31 Verfahren zur Herstellung von Gebilden, wie Faeden oder Filmen, aus regenerierter Cellulose

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Cited By (9)

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US2813038A (en) * 1953-04-07 1957-11-12 Courtaulds Ltd Production of artificial filaments, threads and the like
DE1023186B (de) * 1956-02-20 1958-01-23 Glanzstoff Ag Verfahren zum Herstellen von Kuenstlichen Faeden nach dem Viskosespinnverfahren
US2852333A (en) * 1954-05-21 1958-09-16 Du Pont Viscose spinning process
US2860480A (en) * 1956-04-18 1958-11-18 Du Pont Regenerated cellulose structures and process for producing them
US2891836A (en) * 1955-04-26 1959-06-23 Du Pont Viscose process
US2956894A (en) * 1954-12-30 1960-10-18 American Viscose Corp Method of forming all skin viscose rayon
US3002803A (en) * 1956-08-29 1961-10-03 American Enka Corp Method of spinning low elongation viscose rayon
US3019509A (en) * 1954-05-21 1962-02-06 Beaunit Mills Inc Crimped regenerated cellulose fibers
US5482776A (en) * 1988-10-05 1996-01-09 Asahi Kasei Kogyo Kabushiki Kaisha Viscose rayon fiber having superior appearance

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NL87530C (en, 2012) * 1955-06-29 1900-01-01
BE554986A (en, 2012) * 1956-03-02 1900-01-01
US2893820A (en) * 1956-07-16 1959-07-07 Du Pont Process for the production of regenerated cellulose filaments
US2983572A (en) * 1958-06-06 1961-05-09 American Enka Corp Manufacture of viscose rayon

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NL51307C (en, 2012) * 1937-05-11
US1683199A (en) * 1925-06-20 1928-09-04 Lilienfeld Leon Artificial thread and process for making same
FR778947A (fr) * 1933-10-06 1935-03-26 Perfectionnements à la fabrication de textiles artificiels par le procédé à la viscose
US2125031A (en) * 1935-02-16 1938-07-26 American Enka Corp Manufacture of artificial silk
US2174991A (en) * 1939-01-09 1939-10-03 C H Masland & Sons Inc Textile fabric
US2310207A (en) * 1938-10-07 1943-02-09 North American Rayon Corp Surface-active incrustation inhibitor
US2340377A (en) * 1939-12-11 1944-02-01 Graumann Erich Process of making artificial fibers
US2345570A (en) * 1938-10-07 1944-04-04 North American Rayon Corp Coagulating bath containing cationactive inhibitors
US2373712A (en) * 1943-04-19 1945-04-17 Rayonier Inc Viscose production
US2412969A (en) * 1943-04-27 1946-12-24 Du Pont Spinning process
US2517694A (en) * 1943-09-14 1950-08-08 American Viscose Corp Crimped artificial filament

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GB446647A (en) * 1934-07-31 1935-10-14 Willy Schaan An improved process and apparatus for photography
DE744891C (de) * 1938-10-22 1944-01-28 Ig Farbenindustrie Ag Verfahren zur Herstellung von Kunstseide, Fasern und Faeden aus Viscose
GB533309A (en) * 1939-08-10 1941-02-11 Courtaulds Ltd Improvements in or relating to the production of artificial threads from viscose

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1683199A (en) * 1925-06-20 1928-09-04 Lilienfeld Leon Artificial thread and process for making same
FR778947A (fr) * 1933-10-06 1935-03-26 Perfectionnements à la fabrication de textiles artificiels par le procédé à la viscose
US2125031A (en) * 1935-02-16 1938-07-26 American Enka Corp Manufacture of artificial silk
NL51307C (en, 2012) * 1937-05-11
US2310207A (en) * 1938-10-07 1943-02-09 North American Rayon Corp Surface-active incrustation inhibitor
US2345570A (en) * 1938-10-07 1944-04-04 North American Rayon Corp Coagulating bath containing cationactive inhibitors
US2174991A (en) * 1939-01-09 1939-10-03 C H Masland & Sons Inc Textile fabric
US2340377A (en) * 1939-12-11 1944-02-01 Graumann Erich Process of making artificial fibers
US2373712A (en) * 1943-04-19 1945-04-17 Rayonier Inc Viscose production
US2412969A (en) * 1943-04-27 1946-12-24 Du Pont Spinning process
US2517694A (en) * 1943-09-14 1950-08-08 American Viscose Corp Crimped artificial filament

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2813038A (en) * 1953-04-07 1957-11-12 Courtaulds Ltd Production of artificial filaments, threads and the like
US2852333A (en) * 1954-05-21 1958-09-16 Du Pont Viscose spinning process
US3019509A (en) * 1954-05-21 1962-02-06 Beaunit Mills Inc Crimped regenerated cellulose fibers
US2956894A (en) * 1954-12-30 1960-10-18 American Viscose Corp Method of forming all skin viscose rayon
US2891836A (en) * 1955-04-26 1959-06-23 Du Pont Viscose process
DE1023186B (de) * 1956-02-20 1958-01-23 Glanzstoff Ag Verfahren zum Herstellen von Kuenstlichen Faeden nach dem Viskosespinnverfahren
US2860480A (en) * 1956-04-18 1958-11-18 Du Pont Regenerated cellulose structures and process for producing them
US3002803A (en) * 1956-08-29 1961-10-03 American Enka Corp Method of spinning low elongation viscose rayon
US5482776A (en) * 1988-10-05 1996-01-09 Asahi Kasei Kogyo Kabushiki Kaisha Viscose rayon fiber having superior appearance

Also Published As

Publication number Publication date
FR957246A (en, 2012) 1950-02-17
DE974548C (de) 1961-02-02
GB652741A (en) 1951-05-02

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