US2535045A - Spinning of viscose - Google Patents

Spinning of viscose Download PDF

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Publication number
US2535045A
US2535045A US744069A US74406947A US2535045A US 2535045 A US2535045 A US 2535045A US 744069 A US744069 A US 744069A US 74406947 A US74406947 A US 74406947A US 2535045 A US2535045 A US 2535045A
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bath
viscose
spinning
carbon atoms
yarn
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US744069A
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English (en)
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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 FR961353D priority Critical patent/FR961353A/fr
Application filed by EI Du Pont de Nemours and Co filed Critical EI Du Pont de Nemours and Co
Priority to US744069A priority patent/US2535045A/en
Priority to GB603/48A priority patent/GB652746A/en
Priority to DEP28795D priority patent/DE829649C/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

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 by methods known to the art 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-tenacity regenerated cellulose fiber having a non-crenulated surface. Other objects will appear hereinafter.
  • Another object which was unexpectedly found possible to accomplish through the invention described below, was the production of very highstrength yarns having smooth (non-crenulated) surfaces with improved soil resistance and abrasion resistance.
  • the combination of high tenacity and high fatigue resistance with smooth surface had not heretofore been achieved.
  • bath-soluble monoamine modifiers those monoamines the organic groups of which total from four to ten carbon atoms, no single group within the molecule having more than six carbon atoms and the solubility of which is at least 0,2%, on a weight basis, in an aqueous sulfuric acid spinning bath containing at least 2% of zinc sulfate and 13% or more of sodium sulfate.
  • Figure l is a dyed cross-section of a filament regenerated from unripened, unmodified viscose
  • Figure 2 is a dyed cross-section of a filament, regenerated from viscose unripened, but modified with the agents of and by the processes of this invention.
  • the gel thread is 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 is centrifuged (1400 R. P. M.) for a minute, cut off, and weighed in a closed bottle.
  • the sample is washed free of acid, dried in an oven at 105 C., and weighed.
  • the ratio of gel weight to cellulose weight (gramsof 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. In the case of films, excess bath is removed by blotting with pulp sheet and the gel swelling value is expressed as for filaments.
  • 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 5.2-6.8), and observing the distance in inches from the spinneret at which the purple color completely disappears in the traveling filament. This distance is the D value.
  • the selected amines suitable for use in this invention reduce the rate of neutralization of the spinning filaments, and, hence, increase the "D" value over that of unmodified viscose. It has been found that, in general, the greater the D value, the better the yarn properties. The increased D value is believed to indicate 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 includes free sodium hydroxide and that combined in the form of sodium carbonate, sodium trithiocarbonate, and sodium cellulose xanthate.
  • Viscose was prepared in the following manner, using 7% cellulose and 6% total sodium hydroxide (7-6 viscose). Alkali cellulose, aged to get the desired viscose viscosity (40-60 poises) is xanthated for 2 hours using 35% carbon disulfide (based on the recoverable bone-dry cellulose). After mixing 1%; hours at 0 C., the freshly prepared viscose is filtered while it is cold, deaerated, and kept at 0 C. until spun, i. e., it is spun in the unripened state and has a high salt index value, high xanthate sulfur content, and low sodium trithiocarbonate concentration.
  • the viscose is spun into 275 denier-100 filament yarn by extruding through a spinneret having holes of 0.0025" diameter into primary coagulating and regenerating baths comprising 8.5% H2804, 23% Na2SO4, and4% 211504, and 0.0, 0.2, and 0.4% of triethylamine, respectively.
  • the yarn is given a primary bath travel of 28" by using a roller guide.
  • the specific conditions include a bath temperature of 50 C. and first feed-wheel speed of 485 inches per minute.
  • the filaments are carried through a water bath at 95-100 C. and wound up at such a speed as to give stretch beyond the feed wheel.
  • the resulting regenerated gel yarn is washed free of acid and salt and then processed.
  • the yarns which are dried on the bobbin or, alternately, partially relaxed before drying by rewinding on another bobbin, are twisted four turns per inch and tested after conditioning at 21 C. and 60% relative humidity for 48 hours.
  • the yarn produced by this and other examples has a number of properties which distinguish it sharply from other regenerated cellulose yarn. Its properties are similar to those produced through modification of viscose with short-chain quaternary ammonium compounds which are described and claimed in copending application Serial No. 716,415. The most readily apparent modifications are the new cross-section and surface features. For conventional yarns prepared from viscose spun into zinc baths, a skin or outer shell which swells to a different extent in water than that of the core is visible. These yarn crosssections show both deep and shallow crenulations around the periphery of the filament. However, for yarns spun into zinc baths containing the amine modifiers of this invention, the boundary between the skin and core is very diffuse and crenulations are absent, giving the yarn a smooth surface.
  • the filaments of the invention have smooth surface and considerably lower sec 7 ondary swelling (water take-up by dried yarns) results in more resistance to flbrillating, laundering, fatiguing, and soiling action than exhibited by normal crenulated viscose yarns.
  • EXAMPLE II A 7-6 viscose is prepared and spun in the unripened state in the manner described in Example I.
  • yarns were collected in separate coagulating baths containing 0.0, 0.2, and 0.4% dibutylamine, respectively.
  • the yarns were partially relaxed before drying on the bobbin.
  • the yarn properties are tabulated below for both control and modified conditions. It will be noted that the use. of the amine modifier in the coagulating bath gives lower gel swelling, lower rate of neutralization (higher "D value), and improved yarn prop-f erties.
  • EXAIWPLE III A cotton linters viscose containing 7% cellulose and 6% caustic is prepared and spun as described in Example I. In this case, however, the modifier added to the bath is cyclohexylamine. Yarns with smooth surface and improved properties are obtained by adding 0.3 and 0.5% of this modifier to the bath:
  • EXAIWPLE V A cotton linters viscose containing 7% cellulose and 6% total caustic is prepared and ripened to a salt index of 5.0, as is normally done in com truckal production, and then spun into filaments using all the conditions of Example I for collection and processing.
  • the modifier used in the coagulating bath is 0.3% butylmonoethanolamine.
  • Considerable decrease in gel swelling and increase in "D value are obtained, which are reflected in a measurable increase in physical properties of the yarn (see table below).
  • the character of the filament is changed in the same manner as noted with unripened viscose.
  • EXAMPLE VI A cotton linters viscose containing 7% cellulose and 6% caustic is prepared as in Example I and ripened as described in Example V. A layer of this viscose 0.015 inch thick is spread on a glass plate and then immersed in a coagulating bath at 50 C. Baths containing 6% sulfuric acid, 23% sodium sulfate, and 1, 3, and 4% zinc sulfate, respectively, were used. The following modifiers were added to the coagulating baths: amylamine, cyclohexylamine, dibutylamine, triethylamine, and tributylamine.
  • the modifying agents suitable for the purpose of this invention are primary, secondary, and tertiary monoamines which are soluble in the coagulating bath to at least 0.2%. It should be noted in this connection that many amines are practically completely insoluble in the normal coagulating baths, e. g., baths containing 13% or more of sodium sulfate, in spite of the fact that the baths are acidic. This is true in particular of the long-chain amines, and even of relatively short-chain amines such as triamylamine, which is not soluble in such coagulating baths even to the extent of 0.2%. Tributylamine is soluble to 0.2% in coagulating baths but 0.5% will not dissolve. If the amine has the solubility requirement, it must also fulfill the following additional conditions previously stated, namely:
  • the preferred modifiers are those in which the amino nitrogen is attached to hydrocarbon groups, preferably alkyl groups, and/or to hydroxyalkyl groups.
  • Suitable agents which may be mentioned in addition to those used in the examples are diethylamine, dipropylamine, butylamine, ethyldiethanolamine, pyridine, piperidine, aniline, triethanolamine, dipropanolamine, propylpropanolamine, hexanolamine, amyldiethanolamine, butylmethylethanolamine, propylethanolamine, cyclohexylethanolamine, and hexyldiethanolamine.
  • the amine modifiers for effective results should be used in the coagulating bath in concentrations of at least 0.2%, based on the weight of the bath, and, in general, it is unnecessary to use more than 1.0% of agent, a generally useful range being 0.20.5%.
  • concentrations of any given agent depends on its eflectiveness and on its molecular weight. For example. larger concentrations of amylamine are needed than for triethylamine. It also depends to some extent on process variables such as the spinning speed, since at the high spinning speeds used in industrial practice less agent is desired than at lower speeds, for the reason that the rate of neutralization of the filament should be retarded only to the extent compatible with complete coagulathose skilled in the art.
  • 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 amount of carbon disulfide used in xanthation can be from 25-50% (based on the recoverable bone-dry cellulose).
  • the spinning baths suitable for use in the invention contain sulfuric acid, sodium sulfate, and zinc sulfate.
  • Zinc sulfate is an essential component of the spinning bath since, in its absence, or if it is present in insufficient amount, the amine 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, magnesium sulfate, nickel sulfate, or chromic sulfate, particularly the first-named salt. When one or any of these supplementary metal salts are used, smaller amounts of zinc sulfate are required.
  • the spinning bath contains from 4 to 12% of sulfuric acid, from 13 to 25% of sodium sulfate, and from 2 to 15% of zinc sulfate, optionally with 1 to about 5% of ferrous sulfate.
  • the optimum quantity of zinc sulfate for industrial practice appears. to be 3 to 5%; however, 15% zinc sulfate is quite satisfactory for reducing gel swelling and improving yarn properties.
  • With the addition .of amines to the baths it is possible to obtain excellent yarns in the upper range of bath acidity under which conditions normal, unmodified viscoses give yarns of decreased quality.
  • the temperature range of best spinnability is from 40 C. to 65 C.
  • the filaments may be given a long travel of 130 to 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 preferred method is to apply a part or all of the stretch beyond the primary bath in a secondary bath or to use a combination of air and hot-bath stretch.
  • the secondary bath may consist simply of water or of dilute (1% to 3%) sulfuric acid, or it may have the same composition as the coagulating bath but at a greater dilution, e. g., onei'ourth of the concentration of the coagulating bath.
  • the temperature of the secondary bath is preferably between 50 C. and 100 C.
  • Stretches of 80% to 100% are preferred for producing high-tenacity yarn and 20% to 30% for textile type yarns.
  • the bobbin process has been used in the example, but it is immaterial whether spinning is by bobbin. bucket, or continuous process.
  • the yarn cake is washed free of acid and salt, then dried under tension. If preferred, it may be twisteror 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 to 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 have substantially improved Wet tenacities and can, in general, be used instead of regular regenerated cellulose fibers for any purpose where the latter are finding applications, more particularly in the textile and tire cord industries.
  • a method of producing regenerated cellulosic structures which comprises the step of spinning viscose into an aqueous 4 to 12% sulfuric acid spinning bath containing at least 2% of zinc sulfate and at least 0.2% of a. bath-soluble monoamine which contains from 4 to 10 carbon atoms and which contains no radical having more than 6 carbon atoms.
  • a method of producing regenerated cellulosic structures which comprises the step of spinning viscose into an aqueous 4 to 12% sulfuric acid bath containing from 2% to 15% of zinc sulfate and from 0.2% to 0.5% of a bath-soluble monoamine which contains from 4 to 10 carbon atoms and which contains no radical having more than 6 carbon atoms.
  • step 3 which comprises incorporating in the said bath at least 0.2% by weight of a bath-soluble monoamine which con-. tains from 4 to 10 carbon atoms and which contains no radical having more than 6 carbon atoms.
  • a method of producing regenerated cellulosic structures which comprises the ste s of spinning viscose in an aqueous 4 to 12% sulfuric acid spinning bath containing from 2% to 15% zinc sulfate and at least 0.2% of a bath-soluble monoamine which contains from 4 to 10 carbon atoms and which contains no radical having more than 6 carbon atoms, passing the said structures into a second bath and stretching said structures in the said second bath to an extent of at least 20%.
  • a process of producing regenerated cellulosic structures which comprises extruding vis cose into a coagulating bath comprising an aqueous solution of 4% to 12% sulfuric acid, 13% to 25% sodium sulfate, 2% to 15% zinc sulfate and at least 0.2% of a bath-soluble monoaminewhich contains from 4 to 10 carbon atoms and which contains no radical having more than 6 carbon atoms.
  • An aqueous 4 'to 12% sulfuric acid spinning bath for the spinning of regenerated cellulosic structures from viscose said bath containing from 2% to 15% zinc sulfate together with at least 0.2% of a bath-soluble monoamine which contains from 4 to 10 carbon atoms and which contains no radical having more than 6 carbon atoms.
  • 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, 2% to 15% zinc sulfate and at least 0.2% of a bathsoluble monoamine which contains from 4 to 10 carbon atoms and which contains no radical having more than 6 carbon atoms.
  • An aqueous sulfuric acid bath for the spinning of regenerated cellulosic structures from viscose containing from 4% to 12% sulfuric acid, 13% to 25% sodium sulfate, 2% to 15% zinc sulfate, 1% to 5% fe1rous sulfate and 0.2% to 0.5% of a bath-soluble monoamine which contains from 4 to 10 carbon atoms and which contains no radical having more than 6 carbon atoms.
  • a method of producing regenerated cellulosic structures which comprises the step of spinning unripened viscose into an aqueous 4 to 12% sulfuril; acid spinning bath containing at least 1 11 2% of zinc sulfate and at least 0.2% of a bathsoluble monoamine which contains from 4 to carbon atoms and which contains no radical having more than 6 carbon atoms.
  • a method of producing regenerated cellulosic structures which comprises the step of spinning unripened viscose into an aqueous 4 to 12% sulfuric acid bath containing from 2% to of zinc sulfate and from 0.2% to 0.5% of a bathsoluble monoamine which contains from 4 to 10 carbon atoms and which contains no radical having more than 6 carbon atoms.
  • step 12 In a method of producing regenerated cellulosic structures by extruding unripened viscose in an aqueous 4 to 12% sulfuric acid bath containing from 2% to 15% zinc sulfate, the step which comprises incorporating in the said bath at least 0.2% by weight of a bath-soluble monoamine which contains from 4 to 10 carbon atoms and which contains no radical having more than 6 carbon atoms.
  • a method of producing regenerated cellulosic structures which comprises the steps of spinning unripened viscose in an aqueous 4 to 12% sulfuric acid spinning bath containing from 2% to 15% zinc sulfate and at least 0.2% of a bath-soluble monoamine which contains from 4 to 10 carbon atoms and which contains no radical having more than 6 carbon atoms, passing the said structures into a second bath and stretching said structures in the said second bath' to an extent of at least 14.
  • a process of producing regenerated cellulosic structures which comprises extruding unripened viscose into a coagulating bath comprising an aqueous solution of 4% to 12% sulfuric acid, 13% to sodium sulfate, 2% to 15% zinc sulfate and at least 0.2% of a bath-soluble monoamine which contains from 4 to 10 carbon atoms and which contains no radical having more than 6 carbon atoms.
  • An aqueous 4 to 12% sulfuric acid spinning bath for the spinning of regenerated cellulosic structures from unripened viscose said bath containing from 2% to 15% zinc sulfate together with at least 0.2% of a bath-soluble monoamine which contains from 4 to 10 carbon atoms and which contains no radical having more than 8 carbon atoms.
  • An aqueous sulfuric acid bath for the spinning of regenerated cellulosic structures from unripened viscose said bath containing from 4% to 12% sulfuric acid, 13% to 25% sodium sulfate, to 15% zinc sulfate and at least 0.2% of a bath-soluble monoamine which contains from 4 to 10 carbon atoms and which contains no radical having more than 6 carbon atoms.
  • An aqueous sulfuric acid bath for the spinning of regenerated cellulosic structures from unripened viscose said bath containing from 4% to 12% sulfuric acid, 13% to 25% sodium sulfate, 2% to 15% zinc sulfate, 1% to 5% ferrous sulfate and 0.2% to 0.5% of a bath-soluble monoamine which contains from 4 to 10 carbon atoms and which contains no radical having more than 6 carbon atoms.

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  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Artificial Filaments (AREA)
US744069A 1947-04-26 1947-04-26 Spinning of viscose Expired - Lifetime US2535045A (en)

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FR961353D FR961353A (zh) 1947-04-26
US744069A US2535045A (en) 1947-04-26 1947-04-26 Spinning of viscose
GB603/48A GB652746A (en) 1947-04-26 1948-01-08 Improvements in the spinning of viscose
DEP28795D DE829649C (de) 1947-04-26 1948-12-31 Verfahren zur Herstellung von Gebilden aus regenerierter Cellulose

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Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2810658A (en) * 1954-08-16 1957-10-22 Du Pont Process for spinning modified viscose solution
US2813038A (en) * 1953-04-07 1957-11-12 Courtaulds Ltd Production of artificial filaments, threads and the like
US2855321A (en) * 1955-03-30 1958-10-07 Du Pont Viscose process
US2908581A (en) * 1954-11-03 1959-10-13 American Viscose Corp Producing all skin viscose rayon
US2937922A (en) * 1954-03-24 1960-05-24 Rayonier Inc Viscose process
US2947597A (en) * 1956-02-20 1960-08-02 American Enka Corp Manufacture of viscose rayon
US2952508A (en) * 1953-09-16 1960-09-13 Rayonier Inc Viscose process and products produced thereby
US2971817A (en) * 1955-06-29 1961-02-14 American Viscose Corp Producing all skin rayon
US3007764A (en) * 1957-10-01 1961-11-07 Du Pont Process of preparing viscose rayon
US3016305A (en) * 1956-05-10 1962-01-09 Kunstzijdespinnerij Nyma Nv Manufacture of thick-skinned or allskin shaped articles from viscose
US3018158A (en) * 1959-05-05 1962-01-23 Rayonier Inc Viscose process
DE1144000B (de) * 1958-12-13 1963-02-21 Stockhausen & Cie Chem Fab Verfahren zum Koagulieren von Viskose
US3097414A (en) * 1958-10-30 1963-07-16 Woodell
US3112158A (en) * 1959-07-02 1963-11-26 Fmc Corp Method of producing shaped bodies of regenerated cellulose from viscose and spinning solution and bath therefor
US3112986A (en) * 1958-10-30 1963-12-03 Beaunit Corp Process for the production of crimpable regenerated cellulose fibers and yarn
US3194861A (en) * 1957-03-25 1965-07-13 Beaunit Corp Viscose spinning process and bath
US3531560A (en) * 1968-10-28 1970-09-29 Int Paper Canada Spinning of viscose

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1090373B (de) * 1955-07-27 1960-10-06 Du Pont Verfahren zur Herstellung von Gebilden, insbesondere Faeden, aus regenerierter Cellulose
BE558773A (zh) * 1956-08-29
CN112402095B (zh) * 2020-11-17 2022-05-31 新领医药技术(深圳)有限公司 一种硫酸镁冷敷贴及其制备工艺

Citations (5)

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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
US2125031A (en) * 1935-02-16 1938-07-26 American Enka Corp Manufacture of artificial silk
US2294379A (en) * 1938-10-07 1942-09-01 North American Rayon Corp Surface-active incrustation inhibitor
US2340377A (en) * 1939-12-11 1944-02-01 Graumann Erich Process of making artificial fibers
US2364273A (en) * 1941-11-22 1944-12-05 Du Pont Production of cellulosic structures

Patent Citations (5)

* 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
US2125031A (en) * 1935-02-16 1938-07-26 American Enka Corp Manufacture of artificial silk
US2294379A (en) * 1938-10-07 1942-09-01 North American Rayon Corp Surface-active incrustation inhibitor
US2340377A (en) * 1939-12-11 1944-02-01 Graumann Erich Process of making artificial fibers
US2364273A (en) * 1941-11-22 1944-12-05 Du Pont Production of cellulosic structures

Cited By (18)

* 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
US2952508A (en) * 1953-09-16 1960-09-13 Rayonier Inc Viscose process and products produced thereby
US2937922A (en) * 1954-03-24 1960-05-24 Rayonier Inc Viscose process
US2810658A (en) * 1954-08-16 1957-10-22 Du Pont Process for spinning modified viscose solution
US2908581A (en) * 1954-11-03 1959-10-13 American Viscose Corp Producing all skin viscose rayon
US2855321A (en) * 1955-03-30 1958-10-07 Du Pont Viscose process
US2971817A (en) * 1955-06-29 1961-02-14 American Viscose Corp Producing all skin rayon
US2947597A (en) * 1956-02-20 1960-08-02 American Enka Corp Manufacture of viscose rayon
US3016305A (en) * 1956-05-10 1962-01-09 Kunstzijdespinnerij Nyma Nv Manufacture of thick-skinned or allskin shaped articles from viscose
US3194861A (en) * 1957-03-25 1965-07-13 Beaunit Corp Viscose spinning process and bath
US3007764A (en) * 1957-10-01 1961-11-07 Du Pont Process of preparing viscose rayon
US3097414A (en) * 1958-10-30 1963-07-16 Woodell
US3112986A (en) * 1958-10-30 1963-12-03 Beaunit Corp Process for the production of crimpable regenerated cellulose fibers and yarn
US3248466A (en) * 1958-10-30 1966-04-26 Beaunit Corp Process for producing two component crimpable regenerated cellulose fiber
DE1144000B (de) * 1958-12-13 1963-02-21 Stockhausen & Cie Chem Fab Verfahren zum Koagulieren von Viskose
US3018158A (en) * 1959-05-05 1962-01-23 Rayonier Inc Viscose process
US3112158A (en) * 1959-07-02 1963-11-26 Fmc Corp Method of producing shaped bodies of regenerated cellulose from viscose and spinning solution and bath therefor
US3531560A (en) * 1968-10-28 1970-09-29 Int Paper Canada Spinning of viscose

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FR961353A (zh) 1950-05-11
GB652746A (en) 1951-05-02

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