US2853360A - Viscose spinning process - Google Patents
Viscose spinning process Download PDFInfo
- Publication number
- US2853360A US2853360A US466674A US46667454A US2853360A US 2853360 A US2853360 A US 2853360A US 466674 A US466674 A US 466674A US 46667454 A US46667454 A US 46667454A US 2853360 A US2853360 A US 2853360A
- Authority
- US
- United States
- Prior art keywords
- viscose
- filaments
- skin
- water
- cellulose
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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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
- D01F2/10—Addition to the spinning solution or spinning bath of substances which exert their effect equally well in either
Definitions
- a suitable cellulosic material such as purified cotton linters, wood pulp, mixtures thereof, and the like is first converted to an alkali cellulose by treatment with a caustic soda solution and after shredding the treated cellulose material, it is allowed to age.
- the aged alkali cellulose is then converted to a xanthate by treatment with carbon disulfide.
- the cellulose xanthate is subsequently dissolved in a caustic soda solution in an amount calculated to provide a viscose of the desired cellulose and alkali content.
- the viscose solution is allowed to ripen and is subsequently extruded through a shaped orifice into a suitable coagulating and regenerating bath.
- the filaments as formed by the conventional methods consist of a skin or outer'shell portion and a core portion with a sharp line of demarkation between the .two.
- the cross-section of the'filarnents exhibits a very irregular or crenulated 'exteriorsurface when even small amounts of zinc salts or certain other polyvalent metal saltssare present in thespinning bath.
- the skin and core .portions of 'the filament representdiiferences in structure and these different portions possess different swelling. and staining characteristics, the latter permitting a ready identification of skin and core.
- the sharply 'irregularand crenulated surface structure has a relatively low abrasion resistance and readily picks up foreign particles such as dirt.
- the coreportion possess 'a re'latively'high tensile strength, it has a low abrasion resistance and a'low flex-life, is subject to fibrillation "and is re'lativelystiff.
- This invention contemplates the use of alkylene oxide adducts of morpholine'havingfrom 1 to about 50.or more alkylene oxide groups per molecule, preferably from 1 to about 20 alkylene oxide units per molecule of morpholine. It is obvious that for all practical purposes con sidering cost, ease of preparation, commercial availability and solubility in water, in alkali solutions and in acid solutions, the ethylene oxide adducts are preferred.
- n is from 1 to about 50. It is not necessary to employ individual specific compounds of the type described and the reaction product which may consist of a mixture of specific compounds, the average alkylene oxide content per molecule of morpholine being within the stated range are satisfactory.
- the amount of the adduct which is incorporated in the viscose "must be at least about 0.25% by weight of ⁇ the cellulose in the viscose and may vary up to about 4% preferably, the amountvaries-from-0.5 to 2%. Lesser amounts do not result in the production of products consisting entirely of skin and greater amounts aflect adversely the physical properties of the products. Amounts withinthe preferred range are most effective in enhancing the characteristics and properties of the products.
- the adduct of morpholine may be added at any desired stage in the production-of the viscose such as in the preparation of the refined wood pulp for the manufacture of viscose, before or duringthe shredding of the alkali cellulose, -to the -xanthated cellulose while it is being dissolved inthe caustic solution or to the viscose solution before ,or after filtration.
- the adduct is preferably added after the cellulose xanthate has been dissolved in the caustic solution and prior tofiltration.
- the viscose may contain from about 6% to about 8% cellulose, the particular source of the cellulose being 'se "lected for the ultimate use of the regenerated cellulose product.
- the caustic soda content may be from about 4% to about 8% and the carbon disulfide content may be from about 30% to about 50% based upon the weight of the cellulose.
- the modified viscose that is, a viscose containing 'the small amount of adduct, may have a salt 'test above about '7 and preferably above about '8 at the time of spinning or extrusion.
- salt test as used herein refers to the conventional sodium chloride salt test.
- the .spinning bath contain in solution at least about 0.01% of the adduct.
- the presence of the alkylene oxide adducts of morpholine in the viscose and in the spinning bath combined with these limited spinning baths results in the production of yarns of improved properties such as high tenacity, high abrasion resistance, high fatigue resistance and consisting of filaments composed entirely of skin.
- the spinning bath is a low acid-high zinc spinning bath to which is added the adduct of morpholine in amounts of from about 0.01% to about 0.1%, preferably about 0.05%.
- the bath should contain from about to about 25% sodium sulfate and from about 3% to about zinc sulfate, preferably from 15% to 22% sodium sulfate and from 4% to 9% zinc sulfate.
- Other metal sulfates such as iron, manganese, nickel and the like may be present and may replace some of the Zinc sulfate.
- the temperature of the spinning bath may vary from about 25 C. to about 80 C., preferably between about 45 C. and about 70 C.
- the temperature of the spinning bath is not critical, however, as is well known in the conventional practice in the art, certain of the physical properties such as tensile strength vary directly with the temperature of the spinning bath.
- the spinning bath is preferably maintained at a temperature between about 55 C. and 65 C. so as to obtain the desired high tensile strength.
- the acid content of the spinning bath is balanced against the composition of the viscose.
- the lower limit of the acid concentration is just furic acid result in the production of products having skin and core.
- a lowering of the amount of adduct of morpholine, the lowering of the caustic soda content or the lowering of the salt test of the viscose reduces the maximum permissible acid concentration for the production of all skin filaments. It has been determined that the maximum concentration of acid which is permissible for the production of all skin products is about 8.5%.
- the acid concentration of the spinning bath is generally maintained about 0.4% to 0.5% above the For any specific viscose composition, the acid concentration of the spinning bath must be maintained above the slubbing point and below the point at which the neutralization of the caustic of the viscose is sufiiciently rapid to form a filament having a skin and core.
- the adduct is employed in amounts within the lower portion of the range, for example, about 0.5
- the determination of the specific maximum and optimum concentration of acid for any specific viscose, spinning bath and spinning speed is a matter of simple experimentation for those skilled in the art.
- the extruded viscose must, of course, be immersed or maintained in the spinning bath for a period suificient to eifect relatively complete coagulation of the viscose, that is, the coagulation must be sufiicient so that the filaments will not adhere to each other as they are brought together and withdrawn from the bath.
- the filaments may then be passed through a final regenerating bath which may contain from about 1% to about 5% sulfuric acid and from about 1% to about 5% sodium sulfate with or without small amounts of zinc sulfate if regeneration has not previously been completed.
- the treatment following the final regenerating bath, or the stretching operation where regeneration has been completed may consist of a washing step, a desulfurizing step, the application of a finishing or plasticizing material and drying before or after collecting, or may include other desired and conventional steps such as bleaching and the like.
- the treatment after regeneration will be dictated by the specific type of shaped body and the proposed use thereof.
- the invention may be illustrated by reference to the preparation of regenerated cellulose filaments from a viscose containing about 7% cellulose, about 6% caustic soda, and having a total carbon disulfide content of about 41% based on the weight of the cellulose.
- the viscose solutions were prepared by xanthating alkali cellulose by the introduction of 36% carbon disulfide based on the weight of the cellulose and churning for about 2% hours. The cellulose xanthate was then dissolved in caustic soda solution. An additional carbon disu'lfide was then added to the mixer and the (mass mixed for about one hour. The desired amount of an ethylene oxide adduct of morpholine was added to the solution and mixed for about /2 hour. The viscose was then allowed to ripen for about 30 hours at 18 C.
- Example 1 Approximately 1% (based on the weight of the cellulose) of an ethylene oxide adduct of morpholine containing 1 ethylene oxide unit per molecule (N-beta-hydroxy- :ethylmorpholine or 4-rnorpholine ethanol) was added to andincorporated in the viscose as described above.
- ethylene oxide adduct of morpholine containing 1 ethylene oxide unit per molecule N-beta-hydroxy- :ethylmorpholine or 4-rnorpholine ethanol
- the coagulating and regenerating bath was maintained at a temperature-of about 60 C. and contained 7.3% sulfuric acid, 8.2% zinc sulfate, 18% sodium sulfate and 0.05% of the ethylene oxide adduct of morpholine.
- the yarn was stretched about 90% while passing through a hot water bath at 95 C. The'yarn was collected in a spinning box, washed free of acids and salts and dried.
- the individual filaments have a smooth, non-crenulated exterior surface and consist entirely of skin, no core being detectable at high magnification (e. g. 1500X).
- Other physical properties are set forth in the table which follows the examples.
- Example 2 To a viscose as described above, there was added 2% of an ethylene oxide adduct of morpholine containing 20 ethylene oxide units per molecule (a 4-morpholinepoly (oxyethylene)ethanol).
- the viscose had a salt test of 8.2 and was spun into a 210 denier, 120 filament yarn by extrusion into a spinning bath containing 7.6% sulfuric acid, 8.6% zinc sulfate, 20% sodium sulfate, and 0.05 of an ethylene oxide adduct of morpholine containing 20 ethylene oxide units per molecule.
- the bath was maintained at 60 C. and the extrusion rate was about 22 meters per minute.
- the filaments were subsequently passed through a hot water bath at 95 C. and stretched about 48%.
- the yarn was collected in a spinning box, washed free of acids and salts and dried.
- control filaments were readily distinguishable from control filaments in that they have a smooth, noncrenulated surface and consist entirely of skin while the control filaments have a very irregular and serrated surface and consist of about 75% skin and the balance core with a sharp line of demarkation between the skin and core.
- Other physical properties are set forth in the table which follows the examples.
- Example 3 As a control for the foregoing examples, a viscose solution, prepared as described above, having a salt test of 10 was spun into a 210 denier, 120 filament yarn by extrusion into a bath containing 7.6% sulfuric acid, 8% zinc sulfate and 18% sodium sulfate. The bath was maintained at a temperature of about 61 C. The extrusion rate was about 22 meters per minute. The water bath was maintained at a temperature of about 95 C. and the filaments were stretched 82% while passing through the hot water. The yarn was collected in a spinning box, washed free of acid and salts and dried.
- the individual filaments have a very irregular and serrated surface and consist of about 75% skin .and the balance core with a sharp line of demarkation between the skin and the core. Other characteristics are set forth in the table which follows:
- tenacity and elongation are the only properties set forth, they have been chosen because of the ease and simplicity with which such properties may be determined. In some instances, products made in accordance with this invention do not exhibit large or great improvements in tenacity and elongation, however, the products consist of a smooth-surfaced, all skin structure and possess improved abrasion resistance, flex-life and other properties as disclosed hereinbefore.
- the modifier of this invention may be added to'any desired viscose such as those normally used in industry, the specific viscose composition set forth above, being merely for illustrative purposes.
- the alkylene oxide adduct of morpholine may be added at any desired stage in the production of the viscose and may be present in the cellulosic raw material although it may be necessary to adjust the amount present to produce a viscose having the proper proportions of the adduct at the time of spinning.
- the term skin is employed to designate that portion of regenerated cellulose filaments which is permanently stained or dyed by the following procedure: A microtome section of one or more of the filaments mounted in a wax block is taken and mounted on a slide with Meyers albumin fixative. After dewaxing in xylene, the section is placed in successive baths of 60% and 30% alcohol for a few moments each, and it is then stained in 2% aqueous solution of Victoria Blue BS conc. (General Dyestuffs Corp.) for l to 2 hours; At this point, the entire section is blue.
- Victoria Blue BS conc. General Dyestuffs Corp.
- the dye By rinsing the section first in distilled Water and then in one or more baths composed of 10% water and dioxane for a period varying from 5 to 30minutes depending on the particular filament, the dye is entirely removed from the core, leaving it restricted to the skin areas.
- a method of producing shaped bodies of regenerated cellulose consisting substantially entirely of skin the step which comprises extruding a viscose containing from about 0.25% to about 4%, based on the weight of the cellulose in the viscose, of a water-soluble morpholine derivative into an aqueous spinning bath containing from about 10% to 25% sodium sulfate, from about 3% to zinc sulfate, at least about 0.01% of a water-soluble morpholine derivative and sulfuric acid, the sulfuric acid content of the spinning bath exceeding the slubbing point but not evceeding about 8.5%, the morpholine derivative being selected from the group consisting of Water-soluble compounds and mixtures of water-soluble compounds represented by the formula C H2 C H2 0 N -(alkylene oxide) "H 0 Hg 0 H3 wherein n is from 1 to about 50.
- the morpholine derivative is selected from the group consisting of water-soluble compounds and mixtures of water-soluble compounds represented by the formula set forth in claim 1 wherein the alkylene oxide is ethylene oxide and n is from 1 to 30.
- n is from 1 to about 50.
- the morpholine derivative is selected from the group consisting of water-soluble compounds and mixtures of water-soluble compounds represented by the formula set forth in claim 3 wherein the alkylene oxide is ethylene oxide and n is from 1 to 30.
- An aqueous spinning bath for the production of regenerated cellulose products consisting substantially entirely of skin from viscose containing from about 10% to 25% sodium sulfate, from about 3% to 15% zinc sulfate, at least about 0.01% of a water-soluble morpholine derivative and up to about 8.5% sulfuric acid, the morpholine derivative being selected from the group consisting of water-soluble compounds and mixtures of water-soluble compounds represented by the formula CIEQC'H:
- morpholine derivative is selected from the group consisting of water-soluble compounds and mixtures of water-soluble compounds represented by the formula set forth in claim 5 wherein the alkylene oxide is ethylene oxide and n is from 1 to 30.
Description
Claims (1)
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US466674A US2853360A (en) | 1954-11-03 | 1954-11-03 | Viscose spinning process |
US667667A US2888356A (en) | 1954-11-03 | 1957-06-24 | All skin viscose rayon |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US466674A US2853360A (en) | 1954-11-03 | 1954-11-03 | Viscose spinning process |
Publications (1)
Publication Number | Publication Date |
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US2853360A true US2853360A (en) | 1958-09-23 |
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Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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US466674A Expired - Lifetime US2853360A (en) | 1954-11-03 | 1954-11-03 | Viscose spinning process |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2974004A (en) * | 1954-11-25 | 1961-03-07 | American Enka Corp | Production of shaped objects from viscose |
US3049398A (en) * | 1955-12-05 | 1962-08-14 | American Viscose Corp | Method of producing all skin rayon |
US3063789A (en) * | 1960-11-29 | 1962-11-13 | American Viscose Corp | Method for producing viscose rayon |
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 |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2125031A (en) * | 1935-02-16 | 1938-07-26 | American Enka Corp | Manufacture of artificial silk |
US2312152A (en) * | 1941-12-10 | 1943-02-23 | American Viscose Corp | Rayon and method of manufacturing same |
US2373712A (en) * | 1943-04-19 | 1945-04-17 | Rayonier Inc | Viscose production |
US2593466A (en) * | 1948-07-16 | 1952-04-22 | Ind Rayon Corp | Viscose spinning solution |
-
1954
- 1954-11-03 US US466674A patent/US2853360A/en not_active Expired - Lifetime
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2125031A (en) * | 1935-02-16 | 1938-07-26 | American Enka Corp | Manufacture of artificial silk |
US2312152A (en) * | 1941-12-10 | 1943-02-23 | American Viscose Corp | Rayon and method of manufacturing same |
US2373712A (en) * | 1943-04-19 | 1945-04-17 | Rayonier Inc | Viscose production |
US2593466A (en) * | 1948-07-16 | 1952-04-22 | Ind Rayon Corp | Viscose spinning solution |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2974004A (en) * | 1954-11-25 | 1961-03-07 | American Enka Corp | Production of shaped objects from viscose |
US3049398A (en) * | 1955-12-05 | 1962-08-14 | American Viscose Corp | Method of producing all skin rayon |
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 |
US3063789A (en) * | 1960-11-29 | 1962-11-13 | American Viscose Corp | Method for producing viscose rayon |
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Owner name: PAUL REVERE LIFE INSURANCE COMPANY THE C/O THE PAU Free format text: AS SECURITY FOR INDEBTEDNESS RECITED ASSIGNOR GRANTS , BARGAINS, MORTGAGES, PLEDGES, SELLS AND CREATES A SECURITY INTEREST WITH A LIEN UNDER SAID PATENTS, SUBJECT TO CONDITIONS RECITED.;ASSIGNOR:AVTEX FIBERS INC. A NY CORP.;REEL/FRAME:003959/0219 Effective date: 19810301 Owner name: WESTERN AND SOUTHERN LIFE INSURANCE COMPANY THE C/ Free format text: AS SECURITY FOR INDEBTEDNESS RECITED ASSIGNOR GRANTS , BARGAINS, MORTGAGES, PLEDGES, SELLS AND CREATES A SECURITY INTEREST WITH A LIEN UNDER SAID PATENTS, SUBJECT TO CONDITIONS RECITED.;ASSIGNOR:AVTEX FIBERS INC. A NY CORP.;REEL/FRAME:003959/0219 Effective date: 19810301 Owner name: PROVIDENT ALLIANCE LIFE INSURANCE COMPANY C/O THE Free format text: AS SECURITY FOR INDEBTEDNESS RECITED ASSIGNOR GRANTS , BARGAINS, MORTGAGES, PLEDGES, SELLS AND CREATES A SECURITY INTEREST WITH A LIEN UNDER SAID PATENTS, SUBJECT TO CONDITIONS RECITED.;ASSIGNOR:AVTEX FIBERS INC. A NY CORP.;REEL/FRAME:003959/0219 Effective date: 19810301 Owner name: WALTER E. HELLER & COMPANY, INC., A CORP. OF DEL. Free format text: AGREEMENT WHEREBY AETNA RELEASES AVTEX FROM ALL MORTAGES AND SECURITY INTERESTS IN SAID INVENTIONS AS OF JANUARY 11,1979, AND ASSIGNS TO ASSIGNEE THE ENTIRE INTEREST IN SAID MORTAGE AGREEMENT TO ASSIGNEE;ASSIGNORS:AETNA BUSINESS CREDIT, INC., A CORP. OF N.Y.;AVTEX FIBERS, INC, A CORP. OF NY;KELLOGG CREDIT CORP., A CORP. OF DEL.;REEL/FRAME:003959/0250 Effective date: 19800326 Owner name: KELLOGG CREDIT CORPORATION A DE CORP. Free format text: AGREEMENT WHEREBY SAID HELLER AND RAYONIER RELEASES ALL MORTGAGES AND SECURITY INTERESTS HELD BY AVTEX ON APRIL 28, 1978, AND JAN. 11, 1979, RESPECTIVELY AND ASSIGNS ITS ENTIRE INTEREST IN SAID MORT-AGAGE AGREEMENT TO ASSIGNEE;ASSIGNORS:WALTER E. HELLER & COMPANY, INC. A NY CORP.;ITT RAYONIER INCORPORATED, A DE CORP.;AVTEX FIBERS INC., A NY CORP.;REEL/FRAME:003959/0350 Effective date: 19800326 Owner name: BALBOA INSURANCE COMPANY C/O THE PAUL REVERE EQUIT Free format text: AS SECURITY FOR INDEBTEDNESS RECITED ASSIGNOR GRANTS , BARGAINS, MORTGAGES, PLEDGES, SELLS AND CREATES A SECURITY INTEREST WITH A LIEN UNDER SAID PATENTS, SUBJECT TO CONDITIONS RECITED.;ASSIGNOR:AVTEX FIBERS INC. A NY CORP.;REEL/FRAME:003959/0219 Effective date: 19810301 Owner name: NEW ENGLAND MUTUAL LIFE INSURANCE COMPANY 501 BOYL Free format text: AS SECURITY FOR INDEBTEDNESS RECITED ASSIGNOR GRANTS , BARGAINS, MORTGAGES, PLEDGES, SELLS AND CREATES A SECURITY INTEREST WITH A LIEN UNDER SAID PATENTS, SUBJECT TO CONDITIONS RECITED.;ASSIGNOR:AVTEX FIBERS INC. A NY CORP.;REEL/FRAME:003959/0219 Effective date: 19810301 Owner name: JOHN HANCOCK MUTUAL LIFE INSURANCE COMPANY JOHN HA Free format text: AS SECURITY FOR INDEBTEDNESS RECITED ASSIGNOR GRANTS , BARGAINS, MORTGAGES, PLEDGES, SELLS AND CREATES A SECURITY INTEREST WITH A LIEN UNDER SAID PATENTS, SUBJECT TO CONDITIONS RECITED.;ASSIGNOR:AVTEX FIBERS INC. A NY CORP.;REEL/FRAME:003959/0219 Effective date: 19810301 |