US2956894A - Method of forming all skin viscose rayon - Google Patents
Method of forming all skin viscose rayon Download PDFInfo
- Publication number
- US2956894A US2956894A US775352A US77535258A US2956894A US 2956894 A US2956894 A US 2956894A US 775352 A US775352 A US 775352A US 77535258 A US77535258 A US 77535258A US 2956894 A US2956894 A US 2956894A
- Authority
- US
- United States
- Prior art keywords
- viscose
- choline
- filaments
- skin
- spinning
- 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
- asuitable cellulosic material such as purified cotton linte'rs, wood pulp, mixtures thereof, and the like is first co'nverted 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 their con verted to a xanthate by treatment with carbon disulfide.
- the cellulose x-anthate is subsequently dissolved in a caustic soda solutionin an amount calculated to providea viscose of: the desired cellulose and alkali content.
- the viscose-solution is allowed to river! and is subsequently extruded through a: shaped orifice into a suitable coagulating and regenerating bath.
- the viscose solution is extruded through a spinneret into a coagulating and regenerating bath consisting of an aqueous acid solution containing Zinc sulfate.
- the filament may then be passed through a diluteaqueous solution. of" sulfuric acid and sodium sulfate to complete the regeneration of the cellulose, in case it is not completely regenerated upon leav ing the stretching stage.
- the filament is subsequently subjected: to Washing, purification, bleaching, possibly other treating operations and drying, being collected either before or after these treatments.
- the filaments as formed by the conventional methods consist of: a skin or outer shell portion and a core-por tion with a sharp line of demarkation between the two.
- the cross-section of the filaments exhibits a very irregular or crenulated exterior surface when" even small amounts of zine salts or certain other polyvalent metal salts are present in the spinning bath.
- the skin and core portions of the filamentr epresent'differences in struc ture and these diiferentporti'ons possess different swelling and staining characteristics, the latter permitting a ready identification of skin and core.
- cr enul'at'ed surfacestructure has arelatively low abrasion resistance and readily picks-up foreign particles such as dirt.
- the core portion possesses a relatively high tensile strength, it has a low abrasion resistance and a low flex-life, is-subj'ect to fibrillation? andis' relatively stiff.
- Choline salts which are satisfactory for the purposes of this invention include both inorganic and organic anionssuoh as the halides, for example, the chloride and the bromide, sulfates, for example, the sulfate andthe bisulfate, the acetate, the propionate, etc. Mixtures of choline with one or more salts and mixtures of the salts are also satisfactory.
- the modifier maybe conveniently added in the form of a solution in water or in a caustic soda solution.
- the caustic soda content may be from about 4% to about 8% and the carbondisulfide 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 choline or a choline salt, may. have a salt test above about 7 and preferably above about 9 at the time of spinning .or extrusion.
- the composition of. the spinning bath be maintained within awell defined range.
- the presence of the choline or choline salt in the viscose combined with these limited spinning baths results in the production of yarns of improved properties such as high tenacity, high abrasion resistance,v high fatigue resistance and consisting of filaments. composed entirely of skin.
- the acid content of the spinning bath is balanced against the composition of the viscose.
- the lower limit of the acid concentration is just above the slubbing point, that is, the concentration at which small slubs of uncoagulated viscose appear in the strand as it leaves the spinning bath.
- the acid concentration of the spinning bath is generally maintained about 0.4% to 0.5% above the slubbing point.
- 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 sufficiently rapid to form a filament having a skin and core.
- 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.
- Regenerated cellulose filaments prepared from viscose containing the small amounts of choline or choline salts and spun in the spinning baths of limited acid content have a smooth or non-crenulated surface and consist entirely of skin. Because of the uniformity of structure throughout the filament, the swelling and staining characteristics are uniform throughout the cross-section of the filament. Filaments produced pursuant to this invention and consisting entirely of skin have a high toughness and a greater flexing life than filaments as produced according to prior methods which may be attributed by the uniformity in skin structure throughout the filament.
- the invention may be illustrated by reference to the preparation of regenerated cellulose filaments from a viscose modified with choline chloride and 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 /2 hours. The cellulose xanthate was then dissolved in caustic soda solution. An additional 5% carbon disulfide was then added to the mixer and the mass mixed for about one hour. The desired amount of modifier was added to the solution and mixed for about' /zhour. The viscose was then allowed to ripen for about 30 hours at 18 C.
- Example 1 Approximately 0.7% (based on the weight of the cellulose) choline chloride was added to and incorporated in the viscose as described above.
- the viscose employed in the spinning of filaments had a salt test of 11.
- the viscose was extruded through a spinneret to form a 200 denier, 1 2! filament yarn at a rate of about 22 meters per minute.
- the coagulating and regenerating bath was maintained" at a. temperature, of about 60 C. and contained 7.7%. sulfuric. acid, 8.3% zinc sulfate and 18% sodium sulfate.
- the yarn was stretched about 82% 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. 1500).
- Other physical properties are set forth in the table which follows the examples.
- Example 2 To a viscose as described above, there was added 1.4% choline chloride. The viscose had a salt test of 10.8 and was spun into a 200 denier, 120 filament yarn by extrusion into a spinning bath containing 7.8% sulfuric acid, 8.3% zinc sulfate and 18% sodium sulfate. The bath was maintained at 61 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 82%. 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 To a viscose solution as described above, there was added 1% choline chloride.
- the viscose had a salt test of and was spun into a 1650 denier, 720 filament cord by extrusion into a bath containing 7.2% sulfuric acid, 8% zinc sulfate and 17% sodium sulfate. The bath was maintained at a temperature of 60 C. The extrusion rate was about 21 meters per minute. The water bath was maintained at about 95 C. and the filaments were stretched approximately 90% while passing through the hot water. The cord was washed free of acid and salts by treatment with water at about 95 C. on thread-advancing reels, dried and collected on cones.
- control filaments were readily distinguishable from control filaments prepared from viscose containing no modifier in that they have a smooth, non-crenulated surface and consist entirely of skin. 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 4 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 60 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 choline or choline salt 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 modifying agent 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 oonc. (General Dyestuffs Corp.) for 1 to 2 hours. At this point, the entire section is blue.
- Victoria Blue BS oonc 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 30 minutes depending on the particular filament, the dye is entirely removed from the core, leaving it restricted to the skin areas.
- a viscose spinning solution containing a small amount of a modifying agent selected from the group consisting of choline, choline halides, choline sulfate, choline bisulfate, choline acetate, choline propionate and mixtures thereof, said small amount of the modifying agent being a quantity suflicient to impart a smooth, noncrenulated surface and a substantially all skin structure to products formed by spinning the viscose at a sodium chloride salt test of at least 7 into an aqueous bath containing from 15% to 22% sodium sulfate, from 4% to 9% zinc sulfate and sulfuric acid in an amount not exceeding 8.5%, but the quantity being insuflicient to adversely afiect the physical properties of such products.
- a modifying agent selected from the group consisting of choline, choline halides, choline sulfate, choline bisulfate, choline acetate, choline propionate
- a viscose spinning solution containing from about 0.3% to about 4.5%, based on the Weight of the cellulose in the viscose, of a modifying agent selected from the group consisting of choline, choline halides, choline sulfate, choline bisulfate, choline acetate, choline propionate and mixtures thereof.
Description
Claims (1)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US775352A US2956894A (en) | 1954-12-30 | 1958-11-21 | Method of forming all skin viscose rayon |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US478914A US2895788A (en) | 1954-12-30 | 1954-12-30 | Method of forming all skin viscose rayon |
US775352A US2956894A (en) | 1954-12-30 | 1958-11-21 | Method of forming all skin viscose rayon |
Publications (1)
Publication Number | Publication Date |
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US2956894A true US2956894A (en) | 1960-10-18 |
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Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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US775352A Expired - Lifetime US2956894A (en) | 1954-12-30 | 1958-11-21 | Method of forming all skin viscose rayon |
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Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB379260A (en) * | 1931-04-29 | 1932-08-25 | Fride Koerner | Improvements in and relating to the production of choline compounds |
US2536014A (en) * | 1946-12-14 | 1950-12-26 | Du Pont | Spinning of viscose |
-
1958
- 1958-11-21 US US775352A patent/US2956894A/en not_active Expired - Lifetime
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB379260A (en) * | 1931-04-29 | 1932-08-25 | Fride Koerner | Improvements in and relating to the production of choline compounds |
US2536014A (en) * | 1946-12-14 | 1950-12-26 | Du Pont | Spinning of viscose |
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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: 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: 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: 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 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: 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 |