US2840449A - Method of producing all skin rayon - Google Patents
Method of producing all skin rayon Download PDFInfo
- Publication number
- US2840449A US2840449A US518988A US51898855A US2840449A US 2840449 A US2840449 A US 2840449A US 518988 A US518988 A US 518988A US 51898855 A US51898855 A US 51898855A US 2840449 A US2840449 A US 2840449A
- Authority
- US
- United States
- Prior art keywords
- viscose
- cellulose
- skin
- filaments
- bath
- 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
- This invention relates to the production of shaped bodies of regenerated cellulose from viscose and more particularly to filaments and fibers of regenerated cellulose from viscose.
- 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 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 subsequently be passed through a hot aqueous bath where it is stretched to improve its properties such as tensile strength.
- the filament may then be passed through a dilute aqueous solution of sulfuric acid and sodium sulfate to complete the regeneration of the cellulose, in case it is not completely regenerated upon leaving
- 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 portion 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 zinc salts or certain other polyvalent metal salts are present in the spinning bath.
- the skin and core portions of the filament represent differences in structure and these differentportions possess different swelling and staining characteristics, the latter permitting a ready idenamounts of B-hydroxyethyl hydrazine in viscose results I,
- the amountof B-hydroxyethyl hydrazine which isincorporated in the viscose must be at least about 0.5 by weight of the cellulose in theviscose and may vary up to about 4%, .preferably, the amount varies from about 1% to 2%. Lesser amounts do not result in the production of products consisting entirely of skin and greater amounts affect adversely the physical properties of the products. Amounts within the preferred range aremost effective in enhancing the characteristics and properties of the products.
- the B-hydroxyethyl hydrazine may be added at any desired stage in the production of the viscose such as in the preparation of the refined wood pulp.
- the B-hydroxyethyl hydrazine is preferably added after the cellu- V lose xanthate has beendissolved in the caustic solution and prior to filtration.
- the viscose may contain from about 6% to about 10% cellulose, the particular source of the cellulose being selected for the ultimate use of the regenerated cellulose product.
- the caustic soda content may be from about 4% to about 8% and the carbon disulfidecontent 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 B-hydroxyethyl hydrazine should have a sodium chloride salt test above about 6 and preferably above about 7 at the time of spinning or extrusion.
- salt test as used herein refers to the conventional sodium chloride salt test.
- the spinning bath is a low acid-high spinning bath containing from about 10% to about 25% soduim sulfate and from about 3% to about 15% zinc sulfate, preferably from 15% to 22% sodium sulfate and from 4% to 9% zinc sulfate.
- Other metal sulfates such asiron, 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 C., preferably between about 45 C. and about 70 C..
- 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 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 main tained above the slubbing point and below the point sulfici'ently rapid to produciejfilaments having a skin andcore. 'For example, in general, the acid concentration of the spinning baths which are satisfactory for the production of the all skin products from a 7% cellulose,
- 6% caustic-viscose and containing B-hydroxyethyl hydrazine lies between about 6%Land about 8%.
- the acid concentration maybe increasedas" the amount of B-hydroxethyl hydrazine is increased and also as the salt testfof the viscose is increased.
- a lowering of the amount of the B- hydroxyethyl hydrazine, the lowering of the caustic soda content or the lowering of the salttest of the viscose reducesthe maximum permissible acid concentration for theproduction of allskin filaments; It has been determined that the maximum concentration of acid which is permissible for the production of all skin products is about 8.7% to 8.9%.
- theB-hydroxyethyl hydrazine is employed in amounts within the lower portion of the range, for example, about 1%.
- the determination of the specific maximum and optimum concentrationof acid for any specific viscose, spinning bath and spinning speed is a matter of simple' experimentation for those skilled in the art.
- the extruded viscosemust of course, be immersed or maintained in the spinning bathfor a period sufiicient toetfect relatively complete coagulation of the viscose, that is, the coagulation must besufficient so that the filaments will not adhereto eachother as they are brought together andwithdrawn from the bath,
- the filaments are preferably stretched after removal-from the initial coagulating and regenerating bath.
- the filaments may be passed through a hotaqueous bath which may consist of hot water or a dilute acid solution and may be stretched from about 70% to about 120%, preferably between 80% and 100%.
- Yarns for other textile purposes may be stretchedas low as 20%. The precise amount of stret'ching will be dependent upon the desired tenacity and other properties and the'specific type of product being produced.
- thefilaments may bestretched in air. It is to beunderstood that the inven# tion is' not restricted to the production of filaments and yarns but his also applicable to other shaped bodies such as sheets, films, tubes] andthe like.
- the filaments 'the filament.
- 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.
- Regenerated cellulose filaments prepared from viscose containing the small amounts of B-hydroxyethyl hydrazine and spun in the spinning baths of limited acid content have a smooth or non-crenulated surface and consist substantially entirely of skin. Because of the uniformity of structure throughout the filament, the swelling and staining characteristics are uniform throughout the crosssection of the filament.
- Filaments produced pursuant to this invention and consisting entirely of skin have a high toughness and a greater flexing lifethan filaments as produced'according to prior methods which may be at tributed by the uniformity in skin'structure throughout
- the twisting of conventional filaments, as in the production of tire cord results in an appreciable loss of tensile strength, there is appreciably less loss in tensile strength in the production of twisted cords from the filaments consisting entirely of skin.
- Filaments prepared from'viscose containing B-hydroxyethyl hydrazine have a superior abrasion and "fatigue resistance characteristics and have a high flex-life.
- Such filaments are highly satisfactory for the production of cords for the reinforcement of rubber products such as pneumatic tire casings, but the filaments are not restricted to such uses and may be used for other textile applications.
- the invention may be illustrated'by reference to the preparation of regenerated cellulose filaments from a viscose containing about 7% cellulose, about 6.5% caustic soda, and having a total carbon disulfide content of about 35% based on the weight of the cellulose.
- the viscose solution was prepared by xanthating alkali cellulose by the introduction of 35% 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.
- About 1% B-hydroxyethyl hydrazine, based on the weight of the cellulose, 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. at The viscose was extruded through a spinneret to form a 210 denier, 120
- the coagulating and regenerating bath was maintained at a temperature of about 60 C. and contained 8% sulfuric acid, 8% zinc'sulfate and 18% sodium sulfate.
- the yarn was stretched about 82% while passing through a hot water bath at C.
- the yarn was collected in a spinning box,.washed free of acids and salts, and jdried.
- the individual filaments have a smooth, non-crenulated exterior surface and consist entirely of skin, no core being detectable athigh magnification (e. g.
- a viscose solution prepared as described above but without the addition of B-hydroxyethyl hydrazineand having a salt test of 9.2, was spun into a 210 denier, filament yarn by extrusioninto a bath containing 7.9% sulfuric acid, 8% zinc sulfate and 20% sodium sulfate.
- the bath was maintained at a temperature of about 60 C. and 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. about 82% while passing through; the hot water.
- the yarn was Tenacity, Elongation, Grams per Percent Viscose denier Skin,
- the B-hydroxyethyl hydrazine 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 B-hydroxyethyl hydrazine may be added at any desired stage in the producti'on 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 B-hydroxyethyl hydrazine 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 6 in a Wax block is taken and mounted on a slide with Meyers albumin fixative. After dewaxing in xylene, the
- a method of producing shaped bodies of regenerated cellulose consisting substantially entirely of skin the steps which comprise adding to and incorporating in viscose from about 0.5% to about 4%, based on the weight of the cellulose, of B-hydroxyethyl hydrazine, and extruding the viscose into an aqueous spinning bath containing from about 10% to 25% sodium sulfate, from about 3% to 15% zinc sulfate and sulfuric acid, the sulfuric acid content of the bath exceeding the slubbing point but not exceeding about 9%.
- the method of producing shaped bodies of regenerated cellulose consisting substantially entirely of skin which comprises adding to and incorporating in a viscose from about 0.5% to about 4%, based on the weight of the cellulose, of B-hydroxyethyl hydrazine, ripening the viscose to a sodium chloride salt point of not less than 6 and extruding the viscose into an aqueous spinning bath containing from about 16% to 20% sodium sulfate, from about 4% to 9% zinc sulfate and sulfuric acid, the sulfuric acid content of the spinning bath exceeding the slubbing point but not exceeding about 8.9%.
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Artificial Filaments (AREA)
Description
Claims (1)
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US518988A US2840449A (en) | 1955-06-29 | 1955-06-29 | Method of producing all skin rayon |
US674290A US2890131A (en) | 1955-06-29 | 1957-07-26 | Method of producing all skin rayon |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US518988A US2840449A (en) | 1955-06-29 | 1955-06-29 | Method of producing all skin rayon |
Publications (1)
Publication Number | Publication Date |
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US2840449A true US2840449A (en) | 1958-06-24 |
Family
ID=24066323
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US518988A Expired - Lifetime US2840449A (en) | 1955-06-29 | 1955-06-29 | Method of producing all skin rayon |
Country Status (1)
Country | Link |
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US (1) | US2840449A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2993798A (en) * | 1955-09-13 | 1961-07-25 | Spinnfaser Ag | Viscose spinning solution containing xanthated lower alcohol |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
US2535044A (en) * | 1947-04-26 | 1950-12-26 | Du Pont | Spinning of viscose |
US2593466A (en) * | 1948-07-16 | 1952-04-22 | Ind Rayon Corp | Viscose spinning solution |
-
1955
- 1955-06-29 US US518988A patent/US2840449A/en not_active Expired - Lifetime
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
US2535044A (en) * | 1947-04-26 | 1950-12-26 | Du Pont | Spinning of viscose |
US2593466A (en) * | 1948-07-16 | 1952-04-22 | Ind Rayon Corp | Viscose spinning solution |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2993798A (en) * | 1955-09-13 | 1961-07-25 | Spinnfaser Ag | Viscose spinning solution containing xanthated lower alcohol |
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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: 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: 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: 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: 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: 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: 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 |