US2923637A - Viscose solution - Google Patents
Viscose solution Download PDFInfo
- Publication number
- US2923637A US2923637A US667668A US66766857A US2923637A US 2923637 A US2923637 A US 2923637A US 667668 A US667668 A US 667668A US 66766857 A US66766857 A US 66766857A US 2923637 A US2923637 A US 2923637A
- Authority
- US
- United States
- Prior art keywords
- viscose
- aniline
- adduct
- filaments
- skin
- 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
Links
- 229920000297 Rayon Polymers 0.000 title claims description 75
- 238000009987 spinning Methods 0.000 claims description 50
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 22
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 20
- 150000003839 salts Chemical class 0.000 claims description 15
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 11
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 11
- 235000011152 sodium sulphate Nutrition 0.000 claims description 11
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 11
- 229960001763 zinc sulfate Drugs 0.000 claims description 11
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 11
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 10
- 230000000704 physical effect Effects 0.000 claims description 6
- 230000002411 adverse Effects 0.000 claims description 2
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 72
- 229920002678 cellulose Polymers 0.000 description 24
- 239000001913 cellulose Substances 0.000 description 24
- 239000002253 acid Substances 0.000 description 21
- 239000000243 solution Substances 0.000 description 21
- 238000004519 manufacturing process Methods 0.000 description 20
- 125000002947 alkylene group Chemical group 0.000 description 19
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 12
- 239000000203 mixture Substances 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 239000004627 regenerated cellulose Substances 0.000 description 9
- 238000001125 extrusion Methods 0.000 description 7
- 239000003513 alkali Substances 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- 230000001965 increasing effect Effects 0.000 description 6
- 230000001788 irregular Effects 0.000 description 6
- 230000001172 regenerating effect Effects 0.000 description 6
- 230000008961 swelling Effects 0.000 description 6
- 238000011282 treatment Methods 0.000 description 6
- 239000003518 caustics Substances 0.000 description 5
- 238000005299 abrasion Methods 0.000 description 4
- 230000001112 coagulating effect Effects 0.000 description 4
- ZOOODBUHSVUZEM-UHFFFAOYSA-N ethoxymethanedithioic acid Chemical compound CCOC(S)=S ZOOODBUHSVUZEM-UHFFFAOYSA-N 0.000 description 4
- 230000008929 regeneration Effects 0.000 description 4
- 238000011069 regeneration method Methods 0.000 description 4
- 239000012991 xanthate Substances 0.000 description 4
- 230000015271 coagulation Effects 0.000 description 3
- 238000005345 coagulation Methods 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000003607 modifier Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000004061 bleaching Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000001419 dependent effect Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000002964 rayon Substances 0.000 description 2
- 238000010186 staining Methods 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- 102000009027 Albumins Human genes 0.000 description 1
- 108010088751 Albumins Proteins 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- BWGNESOTFCXPMA-UHFFFAOYSA-N Dihydrogen disulfide Chemical compound SS BWGNESOTFCXPMA-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 150000001448 anilines Chemical class 0.000 description 1
- 239000011260 aqueous acid Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- QGJOPFRUJISHPQ-NJFSPNSNSA-N carbon disulfide-14c Chemical compound S=[14C]=S QGJOPFRUJISHPQ-NJFSPNSNSA-N 0.000 description 1
- 206010061592 cardiac fibrillation Diseases 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000003009 desulfurizing effect Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000002600 fibrillogenic effect Effects 0.000 description 1
- 239000000834 fixative Substances 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920001515 polyalkylene glycol Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000036555 skin type Effects 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- LLWJPGAKXJBKKA-UHFFFAOYSA-N victoria blue B Chemical compound [Cl-].C1=CC(N(C)C)=CC=C1C(C=1C=CC(=CC=1)N(C)C)=C(C=C1)C2=CC=CC=C2C1=[NH+]C1=CC=CC=C1 LLWJPGAKXJBKKA-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
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 productionof 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.
- Theaged alkali cellulose is then converted tov 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 stretching stage.
- Thefilament is subsequently subjected to washing, purification, bleaching, possibly other"treating operations and' drying, being collected either'befor'e 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 ofdemarkation between the two.
- the cross-section of the filaments exhibits a very irregular or crenulated exterior surface when even small amounts of zinc salts for certain other polyvalent metal salts are present in the spinning bath.
- the skin and core portions of the filament represent diiferences in structure and these diiferentportions possess different swelling and staining characteristics, the latter permitting a ready identification of skin and core.
- the sharply irregular and crenulated surface structure has a relatively low abrasion resistance and 'readily picks up foreign particles such as dirt.
- the" core portion possesses a relatively hightensile strength, ithas a lowabrasion resistance and a low flex-life, is subject to fibrillation and is relatively stiff.
- bodies of regenerated cellulose suchas filaments, films,
- alkylene oxide adducts of aniline having from about 2 to about 50 or more alkylene oxide groups per molecule, preferably from about 4 to about 30 alkylene oxide units per molecule of aniline. It is obvious that for all practical purposes considering cost, ease of preparation, commercial availabilityand solubility in water, in alkali solutions and in acid solutions, the ethylene oxide adductsare preferred.
- an alkylene oxide adduct such as ethylene oxide adduct of aniline containing 4 ethylene oxide units per molecule of aniline would consist of a compound in which each of the amino hydrogen atoms has been replaced with a chain of two ethylene oxide units. It is not necessary, however, that all of the amino hydrogens be replaced nor is it necessary that the ethylene oxide chains-replacing the difierent hydrogenatoms be the same in each'instance.
- adduct is used herein to simplify the disclosure and description and designates a water-soluble N-substitlited aniline formed by the reaction between an alkylene oxide andaniline wherein the alkylene oxide or a polyoxyalkylene chain replaces one or both of the hydrogen atoms attached'to the nitrogen atom. It is not necessary to' employ individual specific compounds of the type described and the reaction. products which probably consist of mixture of specific compounds, the average alkylene oxide content per molecule of aniline being within the stated ranges, are satisfactory. Where, for example, each of the amino hydrogen atoms has been replaced with an alkylene oxide group, the compound is a N,N-di(beta-hydroxyalkyl)aniline.
- the amino hydrogen atoms has been replaced with a polyalkylene glycol radical, the compound is a N-mono- (omega-hydroxy polyoxyalkylene) aniline.
- Compounds in which both amino hydrogen atoms have been replaced withalkylene oxide chains are N,N-di(omega-hydroxy polyoxyalkylene) anilines.
- the alkylene oxide adduct must have sufficient solubility topermit the minimum amount of the adduct to be dissolved in the viscose or the spinning bath or both.
- the adduct may be conveniently added to the viscose in the form of a' solution in alkali or water and to the spinning bath in a solution of water or of the spinning bath.
- the amount of the adduct which is incorporated in viscose must be at least about 0.2% by weight of the cellulose in the viscose and may vary up to about 4%, preferably, the amount varies from 0.5% to 2%. Lesser amounts do not result in the production of products consisting entirely of skin and greater amountsafiectadversely the physical properties of the products. Amou nts'within the preferred range are most effective in enhancing the characteristics and properties of the products.
- the adduct of aniline may be added at any desired stage. in the production of the viscose such.
- the viscose may contain fromabout 6% to about 8% 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,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 9 at the time of spinning or extrusion.
- the composition of the spinning bath be maintained within a well defined range.
- the presence of the alkylene oxide adducts of aniline in the viscose or 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.
- the bath should contain from about 10% to about 25% sodium 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 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 above the slubbing point, that is, the concentration at which small slubs of uncoagulated viscose appears 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 sufiiciently rapid to form a filament having a skin and core.
- 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 the adducts of aniline lies between about and about 7.8%.
- the acid concentration may be increased as the amount of adduct is increased and also as the salt test of the viscose is increased.
- ,4 cellulose about 6% caustic soda, about 41% carbon disulfide, based on the weight of the cellulose, 1%, based on the weight of the cellulose, of an ethylene oxide adduct of aniline containing about 6 ethylene oxide units per molecule and having a salt test of about 10 when extruded into spinning baths containing 16 to 20% sodium sulfate, 4 to 8% zinc sulfate and sulfuric acid not more than about 7.8%, results in the production of all skin filaments. Lesser amounts of sulfuric acid may be employed. Greater amounts of sulfuric acid results in the production of products having skin and core.
- a lowering of the amount of adduct of aniline, 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 1.35 times the percentage caustic soda content of the viscose and is preferably held between about 1.15 and 1.25 times the percentage caustic soda content of the viscose.
- the adducts of aniline in the viscose retards the coagulation and, therefore, the amount of adduct employed must be reduced at high spinning speeds
- the adduct is employed in amounts within the lower portion of the range, for example, about 0.5%.
- the filaments are preferably stretched after removal from the initial coagulating and regenerating bath.
- the filaments may be passed through a hot aqueous bath which may consist of hot water or a dilute acid solution and may be stretched from about 70% to about 120%, preferably between and Yarns for other textile purposes may be stretched as low as 20%.
- the precise amount of stretching will be dependent upon the desired tenacity and other properties and the specific type of product being produced. It is to be understood that the invention is not restricted to the production of filaments and yarns but it is also applicable to other shaped bodies such as sheets, films, tubes and the like.
- 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 washnig 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 the water-soluble alkylene oxide adducts of aniline and spun in the spinning baths of limited acid content have a smooth or noncrenulated 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 cross-section of the filament.
- Filaments producedpursuant to this invention and consisting entirely of skin have a high toughness and a greater flexing life than filaments as produced according to prior inthe production of twisted cords from the filaments' consisting entirely of skin.
- .Filaments prepared from viscose containing the alkylene oxide adducts of aniline have a high tensile strengtha's compared to normal regenerated cellulose filaments, have superior abrasion and fatigue resistance characteristics and have a high flexlife.
- 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 alkylene oxide adducts of aniline in the spinning bath in place of adding the adduct to the viscose. It is essential that the composition of the spinning bath, particularly the acid concentration be maintained within the limits set forth hereinbefore.
- the amount ofthe alkylene oxide adduct of aniline dissolved. in the spinning bath must be at least about 0.05% .by weight and is preferably maintained at about 0.1%.
- the upper limit does not appear to be critical as'in the incorporation of the adducts in the viscose. The upper. limit is dependent upon the solubility of the particular adduct and by economic considerations since "amounts exceeding about 0.2% are not more effective in improving the properties of the products.
- the adducts may be added to both the viscose and the spinning bath, if desired.v In such instance, it is also essential to maintain the amounts of the adduct of the viscoseand in the spinning bath, and the composition of the spinning bath within the stated limits.
- the all skin products of improved properties are obtained only when the spinning operation in the presence of the alkylene oxide adducts of aniline is carried out within the spinning bath composition as .set forth hereinbefore.
- 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 5% carbon disulfide was then added to the mixer and the mass mixed for about one hour. The viscose was then allowed to ripen for about 30 hours at 18 C. In those instances where the modifier was incorporated in the viscose, the desired amount of an ethylene oxide adduct of aniline was added to the solution and mixed for about /2 hour before allowing the viscose to ripen.
- Example 1 Approximately 1% (based on the weight of the cellulose) of an ethylene oxide adduct of aniline containing about 6 ethylene oxide units per molecule of aniline was added to and incorporated in the viscose as described above.
- the viscose employed in the spinning of filaments had a salt test of 10.
- the viscose was extruded through a spinneret to form a 1650 denier, 720 filament cord at a rate of about 22 meters per minute.
- the coagulating and regenerating bath was maintained at a temperature of about 60 and contained 7.1% sulfuric acid, 8%
- the cord was stretched about washed free of acids and salts by treatment with water at about C. on thread advancing reels, dried and collected on cones.
- 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 A viscose solution as described above (no adduct added) having a salt test of 10.7 was spun into a 210 denier, filament yarn by extrusion into a spinning bath containing'7.7% sulfuric acid, 8% zinc sulfate, 17% sodium sulfate and 0.1% of an ethylene oxide adduct of aniline containing about 6 ethylene oxide units per molecule of aniline. The bath was maintained at 60 C. and the extrusion rate was about 22 meters per minute. The filaments were. passed through a hot water bath maintained at about 95 C. and stretched about 82%. The yarn was collected in a spinning box, washed free of acid and salts anddried.
- the filaments have a smooth, non-crenulated surface and consist entirely of skin 'while 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 characteristics are set forth in the table which follows the examples.
- Example 3 To a viscose as describedabove, there was added 1% of an ethylene oxide adduct of aniline. containing 6 ethylene oxide units per'molecule of aniline.
- the viscose had a salt test of 10.7 and was spun into a 210 denier, 120 filament yarn by extrusion into a spinning bath containing 7.7% sulfuric acid, 8.3% zinc'sulfate, 17% sodium sulfate, and 0.1%, based on the weight of the cellulose in the viscose, of an ethylene oxide adduct of aniline containing 6 ethylene oxide units per molecule of aniline.
- 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 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 the 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 7.5% 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:
- 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 aniline 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 and 30% alcohol for a few moments each, and it is then stained in 2% aqueous solution of Victoria Blue BS conc. (General Dyestulfs Corp.) for 1 to 2 ho rs. At this point, the entire section is blue.
- Victoria Blue BS conc. General Dyestulfs Corp.
- the dye By rinsing the section first in dis tilled 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 water-soluble adduct of aniline with ethylene oxide, the adduct containing from about 2 to about 50 ethylene oxide units per molecule of aniline, said small amount of the adduct being a quantity sufficient to impart a smooth, non-crenulated surface and a substantially all skin structure to products formed by spinning the viscose at a salt test of at least 7 into an aqueous bath containing from 10% to 25% sodium sulfate, from 3% to 15% zinc sulfate and sulfuric acid in a percentage not exceeding about 1.25 times the percentage of caustic soda in the viscose, but the quantity being insufficient to adversely affect the physical properties of such products.
- a viscose spinning solution containing from about 0.2% to about 4%, based on the weight of the cellulose in the viscose, of a water-soluble adduct of aniline with ethylene oxide, the adduct containing from about 2 to about 50 ethylene oxide units per molecule of aniline.
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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 (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US667668A US2923637A (en) | 1954-11-03 | 1957-06-24 | Viscose solution |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US466677A US2975020A (en) | 1954-11-03 | 1954-11-03 | Producing all skin viscose rayon |
US667668A US2923637A (en) | 1954-11-03 | 1957-06-24 | Viscose solution |
Publications (1)
Publication Number | Publication Date |
---|---|
US2923637A true US2923637A (en) | 1960-02-02 |
Family
ID=27041743
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US667668A Expired - Lifetime US2923637A (en) | 1954-11-03 | 1957-06-24 | Viscose solution |
Country Status (1)
Country | Link |
---|---|
US (1) | US2923637A (en) |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2125031A (en) * | 1935-02-16 | 1938-07-26 | American Enka Corp | Manufacture of artificial silk |
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 |
-
1957
- 1957-06-24 US US667668A patent/US2923637A/en not_active Expired - Lifetime
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2125031A (en) * | 1935-02-16 | 1938-07-26 | American Enka Corp | Manufacture of artificial silk |
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 |
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