US2194470A - Process and apparatus for the manufacture of artificial silk - Google Patents

Process and apparatus for the manufacture of artificial silk Download PDF

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Publication number
US2194470A
US2194470A US131942A US13194237A US2194470A US 2194470 A US2194470 A US 2194470A US 131942 A US131942 A US 131942A US 13194237 A US13194237 A US 13194237A US 2194470 A US2194470 A US 2194470A
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US
United States
Prior art keywords
sulphur
thread
water
rollers
viscose
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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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US131942A
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English (en)
Inventor
Hartmann August
Uytenbogaart Johannes
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North American Rayon Corp
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North American Rayon Corp
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Publication date
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Publication of US2194470A publication Critical patent/US2194470A/en
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Classifications

    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
    • D01D10/06—Washing or drying
    • 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
    • D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
    • D01F11/02—Chemical after-treatment of artificial filaments or the like during manufacture of cellulose, cellulose derivatives, or proteins

Definitions

  • the present invention relates to the manufacture of filaments of artificial origin but more particularly has for its object to devise a process of and apparatus for the desulphurization of viscose rayon in a continuous process.
  • the continuously progressing thread should be treated within a few seconds, or fraction thereof, after leaving the spinning bath or while the sulphur is in a colloidal state.
  • the novel process is especially adaptable to the so-called continuous spinning process in which rollers, described for example in French Patent No. 745,254, or the United States equivalent Patent 2,002,995 may be used.
  • Another object of the present invention is to provide a precipitatory bath for viscose rayon which precipitates the sulphur in the filaments in a state which allows ready removal of the sulphur.
  • Still another object of the present invention is to provide an after-treatment process for viscose rayon which removes the greater part of the sulphur therefrom.
  • the numeral l indicates a spinning nozzle from which is drawn the thread 3.
  • the nozzle I is immersed in the spinning or precipitating bath 2 through which the threads 3 are drawn and coagulated.
  • a driven roller 4 delivers the thread to the inclined treating cylinders 5 and 6 over which the thread is passed in an approximately helical path.
  • These rollers 5 and 6 which are inclined for a purpose to be later explained, are also in- 26 clined with respect to each other whereby the thread which is looped a plurality of times around the rollers is fed from one end of the said rollers to the other end thereof.
  • the thread 3 is then carried from the lower roller to a stationary 30 guide 1 and from there passes to any suitable collecting device (not shown).
  • the said thread 3 may first becarried from the rollers 5 and 6 to other treating steps such as washing and drying before being passed to a collecting device.
  • a sulphuric acid solution is sprayed from the nozzle 8 which is mounted on the end of a supply pipe 9.
  • the sulphuric acid is sprayed onto the top roller 5 in a regulated amount whereby it spreads in a film down over the surface of the cylinder and the loops of thread conveyed thereon.
  • the acid flows in a film evenly down the cylinder 5 and drips oil the lower edge thereof and is caught by a drip pan III. From the drip pan ill the spent acid is. carried off by a drain pipe II.
  • a supply pipe l2 carries water to a nozzle 13 which sprays the lower roller or cylinder 6 in a regulated quantity so that no spraying of the water results.
  • the water flows down in an even film over the roller 6 and across the thread winding to the lower edge of the roller from where it drips into a drip pan l4.
  • a drain pipe l5 carries off the waste water.
  • the spent sulphuric acid which is carried away bythe drain pipe ll may be recovered by carrying it to storage tanks in which the colloidal sulphur carried by the acid may be allowed to settle. After removal of this sulphur, which is done by allowing it to settle out and filtering, the acid may again be used.
  • the viscose spinning solution is extruded 'through the spinning nozzle I into a precipitating bath which is preferably maintained at a temperature of about -'70 C. (preferably -60) and which consists of an aqueous solution containing about 80 to 200 gr. sulphuric acid (1.84 specific gravity) (preferably about 119-121 gr.), about 240-300 gr. of sodium sulphate, (preferably about 280-285 gr.), and about 5-25 gr. of zinc sulphate, (preferably about 16.0-16.5 gr.), per liter.
  • sulphuric acid (1.84 specific gravity
  • sodium sulphate preferably about 280-285 gr.
  • zinc sulphate preferably about 16.0-16.5 gr.
  • This bath which is low in acid concentration and high in salt concentration, is used because it is necessary to keep the viscose from becoming fully regenerated so that in the immediate after-treatment with sulphuric acid on the rollers the said acid may have full access throughout the thread to more readily wash out the collodial sulphur precipitated therein.
  • This type of bath also produces a thread which minimizes shrinkage particularly longitudinally and imparts a definite elastic tension whereby it may more readily feed along the rollers.
  • a further advantage to be gained by the use of such a bath is that a thread is produced which is in a low hydrated state, making it an easy matter to wash out the residual acid.
  • salts which might be used in place of sodium sulphate are aluminum sulphate, magnesium sulphate, ammonium sulphate, zinc sulphate, or potassium sulphate.
  • the high zinc sulphate concentration in the bath is used because the hydrated zinc groups are more slowly decomposed than the sodium groups. This has the effect of acting as a buffer against the action of the sulphuric acid on the threads.
  • a further advantage of the high zinc concentration is that the threads which are treated thereby have deeper dyeing qualities.
  • the somewhat high temperature of the bath compensates somewhat for the slowness of coagulation of the viscose and at the same time results on keeping the volume of the spin bath as near constant as possible due to evaporation.
  • the threads after passing through the spinm'ng bath, described above, are drawn therefrom by the drawing roller 4 and passed to the rollers 5 and 6 for treatment with acid and water.
  • the sulphuric acid which is applied to the roller 5 is an aqueous solution containing about to 170 gr. of sulphuric acid (preferably to gr.), per liter.
  • This sulphuric acid solution is applied to the roller at a temperature of about 20 to 60 C. although it is preferably about 40 to 45 C. and the water which is applied to the other roller 6 is at a temperature above 80 C.
  • the sulphur may be removed from the filaments by the action of the sulphuric acid solution which contacts it very shortly after the initial regeneration of the cellulose and before the regeneration of the cellulose is completed, and also before the sulphur fiocculates or while it is .in a collodial state.
  • This treatment with acid may continue for a considerable distance, i. e., 5, 15, or 20 meters.
  • the threads passing from the precipitating bath to the spaced roller may be and preferably are stretched therebetween. Due to the fact that the threads have been only partially coagulated or regenerated a more satisfactory stretching may be given or imparted to the filament.
  • the sulphur while in a colloidal or semi-colloidal state and before flocculation thereof is easily removed physically by the acid on the roller and retained and carried away thereby.
  • the removal of the sulphur in this state is differentiated from a chemical separation which takes place after complete regeneration of the cellulose and flocculation of the sulphur.
  • the result is a golden-yellow, dilute sulphuric acid solution in which the sulphur is present in a collodial or semi-collodial form, which, when the said acid solution is carried to a settling tank and allowed to stand, will settlefto the bottom of the tank.
  • the acid may then be carried off from the top of the tank and filtered. This acid may then be re-used.
  • the invention as disclosed comprises extruding a viscose solution into a setting bath which partially coagulates them and precipitates the sulphur in a form whereby the sulphur may be readily removed by immediate treatment of the thread with a pure substantially salt-free sulphuric acid while the sulphur is still in a colloidal state, and also serves to further regenerate the cellulosic filaments.
  • the filaments proceed under the nozzle l3 they are subjected to a washing action, whereby the acid solution and sulphur, zinc, etc., carried by it are removed.
  • the application of the acid and water causes the thread to shrink longitudinally and maintain the necessary tension in order to cause the filaments to be fed upwardly by the rotating rollers.
  • the operations are preferably conducted so as to keep the degree of hydration of the filaments as low as possible in order that lateral shrinkage of the filaments will be minimized.
  • the threads made as described herein will have uniform properties, such as, uniform dyeing properties, uniform shrinkage properties and uniform denier, strength and elongation thoughout every length.
  • An apparatus for continuously spinning and treating filaments of artificial origin comprising, a spinning nozzle, a precipitating bath, a plurality of spaced rotors over which said filaments are conveyed alternately from one to the other of said rotors in a plurality of loops after leaving said precipitating bath, and means to supply a different treating liquid to each of said rotors.
  • An apparatus for continuously spinning and treating filaments of artificial origin comprising, a spinning nozzle, a precipitating bath, a plurality of spaced rotors over which said filaments are conveyed in plurality of loops after leaving said precipitating bath, said rotors having their axes at an angle to the horizontal, and means to supply a different treating liquid to each of said rotors.
  • An apparatus for continuously spinning and treating filaments of artificial origin comprising, a spinning nozzle, a precipitating bath, a plurality of spaced rotors over which said filaments are conveyed in plurality of loops after leaving said precipitating bath, said rotors having their axes at an angle to the horizontal, and means to supply a different treating liquid to each of said rotors in such quantities that they will substantially vertically drip from the lower ends of said rollers.
  • An apparatus for continuously spinning and treating filaments of artificial origin comprising, a spinning nozzle, a precipitating bath, a pair of spaced rollers about which the filaments are looped a plurality of times after leaving said precipitating bath, said rollers having their axes at an angle to the horizontal, and means to supply a diiferent treating liquid to each of said rollers in such regulated amounts that they will substantially vertically drip from the lower ends of said rollers.
  • the process of desulphurizing viscose rayon comprising treating a freshly spun viscose thread immediately after coagulation in successive lengths of a plurality of meters with a dilute and substantially salt-free sulphuric acid, and subsequently washing said thread with water, said acid containing about 80 to 170 grams of H2804 per liter of H20.
  • said precipitating bath containing about 80 to 200 g. of H2804 and about 245 to-325 g. of soluble salts per liter of water, and said salt-free sulphuric acid solution containing about 80 to 170 g. of H2804 per liter of water.

Landscapes

  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Artificial Filaments (AREA)
  • Treatment Of Fiber Materials (AREA)
  • Materials For Medical Uses (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
US131942A 1934-02-05 1937-03-19 Process and apparatus for the manufacture of artificial silk Expired - Lifetime US2194470A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEV30385D DE625355C (de) 1934-02-05 1934-02-05 Verfahren zum Nachbehandeln von Viscosekunstseide

Publications (1)

Publication Number Publication Date
US2194470A true US2194470A (en) 1940-03-26

Family

ID=41057579

Family Applications (2)

Application Number Title Priority Date Filing Date
US131942A Expired - Lifetime US2194470A (en) 1934-02-05 1937-03-19 Process and apparatus for the manufacture of artificial silk
US229038A Expired - Lifetime US2254251A (en) 1934-02-05 1938-09-08 Device for use in the aftertreatment of artificial silk

Family Applications After (1)

Application Number Title Priority Date Filing Date
US229038A Expired - Lifetime US2254251A (en) 1934-02-05 1938-09-08 Device for use in the aftertreatment of artificial silk

Country Status (5)

Country Link
US (2) US2194470A (enrdf_load_stackoverflow)
DE (4) DE625355C (enrdf_load_stackoverflow)
FR (2) FR783933A (enrdf_load_stackoverflow)
GB (2) GB432692A (enrdf_load_stackoverflow)
NL (2) NL39083C (enrdf_load_stackoverflow)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2418660A (en) * 1943-04-24 1947-04-08 Du Pont Manufacture of regenerated cellulose structures
US2516157A (en) * 1944-04-22 1950-07-25 American Viseose Corp Apparatus for spinning artificial filaments
US2582293A (en) * 1944-02-22 1952-01-15 American Viscose Corp Reel for fluid treatment of filamentary materials
US2622182A (en) * 1951-06-23 1952-12-16 American Cyanamid Co Apparatus for drying continuous filament yarn and the like
US2707668A (en) * 1943-10-02 1955-05-03 American Viscose Corp Method and apparatus for fluid treating yarn in a helical path
US2764012A (en) * 1953-08-05 1956-09-25 American Viscose Corp Fluid processing system for running strand
US2892336A (en) * 1954-02-02 1959-06-30 Pensotti Ambrogio Apparatus for wet-treating threads, particularly viscose rayon threads

Families Citing this family (30)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE740392C (de) * 1940-06-26 1943-10-20 Barmag Barmer Maschf Vorrichtung zur Nachbehandlung von Kunstseidefaeden im fortlaufenden Arbeitsgang
NL68203C (enrdf_load_stackoverflow) * 1942-07-14
BE476720A (enrdf_load_stackoverflow) * 1943-01-04
US2634597A (en) * 1945-04-06 1953-04-14 American Viscose Corp Apparatus for liquid treatment of strands
US2541149A (en) * 1945-08-29 1951-02-13 Du Pont Draw roll mechanism for hot stretching of artificial filaments
US2513381A (en) * 1945-12-06 1950-07-04 American Viscose Corp Method for treatment of filaments
US2616155A (en) * 1947-04-30 1952-11-04 Kuljian Harry Asdour Apparatus for manufacture of threads
US2647389A (en) * 1948-02-06 1953-08-04 American Viscose Corp Yarn advancing reel having liquid applying and liquid stripping means
US2608850A (en) * 1948-02-06 1952-09-02 American Viscose Corp Apparatus for the liquid treatment of yarns and the like
NL65265C (enrdf_load_stackoverflow) * 1948-05-07
US2625811A (en) * 1949-01-28 1953-01-20 Kuljian Corp Thread processing reel having liquid applying and liquid removing means
DE967950C (de) * 1949-10-13 1958-01-02 Bayer Ag Verfahren zur Herstellung von Faeden aus Loesungen oder Schmelzen von organischen Hochpolymeren
US2720100A (en) * 1950-06-22 1955-10-11 Wiskemann Franz Apparatus for the fluid treatment of filamentary material
DE927949C (de) * 1950-09-10 1955-05-20 Harry Asdour Kuljian Vorrichtung zur Behandlung von endlosen kuenstlichen Faeden
US2688863A (en) * 1950-10-09 1954-09-14 William F Luther Apparatus for the continuous mercerization of cotton
DE934302C (de) * 1951-05-09 1955-10-20 Harry Asdour Kuljian Vorrichtung zum Trocknen eines laufenden Fadens, insbesondere Kunstseidefadens, in Gestalt eines Fadenfoerderhaspels
BE512824A (enrdf_load_stackoverflow) * 1951-07-18
IT535752A (enrdf_load_stackoverflow) * 1951-11-08
NL175547B (nl) * 1952-01-25 Oerlikon Buehrle Ag Automatisch vuurwapen.
BE518965A (enrdf_load_stackoverflow) * 1952-04-05
US2714052A (en) * 1952-04-11 1955-07-26 American Cyanamid Co Method of washing a gelled thread of an acrylonitrile polymerization product
NL98387C (enrdf_load_stackoverflow) * 1952-04-30
BE519507A (enrdf_load_stackoverflow) * 1952-04-30
US2788256A (en) * 1952-06-02 1957-04-09 American Viscose Corp Method of spinning filamentary strands
US2750780A (en) * 1952-06-18 1956-06-19 Ind Rayon Corp Thread advancing reel having liquid applicator and wiper
NL86762C (enrdf_load_stackoverflow) * 1953-08-28
BE537745A (enrdf_load_stackoverflow) * 1954-04-30 1900-01-01
NL95876C (enrdf_load_stackoverflow) * 1955-01-05 1960-11-15
US2998620A (en) * 1958-06-09 1961-09-05 Owens Corning Fiberglass Corp Method and means for centrifuging curly fibers
US3554422A (en) * 1969-03-05 1971-01-12 Maremont Corp Yarn-processing apparatus

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2418660A (en) * 1943-04-24 1947-04-08 Du Pont Manufacture of regenerated cellulose structures
US2707668A (en) * 1943-10-02 1955-05-03 American Viscose Corp Method and apparatus for fluid treating yarn in a helical path
US2582293A (en) * 1944-02-22 1952-01-15 American Viscose Corp Reel for fluid treatment of filamentary materials
US2516157A (en) * 1944-04-22 1950-07-25 American Viseose Corp Apparatus for spinning artificial filaments
US2622182A (en) * 1951-06-23 1952-12-16 American Cyanamid Co Apparatus for drying continuous filament yarn and the like
US2764012A (en) * 1953-08-05 1956-09-25 American Viscose Corp Fluid processing system for running strand
US2892336A (en) * 1954-02-02 1959-06-30 Pensotti Ambrogio Apparatus for wet-treating threads, particularly viscose rayon threads

Also Published As

Publication number Publication date
DE625355C (de) 1936-02-10
DE744026C (de) 1944-01-07
NL39083C (enrdf_load_stackoverflow) 1936-09-15
US2254251A (en) 1941-09-02
GB499478A (en) 1939-01-24
DE711207C (de) 1941-09-27
GB432692A (en) 1935-07-31
NL50169C (enrdf_load_stackoverflow) 1941-04-15
FR783933A (fr) 1935-07-19
DE739537C (de) 1943-09-29
FR49674E (fr) 1939-05-30

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