US3055728A - Method of producing crimped viscose fibers - Google Patents

Method of producing crimped viscose fibers Download PDF

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Publication number
US3055728A
US3055728A US675407A US67540757A US3055728A US 3055728 A US3055728 A US 3055728A US 675407 A US675407 A US 675407A US 67540757 A US67540757 A US 67540757A US 3055728 A US3055728 A US 3055728A
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Prior art keywords
fiber
cellulose
bath
stretch
fibers
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Expired - Lifetime
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US675407A
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English (en)
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Kaiser Franz
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Phrix Werke AG
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Phrix Werke AG
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/22Formation of filaments, threads, or the like with a crimped or curled structure; with a special structure to simulate wool
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • D01F2/06Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
    • D01F2/08Composition of the spinning solution or the bath

Definitions

  • the present invention relates to a new method of producing crimped viscose fibers, and more particularly to a method of producing crimped viscose fibers from freshly spun viscose whereby a high degree of crimping is obtained.
  • the degree of crimping depends upon numerous factors such as the degree of ripeness of the viscose, the composition of the spinning bath, the temperature of stretching of the fibers and other conditions.
  • the degree of crimping depends upon numerous factors such as the degree of ripeness of the viscose, the composition of the spinning bath, the temperature of stretching of the fibers and other conditions.
  • a good crimping is obtained, that is the fibers are sharply bent, and in other cases only a weak degree of crimping is obtained, that is the arc length of the crimped fiber is many times the desired arc length.
  • the present invention mainly consists in a method of producing crimped regenerated cellulose fibers from viscose by subjecting freshly spun viscose fibers to a predetermined stretch, according to which method the freshly spun viscose fibers still in plastic state and consisting in this state mainly of cellulose xanthogenate is subjected to a first or pre-stretch corresponding at most to one-third of the total of the predetermined stretch, subjecting the thus partially stretched viscose fiber after partial conversion of the same to cellulose hydrate to a second stretch corresponding to the difference between the first stretch and the total of the predetermined stretch so as to further stretch the fiber, and completing conversion of the thus further stretched fiber to regenerated cellulose, whereby the thus obtained regenerated cellulose fiber is highly crimped.
  • the thus partially converted fiber-s are subjected to the remaining stretch either in a single stretching operation or in a plurality of stretching operations. This further stretching of the partially converted fibers must be carried out before the fibers have been completely converted to cellulose hydrate because after complete conversion of the fibers to cellulose hydrate a strong degree of stretching will result in tearing of the fibers.
  • the further stretching of the partially stretched fiber that is the stretching of the fibers after partial conversion of the same to mainly cellulose hydrate is about double the pre-stretching or stretching of the fibers while the same are mainly in the form of cellulose Xathogenate.
  • the total amount of stretching of the fibers is to an extent such that the stretched fiber is about 60-65% of the thickness of the original fiber before stretching. In other words, the total amount of stretching is such that the diameter of the original fiber is reduced so as to be between 6065% of the original diameter.
  • up to one-third of the stretching is carried out in the pre-stretched step when the fiber is mainly in the form of cellulose xanthogenate, that is up to one-third of the total reduction in diameter, or up to about 12-13% of the diameter reduction occurs during the first stretching step while the remaining twothirds of the total diameter reduction, or 24-26% of the diameter reduction occurs in the second stretching operation when the fiber is partially converted to cellulose hydrate.
  • the fiber After the final stretching, that is after the fiber has been stretched so that the diameter of the fiber is between 6065% of the diameter of the original fiber the fiber is finally completely converted into the form of regenerated cellulose or cellulose hydrate.
  • the resulting fiber is highly crimped.
  • the time that the fiber remains in the spinning bath is not sufficient under any circumstances to substantially convert the fiber into the form of cellulose hydrate.
  • the stretching is accomplished in accordance with the present invention by withdrawing the fiber from the spinning bath at a predetermined speed, for example at a speed of 40 m./ minute.
  • the fiber is then drawn onto a second roller at a greater speed, for example at a speed of 50 m./ minute. This increase of speed between the first and second roller results in a stretching of the fiber, and this stretching is the first or pre-stretching while the fiber is still mainly in the form of cellulose xanthogenate.
  • the fiber After the fiber has to a great extent been converted to cellulose hydrate, for example 75-95% of the original cellulose xanthogenate has been converted to cellulose hydrate, this being accomplished if necessary by passage of the pre-stretched fiber through a second bath, the fiber is then withdrawn on a third roller at a still greater speed, for example at a speed of 65 m./minute to accomplish the final stretching, e.g. the remaining two-thirds of the predetermined stretch. Since the length of the fiber remaining in the first precipitating bath from which the fiber is spun is about 10-15 cm.
  • the fiber After emerging from the spinning bath there is practically no further conversion of the cellulose xanthogenate into cellulose hydrate because the acid still remaining on the fiber becomes very quickly exhausted. Therefore, the fiber is passed into a second acid bath in accordance with the present invention to further convert the cellulose xanthogenate to cellulose hydrate, though not yet completely, and after emerging from this second acid bath the fiber which is now partially converted to cellulose hydrate is, in accordance with the present invention, subjected to the final stretching operation to stretch the remaining two-thirds of the predetermined stretch, that is to stretch it so that the thickness of the fiber is reduced the final 24-27% to a thickness which is about 6065% of the thickness of the original fiber.
  • this final or after stretching is preferably carried out in an acid medium in which the acid content amounts to about 10 g. per liter of H 80
  • This acid content can easily be arrived at by treating the freshly spun fiber or cable of fibers, which still contain certain amounts of acid from the precipitating bath, with measured amounts of hot water during this final stretching operation.
  • a temperature of 50-100 C. of the hot water is particularly suitable.
  • a relatively unripe viscose having a Hottenroth degree of ripeness of 14 or about should be used.
  • the alkali content of the viscose plays a decisive role for obtaining such degree of ripeness.
  • a viscose of this type of which the alkali factor (that is the relationship between the NaOH and the alpha cellulose) is below 0.9, and preferably is between 0.8 and 0.85 is particularly suitable for crimping in accordance with the method of the present invention.
  • the precipitating baths are of the same type and composition as the usual precipitating baths, baths with a sulfuric acid content of more than 100 g./l. of sulfuric acid and high sodium sulfate content of more than 300 g./l. with the addition of small amounts of zinc salts being preferred.
  • the fibers which in accordance with the present invention have been subjected to a first stretching operation while the fibers are mainly in the form of cellulose xanthogenate and to a second stretching operation while the fibers are partially converted to cellulose hydrtae are, after practically complete conversion to cellulose hydrate or regenerated cellulose, without any particular further tension conducted to a cutting device in which the fibers are cut and then finally in loose condition subjected to the usual final treatment.
  • the cut fibers are immediately dropped into a hot treating bath, this first treating bath being as usual an alkali bath.
  • the use of such bath is not essential for obtaining the desired crimping since by properly stretching the fibers in accordance with the present invention the crimping can finally be obtained by introducing the cut and stretched fibens into a bath of only hot water. After this suspending operation the fibers are subjected to the customary after treatment such as desulfurization, washing, bleaching, brightening and drying of the finally cut fibers which are obtained at the end of the preferably continuous process in a condition which, with respect to crimping, closely corresponds to natural wool fibers.
  • the viscose solution flowing in through the conduit 1 through the nozzle 2 into the spinning bath 3 which is contained in the spinning vat 4- is formed into fibers at the nozzle and these fibers are drawn from the bath by means of a roller 5 which, for example, rotates at a speed such that the peripheral speed is 40 m./minute.
  • the distance between the nozzle 2 and the roller 5 is about 15 cm.
  • the fresh fiber 6 from the roller 5 is wound about a roller 7 which runs at a peripheral speed of about 48 m./minute.
  • the fiber is wound several times around this roller 7 and for this purpose is passed over a glass fiber conductor 8.
  • the fiber is passed into a hot stretching bath 9, which bath is heated by means of heating devices which are not shown so that the bath is maintained at a temperature of preferably C.
  • the acid bath liquid is passed into the vat 9 through the inlet 10 and out of the same through the outlet 11.
  • glass fiber guides 12 and 13 are arranged at the beginning and the end of the bath respectively.
  • the fiber emerging from the bath 9 is conducted over a three member roller arrangement consisting of rollers 14, 15 and 16 which run with a starting peripheral speed of 53 m./minute.
  • the rollers serve partly to squeeze out the excess bath liquid from the fiber.
  • the spray nozzles 17 which are arranged above the rollers 14, 15 and 16 serve the same purpose and the nozzles run hot water over the rollers.
  • the liquid running over the rollers is caught in trough 18 and can be utilized for example in the stretching bath trough 9.
  • the change in the thickness of the fiber is given by relationship to the change in deniers. It is understood that a fiber has a denier value of one denier when 9000 meters of this fiber weighs 1 g. Thus, if 9000 meters of the fiber weighs 2 g. the fiber has a denier value of 2 denier, etc.
  • the absolute thickness in millimeters is not given because of the extremely small absolute thickness, for example a fiber having a denier value of 3 deniers actually has a diameter of 0.017 mm. It is for this reason that the fiber thickness is given in relationship to the denier value thereof.
  • Example A viscose containing 8.9% alpha cellulose and 7.3 NaOH and having a degree of ripeness according to Hottenroth of 15 is spun in a bath which contains 120-135 g. of H 80 about 340 g. of Na S and 5-10 g. of ZnSO per liter.
  • the fiber is drawn from the bath at a speed of 40 m./minute and while still mainly in the form of cellulose xanthogenate is by means of .a correspondingly faster running roller drawn at a rate of 47-50 m./ minute.
  • the fiber drawn from the spinning bath has a denier value of about 5 denier. After being drawn onto the second roller at the faster Speed and thereby somewhat stretched the fiber has a denier value of about 4 denier.
  • the fiber is then passed through an intermediate bath containing -30 g./l. of H 80 per liter of hot water, the temperature of the bath being between 50-l00 C., and the bath also containing a small amount of salt.
  • the fiber is drawn onto a three roller arrangement moving at a peripheral speed of 60-65 m./minute.
  • the fiber is first sprayed with Water and is then passed over a second three roller arangement moving at a starting peripheral speed of 65 m./minute whereby the fiber is drawn and without tension passed into a cutting device.
  • the fiber which is passed into the cutting device has a final denier value of about 3 denier.
  • the still acid fiber is then cut into the desired lengths and the cut fibers fall into a bath containing about 0.1-0.15 g./l.
  • the fibers coming from the bath are then subjected in the usual manner to washing, bleaching, brightening and drying.
  • the resulting fibers are crimped and with respect to the crimping have the appearance of natural wool.
  • a method of producing crimped regenerated cellulose fibers from viscose by subjecting freshly spun viscose fibers to a predetermined stretch corresponding to a reduction in the diameter of the fiber to between 60- 65% of the original diameter, the steps of subjecting a viscose fiber emerging from a sulfuric acid precipitating bath containing more than g./l. of sulfuric acid and more than 300 g./l.
  • a method of producing crimped regenerated celluose fibers from viscose comprising the steps of spinning viscose fibers in a sulfuric acid precipitating bath containing more than 100 g./l. of sulfuric acid and more than 300 g./l.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Artificial Filaments (AREA)
US675407A 1956-08-09 1957-07-31 Method of producing crimped viscose fibers Expired - Lifetime US3055728A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEP16816A DE1203418B (de) 1956-08-09 1956-08-09 Herstellen gekraeuselter Zellwolle aus Viskose

Publications (1)

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US3055728A true US3055728A (en) 1962-09-25

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US675407A Expired - Lifetime US3055728A (en) 1956-08-09 1957-07-31 Method of producing crimped viscose fibers

Country Status (6)

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US (1) US3055728A (xx)
BE (1) BE558974A (xx)
DE (1) DE1203418B (xx)
FR (1) FR1177664A (xx)
GB (1) GB827558A (xx)
NL (2) NL109311C (xx)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3302385A (en) * 1961-08-26 1967-02-07 Ruddell James Nelson Modification of filaments
US6051172A (en) * 1997-07-31 2000-04-18 Robert L. Phillips Method of manufacture for flexible cutting line
CN113089112A (zh) * 2019-12-23 2021-07-09 连津格股份公司 用于制造纤维素纤维的纺丝机及其操作方法

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3423499A (en) * 1965-02-18 1969-01-21 Fmc Corp Process for spinning modified xanthated polymers

Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1930803A (en) * 1927-11-01 1933-10-17 Harrison William Manufacture of artificial filaments
US2302971A (en) * 1940-06-11 1942-11-24 American Enka Corp Manufacture of rayon
US2340377A (en) * 1939-12-11 1944-02-01 Graumann Erich Process of making artificial fibers
US2364273A (en) * 1941-11-22 1944-12-05 Du Pont Production of cellulosic structures
US2369191A (en) * 1939-03-01 1945-02-13 American Enka Corp Manufacture of rayon
GB570159A (en) * 1943-11-18 1945-06-25 Courtaulds Ltd Improvements in and relating to the production of crimped artificial threads by the viscose process
US2427993A (en) * 1944-07-26 1947-09-23 Ind Rayon Corp Production of rayon
US2440057A (en) * 1944-03-15 1948-04-20 Du Pont Production of viscose rayon
US2515834A (en) * 1942-11-13 1950-07-18 Du Pont Cellulose filaments and method of producing same
US2515889A (en) * 1949-01-28 1950-07-18 Du Pont Process for producing artificial filaments
US2723900A (en) * 1952-12-03 1955-11-15 Ind Rayon Corp Spinning of acrylonitrile polymers

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US808149A (en) * 1905-06-19 1905-12-26 Silas W Pettit Apparatus for producing or forming filaments from viscose, &c.
DE743307C (de) * 1936-08-21 1943-12-22 Schlesische Zellwolle Ag Verfahren zur Herstellung gekraeuselter Zellwolle aus Viskose
CH244571A (de) * 1943-12-16 1946-09-30 Haederli Charles Vorrichtung zur Streckung von künstlichen Fadengebilden, wie Einzelfäden, Bänder oder Kabel.
NL61100C (xx) * 1944-02-15

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1930803A (en) * 1927-11-01 1933-10-17 Harrison William Manufacture of artificial filaments
US2369191A (en) * 1939-03-01 1945-02-13 American Enka Corp Manufacture of rayon
US2340377A (en) * 1939-12-11 1944-02-01 Graumann Erich Process of making artificial fibers
US2302971A (en) * 1940-06-11 1942-11-24 American Enka Corp Manufacture of rayon
US2364273A (en) * 1941-11-22 1944-12-05 Du Pont Production of cellulosic structures
US2515834A (en) * 1942-11-13 1950-07-18 Du Pont Cellulose filaments and method of producing same
GB570159A (en) * 1943-11-18 1945-06-25 Courtaulds Ltd Improvements in and relating to the production of crimped artificial threads by the viscose process
US2440057A (en) * 1944-03-15 1948-04-20 Du Pont Production of viscose rayon
US2427993A (en) * 1944-07-26 1947-09-23 Ind Rayon Corp Production of rayon
US2515889A (en) * 1949-01-28 1950-07-18 Du Pont Process for producing artificial filaments
US2723900A (en) * 1952-12-03 1955-11-15 Ind Rayon Corp Spinning of acrylonitrile polymers

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3302385A (en) * 1961-08-26 1967-02-07 Ruddell James Nelson Modification of filaments
US6051172A (en) * 1997-07-31 2000-04-18 Robert L. Phillips Method of manufacture for flexible cutting line
CN113089112A (zh) * 2019-12-23 2021-07-09 连津格股份公司 用于制造纤维素纤维的纺丝机及其操作方法

Also Published As

Publication number Publication date
NL218225A (xx)
DE1203418B (de) 1965-10-21
GB827558A (en) 1960-02-10
NL109311C (xx)
FR1177664A (fr) 1959-04-28
BE558974A (xx)

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