US3352957A - Process for spinning cellulosic fibers - Google Patents

Process for spinning cellulosic fibers Download PDF

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Publication number
US3352957A
US3352957A US321063A US32106363A US3352957A US 3352957 A US3352957 A US 3352957A US 321063 A US321063 A US 321063A US 32106363 A US32106363 A US 32106363A US 3352957 A US3352957 A US 3352957A
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Prior art keywords
bath
filaments
cellulose
spinning
viscose
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US321063A
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English (en)
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Drisch Nicolas
Herrbach Paul
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Chimiotex SA
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Chimiotex
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Priority claimed from FR914533A external-priority patent/FR1468625A/fr
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    • 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
    • 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

  • filaments having improved characteristics are obtained, notably filaments of high tenacity both in the conditioned state and in the wet state, by spinning viscose as described in French Patent No. 1,266,492 into a bath of low acid content, the essential element of the invention being that this first bath is maintained, not at ambient temperature, but at an extremely low temperature, below C., and not-ably between 10 C. and 0 C.
  • the process according to the invention makes it possible to obtain a high stretching capacity by physical means, namely the use of very low bath temperatures, whereby their regeneration power is further increased and very high gamma indices can thus be obtained.
  • the stretching it has been found (and other elements) that with a cold bath and a low acid concentration, the possible, degree of stretching of the gel is higher in proportion as the zinc sulphate content of the bath is lower. With the same temperature and the same zinc sulphate content, it is possible to stretch the gel to a greater extent as the sodium sulphate concentration of the bath is lower.
  • a viscose containing at least 3% of cellulose and 1.59% of sodium hydroxide, and of which the carbon disulphide content is at least 35% based upon the alpha-cellulose employed.
  • the gamma index of the viscose at the time of the spinning must be between 45 and and the cellulose contained in the viscose must have a DR of at least 400, and preferably above 500.
  • the viscosity of the viscose must be between and 1000 poises, and it is preferably higher than 400 poises.
  • the viscose which contains in addition 0.1-5% of a surface-active protecting agent such as sodium oleate, for example (based upon the alpha-cellulose) is spun into a bath which contains less than 40 g./l. of acid, preferably from 5 to 25 g. of acid per litre, from 10 to 100 g. per litre of sodium sulphate, preferably less than 40 g./l., and little or no zinc sulphate (less than 1 g./litre).
  • zinc sulphate tends to reduce the possible degrees of stretch, it is nevertheless preferable to use small quantities thereof because under these conditions a fibre of better quality is obtained.
  • the temperature of the bath is extremely low and is below 10 C., preferably between 10 and 0 C.
  • formaldehyde may be incorporated in the bath, or small quantities of retarding agents such as N-methylcyclohexylamine, polyhydroxyalkylamines, ethylene polyoxides, etc., may be added to this bath.
  • the excess solution is rea slight reduction in tension through a third degassing bath consisting of hot dilute acid. They are finally re-' ceived on an appropriate support without tension. After a relaxation period of several hours, the filaments are cut in the acid state in order to produce dis-' continuously fibres, these fibres are washed and they are treated in order to improve their transverse characteristics and their dye aflinity.
  • the filaments which are produced by the process described possess the so-called Polynosic structure, which means that their structural characteristics are stable and are not appreciably modified by a subsequent treatment with 5% sodium hydroxide, while under the same conditions filaments of ordinary rayon and pneumatic tire rayon are thoroughly disorganized.
  • the filaments according to the invention have a high tenacity which exceeds 4 g./den. in the wet state and 4.5 g./ den. in the conditioned state and they possess a high modulus of elasticity in the wet state, which results in a wet elongation of less than 3% under a load of 0.5 g./den. They have a circular cross-section and their swelling is currently lower than 65%.
  • Example 1 A cellulose pulp having a high alpha-cellulose content is immersed for 30 minutes in sodium hydroxide in a proportion of 242 g./l., at a temperature of 22 C., and thereafter pressed to a proportion of 3.13 in relation to the alpha-cellulose.
  • the alpha-cellulose formed is not subjected to any ripening and there is directly added thereto 43% of carbon disulphide (based on the alpha-cellulose).
  • the xanthate formed is thereafter dissolved in dilute sodium hydroxide at low temperature, but there is added to the mass an additional quantity of 5% of carbon disulphide together with 2% of sodium oleate and also 0.25% of Intrasol FSW (the condensation product of a fatty alcohol with ethylene oxide) and 0.15% of Nonanol, an alcohol with nine carbon atoms and a primary alcohol group (based on the alpha-cellulose).
  • Intrasol FSW the condensation product of a fatty alcohol with ethylene oxide
  • Nonanol an alcohol with nine carbon atoms and a primary alcohol group (based on the alpha-cellulose).
  • the viscose is spun with the aid of a spinneret having 8000 holes of .06 mm. diameter and a tube 5 cm. in diameter and 20 cm. long, into a first bath containing 12 g. of sulphuric acid, 25 g. of sodium sulphate and 0.3 g. of zinc sulphate per litre, as also small quantities of Ceponol TS (a dodecal toluene sulfonate) at a temperature of 8 C.
  • Ceponol TS a dodecal toluene sulfonate
  • the gamma index of the filaments leaving the first bath is 45.7 and it falls to 28 at the end of the stretching.
  • the filaments thereafter pass, through a second bath of the same composition and at the same temperature as the first bath, the length of immersion being 230 cm., and they then enter a third degassing bath at a temperature of 95 C., obtained by dilution of the first bath so that its sulphuric acid content is between 6 and 8 g. per litre, the sodium sulphate and the zinc sulphate being diluted in the same ratio.
  • the length of travel through this bath is 490 cm. and the filaments undergo therein a detensioning of 0. 8%.
  • the tow There is received in the pot the tow of 12,000 den., at a final speed of 12.5 metres per minute. After standing for a number of hours, the tow is divided in the acid state.
  • the fibres formed are then deacidified by washing with softened water, and are treated with a sodium hydroxide solution in a concentration of 40 g./l. at 30 C. for 30 minutes, in the state of primary swelling and then subjected to rinsing, desulphur-ising, washing, sizing and drying operations.
  • the characteristics of the filaments obtained are indicated in Table III as compared with those of filaments spun under the same conditions, but into baths at ambient temperature (20 C.).
  • a fabric of a texture of 47 x 27 woven with yarns having a metric count of 70, themselves obtained from filaments according to the invention shows a warp abrasion (on the Stoll-Flex apparatus) of 2700, in contrast to an abrasion of 1460 in the case of a similar fabric based on known filaments (spun into a bath at 20 C. under otherwise equal conditions).
  • Example 2 A viscose containing 5.5% of cellulose and 3.2% sodium hydroxide, prepared in the same way as that indicated in Example 1 is spun with the aid of the same tube arrangement into a first bath containing 12 g.- of sulphuric acid and 26 g. of sodium sulphate per litre, but completely free from zinc sulphate, at a temperature of 3 C. After a passage of 100 cm. the filaments are extracted from the bath, are freed from sulphur solution between two compression rollers and are stretched in air by 230 C. The gamma index of the filaments is 53 when they leave the first bath and 31 at the end of the primary stretch.
  • the filaments thereafter pass through a second bath of the same composition and at the same temperature as the first, the length of immersion being 230 cm., and then through a third degassing bath at a temperature of C. obtained by dilution of the first bath, so that the sulphuric acid content is between 6 and 8 g. per litre, the sodium sulphate having the same dilution ratio.
  • the length of passage through this bath is 550 cm. and the filaments undergo therein a detensioning of 1.5%.
  • There is received in the pot a tow of 12,000 den. at a speed of 12.8 metres per minute.
  • the finishing operation and notably the sodium hydroxide treatment are carried out as in Example 1. Filaments are obtained which have the following characteristics:
  • Example 3 A pulp of linters is immersed for 35 minutes in sodium hydroxide in a concentration of 240 g. per litre at a temperature of 20 C., and the alkali cellulose obtained is pressed to a proportion of 3.1 in relation to the alpha-cellulose. The alkali cellulose is thereafter ground and then treated without any ripening with 44% of carbon disulphide (calculated on the alpha-cellulose). The xanthate formed is dissolved in cold sodium hydroxide, while there are incorporated at the same time 0.6% of Ceponol and small quantities of surface-active products. Finally, there is added a further quantity of 5% of carbon disulphide. The viscose obtained contains 6% of cellulose and 4% of sodium hydroxide. Its DP is 600, its viscosity 650 poises and its gamma index 67.
  • Spinning is effected as in Example 1 with the aid of an 8000-hole spinneret and with a tube 5 cm. in diameter and 20 cm. long into a bath containing 16 g. of sulphuric acid, 52 g. of sodium sulphate and 0.3 g. of zinc sulphate per litre, at a temperature of 3 C.
  • the filaments formed travel a distance of 90 cm. through the bath, whereafter they are extracted therefrom, freed from the excess solution by which they are impregnated by passing them between two compression rollers, and are stretched by 215% during their travel through the air between the first and second baths.
  • the gamma index is 53 at discharge from the first bath and still amounts to 31 at the end of the stretching.
  • the filaments thereafter pass through a second bath having the same composition and at the same temperature as the first, the length of travel being 230 cm., and then through a third degassing bath at a temperature of 95 C., obtained by dilution of the first bath, so that its sulphuric acid content is between 6 and 8 g. per litre, the sodium sulphate and the zinc sulphate being in the same dilution ratio.
  • the length of travel through the third bath is 550 cm. and the filaments undergo therein a detensioning of 1.5%.
  • the tow of 12,000 den. is received in the pot at a speed of 12.5 metres per minute.
  • the finishing operations and notably the treatment with sodium hydroxide are carried out as in Example 1. Filaments are obtained which have the following characteristics:
  • the filaments derived from the first bath may be passed through a cold intermediate bath containing an aldehyde and then stretched in a second bath, preferably cold, which also contains an aldehyde.
  • a cold intermediate bath containing an aldehyde
  • a second bath preferably cold, which also contains an aldehyde.
  • the presence of the aldehyde results in the formation of a more stable complex of xanthate and the lowering of the gamma index of the filaments in the gel form is very rapidly blocked at a relatively short distance after it leaves the first bath.
  • the filaments have an even higher gamma index during the stretching operation in addition this index falls much more slowly.
  • filaments stretched in air may undergo a further stretch in a cold secondary bath, in contrast to the usual practice, which consists in using a hot second bath. Under these conditions, it is possible to reach substantially greater stretches, and consequently exceptional tenacities.
  • a viscose containing at least 3% of cellulose and 1.5-9% of sodium hydroxide the percentage of carbon disulphide added being 35% at least calculated on the alpha-cellulose employed.
  • the gamma index of the viscose at the time of spinning being between 45 and 100 and the cellulose contained in the viscose having a DP of at least 400, preferably higher than 500, the viscosity of the viscose being between 150 and 1000 poises,
  • This viscose is spun into a first bath which contains at least 40 g. of acid, preferably from 5 g. to 25 g. of acid per liter, from 10 g. to g., preferably less than 40 g., per litre of sodium sulphate, and less than 1 g. per litre zinc sulphate.
  • the bath may contain in addition small quantities of a modifying agent such as an ethylene polyhydroxide, or an amine.
  • the temperature of the first bath is extremely low and is between 0 and 10 C., preferably between 2 and 8 C.
  • the filaments are freed from surplus solution by squeezing between rollers and they thereafter pass around a roller which is partially immersed in a cold intermediate bath containing formaldehyde, which bath may have, apart from the aldehyde, the same composition and the same temperature as the first bath.
  • the filaments are thereafter stretched -by at least while travelling through air, and again by at least 20% in a second cold dilute acid bath containing an aldehyde, which second bath may have the same composition and. the same temperature as the intermediate bath.
  • the filaments are subjected to a regenerating treatment in a third bath, under slight detensioning, and they are received in pots. After a period of relaxation of a number of hours the filaments in the acid state are cut to produce discontinuous fibres, and these fibres are washed and given a primary swelling treatment with 5% sodium hydroxide in order to improve their transverse characteristics and their affinity.
  • the filaments produced by the described process possess the so-called Polynosic structure and their charac teristics are stable and only slightly modified by a subsequent treatment with 5% sodium hydroxide, while under the same conditions ordinary rayon filaments and rayon filaments for pneumatic tires are thoroughly disorganized.
  • These filaments have a high tenacity which exceeds 4 g./den. in the wet state and 4.5 g./den. in the conditioned state and they possess a high modulus of elasticity in the wet state, which results in an elongation of less than 3% under a load of 0.5 g./den. They have a circular crosssection and their swelling is currently below 65%.
  • Example 4 In a first embodiment a cellulose pulp having a high alpha-cellulose content is immersed for 30 minutes in sodium hydroxide in a concentration of 242 g./litre, at a temperature of 22 C., and is thereafter pressed to a proportion of 3.1 calculated on the alphacellulose.
  • the alkali cellulose formed is not subjected to any ripening and 43% of carbon disulphide are directly added thereto (calculated on the alpha-cellulose).
  • the xanthate formed is thereafter dissolved in dilute sodium hydroxide at low temperature, while there is added to the mass an additional quantity of 5% of carbon disulphide, simultaneously with 0.25% of Intrasol FSW, and 0.15% of Nonanol (calculated on the alpha-cellulose).
  • the viscose is spun with the aid of a spinneret having 8000 holes of mm., and with a tube 5 cm. in diameter and 20 cm. long into a first bath containing 15 g. of sulphuric acid, 25 g. of sodium sulphate and 0.3 g. of zinc sulphate per litre, as also small quantities of Ceponol TS, at a temperature of 8 C.
  • the filaments are extracted from the bath and are freed from surplus solution between two pressure rolls, and they pass around a roller which is partially immersed in an intermediate bath at 80 C., having the same composition as the first bath, but containing in 7 addition 10 g. of formaldehyde per litre.
  • the filaments are thereafter stretched by 150% while travelling in the air, and again by 30% in a second bath, which has the same conditions and the same temperature as the inter- 8 viscose having a viscosity of at least 400 poises, a gamma index of at least 45 and containing a cellulose having a DP of at least 500 into a spinning bath containing less than 40 g./l. of sulphuric acid, from 10 to 100 g./l. of
  • the filaments then pass, with a length of immerf i f and less than 1 of Zmc Sulphate sion of 490 cm. through a third bath at obtained wh1le maintaining the bath at a temperature below C., by dilution of the first bath, so that it contains 6-8 g. Yvlthdrawing the filaments from the Spinning bath, m per litre of sulphuric acid, the sodium and zinc sulphates g the cess S lution from said filaments by pressure, having the same ratio of dilution, while these filaments then passing the filaments into a second cold bath havin 10 g are sub ected at the same time to a relaxation of 0.8%.
  • this table illustrates the fact that properties oi the 3,083,075 3/ 1963 Saxton et al. 264 197 filaments obtained in embodiment 1 of Example 5 (cold 3,108,849 0/ 1963 Owashi et al 264 197 stretching bath) are slightly superior to the properties of f the filaments obtained in embodiment 2 of Example 5 W et 264-198 h 0b h t M dt 1 3,153,687 10/1964 Eskridge 264 19 X ot stre tc m at no a y in regar o e onga ion.

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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)
US321063A 1962-11-06 1963-11-04 Process for spinning cellulosic fibers Expired - Lifetime US3352957A (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR914533A FR1468625A (fr) 1962-11-06 1962-11-06 Nouveau procédé de filature de fibres dites polynosiques
FR917772A FR89302E (fr) 1962-11-06 1962-12-06 Nouveau procédé de filature de fibres dites polynosiques
CH1330763A CH406515A (fr) 1962-11-06 1963-10-30 Procédé de filature de fils de cellulose régénérée à haut module au mouillé

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US3352957A true US3352957A (en) 1967-11-14

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US (1) US3352957A (xx)
BE (2) BE638523A (xx)
CH (2) CH406515A (xx)
DE (2) DE1291050B (xx)
FR (1) FR89302E (xx)
GB (1) GB1020169A (xx)
NL (1) NL299635A (xx)
SE (1) SE315682B (xx)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3420814A (en) * 1964-07-31 1969-01-07 American Enka Corp Process for producing artificial staple fibers
US3458901A (en) * 1965-08-19 1969-08-05 Phrix Werke Ag Device for spinning viscose
US3539679A (en) * 1965-08-03 1970-11-10 Mitsubishi Rayon Co Process for producing polynosic fibers
US4383962A (en) * 1979-09-27 1983-05-17 Asahi Kasei Kogyo Kabushiki Kaisha Process for producing viscose rayon filament yarn
US20080275231A1 (en) * 2005-05-30 2008-11-06 Jiangsu Long-Ma Green Fibers Co., Ltd. Method for Preparing Regenerated Cellulose Fiber by Two-Step Coagulating Bath Process

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
IT1129651B (it) * 1980-01-09 1986-06-11 Snia Viscosa Procedimento perfezionato per la filatura in continuo di rayon viscosa
US9422641B2 (en) 2012-10-31 2016-08-23 Kimberly-Clark Worldwide, Inc. Filaments comprising microfibrillar cellulose, fibrous nonwoven webs and process for making the same

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2607955A (en) * 1949-08-25 1952-08-26 Textile & Chem Res Co Ltd Spinning of viscose
US2703270A (en) * 1951-07-31 1955-03-01 Schweizerische Viscose Production by spinning of cellulose hydrate filaments
GB915803A (en) * 1958-08-12 1963-01-16 Courtaulds Ltd Improvements relating to the production of regenerated cellulose filaments
US3083075A (en) * 1962-07-09 1963-03-26 William R Saxton Process of manufacturing regenerated cellulose fiber
US3108849A (en) * 1960-10-27 1963-10-29 Mitsubishi Rayon Co Process for producing viscose regenerated cellulose fibers
US3109700A (en) * 1962-05-04 1963-11-05 Courtaulds North America Inc Method for making rayon filaments
US3139467A (en) * 1962-11-14 1964-06-30 Chimiotex Method for spinning viscose
US3153687A (en) * 1962-01-17 1964-10-20 American Enka Corp Production of viscose rayon
US3226461A (en) * 1962-02-27 1965-12-28 Courtaulds North America Inc Manufacture of regenerated cellulose fibers from viscose

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR704279A (fr) * 1929-11-05 1931-05-16 Perfectionnements à la fabrication des filaments, fils, rubans, films, etc. en matières artificielles
NL88549C (xx) * 1948-05-11

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2607955A (en) * 1949-08-25 1952-08-26 Textile & Chem Res Co Ltd Spinning of viscose
US2705184A (en) * 1949-08-25 1955-03-29 Textile & Chemical Res Company Process for the production of rayon products
US2703270A (en) * 1951-07-31 1955-03-01 Schweizerische Viscose Production by spinning of cellulose hydrate filaments
GB915803A (en) * 1958-08-12 1963-01-16 Courtaulds Ltd Improvements relating to the production of regenerated cellulose filaments
US3108849A (en) * 1960-10-27 1963-10-29 Mitsubishi Rayon Co Process for producing viscose regenerated cellulose fibers
US3153687A (en) * 1962-01-17 1964-10-20 American Enka Corp Production of viscose rayon
US3226461A (en) * 1962-02-27 1965-12-28 Courtaulds North America Inc Manufacture of regenerated cellulose fibers from viscose
US3109700A (en) * 1962-05-04 1963-11-05 Courtaulds North America Inc Method for making rayon filaments
US3083075A (en) * 1962-07-09 1963-03-26 William R Saxton Process of manufacturing regenerated cellulose fiber
US3139467A (en) * 1962-11-14 1964-06-30 Chimiotex Method for spinning viscose

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3420814A (en) * 1964-07-31 1969-01-07 American Enka Corp Process for producing artificial staple fibers
US3539679A (en) * 1965-08-03 1970-11-10 Mitsubishi Rayon Co Process for producing polynosic fibers
US3458901A (en) * 1965-08-19 1969-08-05 Phrix Werke Ag Device for spinning viscose
US4383962A (en) * 1979-09-27 1983-05-17 Asahi Kasei Kogyo Kabushiki Kaisha Process for producing viscose rayon filament yarn
US20080275231A1 (en) * 2005-05-30 2008-11-06 Jiangsu Long-Ma Green Fibers Co., Ltd. Method for Preparing Regenerated Cellulose Fiber by Two-Step Coagulating Bath Process

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Publication number Publication date
GB1020169A (en) 1966-02-16
DE1469064A1 (de) 1968-11-07
BE638775A (xx)
NL299635A (xx)
DE1291050B (de) 1969-03-20
CH406515A (fr) 1966-01-31
FR89302E (fr) 1967-06-09
SE315682B (xx) 1969-10-06
BE638523A (xx)
CH423085A (fr) 1966-10-31

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