US2947597A - Manufacture of viscose rayon - Google Patents

Manufacture of viscose rayon Download PDF

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Publication number
US2947597A
US2947597A US640617A US64061757A US2947597A US 2947597 A US2947597 A US 2947597A US 640617 A US640617 A US 640617A US 64061757 A US64061757 A US 64061757A US 2947597 A US2947597 A US 2947597A
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US
United States
Prior art keywords
viscose
yarn
spinbath
skin
sulphuric acid
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
Application number
US640617A
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English (en)
Inventor
Brotz August
Richter Kurt
Wachtendorf Wilhelm
Heuer Kurt
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Akzona Inc
Original Assignee
American Enka Corp
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Filing date
Publication date
Application filed by American Enka Corp filed Critical American Enka Corp
Application granted granted Critical
Publication of US2947597A publication Critical patent/US2947597A/en
Anticipated expiration legal-status Critical
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Classifications

    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
    • D01F2/08—Composition of the spinning solution or the bath

Definitions

  • this invention relates to the production of said articles having substantially all skin area, high strength and high fatigue rei sistance.
  • a need for a very high tenacity viscose rayon yarn [exists inthe industry today in order to compete with "other synthetic fibers.
  • textile rayons which have a very thin skin.
  • the strength of the yarn increases as the percentage of skin. area increases and the percentage of core decreases.
  • yarns havri-ing a large degree of skin have a lower swelling value as 2 compared to yarn of little or no skin.
  • the skin and core as referred to herein are not different types of material but occur from the same stream of viscose. However, it has been established that the orientation and crystallinity of the cellulose molecule The formation of a yarn having a considerable de- I gree of skin area may be influenced in ditferent ways.
  • viscose rayon yarns which have a -relatively thick skin may be produced by regenerating the cellulose in the presence of a viscose additive which modifies the regeneration-coagulation process of the visc'ose 'in the acid spinbath.
  • Rayons of the high tenacity type have a com-.
  • the spinbath in the viscose process is constantly being spent in operation and must be regenerated by adding fresh sulphuric acid and removing the excess sodium sulphate. Regeneration of spinbath containing these additives present many operational problems. Thus, it would be desirable to operate without the additives Also, by varying the spinningconstants a yarn of varying degrees of skin thickness may be produced. By varying the acid concentration the skin thickness can be increased by either increasing or decreasing the acid concentration depending upon other spinning constants.
  • the viscose may be varied to influence skin formation such as increasing or decreasing the sodium hydroxide content, decreasing the aging of the viscose, increasing the amount of CS used during xanthation and increasing the cellulose content thereof.
  • a very high strength yarn may be produced by the so-called Lilienfeld process in which viscose is extruded into a coagulating bath containing sulphuric acid generally in the amount of -70% by weight.
  • the spinning or coagulation bath treatment may be followed by a secondary bath also having a relatively high sulphuric acid content.
  • other physical properties are not improved and, in most instances, are poorer. Theyarn produced by the Lilienfeld process is very brittle and is almost worthless for use in articles which require good extensibility and good fatigue resistance.
  • viscose having sodium hydroxide in the amount of 6% or less by weight and a maturity of about 4046 gamma number is spun into a coagulating spinbath containing about 17-19% sodium sulphate, 45-60% sulphuric acid, and zinc sul- Q phate, the concentration. of which is dependent upon the concentration. of the sulphuricacid. It is preferred that v the ratio of the acid content to the zinc sulphate content be 1.2408 to 1. After a short travel through the spinbath, the freshly spun. yarn is directed into a second hot 7 weakly acid bath where the yarn is stretched in the .con-
  • the freshly spun yarn was directed throu'ghthe' spinbath for a distance of 17 cm. and out of this first'bath into a: second bath.
  • this second bath which contained 2% H SO and had a temperature of 90 C.
  • the yarn was given a stretch of 90%.
  • the drawo'lf speedof the yarn was 60 meters per minute.
  • the yarn was aftertreated in the usual manner, such as Washing, desulphurizing, drying, etc. However, before finally drying the yarn was given an additional stretch of 3-l0%'
  • the dried thread was given a twist of I20 turnsper meter.
  • the physical properties of 1650 denier yarn produced in the above manner were as follows. In. the dry state Itis. important to the present invention that the percentage of sodium hydroxide in the viscose benot. more than 6%. There appears to be no defined lower value for the percent caustic. Generally, it is preferred that thealkali content be no lower than 4.5. However, a. viscose with even a lower alkali may be used. In any case/the sodium hydnoxid'e should be sufficiently high to render the viscose amenable tozthe conventional filtering and-spinningprocesses. The maturity of the viscose is not critical in: the
  • the viscose be aged to aa ripeness of about 4046 gamma number.
  • AnLsonit' is. importantthat the concentration of materials in the spinbath. be maintained between certain defined ranges- It is necessary that the sulphuricv acid be kept at 4.5.-.6.0.%. Above 6.0% thev skin. thickness of the-yarn notably decreases, below 4.0% many spinningproblems? arise.
  • The. concentration of salts in the spinbath should be. maintained at. certain levels in order to retaintheir skin formation effect. For example, the optimum concentration of sodium sulphate in the present invention is l 7-l'9%:. depending upon the amount of acid in the spinbath. 'It has been established that the optimum concentration of the zinc salt is reached when the ratio of acid to zinc salts is 1.2-0.8 to 1.
  • Example I Alkali cellulose prepared from cotton linters and aged The concentration of zinc sulphate is varied) the strength or the yarn was 435 g./100 denier and the elongation was 7.8%. In the conditioned state" the strength of the yarn was 291 g;/ 100 denier and the" elongation; was 24.4%. The swelling value of the yarii 70.9%.
  • viscose prepared in. identical manner asiin Example'l-wasextruded into a spinbath' containing 6.5%
  • A'process for the production of regeneratedcellulose articles having substantially all skin fromviscose comprising spinning a solution consisting essentially" of viscose containing sodium hydroxide in the amount of less 6% by weight into acoagulating spinbath consisting essentially of 1 7-19 sodium sulphate, 45-60% sulphuric acid, andzinc sulphate, directing the spunarticle out of said spinbathinto a second bath containing dilute sulphuric-acid, and stretching the spun article; in the second bath to an extent of at least the concentration of zinc sulphate being adjusted so that the ratio of sulphuric acid insaid spinbath to zinc sulphate is 142-08 2.
  • a process for the production of regenerated cellulose articles having substantially all skin froni vi'scose comprising; spinning a solution consisting es's'enti'ally Qof "viscose containing 4.5'-6.0% by weight of sodium hydioxide into a coagulatingspinbath. consisting essentially co'nsistingf essentially of viscosecontaining-4.59550 by :3 weight of sodium hydroxide into a coagulating spinbath consisting essentially of 17-19% sodium sulphate, 4.5- 6.0% sulphuric acid, and zinc sulphate, directing the spun yarn out of said spinbath into a second bath containing about 2% sulphuric acid and having a temperature of about 90 C. and stretching the yarn in the second bath at least 85%, the concentration of zinc sulphate being adjusted so that the ratio of sulphuric acid in said spinbath to zinc sulphate is 12 0.8 to 1.

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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)
US640617A 1956-02-20 1957-02-18 Manufacture of viscose rayon Expired - Lifetime US2947597A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE2947597X 1956-02-20

Publications (1)

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US2947597A true US2947597A (en) 1960-08-02

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US640617A Expired - Lifetime US2947597A (en) 1956-02-20 1957-02-18 Manufacture of viscose rayon

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BE (1) BE553819A (enrdf_load_stackoverflow)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3720743A (en) * 1970-10-20 1973-03-13 Itt Process for producing high performance crimped rayon staple fiber

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2535045A (en) * 1947-04-26 1950-12-26 Du Pont Spinning of viscose
US2535044A (en) * 1947-04-26 1950-12-26 Du Pont Spinning of viscose

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2535045A (en) * 1947-04-26 1950-12-26 Du Pont Spinning of viscose
US2535044A (en) * 1947-04-26 1950-12-26 Du Pont Spinning of viscose

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3720743A (en) * 1970-10-20 1973-03-13 Itt Process for producing high performance crimped rayon staple fiber

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Publication number Publication date
BE553819A (enrdf_load_stackoverflow) 1900-01-01

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