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
• • 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
  • D01D5/00—Formation of filaments, threads, or the like
  • D01D5/22—Formation of filaments, threads, or the like with a crimped or curled structure; with a special structure to simulate wool

Definitions

• This invention in general relates to the production of synthetic fibers from viscose and more particularly to the production of crimped fibers having high crimping values.
• Regenerated cellulose filaments may be manufactured by spinning viscose solutions in an acid bath.
• viscose solutions are solutions of alkali cellulose xanthate in dilute caustic soda.
• Alkali cellulose xanthate is prepared by first forming alkali cellulose by immersing cellulose in strong caustic soda solution. The alkali cellulose is then contacted with carbon disulfide to form the alkali cellulose xanthate which may be put in solution form by dissolving the composition in dilute alkali.
• the cellulose is regenerated when the carbon disulfide splits oif of the cellulose glucose side chain and the sodium cellulose is reduced to cellulose in an acid medium.
• the viscose solution is allowed to ripen to a point just before the alkali cellulose begins to precipitate or come out of solution.
• some of the cellulose xanthate decomposes into alkali cellulose and carbon disulfide.
• the alkali cellulose is held in the viscose solution as an emulsion by the remaining alkali cellulose xanthate.
• the remaining cellulose xanthate is decomposed in the first acid spinning bath.
• the ripening, or decomposition, of the alkali cellulose xanthate does not proceed as far as in the usual viscose process.
• complete regeneration of cellulose from the incompletely ripened viscose occurs, not in the dilute acid solution used in spinning and stretching, but after the fibers in a lax state are contacted with additional dilute acid after the spinning and stretching operations.
• Another object of this invention is to provide a process for the manufacture of regenerated cellulose fibers with high crimping properties and high stretching and abrasion resistance values.
• EXAMPLE I In the spinning of a 2.2 denier, highly crimped filament with a staple length of 40 millimeters, a viscose of the composition: cellulose, 8.6%; NaOH, 6.5%; and CS 37%, is spun at a ripeness of 19 H. in a spinning bath of the following compositions: 92-97 grams per liter sulfuric acid, 345-355 grams per liter sodium sulfate, and 10-l2 grams per liter of zinc sulfate.
• the spinning bath has a specific gravity at 43 C. of 1.305 to 1.31.
• the temperature of the bath is 70 C.
• the work is accomplished at a drawing off rate of 60 meters per minute, and after the removal from the first bath, stretching by 35% is done in a second bath which contains approximately 15-20 grams per liter sulfuric acid at a temperature of 95 C.
• the filaments are cut into the desired staple length they are immersed in another dilute acid bath at approximately 80 C. Here decomposition of the remaining cellulose xanthate is completed and the crimping of the filament occurs.
• EXAMPLE II result is transposed to a 100 millimeter length basis by
• a viscose of the composition cellulose, 8.6%; NaOH, 6.5%; and CS 35.0% or 37.0%, is spun at a ripeness of 19 H. in a spinning bath of the following composition: 105-110 grams per liter sulfuric acid, 345- 355 grams per liter sodium sulfate, and -12 grams per liter zinc sulfate.
• the bath has a specific gravity at 43 C. of 1310-1320.
• the temperature of the bath is 70 C.
• the spun filaments are drawn off at a rate of 55 meters per minute and after removal from the spinning bath are stretched by 35-40% in a second bath which contains 20-30 grams per liter of sulfuric acid.
• the uncrimping resistance is the force in milligrams at which no further change occurs in the length of the fiber with additional loading.
• the amount of crimping reported on a percentage basis, is determined by multiplying 100 times the quotient of the stretched length of the crimped fiber minus the the length of the crimped fiber in the unstretched state, the difference being divided by the length of the stretched fiber.
• the crimping constancy or stability is a measure of the recovery capacity in percent of the fiber crimping after a loading for 5 minutes with a weight equal to the uncrimping resistance plus an additional 50 milligrams.
• the abrasion values are determined on an apparatus consisting of an unglazed ceramic cylinder of 10 mm. diameter rotating at 80 r.p.m.
• the rotating cylinder is Arcs on Unmm Grim Grim continuously moistened with distilled water containing an Experiment; Temp, 100 mm ing ing ing 3. anionic sodium alkylnaphthalene sulfonate.
• the fiber is Q Fiber g r Percent ifg ggi in contact with the rotating cylinder over approxlmately one quarter of its circumference and is given a 1.5 fiberkilometer load during the test.
• the abrasion value is 48 66 250 19.1 49.3 55 70 255 20. 5 57.2 the number of revolutions of the cyhnder before the fiber 79 273 22.
• the bending number is the number of bends which the 50 fiber sustains at a 1.5 fiber-kilometer load under a bend- Table IV TEXTILE DATA Strength Stretching Crimp Bend- Experi- Temp, Titre Strength, Abrasion ing ment Dry Value No. Dry Wet Dry Wet
• the ripeness of the viscose solutions is determined by the Hottenroth test. In this test, 20 grams of the viscose to be tested are mixed with 30 ccs.
• the ripeness value H. is the number of ccs. of the ammonium chloride solution used to bring about the coagulation.
• the arcs on millimeters of fiber are determined by counting the number of arcs or bends in a measured length of the crimped fiber and the ing of 180 at a bending velocity of 300 double bends per minute.
• An apparatus which may be used for this test is that of the Knote Company of Leipzig, Germany.
• a process for manufacture from viscose of regenerated cellulose fibers with high crimping properties and high stretching and abrasion resistance values which comprises: spinning unripe viscose having a ripeness value of at least 14 H. in an acid spinning bath maintained at a temperature over 65 C. and being high in sodium sulfate content, the bath containing a small quantity of zinc sulfate and having a specific gravity of at least about 1.3 at 43 C.; stretching the filaments in a dilute acid bath; incompletely regenerating the cellulose in the spinning and stretching steps; and thereafter immersing the filaments in a lax state in dilute acid to complete the regeneration of the cellulose.
• a process for manufacture of regenerated cellulose fibers of high titre with high crimping values the steps which comprise: spinning filaments of at least six denier from unripe viscose having a ripeness value of at least 12 H. in a dilute sulfuric acid spinning bath which contains a small quantity of zinc sulfate and is high in sodium sulfate content, said bath being maintained at a temperature over 65 C.; stretching said filaments; incompletely regenerating the cellulose in the spinning and stretching steps; cutting the filaments into the desired staple length; and immersing the resulting fibers in a lax state in a dilute acid bath to complete the regeneration of the cellulose.
• a process for manufacture of regenerated cellulose fibers of high titre with high crimping values the steps which comprise: spinning filaments of at least six denier from unripe viscose having a ripeness value of at least 12 H. in a dilute sulfuric acid spinning bath Which contains a small quantity of zinc sulfate and is high in sodium sulfate content, said bath being maintained at a temperature over 65 C., the bath having a specific gravity of at least 1.3 at 43 C.; stretching said filaments; incompletely regenerating the cellulose in the spinning and stretching steps; cutting the filaments into the desired staple length; and immersing the resulting fibers in a lax state in a dilute acid bath to complete the regeneration of the cellulose.
• steps which comprise: spinning unripe viscose having a ripeness value of at least 14 H. in a dilute sulfuric acid bath of 92 to 110 grams sulfuric acid per liter of water, said bath being maintained at a temperature over C., and said bath being high in sodium sulfate content, containing a small quantity of zinc sulfate and having a specific gravity of at least about 1.3 at 43 C.
• a process for the manufacture from viscose of regenerated cellulose filaments having a high filament titre and high crimping, stretching and abrasion values the steps which comprise: spinning filaments of at least six denier from unripe viscose having a ripeness value of at least 14 H. in an aqueous bath containing to grams sulfuric acid per liter Water, 345 to 355 grams sodium sulfate per liter water, and 10 to 12 grams zinc sulfate per liter Water, said bath having a specific gravity at 43 C.

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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)

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Cited By (3)

Citations (6)

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• 0
  • NL NL211306D patent/NL211306A/xx unknown
  • BE BE549946D patent/BE549946A/xx unknown
  • NL NL99909D patent/NL99909C/xx active
• 1955
  • 1955-10-12 DE DES45978A patent/DE1031931B/de active Pending
• 1956
  • 1956-08-17 CH CH348235D patent/CH348235A/de unknown
  • 1956-09-12 GB GB27902/56A patent/GB812728A/en not_active Expired
  • 1956-10-04 US US613826A patent/US2966391A/en not_active Expired - Lifetime
  • 1956-10-04 FR FR1158102D patent/FR1158102A/fr not_active Expired

Patent Citations (6)

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