US2784107A - Production of artificial filaments, threads and the like - Google Patents

Production of artificial filaments, threads and the like Download PDF

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Publication number
US2784107A
US2784107A US319956A US31995652A US2784107A US 2784107 A US2784107 A US 2784107A US 319956 A US319956 A US 319956A US 31995652 A US31995652 A US 31995652A US 2784107 A US2784107 A US 2784107A
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United States
Prior art keywords
viscose
filaments
percent
skin
grams
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Expired - Lifetime
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US319956A
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English (en)
Inventor
Tallis Ernest Edward
Edwards John Harold
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Akzo Nobel UK PLC
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Courtaulds PLC
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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
    • 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

Definitions

  • This invention relates to the production of artificial filaments, threads, fibres and the like hereinafter referred to as filaments, from viscose.
  • viscose filaments produced by the normal spinning processes have a crenulated surface and a structure which consists of a skin and a core.
  • the presence of the skin and core can be demonstrated by staining a cross-section cut from the filaments under specific conditions; such methods are described in the Textile Research Journal 1945, page 443.
  • Another method of differentiating between the skin and core is by measuring the rate of axial diffusion of dyestuffs as described in Textile Research Journal 1948, page 9.
  • the cellulose molecules of the skin are believed to be more highly orientated than those of the core and for this reason it is thought that the strength of viscose fibres resides mainly in the skin.
  • the object of the present invention is to provide a further process for obtaining modified viscose filaments.
  • a process for the production of artificial filaments, threads, fibres and the like comprises extruding viscose into a coagulating bath containing sulphuric acid and zinc sulphate wherein the spinning is carried out in the presence of more than A of a millimole and less than millimoles per 100 grams of viscose of a polyalkylene polyamine having at least 3 amino groups which are not directly united to each other and which are primary or secondary amino groups.
  • Figures 1 to 6 are tracings of photornicrographs of yarn treated in difierent ways.
  • Figure 1 shows a cross-section of unmodified yarn.
  • Figure 2 shows yarn into which a polyalkylene polyamine has been introduced in accordance with the invention.
  • Figures 3 to 6 show yarns into which ditferent amounts of a polyalkylene polyamine have been introduced, and demonstrate the effect of varying the quantity of the polyalkylene polyamine.
  • the polyalkylene polyamine is added to the viscose but if desired the polyalkylene polyamine can be added to the coagulating bath or to both the viscose and the coagulating bath.
  • the preferred minimum concentration for addition to the viscose 1s 1 millimole per 100 grams of viscose.
  • the filaments obtained have a much thicker skin, and the boundary between the skin and core is more difiuse than those of filaments obtained under similar conditions but without the addition of the polyalkylene polyamines.
  • concentration of the polyalkylene polyamine the core can be practically elminated.
  • the cross-sectional shape of the filaments is affected by the use of these polyalkylene pplyamines, for example filaments having a bean shape or dog-bone shape can be obtained.
  • the crenulations normally found in viscose rayon filament cross-sections are absent and the filaments obtained have a smooth surface.
  • axial diffusion tests are carried out on filaments of the present invention little or no penetration of the dyestufi occurs. It may be necessary, for any particular polyalkylene pol amine to carry out tests to determine the exact concentration required to give the effects desired.
  • the viscose preferably has a salt figure of at least 4.
  • the coagulating bath may be of any desirable concentration, it may contain sulphuric acid, sodium sulphate and zinc sulphate, and the zinc sulphate concentration is preferably between 0.5 percent and 15 percent.
  • concentration of zinc sulphate used will depend on the type of yarn being spun.
  • Other substances may be added to the spinning bath, such as ammonium sulphate, magnesium sulphate and glucose.
  • the filaments of the present invention have a lower water imbibition which is of considerable advantage for textile applications.
  • the filaments of the present invention are more resistant to soiling and have an improved resistance to laundering and mechanical damage when wet.
  • the distance from the jet at which the filaments become neutral is measured. The actual distance depends primarily upon the alkalinity of the viscose, the spinning speed, the spinning bath acidity, the spinning bath temper ature and the filament denier.
  • the cords made from the filaments are of improved quality and have a greater fatigue life than similar cords produced without the process of the present invention.
  • Example 1 A viscose was prepared to contain 7.5 percent of cellulose and 6.5 percent of caustic soda, using 37 percent of carbon disulphide on the weight of a-ccllulose. The viscose was cooled to Centigrade and 1 millimole of diethylene triamine per 100 grams of viscose were mixed in and the viscose filtered and tie-aerated. When the salt figure had fallen to 6.0 the viscose was spun through a jet having 750 holes each 0.003 in diameter into a coagulating bath containing 9.5 percent of sulphuric acid, 4.0 percent of zinc sulphate and 20 percent of sodium sulphate at 48 centigrade.
  • the length of immersion in the coagulating bath was 18 inches and it was withdrawn from the bath on to a godet at a rate of 48 metres per minute.
  • the filaments were then stretched 65 percent between the first and second godets while they were passed through a hot stretch bath at 95 centigrade and 70 inches long.
  • the hot stretch liquor was made by diluting spinning bath to three times its volume.
  • the yarn, of 1650 denier 750 filaments, was subsequently washed, desulphurized, a finish was applied and the yarn was dried and collected on bobbins by means of a cap twister.
  • the yarn obtained had a water imbibition of 90 percent compared with 121.3 percent for an unmodified yarn spun at the same time and under the same conditions.
  • the bone dry yarn strength of the yarn was 4.70 grams per denier compared with 4.20 grams per denier for the unmodified yarn.
  • the conditioned yarn had a strength of 3.29 grams per denier compared with 2.94 grams per denier for the conditioned unmodified yarn.
  • Figure 2 shows clearly the dog-bone or bean-shaped form of the modified yarn, its non-crenulated surface, I
  • Example 2 A viscose was prepared by the method described in Example 1 but was modified by the addition of 1 millimole of triethylene tetramine per 100 grams of viscose. The viscose was spun under similar conditions to those described for Example 1 except that the salt figure was 12.5, the spinning speed was 30 yards per minute and the hot stretch bath contained boiling water and was two feet long. The cross-section of the yarn produced was similar to that shown by Example 1.
  • Example 3 Viscose containing 7.8 percent of cellulose, 6.5 percent of caustic soda and 2.15 percent of combined sulphur was prepared in the usual manner. When the viscose was 33 hours old from the beginning of the mixingstage and the salt figure was 6.5, 0.5 percent of carbon.v disulphide on the weight of the viscose was added and was mixed in for half an hour at centigrade. 4 millimoles per 100 grams of viscose of diet hylene triamine was added and the viscose was mixed for a further half an hour. When the viscose was hours old and had a salt figure of 7.6 it was ready for spinning.
  • the viscose was extruded through a jet having 40 holes, 0.003 inch in diameter into a coagulating bath containing 9.0 percent of sulphuric acid, 20.0 percent of sodium sulphate and 4.0 percent of zinc sulphate to give a thread of 150 denier and 40 filaments.
  • the length of immersion in the bath was 21 inches and the temperature of the bath was 48 Centigrade.
  • the thread was drawn from the bath at a rate of 48.6 metres per minute by a godet and then travelled to a second godet rotating at a higher speed than the first godet, to impart a 20 percent stretch to the thread.
  • the thread was collected in a centrifugal spinning box rotating at 7,000 R. P. M.
  • the cake obtained was washed free from acid and dried.
  • the distance from the jet at which the freshly coagulated thread became neutral was 8 inches whereas an unmodified viscose extruded under similar conditions became neutral 2% inches from the jet.
  • the percentage of cellulose in the cake was 40 percent compared with 28.5 percent for an unmodified viscose.
  • the water imbibition of the finished thread was percent compared with 101 percent for a similar thread from an unmodified viscose. Determination of the axial diffusion of the thread was carried out as described by Hermanns in the Textile Research Journal 1948, page 9, using Solophenyl East Blue-green BL; no penetration of dyestuff was obtained, but for thread from an unmodified viscose it was 50 11.
  • Example 4 Viscose containing 7.8 percent cellulose, 6.5 percent caustic soda and 2. .5 percent combined sulphur was prepared in the usual manner and filtered. When the viscose was 16 hours old 0.5 percent of carbon disulphide was added to it and mixed in for 15 minutes. The temperature of the viscose was reduced by cooling to 1 centigrade and divided into four parts to which were added 1.0, 2.0, 3.0 and 6.0 millimoles per grams viscose triethylone tetrainine.
  • the viscoses were mi .ed for 15 minutes, evacuated for eight hours and spun through a jet having 500 holes, .003 inch in diameter in bath containing 9.5 percent of sulphuric acid, 20.0 percent of sodium sulphate and 4.0 percent of zinc sulphate at 48 centigrade.
  • the filaments were drawn oil? by a godet at 18 yards per n1inrte and stretched through a boiling water bath, by means of a second godet having a peripheral speed oi: yards per minute.
  • the thread was collected in a Tcpham box revolving at 4,000 R. P. M.
  • the yarn was subsequently washed and dried.
  • the salt figures of the viscose at the time of spinning were 12.5, 11.4, ll.6 and 10.2 respectively.
  • the stained cross-sections of the yarns are shown in Figures 3, 4, 5 and 6. in which Figure 3 is from viscose having 1.0 millimolc of triethylene tetraminc per 100 grams of viscose, Figure 4 is from viscose having 2.0 millimoles of triethylene tetramine per 100 grams of viscose, Figure 5 is from viscose having 3 millimoles of triethylene tctramin-e per 100 grams of viscose and Figure 6 is from viscose having 6.0 millimoies of triethylene tetramine per 100 grams ct viscose.
  • a process for the production of viscose rayon filaments, threads, fibers and the like having a thick skin comprising extruding viscose, in the presence of more than one quarter of a millimole and less than millimoles per 100 grams of viscose of a polyethylene polyamine component selected from the group consisting of polyethylene polyamines having the general formula where n is from 1 to 4 inclusive, and condensation products of said polyamines with aliphatic alkylating agents selected from the group consisting of diehlorohydrin, dichlorethylene and trimethylene bromide, into a coagulating bath containing sulphuric acid and 0.545% of zinc sulphate.
  • a process for the production of viscose rayon filaments, threads, fibers and the like having a thick skin comprising extruding viscose in the presence of more than one quarter of a millimole and less than 5 millimoles per 100 grams of viscose of a polyethylene polyamine component selected from the group consisting of polyethylene polyamines' having the general formula NH2CH2CH2(NHCH2CH2)11NH2 where n is from 1 to 4 inclusive and condensation products of said polyamines with aliphatic alkylating agents selected from the group consisting of dichlorohydrin, dichlorethylene and trimethylene bromide, into a coagulatwhere n is from 1 to 4 inclusive, and condensation products of said polyamines with aliphatic alkylating agents selected from the group consisting of dichlorohydrin, dichlorethylene and trimethylene bromide.

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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)
US319956A 1951-12-13 1952-11-12 Production of artificial filaments, threads and the like Expired - Lifetime US2784107A (en)

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GB312134X 1951-12-13

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US2784107A true US2784107A (en) 1957-03-05

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Country Status (7)

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US (1) US2784107A (fr)
BE (1) BE516207A (fr)
CH (1) CH312134A (fr)
DE (1) DE1034811B (fr)
FR (1) FR1077538A (fr)
GB (1) GB723435A (fr)
NL (1) NL93553C (fr)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2910341A (en) * 1953-11-09 1959-10-27 Du Pont Spinning viscose
US2919203A (en) * 1955-12-05 1959-12-29 American Viscose Corp Producing all skin rayon
US2950208A (en) * 1954-11-25 1960-08-23 American Enka Corp Production of shaped objects from viscose
US2953426A (en) * 1954-11-25 1960-09-20 American Enka Corp Production of shaped objects from viscose
US2953425A (en) * 1954-11-25 1960-09-20 American Enka Corp Production of shaped objects from viscose
US2953468A (en) * 1955-10-25 1960-09-20 American Enka Corp Production of shaped objects from viscose
US2958569A (en) * 1954-10-20 1960-11-01 American Enka Corp Production of threads and other shaped objects from viscose
US2974005A (en) * 1956-09-14 1961-03-07 American Enka Corp Manufacture of rayon
US3034910A (en) * 1959-07-31 1962-05-15 Buckeye Cellulose Corp Production of regenerated cellulose filaments from wood pulp

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BE553231A (fr) * 1955-12-14
BE559502A (fr) * 1956-08-29
DE1093044B (de) * 1956-10-26 1960-11-17 Du Pont Verfahren zur Herstellung von Gebilden aus regenerierter Cellulose

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1929868A (en) * 1930-02-11 1933-10-10 Soc Of Chemical Ind Cellulose derivative having alpha strong affinity for acid dyestuffs, and alpha process of making same
US2300589A (en) * 1938-08-23 1942-11-03 Gen Aniline & Film Corp Animalizing cellulosic fibers
US2312199A (en) * 1939-11-22 1943-02-23 Courtaulds Ltd Treatment of cellulosic textile materials
US2329086A (en) * 1939-05-20 1943-09-07 Nat Oil Prod Co Sulphonated amides and process of producing same
US2345570A (en) * 1938-10-07 1944-04-04 North American Rayon Corp Coagulating bath containing cationactive inhibitors
US2397454A (en) * 1941-09-17 1946-03-26 Du Pont Polymeric cellulose structure and process for making same
US2422021A (en) * 1940-07-29 1947-06-10 Ind Rayon Corp Manufacture of thread or the like
US2535044A (en) * 1947-04-26 1950-12-26 Du Pont Spinning of viscose

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB533309A (en) * 1939-08-10 1941-02-11 Courtaulds Ltd Improvements in or relating to the production of artificial threads from viscose

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1929868A (en) * 1930-02-11 1933-10-10 Soc Of Chemical Ind Cellulose derivative having alpha strong affinity for acid dyestuffs, and alpha process of making same
US2300589A (en) * 1938-08-23 1942-11-03 Gen Aniline & Film Corp Animalizing cellulosic fibers
US2345570A (en) * 1938-10-07 1944-04-04 North American Rayon Corp Coagulating bath containing cationactive inhibitors
US2329086A (en) * 1939-05-20 1943-09-07 Nat Oil Prod Co Sulphonated amides and process of producing same
US2312199A (en) * 1939-11-22 1943-02-23 Courtaulds Ltd Treatment of cellulosic textile materials
US2422021A (en) * 1940-07-29 1947-06-10 Ind Rayon Corp Manufacture of thread or the like
US2397454A (en) * 1941-09-17 1946-03-26 Du Pont Polymeric cellulose structure and process for making same
US2535044A (en) * 1947-04-26 1950-12-26 Du Pont Spinning of viscose

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2910341A (en) * 1953-11-09 1959-10-27 Du Pont Spinning viscose
US2958569A (en) * 1954-10-20 1960-11-01 American Enka Corp Production of threads and other shaped objects from viscose
US2950208A (en) * 1954-11-25 1960-08-23 American Enka Corp Production of shaped objects from viscose
US2953426A (en) * 1954-11-25 1960-09-20 American Enka Corp Production of shaped objects from viscose
US2953425A (en) * 1954-11-25 1960-09-20 American Enka Corp Production of shaped objects from viscose
US2953468A (en) * 1955-10-25 1960-09-20 American Enka Corp Production of shaped objects from viscose
US2919203A (en) * 1955-12-05 1959-12-29 American Viscose Corp Producing all skin rayon
US2974005A (en) * 1956-09-14 1961-03-07 American Enka Corp Manufacture of rayon
US3034910A (en) * 1959-07-31 1962-05-15 Buckeye Cellulose Corp Production of regenerated cellulose filaments from wood pulp

Also Published As

Publication number Publication date
FR1077538A (fr) 1954-11-09
GB723435A (en) 1955-02-09
NL93553C (fr)
BE516207A (fr)
DE1034811B (de) 1958-07-24
CH312134A (de) 1955-12-31

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