US2813038A - Production of artificial filaments, threads and the like - Google Patents

Production of artificial filaments, threads and the like Download PDF

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US2813038A
US2813038A US347360A US34736053A US2813038A US 2813038 A US2813038 A US 2813038A US 347360 A US347360 A US 347360A US 34736053 A US34736053 A US 34736053A US 2813038 A US2813038 A US 2813038A
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viscose
percent
fluorescein
filaments
grams
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US347360A
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John H Edwards
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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
    • 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 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.
  • This skin and core efiect can be demonstrated by staining the cross-section of the filaments under specific conditions with selected dyestuffs.
  • the cellulose molecules of the skin are believed to be more highly orientated than those of the core. Processes have been described in United States patent specifications Nos.
  • 2,536,014, 2,535,045 and 2,535,044 for obtaining modified viscose filaments having a non-crenulated surface and a more diffuse boundary between the skin and core than unmodified filaments by spinning viscose in the presence of specific water-soluble quaternary ammonium compounds, or specific bath-soluble monoamines or specific aliphatic monoamines.
  • the object of the present invention is to provide a further process for obtaining modified viscose filaments which have substantially no skin and core efiect.
  • 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 per 100 grams of viscose of fluorescein.
  • the fluorescein may be used in the form of its salts, for example the sodium salt of fluorescein.
  • fluorescein is added to the viscose but if desired fluorescein may be added to the coagulating bath or to the viscose and the coagulating bath.
  • the preferred minimum concentration for addition to the viscose is 1.5 millimoles per 100 grams of viscose and the preferred maximum concentration is 12 millimoles per 100 grams of viscose.
  • the filaments obtained exhibit substantially no skin and core effect and in some cases a non-crenulated surface is obtained.
  • the cross-sectional shape and the crenulation of the surface of the filaments is dependent on the quantity of fluorescein present during spinning. Tests may be necessary in order to determine the quantity necessary to give a desired cross-sectional shape and a surface free from crenulations.
  • the coagulating bath preferably contains from l/z to 15 percent of zinc sulphate.
  • the filaments obtained by the process of the invention have a lower water-imbibition than unmodified viscose filaments and they have a reduced gel swelling factor.
  • the distance from the jet at which the thread becomes ncutralised is considerably increased by the presence of fluorescein in the viscose or the coagulating bath or both.
  • the process of the present invention enables unripened or so-called green viscoses to be spun.
  • Example 1 Viscosecontaining 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 mixing stage and the salt figure was 6.4, 0.5 percent of carbon disulphide on the weight of the viscose was added and was 3 millimoles per grams of viscose of fluorescein in the form of its sodium salt were added and the viscose was mixed for a further half an hour. When the viscose was 45 hours old and had a salt figure of 8.9 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 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 gel swelling factor was 2.7 compared with 3.5 for an unmodified viscose.
  • the water imbibition of the finished thread was 87 percent compared with 101 percent for a similar thread from an unmodified viscose.
  • the viscoses were mixed for 15 minutes, evacuated for eight hours and spun through a jet having forty holes .003 inch in diameter in a bath containing 9.0 percent of sulphuric acid, 20.0 percent of sodium sulphate and 4.0 percent of zinc sulphate at 48 Centigrade.
  • the filaments were drawn off by a godet at 18 yards per minute and collected in a Topham box revolving at 4,000 R. P. M. The yarn was subsequently washed and dried.
  • the salt figures at the time of spinning were 9.5, 9.8, 8.9, 9.3 and 9.3 respectively.
  • the cross-sections of the yarns are shown in Figures 1 to 5 in which Figure 1 is yarn from unmodified viscose and Figures 2, 3, 4 and 5 are yarns from the viscose having 1.5, 3.0, 6.0 and 9.0 millimoles of fluorescein respectively per 100 grams of viscose. These figures show how the shape and smoothness of outline are affected by the addition of fluorescein.
  • the yarn from unmodified viscose has a substantially circular cross-section and crenulated surface but the other yarns show elongated cross-sections and smoother outlines with the maximum effect at about 3.0 millimoles of fluorescein per 100 grams of viscose.
  • Viscose containing more than /4 of a millimole and less than 12 millimoles per 100 grams of viscose of a compound selected from the group consisting of fluorescein and an alkali metal salt thereof.
  • Viscose containing more than 1.5 and less than 12 millimoles per 100 grams of viscose of a compound selected from the group consisting of fluorescein and an alkali metal salt thereof.
  • a process for the production of artificial filamentary material comprising extruding viscose into an aqueous coagulating bath containing sulphuric acid and zinc sulphate, wherein the viscose contains more than A of a millimole and less than 12 millimoles per 100 grams of viscose of a compound selected from the group consisting of fluorescein and an alkali metal salt thereof.
  • viscose contains more than 1.5 and less than 12 millimoles per 100 grams of viscose of a compound selected from the group consisting of fluorescein and an alkali metal salt thereof.

Description

Nov. 12. 1957 J. H. EDWARDS PRODUCTION OF ARTIFICIAL FILAMENTS, THI QEADS AND THE LIKE Filed April 7. 1953 United States Patent PRODUCTION OF ARTIFICIAL FILAMENTS, I
j THREADS AND THE LIKE John Edwards, Coventry, England, assignor to Courtaulds Limited, London, England, a British company Application April 7, 1953, Serial No. 347,360
4 Claims. (Cl.106165) This invention relates to the'production of artificial filaments, threads, fibres and the like from viscose.
'It is known that viscose filaments produced by the normal spinning processes have a crenulated surface and a structure which consists of a skin and a core. This skin and core efiect can be demonstrated by staining the cross-section of the filaments under specific conditions with selected dyestuffs. In addition to the difference in dyeing affinity and in swelling property between the skin and core, the cellulose molecules of the skin are believed to be more highly orientated than those of the core. Processes have been described in United States patent specifications Nos. 2,536,014, 2,535,045 and 2,535,044 for obtaining modified viscose filaments having a non-crenulated surface and a more diffuse boundary between the skin and core than unmodified filaments by spinning viscose in the presence of specific water-soluble quaternary ammonium compounds, or specific bath-soluble monoamines or specific aliphatic monoamines.
The object of the present invention is to provide a further process for obtaining modified viscose filaments which have substantially no skin and core efiect.
According to the present invention 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 per 100 grams of viscose of fluorescein. If desired, the fluorescein may be used in the form of its salts, for example the sodium salt of fluorescein.
In the preferred process according to the invention fluorescein is added to the viscose but if desired fluorescein may be added to the coagulating bath or to the viscose and the coagulating bath. The preferred minimum concentration for addition to the viscose is 1.5 millimoles per 100 grams of viscose and the preferred maximum concentration is 12 millimoles per 100 grams of viscose. The filaments obtained exhibit substantially no skin and core effect and in some cases a non-crenulated surface is obtained. The cross-sectional shape and the crenulation of the surface of the filaments is dependent on the quantity of fluorescein present during spinning. Tests may be necessary in order to determine the quantity necessary to give a desired cross-sectional shape and a surface free from crenulations. The coagulating bath preferably contains from l/z to 15 percent of zinc sulphate.
In addition to the non-crenulated surface and the reduced skin and core effect the filaments obtained by the process of the invention have a lower water-imbibition than unmodified viscose filaments and they have a reduced gel swelling factor.
When spinning according to the process of the present invention the distance from the jet at which the thread becomes ncutralised is considerably increased by the presence of fluorescein in the viscose or the coagulating bath or both. The process of the present invention enables unripened or so-called green viscoses to be spun.
/ mixed in for half an hour at centigrade.
This invention is illustrated by the following examples in which the percentages are by weight.
Example 1 Viscosecontaining 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 mixing stage and the salt figure was 6.4, 0.5 percent of carbon disulphide on the weight of the viscose was added and was 3 millimoles per grams of viscose of fluorescein in the form of its sodium salt were added and the viscose was mixed for a further half an hour. When the viscose was 45 hours old and had a salt figure of 8.9 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 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 gel swelling factor was 2.7 compared with 3.5 for an unmodified viscose. The water imbibition of the finished thread was 87 percent compared with 101 percent for a similar thread from an unmodified viscose. Determination of the axial difiusion coefiicient of a dyestuff along the core of the thread was carried out as described by Hermans in the Textile Research Journal, 1948, page 9, using Solophenyl Fast Blue-green BL; no penetration of dyestufi" was obtained; but for thread from an unmodified viscose it was 50 a after impregnation for four hours in 1 percent solution of the dyestulf at room temperature, indicating that the thread from the modified viscose showed no skin and core effect. The thread had a non-crennlated surface and the filaments were dog-bone shape in crosssection.
Example 2 Viscose conatining 7.8 percent cellulose, 6.5 percent caustic soda and 2.15 percent combined sulphur was prepared in the usual manner and filtered. When the viscose was 33 hours old 0.5 percent of carbon disulphide was added to it and mixed in for 1 hour. The viscose was divided into five parts one of which was a blank and to the other four were added 1.5, 3.0, 6.0 and 9.0 millimoles per 100 grams of viscose of fluorescein in the form of its sodium salt. The viscoses were mixed for 15 minutes, evacuated for eight hours and spun through a jet having forty holes .003 inch in diameter in a bath containing 9.0 percent of sulphuric acid, 20.0 percent of sodium sulphate and 4.0 percent of zinc sulphate at 48 Centigrade. The filaments were drawn off by a godet at 18 yards per minute and collected in a Topham box revolving at 4,000 R. P. M. The yarn was subsequently washed and dried.
The salt figures at the time of spinning were 9.5, 9.8, 8.9, 9.3 and 9.3 respectively. The cross-sections of the yarns are shown in Figures 1 to 5 in which Figure 1 is yarn from unmodified viscose and Figures 2, 3, 4 and 5 are yarns from the viscose having 1.5, 3.0, 6.0 and 9.0 millimoles of fluorescein respectively per 100 grams of viscose. These figures show how the shape and smoothness of outline are affected by the addition of fluorescein. The yarn from unmodified viscose has a substantially circular cross-section and crenulated surface but the other yarns show elongated cross-sections and smoother outlines with the maximum effect at about 3.0 millimoles of fluorescein per 100 grams of viscose.
What I claim is:
1. Viscose containing more than /4 of a millimole and less than 12 millimoles per 100 grams of viscose of a compound selected from the group consisting of fluorescein and an alkali metal salt thereof.
2. Viscose containing more than 1.5 and less than 12 millimoles per 100 grams of viscose of a compound selected from the group consisting of fluorescein and an alkali metal salt thereof.
3. A process for the production of artificial filamentary material comprising extruding viscose into an aqueous coagulating bath containing sulphuric acid and zinc sulphate, wherein the viscose contains more than A of a millimole and less than 12 millimoles per 100 grams of viscose of a compound selected from the group consisting of fluorescein and an alkali metal salt thereof.
4. A process as claimed in claim 3 wherein the viscose contains more than 1.5 and less than 12 millimoles per 100 grams of viscose of a compound selected from the group consisting of fluorescein and an alkali metal salt thereof.
References Cited in the file of this patent UNITED STATES PATENTS 1,188,777 Hewitt June 27, 1916 1,983,045 Payne Dec. 4, 1934 1,994,709 Holzach et al. Mar. 19, 1935 2,136,201 Whitehead Nov. 8, 1938 2,157,544 Kline May 9, 1939 2,160,839 Dreyfus June 6, 1939 2,307,760 Creadlick Jan. 12, 1943 2,535,044 Cox Dec. 26, 1950 2,535,045 Cox Dec. 26, 1950 2,536,014 Cox Dec. 26, 1950 2,581,059 Witte Jan. 1, 1952 2,658,888 Fischer et a1 Nov. 10, 1953

Claims (1)

1. VISCOSE CONTAINING MORE THAN 1/4 OF A MILLIMOLE AND LESS THAN 12 MILLIMOLES PER 100 GRAMS OF VISCOSE OF A COMPOUND SELECTED FROM THE GROUP CONSISTING OF FLUORESCEIN AND AN ALKALI METAL SALT THEREOF.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3034910A (en) * 1959-07-31 1962-05-15 Buckeye Cellulose Corp Production of regenerated cellulose filaments from wood pulp
WO2004005595A1 (en) * 2002-07-09 2004-01-15 Lenzing Aktiengesellschaft Process for the manufacture of solid regenerated viscose fibres
US20060200103A1 (en) * 2003-03-27 2006-09-07 Josef Schmidtbauer Solid regenerated standard viscose fibres

Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1188777A (en) * 1910-07-23 1916-06-27 Cooper Hewitt Electric Co Light-transforming compositions.
US1983045A (en) * 1930-05-26 1934-12-04 Nat Aniline & Chem Co Inc Coloring matter derived from pyrazolones
US1994709A (en) * 1931-11-25 1935-03-19 Gen Aniline Works Inc Dyestuff salt containing heavy metals in complex combination in the acid component
US2136201A (en) * 1935-09-13 1938-11-08 Celanese Corp Method of spinning artificial filaments
US2157544A (en) * 1934-08-22 1939-05-09 Du Pont Cellulosic structure and process for preparing same
US2160839A (en) * 1936-03-03 1939-06-06 Celanese Corp Method of making textile materials
US2307760A (en) * 1940-07-26 1943-01-12 Du Pont Article of manufacture
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
US2536014A (en) * 1946-12-14 1950-12-26 Du Pont Spinning of viscose
US2581059A (en) * 1948-06-29 1952-01-01 Gen Aniline & Film Corp Process of acylation
US2658888A (en) * 1950-08-03 1953-11-10 Hoechst Ag Heterocyclic monoazodyestuffs

Patent Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1188777A (en) * 1910-07-23 1916-06-27 Cooper Hewitt Electric Co Light-transforming compositions.
US1983045A (en) * 1930-05-26 1934-12-04 Nat Aniline & Chem Co Inc Coloring matter derived from pyrazolones
US1994709A (en) * 1931-11-25 1935-03-19 Gen Aniline Works Inc Dyestuff salt containing heavy metals in complex combination in the acid component
US2157544A (en) * 1934-08-22 1939-05-09 Du Pont Cellulosic structure and process for preparing same
US2136201A (en) * 1935-09-13 1938-11-08 Celanese Corp Method of spinning artificial filaments
US2160839A (en) * 1936-03-03 1939-06-06 Celanese Corp Method of making textile materials
US2307760A (en) * 1940-07-26 1943-01-12 Du Pont Article of manufacture
US2536014A (en) * 1946-12-14 1950-12-26 Du Pont Spinning of viscose
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
US2581059A (en) * 1948-06-29 1952-01-01 Gen Aniline & Film Corp Process of acylation
US2658888A (en) * 1950-08-03 1953-11-10 Hoechst Ag Heterocyclic monoazodyestuffs

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3034910A (en) * 1959-07-31 1962-05-15 Buckeye Cellulose Corp Production of regenerated cellulose filaments from wood pulp
WO2004005595A1 (en) * 2002-07-09 2004-01-15 Lenzing Aktiengesellschaft Process for the manufacture of solid regenerated viscose fibres
US20050179165A1 (en) * 2002-07-09 2005-08-18 Josef Schmidtbauer Process for the manufacture of solid regenerated viscose fibres
US20060200103A1 (en) * 2003-03-27 2006-09-07 Josef Schmidtbauer Solid regenerated standard viscose fibres

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