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
• • 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
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10S264/00—Plastic and nonmetallic article shaping or treating: processes
  • Y10S264/27—Process of spinning viscose where viscose has high degree of polymerization

Definitions

• This invention relates to the production of viscose rayon, artificial staple fibre, hair, braid and the like.
• a process for the production of viscose rayon, artificial staple fibre, 'hairfbraid and the like comprises extruding in filamentary form into a coagulating bath of low acid concentration, at room temperature, a Viscose having a viscosity of at least 400 poises and having a y-value above 60, and thereafter fixing the filamentary product by treatment in hot aqueous liquid.
• the high viscosity viscose employed may be obtained by either of two general methods. In one form of the invention there may be employed viscose produced from an alkali cellulose with a cellulose concentration of 6% to 10% and which has not been ripened (the product is referredto herein as an unripe viscose) and in another form of the invention there may be employed viscose which has a cellulose content of 10 to employed may be achieved by Xanthogenation of.
• the alkali cellulose with-a large excess of car- It is defined by Fink, Stahn cosityof 600 poises or more and the y-value is 70 2 bon disulphide, i e. more than 5 0% calculated on thee cellulose present.
• the viscose employed has a visto 80.
• the viscose employed will have a low concentration of alkali, e. g. 6% or less.
• the high viscosity viscoses are preferably spun through spinnerets having apertures consider-.. ably larger than normal, e. g. of about 0.10 to- 0.15 mm., and the coagulation baths employed are preferably sulphuric acid at a concentration
• the length of travel of the filamentary material through the bath may be,
• the filaments are completely, coagulated when they reach the end of the tube but are still highly plastic and can be easily stretched by 100% or 200% so that the winding speed may be as high as 200 or even 300 metres per minute.
• the fixing of the yarn- is effectedby treatment with hot aqueous baths, e.,g,. hot dilute acids or I saline solutions or hot water. If. the fixing operation is carried out with the yarn under tension;
• fibres vare'obtained, after cutting. which have-very low elongation, less than 7% which yield yarn of relatively low tenacity.
• the fixing is carried out with the filaments in the de-tensioned condition, either by cutting before fixing or by de-tensioning the bundle of filaments before the fixing operation, the fibres have higher elongations, from 7% to 10% or more. They are'very supple and are readily converted by methods known per se, into high quality yarns.
• the filamentary material obtained may be stretched (additionally to the stretching effected as it leaves the nozzle), e. g. by 100 to 200%.
• Yarns of varying denier, e. g. 0.5 to 4 denier, may be obtained by the process.
• EXAIWPLE I Production of the unripe viscose spinning solution greater than 800 and containing less than 2% of molecular chains having a degree of polymerisation below 200, are steeped in caustic soda lye containing 235-240 g./litre of NaOH. The sheets are pressed to expel excess lye until their weight is reduced to 280-285% of the initial alpha-cellulose content. The alkali cellulose thus obtained is shredded but not ripened. It is reacted at 28 C. with carbon disulphide, (50 parts of CS2 per 100 parts of initial alpha-cellulose) for 2 hours. The cellulose xanthate thus obtained is mixed with a small quantity of 9% caustic soda lye at 5 to 10 C. and the resulting pasty, swollen mass is dissolved in 4% caustic soda lye at to C.
• the resulting solution contains about 9.5% of cellulose and 5% of caustic soda. It has a viscosity of 900 poises and the degree of polymerisation of the cellulose contained in it is still in excess of 500. Its salt point lies between 15 and 16.
• the solution is filtered and degassed for 9 hours in a vacuum in the presence of 1 g./litre of a mixture of higher branched aliphatic alcohols as antiscumming agent. It is then ready for use.
• the viscose solution thus prepared, without any ripening, is spun in an apparatus as described in said Patent No. 2,511,699.
• the spinning bath used consists of sulphuric acid at a strength of 1 g./litre and the spinning is eiTected at ordinary room temperature.
• the spinnerets used have a diameter at least about 50% larger than is customary when spinning viscose, e. g. 0.15 mm. to yield filaments of about 1 denier, in order to increase the degree of stretching possible at the spinnerets.
• the stretch at this stage should be positive, i. e. the speed of the filaments leaving the spinnerets should be higher than the speed of the viscose passing through the spinnerets. Using a tube of about 5 mm. diameter metres per minute, or more, are easily obtained.
• the filaments are stretched by a further 150% by means of rollers as in Patent No. 2,511,699.
• the filament may be set by treatment in a bath identical with the spinning bath but heated to 75-80 C., but if this is not done it is preferable to complete the setting of the filaments by 9.1-
• the yarn obtained is washed with hot water and dried. Even without any desulphurisation or bleaching treatment the yarns obtained are remarkably white.
• the conditions being adjusted to yield a yarn of denier/100 filaments, the characteristics of the yarn are:
• the alkali cellulose is not ripened but is shredded for 2 hours with cooling, and then xanthogenated with 55 of carbon disulphide (calculated on the alpha-cellulose content, of the pulp) for 3 hours at between 22 and 30.
• a mixture of the cellulose xanthogenate and alkali is prepared containing 9% of caustic soda and 12% of cellulose and this is then slowly mixed at between 5 and 10 C. with dilute caustic soda to produce a viscose containing 6% to 7% cellulose and 5% to 6% caustic soda.
• the use of stronger caustic soda initially is desirable in order to secure the maximum solubility of the xanthogenate.
• the v-value of the product is about 80.
• the viscose thus obtained has a 'y-value of 70 and a viscosity of about 500 poises.
• a rayon of 400 deniers and containing 260 filaments is spun at 50 m./min. through a spinneret having holes of 0.10 to 0.15 mm. dipping into a bath containing 10 to 15 g./litre of sulphuric acid at 18, the length of the passage de-tensioning.
• This procedure does not afiect the wet and dry tenacity. It has the advantage that it directly de-acidifies the yarn and permits immediate and complete recovery of the carbon disulphide.
• EXANLPLE III Alkali cellulose is prepared as in Example 11, shredded for 2 hours, with cooling, ripened for 30 hours at 21 0., and xanthogenated with 60% of carbon disulphide (calculatedon the alphace1lulose).fcr 3 hours between 22 and 30 C.
• a viscose containing 12% of cellulose and 6% caustic soda is prepared, whereafter the mixture is filtered and degassed. After ripening for 18 hours at 10 C., the -value of the product is 75.
• a bundle of fibres having a total count of 5250 deniers is spun via a spinneret having 3500 holes of a diameter of 0.10 mm., into a sulphuric acid bath of concentration g./litre.
• the filaments are stretched between rollers to 148% and the filaments are then de-tensioned and fixed in water at 85-90 C.
• the filaments are cut to form artificial staple fibre and this product has the following properties:
• the bundle of filaments is passed after de-tensioning, into a second bath composed of very hot Water, for example at 90 C.
• the hot Water treatment produces strongly curled fibres.
• a viscose prepared in accordance with Example ]1 is a spun through a spinneret having slots of 0.25 x 0.05 mm. The conditions are regulated to produce flat filaments of 3 denier, which have the following properties:
• the cross-section is of very elongated form and the filaments may be cut into staple fibre.
• the staple fibre can be easily carded or combed and gives normally regular yarns. In use, it may be mixed with cotton in all proportions. It is an effective substitute for high tenacity staple fibre as previously used in the cotton and linen industry.
• the staple fibre obtained appears under the microscope as twisted fibres of the cotton type.
• Modified yarns may be obtained by including white or coloured pigments or oily substances in the spinning solutions.
• a particular advantage of the process of this invention is that a large proportion of the carbon disulphide used may be readily recovered. Carbon desulphide is regenerated in the spinning bath and remains dispersed therein. Some sinks to the bottom of the spinning bath and can be separated by decantation while the remainder can be recovered by treating the bath with a stream of gas or vapour and adsorbing, absorbing or condensing the carbon disulphide from the gas or vapour stream by any of the usual methods.
• Yarns obtained by the processof this invention have valuable commercia1 properties; for example they may be usedfortheproduction ofjcords for reinforcing pneumatic tyres.
• the prodartificial staple fibre, -hair, braid and the like which comprises extruding in filamentary form into a coagulating bath of sulphuric acid of concentration 1 to 15 g./litre at room temperature,
• a process for the production of viscose rayon, artificial staple fibre, hair, braid and the like which comprises extruding ina filamentary form into a coagulating bath of sulphuric acid of concentration lto 15-g./litre at room temperature, a viscose containing 6% to 15% of cellulose, not over 6% of sodium hydroxide, and prepared from unripened alkali cellulose by xanthogenation with more than 50% carbon disulphide, having a viscosity of at least 400 poises and havin a 'y-value above 60, and thereafter fixing the filamentary product by treatmentin hot aqueous liquid.
• a process for the production of viscoserayon, artificial staple fibre, hair, braid and the like which comprises extruding in filamentary form into a coagulating bath of sulphuric acid of concentration 1 to 15 g./litre at room temperature, a viscose containing 10 to 15% of cellulose, not over 6% of sodium hydroxide, and prepared from ripened alkali cellulose by xanthogenation with more than 50%. of carbon disulphide, having a viscosity of at least 400 poises and having a y-value above 60, and thereafter fixing the filamentary product by treatment inhot aqueous liquid.
• artificial staple fibre, hair, braid and the like which comprises extruding in filamentary form into a coagulating bath containinglo to 15 g. per litre of sulphuric "acid at room temperature, a viscose containing 6% to 15% of cellulose, not over 6% of sodium hydroxide, and prepared from unripened alkali cellulose by xanthogenation with more than 50%carbon disulphide,having a viscosity of at least 400 poises and having a y-value above 60, and thereafter fixing the filamentary product by treatment in hot aqueous liquid.
• A'process for the'pro'duction of viscose rayon, artificial staple'fib-re, hair, braid and the like which comprises extruding in filamentary form into acoagulating bath containing to g. per litre of sulphuric acid at room temperature via spinnerets with holes of 0.10 to 0.15 mm. diameter, a viscose containing 6% to 15% of cellulose, not over 6% of sodium hydroxide, and prepared from unripened alkali cellulose by xanthogenati'on with more than carbon disulphide, having a-viscosity of at least 400 poises and having a y-value above 60, and thereafter fixing the filamentary product by treatment in hot aqueous liquid.
• a process for the production of viscose rayon, artificia1 staple fibre, hair, braidand the like which comprises extruding in filamentary form into a coagulating bath containing 10 to 15 g. per litre of sulphuric acid at room temperature via spinnerets with holes of 0.10 to 0.15 mm. diameter, a viscose containing 10 to 15% of cellulose, not over 6% of sodium hydroxide, and prepared from ripened alkali cellulose by xanthogenation with more than 50% of carbon disulphide, having a viscosity of at least 400 poises and having a v-value above 60, and thereafter fixing the filamentary product by treatment in hot aqueous liquid.
• a process for the production of Viscose rayon, artificial staple fibre, hair, braid and, the'like which comprises extruding in filamentary form into a coagulating bath containing 10 to 15 g. per litre of sulphuric acid at room temperature via spinnerets with holes of 0.10 to 0.15 mm.
• a process for the production of viscose rayon, artificial staple fibre, hair, braid and the like which comprises extruding in filamentary form into a coagulating bath containing 10 to 15g. per litre of sulphuric acid at room temperature via spinnerets with holes of 0.10 to 0.15 mm.
• a process for the production of viscose rayon, artificial staple fibre, hair, braid and the like which comprises extruding in filamentary.
• a process forthe production of viscose rayon, artificial'staple fibre, hair, braid and the like which comprises extruding in filamentary form into a coagulating bath containing 10 to 15 gper litre of sulphuric acid at room temperature via spinnerets with holes of 0.10 to 0.15 mm.
• a process for the production of-viscose rayon, artificial staple fibre, hair, braid and the like which comprises extruding in filamentary form into a coagulating bath containing 10 to 15 g. per litre of sulphuric acid at room tempera- I ture via spinnerets with holes of 0.10 to 0.15 mm.
• a process for the production of viscose rayon, artificial staple fibre, hair, braid and the like which comprises extruding in filamentary form into a coagulating bath containing 10 to 15 g. per litre of sulphuric acid at room temperature via spinnerets with holes of 0.10 to 0.15 mm.
• a process for the production of viscose rayon, artificial staple fibre, hair, braid and the like which comprises extruding in filamentary form into a coagulating bath of sulphuric acid of concentration 1 to 15 g./litre at room temperature, a viscose containing 6% to 15% of cellulose,
• a process for the production of viscose rayon, artificial staple fiber, hair, braid and the like which comprises extruding in filamentary form into a coagulating bath of sulphuric acid of concentration 1 g./litre at room temperature, a viscose containing 6% to 15% of cellulose, not over 6% of sodium hydroxide, and prepared from unripened alkali cellulose by xanthogenation with more than 50% carbon disulphide, having a viscosity of at least 400 poises and having a y-value above 60, and thereafter fixing the filamentary product by treatment in hot aqueous liquid.
• the method of spinning viscose for the manufacture of rayon and the like which comprises ejecting a solution of unripe viscose containing 6% to 15% of cellulose, not over 6% of sodium hydroxide, and having a 'y-value of at least 60 and a viscosity of at least 400 poises at a controlled rate from a spinneret having holes of from .10 mm. to .15 mm. diameter into a coagulating bath, and drawing the filaments in a straight line from said spinneret through a straight tube immersed in said bath and of a diameter such that liquid is drawn through the tube solely by the motion of the filaments.
• the method of spinning viscose for the manufacture of rayon and the like which comprises ejecting a solution of unripe viscose having a 'y-value of at least 60 and a viscosity 01 at least 400 poises, the said viscose solution containing 9.5% to 15% of cellulose and not over 6% of caustic soda, at a controlled rate from a spinneret having holes of .10 mm. to .15 mm. diameter into a coagulating bath, and drawing the filaments in a straight line from said spinneret through a straight tube immersed in said bath and of a diameter such that liquid is drawn through the tube solely by the motion of the filaments.
• the method of spinning viscose for the manufacture of rayon and the like which comprises ejecting a solution of unripe viscose having a 'y-value of at least 60 and a viscosity of at least 400 poises, the said viscose solution containing at least 9.5% of cellulose and at most 6% of caustic soda and having a degree of polymerization in excess of 500, at a controlled rate from a spinneret having holes of .10 mm. to .15 mm. diameter into a coagulating bath, and drawing the filaments in a straight line from said spinneret through a straight tube immersed in said bath and of a diameter such that liquid is drawn through the tube solely by the motion of the filaments.
• the method of spinning viscose for the manufacture of rayon and the like which comprises ejecting a solution of unripe viscose containing 6% to 15% of cellulose, not over 6% of sodium hydroxide, and having a 'y-value of at least 60 and a viscosity of at least 400 poises at a controlled rate from a spinneret having holes of .10 mm. to .15 mm. diameter into a coagulating bath, and drawing the filaments in a straight line from said spinneret through a straight tube immersed in said bath and of a diameter such that liquid is drawn through'the tube solely by the motion of the filaments, the drawing of the filaments being such as to cause a positive stretching of the filaments.
• the method of spinning viscose for the manufacture of rayon and the like which comprises ejecting a solution of unripe viscose containing 6% to 15% of cellulose, not over 6% of sodium hydroxide, and having a -value of at least 60 and a viscosity of at least 400 poises at a controlled rate from a spinneret having holes of .10 mm. to .15 mm.
• the method of spinning viscose for the manufacture of rayon and the like which comprises ejecting a solution of unripe viscose containing 6% to 15% of cellulose, not over 6% of sodium hydroxide, and having a 'y-value of at least 60 and a viscosity of at least 400 poises at a controlled rate from a spinneret having holes of .10 mm. to .15 mm.
• a coagulating bath consisting of a 1% solution of sulphuric acid, and drawing the filaments in a straight line from said spinneret through a straight tube immersed in said bath and of a diameter such that liquid is drawn through the tube solely by the motion of the filaments, the drawing of the filaments being such as to cause a positive stretching of the filaments, and stretching the filaments leaving the coagulating bath by .a further 100% to 200%.
• the method of spinning viscose for the manufacture of rayon and the like which comprises ejecting a solution of unripe viscose containing 6% to 15% of cellulose, not over 6% of sodium hydroxide, and having a 'y-value of at least 60 and a viscosity of at least 400 poises at a controlled rate from a spinneret having .10 mm. to .15 mm.

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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)
• Materials For Medical Uses (AREA)

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