US2319305A - Process of continuously forming cellulose films, staple fibers, and artificial silk - Google Patents

Process of continuously forming cellulose films, staple fibers, and artificial silk Download PDF

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Publication number
US2319305A
US2319305A US183202A US18320238A US2319305A US 2319305 A US2319305 A US 2319305A US 183202 A US183202 A US 183202A US 18320238 A US18320238 A US 18320238A US 2319305 A US2319305 A US 2319305A
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United States
Prior art keywords
cellulose
nozzle
bath
artificial silk
staple fibers
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Expired - Lifetime
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US183202A
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English (en)
Inventor
Nooij Jan Cornelis De
Bleibler Ernest
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Individual
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Individual
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    • 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
    • D01D5/06—Wet spinning methods
    • 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
    • D01F2/02—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from solutions of cellulose in acids, bases or salts

Definitions

  • Our invention relates to improvements in a process for continuously forming cellulose films, transparent sheets, staple fibers and artificial silk, and especially from solutions of cellulose in sulphuric acid, by use of a movable conveyer, the surface of which may be perforated.
  • the first and oldest process uses the'so-called pouring drum.
  • the solution used is poured upon .a rotating drum and fiowed on to the desired thickness.
  • a pouring funnel open at the top is used.
  • the surface of the film is formed on the one side by the surface of the drum, and on the other side by flowing and solidifying without coming into contact with a solid object.
  • This process therefore, requires that the drum have a perfect surface, this being unfavorable especially because of the expense and the possibility of applying the process in actual practice, especially as the surface is chemically affected; moreover the spinning-speed is very limited in practice due to the diameter of the drum.
  • the second process consists in forcing the cellulose solution'into a coagulation bath between two lips or through a nozzle in such a way that the layer entering the bath is a vertical or sloping direction is immediately washed by the bath liquid on two sides.
  • the surface after the cellulose solution leaves the nozzle, is formed on both sides by flowing and solidification without coming into contact with a solid object.
  • the film formed in thi way must be carried upward from the bath which is generally done by leading the product around a driven roller. This process has the disadvantage that the film, whichis at that time only partially coagulated and which is still very weak, is exposed to strong mechanical stresses, since the whole part which travels in an upward direction carries its own weight without any support and must transport itself further.
  • the first process is applied ordinarily, but not exclusively, for solutions of cellulose in volatile solvents, and the second process is used when solutions of cellulose are used which must be coagulated in a liquid.
  • the spinning-solution When using the first process the spinning-solution must not be very viscous because only a small pressure can be used for pressing the liquid out of the pouring funnel.
  • the second.processas has been remarked already-requires that the tensile strength of the film be relatively high even at the beginning.
  • a process is known for dissolving cellulose in sulphuric acid (vide U. S. Patent No. 1,991,141) according to which a relatively thick fiuid solution is formed. When coagulating this solution a strongly swollen gel of relatively small initial strength is obtained.
  • a new coagulation method is used for continuously forming films and transparent sheets, whereby the two principal difficulties as mentioned aboveare removed. Since, however, in spinning staple fibers and artificial silk according to U. S. Patent 1,991,141 the same difficulties are encountered (which are all to be ascribed to the low strength of the product before it has been thoroughly coagulated) our new process may also be applied for the manufacture of both products, the broad nozzle being replaced by one or more spinning nozzles arranged next to each other, in case artificial silk is to be spun.
  • the process according to our invention is characterized by the feature that the layer or one or more jets of cellulose solution is first superficially coagulated on both sides, whereupon it is immediately taken up by the bearing surface and is carried forward in this supported condition in order to be coagulated further.
  • Another feature of our invention is that the liquid to be coagulated is pressed through the nozzle in a horizontal or practically horizontal direction.
  • the bearing surface may consist of a moving band or conveyer running in a horizontal or practically horizontal direction, made of stainless steel or rubber.
  • the bearing surface may also consist of the upper part of a rotating drum.
  • Fig. 1 is a somewhat diagrammatic view, showing a vertical section through an apparatus having means for feeding the solution into the coagulation bath, and means for supporting the resulting weak film or the like on a conveyor while the coagulation proceeds until the film gains strength, and
  • Fig. 2 is a fragmentary plan view correspond-- ing thereto, showing the means for feeding the solution into the bath.
  • the cellulose solution e. g. obtained by the process according to U. S. Patent No. 1,991,141 is supplied from a tank to a channel] which is formed in the interior of a nozzle-piece 2.
  • Said nozzle-piece is pivotally supported by bearings 3 and 4 and may berotated by means of a handwheel 5 acting by means of a worm 6 on teeth on one of the pivots of the nozzle-piece 2.
  • the channel I in the nozzle-piece is connected by a passage 1 to the nozzle which is formed by a fixed part 8 extending throughout the length of the nozzle-piece and a corresponding movable part 9.
  • Said movable part may be adjusted by means of hand-wheels I 0 which are each fixed on a screw I I engaging a threaded hole in a part 12 of the nozzle-piece 2.
  • the number of adjusting means depends upon the length of the movable nozzle-part 9. In the embodiment shown in the drawings four adjusting devices are shown for a nozzle of a width of e. g. 100-150 cm. but it is evident that the number of these maybe varied in accordance with the circumstances.
  • the cellulose solution is supplied to the channel i and forced out of the nozzle under a relatively high pressure of e. g. 8 atmospheres.
  • This solu-- tion leaves the nozzle preferably in a horizontal direction, passing into a coagulation liquid which is contained in a bath l3 so that the cellulose solution is first superficially coagulated on both sides.
  • a coagulation bath it is preferred to use .water or diluted sulphuric acid of about 15% of room temperature.
  • the product thus formed as a film l 4 is immediately taken up and conveyed by a moving surface e. g. a conveyer [5 running through the bath with a speed ofe. g. 30 meters per minute and is further coagulated by the coagulation liquid IS in the bath IS.
  • the conveyer I5 is moved by a roller II which is driven by any suitable known apparatus, e. g. an electric motor and a reduction gear, which are not shown in the drawings.
  • the conveyer, I 5 is further guided by a roller l8 and has a tightener I9.
  • the distance from the nozzle to the conveyer I5 is only small and may generally be about 2 to 10 cm.
  • the film which now consists of a gel, may be lifted from the conveyer after having passed under a roller 20 and may then be guided by other rollers 2
  • the nozzle or nozzles should preferably be acid-proof and capable of resisting high pressures.
  • pressures are applied from 0.1 to 1 kg. per cm., but in the acid process pressures of 2 to 10 kg. per cm. are applied.
  • Solutions made by dissolving cellulose directly in sulphuric acid have two chief properties in common, namely first that such solutions are of extraordinarily high viscosity and second that they can be coagulated only very slowly, and consequently the spinning apparatus according to the present invention presents the only means at present known to us for continuously spinning such solutions.
  • the slowness of coagulation which is characteristic of all these acid solutions, while no doubt due partly to the high viscosity, is caused mainly by the fact that the spinning of such solutions is a physical process (washing out or diffusing of acid into the bath) and not a chemical reaction, in marked contrast to the spinning of viscose, for example.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Artificial Filaments (AREA)
US183202A 1937-01-04 1938-01-03 Process of continuously forming cellulose films, staple fibers, and artificial silk Expired - Lifetime US2319305A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
NL494867X 1937-01-04

Publications (1)

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US2319305A true US2319305A (en) 1943-05-18

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US183202A Expired - Lifetime US2319305A (en) 1937-01-04 1938-01-03 Process of continuously forming cellulose films, staple fibers, and artificial silk

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US (1) US2319305A (en)van)
BE (1) BE425578A (en)van)
FR (1) FR831416A (en)van)
GB (1) GB494867A (en)van)
NL (1) NL47290C (en)van)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2939177A (en) * 1955-02-08 1960-06-07 Celanese Corp Process of cutting partially coagulated esters of cellulose into short lengths
US2962766A (en) * 1957-10-11 1960-12-06 Du Pont Process of producing cellulose film using a flowing coagulating bath
US3024493A (en) * 1958-01-30 1962-03-13 Phrix Werke Ag Adjustably shielded suction drum for circulating bath liquid
US3073733A (en) * 1960-05-31 1963-01-15 Du Pont Film and method of casting film
US3142714A (en) * 1961-12-20 1964-07-28 Nylonge Corp Method for the production of cleaning devices
US5403530A (en) * 1991-02-15 1995-04-04 Courtaulds Plc Elongate member production method
US5958320A (en) * 1997-01-09 1999-09-28 Akzo Nobel Nv Process for the manufacture of cellulosic fibers; and cellulosic fibers

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2939177A (en) * 1955-02-08 1960-06-07 Celanese Corp Process of cutting partially coagulated esters of cellulose into short lengths
US2962766A (en) * 1957-10-11 1960-12-06 Du Pont Process of producing cellulose film using a flowing coagulating bath
US3024493A (en) * 1958-01-30 1962-03-13 Phrix Werke Ag Adjustably shielded suction drum for circulating bath liquid
US3073733A (en) * 1960-05-31 1963-01-15 Du Pont Film and method of casting film
US3142714A (en) * 1961-12-20 1964-07-28 Nylonge Corp Method for the production of cleaning devices
US5403530A (en) * 1991-02-15 1995-04-04 Courtaulds Plc Elongate member production method
US5958320A (en) * 1997-01-09 1999-09-28 Akzo Nobel Nv Process for the manufacture of cellulosic fibers; and cellulosic fibers
US6159601A (en) * 1997-01-09 2000-12-12 Akzo Nobel Nv Process for the manufacture of cellulosic fibers; and cellulosic fibers

Also Published As

Publication number Publication date
BE425578A (en)van)
FR831416A (fr) 1938-09-02
NL47290C (en)van)
GB494867A (en) 1938-11-02

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