US2334615A - Continuous spinning of cellulose solutions in strong mineral acids - Google Patents

Continuous spinning of cellulose solutions in strong mineral acids Download PDF

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Publication number
US2334615A
US2334615A US292254A US29225439A US2334615A US 2334615 A US2334615 A US 2334615A US 292254 A US292254 A US 292254A US 29225439 A US29225439 A US 29225439A US 2334615 A US2334615 A US 2334615A
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Prior art keywords
cellulose
acid
suspension
solution
strong mineral
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US292254A
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English (en)
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Fink Heinrich
Rath Gustav
Hofstadt Richard
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B1/00—Preparatory treatment of cellulose for making derivatives thereof, e.g. pre-treatment, pre-soaking, activation
    • C08B1/003—Preparation of cellulose solutions, i.e. dopes, with different possible solvents, e.g. ionic liquids
    • 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

  • the solutions of cellulose in strong mineral acids are distinguished from cellulose solutions in ammoniacal copper oxide and quaternary bases as well as from viscose by a much higher viscosity with the same content of cellulose, and by the rapid degradation to which the cellulose is subject in. strong mineral acid solutions.
  • the present invention overcomes these dimproperty of cellulose of swelling strongly in mineral acids/of a certain concentration, whereby the union between the ibers is so loosened that there is produced a suspension of fibers of a pasty consistency which can easily be made to ow like a liquid by means of pumps, worms, pistons and the like.
  • Figure l shows diagrammatically a sectional view of an apparatus for carrying the invention into effect
  • Figure 2 is a diagrammatic longitudinal section of an apparatus comprising pressure worms pension slowly forward at a uniform rate by pressure and thoroughly mixing with.' the acid by means of a stirring device, the cellulose dissolves rapidly.
  • a dissolving chamber is arranged in the path to the spinning nozzle, and there may advantageously be a further chamber of a similar kind for homogenizing the solution, whereupon the solution can, if necessary, be
  • the only discontinuous process consists in the production of relatively small batches of the suspension, since in this phase there' is .no danger of ldegradation at the proper temperature, for instance 0 C.
  • the suspension has entered the apparatus as much cellulose is dissolved per unit time as leaves'the apparatus in the same time. Since the dissolution is 4.bubbles is impossible owing rapid the quantity of solution present in the apparatus can be kept very small. For example the total capacity of an apparatus for dissolving 100 kg'.
  • Isuspension is supplied by removing the lid 2 of the cylinder 'l whose piston 3 is for the time beingv .in its lowest position and nlling the cylinder e with suspension;
  • the lid is screwed on the cylinder is'evacuated while the other 'piston 3 makesitsworking 'strokef
  • the cocks I being reversed. In this manner the suspension continually enters the chamber 8 and passes to the spinning nozzles through the pipe II while they cylinders I are charged discontinuously;
  • the cellulose suspension is likewise fed alternately to at least two cylinders I and is deaerated through pipes provided with cocks 8 before proceeding further.
  • the cylinders have no lids ingworm I3 by way of the valve 1a with the lose and the lowest possible content of swelling acid-that are required. Since the batches containing Athe minimum of swelling acid are 'too stiff to be well evacuated the process is so carried out that the suspension is formed with an excess oi' swelling acid and is deaerated, whereupon the suspension under a steady weak pressure.
  • the cylinders I and pistons 3 can in this case be much weaker than those of Figure 1 since the actual feeding of the suspension is performed by the driven worm I3.
  • the latter feeds the suspension into the dissolving chamber I4, which is excess is pressed of! in the apparatus itself. before Y entry of the mass into the dissolving chamber. Thismay-be done for example by forming the feeding device before the dissolving chamber as a pressure worm.
  • the degree of pressure depends on the degree of swelling of the cellulose which is determined by'the concentration oi' theI swelling acid and, for instance, when using' sulfuria acid, increases especially rapidly in the region oi' 5 8560 per cent sulfuric acid.' I
  • I denotes two similar pressure-tight cylinders of acid-resistingmateria] having removable lids 2.
  • Machined pistons 3 having rods! of which .the lower parts are screw-threaded,VA are adapted tobe moved by the driving wheels 5, in the cylinders I
  • the means for driving the wheels I are the motors'M and gears *5a.
  • the cylinders are provided at their upper ends with pipes having cocks 6 and conf" nected with vacuumapparatus.
  • branch pipe I8 may be connected with the ⁇ lower lends of the cylinder.
  • the solution After leaving the dissolving chamber the solution passes to two or more homogenizing worms I5 which feed the solution through pipes II to the spinnerets.
  • Figure 3 s hows apparatus whichv is suited for the production of air-free solutions especially rich in cellulose.. ⁇ Only one charging container I with x .stirrer- Ia and deaerating connection 6 is shown the other or others being assumed to lie outside the plane of the paper behind container vI a yreversal valve suchas 'Ia in Figure 2 being pro ⁇ vided between them. Into the container ⁇ I the suspension is fed with an excess oi' swelling acid while stirring'and is then deaerated'.
  • the mass is ...
  • the worm I3 in this caseacts as apressure worm g circular pipe with alarge number of -perforations
  • the mass is theny fed through the homogenizlns in this case so thin that it runs under its own V'head into the.y chamber provided with .thel worm I3,'the.container's I being againused alternately.
  • the walls of the press-chamber are hollow, the wall I 6 being perforated to allow the excess of swelling acid to be extruded'into the tank 25 where it can be collected andl returned to the mixer in which the I cellulose is swollen.
  • the suspensionv having a reduced content of swelling'acid is then fed into v,the dissolving chamber 22, to which acid is supplied from the pipe I0.
  • v'The dlssolving'chamber 22 is provided with a-kneading pump of theusual worms I5 and pipes I ⁇ I tothe spinnerets.
  • Example 1 With every 3 kg. of cellulose (air-dry) there are stirred, while cooling to 0 C., 30 kg. of sulf-uric acid containing 59.0 per cent of HzSO4 and the mixture is fed into the similarly cooled cylinder l shown in Figure 1 or Figure-2 and evacuated. From there the suspension is ied'continuously during about 30 minutes by means of the piston 3 into the dissolving chamber 8, which is Example 2 4.5 kg. of cellulose (air-dry) in 45 kg. of sulfuric acid containing 59.5 per cent of H2SO4 are introduced into the container shown in Figure 3 and stirred at 0 C. The mixture is then evacuuated. The containers are used alternately.
  • the batch After evacuation the batch is run into the chamber containing the pressure worm i3 which expresses 16 kg. of swelling acid per batch, so that the mass enters the dissolving chamber with a content of 29 kg. of swelling acid to 4.5 kg. of cellulose. 9.5 kg. of sulfuric acid containing '75 per cent of H2SO4 and cooled to 0 C. are supplied to the dissolving chamber.
  • the solution produced contains 9.8 per cent of cellulose and 57 per cent of H2S04.
  • a process of continuously producing solutions of cellulose in a strong mineral acid which comprises suspending the cellulose in a mineral acid of a concentration which will cause swelling of the cellulose, but will not dissolve it, feeding said suspension continuously to an extruding device and adding to said suspension on its way to the extruding device a strong mineral acid in an amount which is necessary to dissolve the cellulose in said suspension, the amount of solution formed per time unit being kept the same as the amount of solution leaving the extruding device.
  • v l5 2.
  • the mineral acid lin the suspension is sulfuric acid with a content of about 59 per cent 'of H2504 and the strong mineral'acid dissolving the suspension is sulfuric acid of about '15 per cent of H2SO4.
  • a process of continuously producing solutions of cellulose in a strong mineral acid which comprises suspending the cellulose in a mineral l acid of a concentration which will cause swelling of the cellulose but will not dissolve it, continuously removing a part of the vsuspension liquid from the suspension, feeding said suspension continuously to an extruding device and adding .to Y
  • a process of continuously producing solutions of cellulose in a strong mineral acid which comprises suspending the cellulose in a minera1 acid of a concentration which will cause swelling of the cellulose but will not dissolve it, de-aerat- 4o ing the suspension, feeding said suspension continuously to an extruding device and adding to said suspension on its way to the extruding device a strong mineral acid in an amount which is necessary to dissolve the cellulose in said sus- 45 pension, the amount of solution formed per time unit being kept the same as the'amount of solution leaving the extruding device.
  • HEINRICH FINK GUSTAV RTH. RICHARD HOFSTADT.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Biochemistry (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Artificial Filaments (AREA)
US292254A 1938-08-30 1939-08-28 Continuous spinning of cellulose solutions in strong mineral acids Expired - Lifetime US2334615A (en)

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DE212205X 1938-08-30

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US2334615A true US2334615A (en) 1943-11-16

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US292254A Expired - Lifetime US2334615A (en) 1938-08-30 1939-08-28 Continuous spinning of cellulose solutions in strong mineral acids

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US (1) US2334615A (en:Method)
BE (1) BE436169A (en:Method)
CH (1) CH212205A (en:Method)
FR (1) FR868729A (en:Method)
NL (1) NL50822C (en:Method)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5456748A (en) * 1993-05-24 1995-10-10 Courtaulds Fibres (Holdings) Ltd. Premix storage hopper

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5456748A (en) * 1993-05-24 1995-10-10 Courtaulds Fibres (Holdings) Ltd. Premix storage hopper

Also Published As

Publication number Publication date
BE436169A (en:Method)
FR868729A (fr) 1942-01-14
NL50822C (en:Method)
CH212205A (de) 1940-11-15

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