US3222198A - Viscose spinning solution for the manufacture of shaped articles from regenerated cellulose - Google Patents

Viscose spinning solution for the manufacture of shaped articles from regenerated cellulose Download PDF

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Publication number
US3222198A
US3222198A US232892A US23289262A US3222198A US 3222198 A US3222198 A US 3222198A US 232892 A US232892 A US 232892A US 23289262 A US23289262 A US 23289262A US 3222198 A US3222198 A US 3222198A
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United States
Prior art keywords
viscose
spinning
spinning solution
manufacture
polyether
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Expired - Lifetime
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US232892A
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English (en)
Inventor
Brachel Hanswilli Von
Jordan Heinz Dietrich
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Bayer AG
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Bayer AG
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Publication date
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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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
    • C08L1/08—Cellulose derivatives
    • C08L1/22—Cellulose xanthate
    • C08L1/24—Viscose

Definitions

  • the subject of the present invention is a process for the manufacture of fibres, threads or films from regenerated cellulose which are characterised by high strength and low swelling.
  • the object of the present invention is to obtain threads which have a lower swelling value and at the same time a higher tensile strength and elongation by using certain additives in the customaryviscose process.
  • Another object of the invention is to provide special additives which may be used in the viscose process for improving the quality of the threads. Further objects of the invention will become evidentin the following description and examples.
  • polyether sulphones in which for every four carbon atoms there is at least "one ether oxygen atom or one sulphone group.
  • processes may be used for preparing the claimed ether sulphones, for example, linear or branched polyether thioethers, such as those described in French patent specification 1,201,171, may be oxidized with hydrogen peroxide, sodium hypochlorite, or similar oxidizing agents, or alternatively mono-, diand polyvinyl sulphones, for example divinyl sulphone, dipropenylsulphone or p-di-vinylsulphonyl benzene may be added to monohydric or polyhydric alcohols, or alternatively the abovementioned monohydric and polyhydric alcohols may be reacted with B-halogen-alkyl-sulphones, such as methylfi-chloroethyl-sulphone, di-fi-chloroethyl-sulphone
  • the polyether sulphones have the particular advantage that they may be mixed homogeneously more easily with the viscose than the other additives previously mentioned, so that they are more effective.
  • the compounds used in accordance with the invention may conveniently be employed by means of the dosing processes which are already known for example for adding dyestulfs to spinning solutions, because when the aqeous or alkaline solutions of these compounds have been injected into the main stream of the viscose and passed through the mixing apparatus which is customarily provided in such plants, they are already present in a completely uniform distribution.
  • the substances incorporated in the viscose in accordance with the present invention may have other effects which promote a satisfactory spinning process, owing to the presence of the polar sulphone groups in these substances.
  • additional effects are: Theviscose may beeasier to filter, the thread may be drawn to a greater extent, the spinnerets may be less liable to get blocked and these, may be less incrustation of the spinnerets, the substances may have a clarifying effect on the spinning bath. This shows an improvement on the polyalkylene oxide compounds previously used.
  • spinning oils which are surface active products of various types. In the method used according to the invention, these spinning oils become superfluous.
  • the quantities of the above-described polysulphones that are added to the viscose vary according to the desired influence on the fibres and on the other conditions of the process, and lie between 0.1 and 4%, preferably 0.1 and 0.6% by weight.
  • the usual apparatus may be used for dosing without additional equipment.
  • the precipitating bath preferably contains at least 3% by weight of zinc sulphate.
  • the fibres and threads obtained with the above additives to viscose are distinguished from those produced without the use of these additives by having a flattened cross-section which may, for example, by kidney shaped, reduced swelling values and increased dry and wet tensile strength without reduced elongation at break.
  • Example 1 A viscose containing 7.2% cellulose and 5.5% total alkali, to which 1.8 g. of the compound described below has been added for each kilogram of viscose, was spun at a state of maturity corresponding to the salt point 8 from a spinneret having 48 apertures of 90a cross section into an acid precipitating bath to produce a thread having a total denier to 180.
  • the bath contained 120 g./l. sulphuric acid, 230 g./l. sodium sulphate and 35 g./l. zinc sulphate and the temperature was 48 C.
  • the thread was stretched in air between 3 rollers by a total of 100%, the last roller having a drawing off speed of 36 in. per minute.
  • the material obtained was then collected in a spinning pot which revolved at 6000 revs. per minute, and the material was then deacidified and treated in the usual manner and dried under tension.
  • the polyether polysulphone which was used was prepared as follows: 1700 g. polyethylene glycol having a molecular weight 1700, 200 g. thiodiglycol and 12 g. orthophosphoric acid were heated in an atmosphere of CO at 185 until the hydroxyl number had fallen below 30. Steam was blown through the reaction product for 4 hours at 120 and 15 mm. Hg pressure and then cooled to 80. The polyether thioether obtained was then slow ly treated with 340 g. hydrogen peroxide (32%) at 80 to 100, and heating was then continued until no more hydrogen peroxide could be detected. The water was then distilled off in vacuo.
  • Example 2 1.9 g. of the compound described below was added per kilogram of viscose to a viscose with 7.0% cellulose and 4.6% alkali. The process was then carried out as described in Example 1 except that the precipitating bath was composed of 95 g./l. sulphuric acid, 215 g./l. sodium sulphate and 45 g./l. zinc sulphate and the temperature of the bath was 50 and the threads were stretched by 100% but only between two rollers.
  • the precipitating bath was composed of 95 g./l. sulphuric acid, 215 g./l. sodium sulphate and 45 g./l. zinc sulphate and the temperature of the bath was 50 and the threads were stretched by 100% but only between two rollers.
  • the polyether polysulphone used was prepared as in Example 1 except that instead of using polyethylene glycol with a molecular weight of 1700, an equivalent quantity of oxyethylated butanediol-(1:4) having a molecular weight 800 was used.
  • Example 3 Observing the same conditions as in Example 1, 1.5 g. of the compound described below was used per kilogram of viscose, and the following improvements in the textile properties were obtained compared with the properties of unmodified viscose: reduction in swelling value, 32%; increase in dry tensile strength, 19%; increase in wet tensile strength, 22%.
  • the polyether polysulphone used was prepared as described in Example 1, except that the polyether thioether had a hydhoxyl number of 20 corresponding to a molecular weight of 5600.
  • Viscose spinning solution which contains 0.1-4.0% by weight of a polyether sulphone compound containing one member of the group consisting of a sulfone group for every four carbon atoms in the polymer chain, an ether group for every four carbon atoms in the polymer chain and a sulfone group plus ether oxygen for every four carbon atoms in the polymer chain, said compound being soluble at least to the extent of 0.1% in 5% aqueous sodium hydroxide solution and having a molecular weight between 300 and 20,000.
  • Viscose spinning solution according to claim 1 which contains a polyether sulphone compound having at least one ether oxygen atom for every four carbon atoms.
  • Viscose spinning solution according to claim 1 which contains a polyether sulphone compound having at least one sulphone group for every four carbon atoms.
  • Viscose spinning solution containing 0.1 to 4.0% by weight of the viscose of a polyether sulphone having an average molecular weight of from 300 to 20,000 and at least one ether oxygen and one sulphone group for every four carbon atoms in the polymer chain, said polyether sulphone being soluble at least to the extent of 0.1 weight percent in a 5 weight percent aqueous sodium hydroxide solution.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Artificial Filaments (AREA)
US232892A 1961-11-02 1962-10-24 Viscose spinning solution for the manufacture of shaped articles from regenerated cellulose Expired - Lifetime US3222198A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEF35263A DE1222201B (de) 1961-11-02 1961-11-02 Herstellen von Faeden durch Verspinnen von Viskose, die einen Polyaether enthaelt

Publications (1)

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US3222198A true US3222198A (en) 1965-12-07

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US232892A Expired - Lifetime US3222198A (en) 1961-11-02 1962-10-24 Viscose spinning solution for the manufacture of shaped articles from regenerated cellulose

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US (1) US3222198A (en))
BE (1) BE624260A (en))
CH (1) CH429014A (en))
DE (1) DE1222201B (en))
NL (1) NL284979A (en))

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2288106A (en) * 1938-08-06 1942-06-30 North American Rayon Corp Viscose spinning solution
US2864866A (en) * 1956-12-28 1958-12-16 Phillips Petroleum Co Process for preparing surface-active materials
US3116353A (en) * 1957-05-02 1963-12-31 Beaunit Corp Spinning viscose

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2288106A (en) * 1938-08-06 1942-06-30 North American Rayon Corp Viscose spinning solution
US2864866A (en) * 1956-12-28 1958-12-16 Phillips Petroleum Co Process for preparing surface-active materials
US3116353A (en) * 1957-05-02 1963-12-31 Beaunit Corp Spinning viscose

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Publication number Publication date
CH429014A (de) 1967-01-31
DE1222201B (de) 1966-08-04
BE624260A (en))
NL284979A (en))

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