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US1820811A - Artificial material and process for making same - Google Patents

Artificial material and process for making same Download PDF

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Publication number
US1820811A
US1820811A US113582A US11358226A US1820811A US 1820811 A US1820811 A US 1820811A US 113582 A US113582 A US 113582A US 11358226 A US11358226 A US 11358226A US 1820811 A US1820811 A US 1820811A
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viscose
sulphuric acid
weight
parts
per cent
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US113582A
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Lilienfeld Leon
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Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F02—COMBUSTION ENGINES; HOT-GAS OR COMBUSTION-PRODUCT ENGINE PLANTS
    • F02M—SUPPLYING COMBUSTION ENGINES IN GENERAL WITH COMBUSTIBLE MIXTURES OR CONSTITUENTS THEREOF
    • F02M21/00—Apparatus for supplying engines with non-liquid fuels, e.g. gaseous fuels stored in liquid form
    • 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
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
    • D06M11/11—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
    • D06M11/11—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
    • D06M11/22—Halides of elements of Groups 5 or 15 of the Periodic Table
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
    • D06M11/40—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table combined with, or in absence of, mechanical tension, e.g. slack mercerising
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/51—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
    • D06M11/53—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with hydrogen sulfide or its salts; with polysulfides
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/51—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
    • D06M11/55—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with sulfur trioxide; with sulfuric acid or thiosulfuric acid or their salts
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/58—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides
    • D06M11/64—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides with nitrogen oxides; with oxyacids of nitrogen or their salts
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
    • D06M11/75—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with phosgene; with compounds containing both carbon and sulfur, e.g. thiophosgene
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F02—COMBUSTION ENGINES; HOT-GAS OR COMBUSTION-PRODUCT ENGINE PLANTS
    • F02M—SUPPLYING COMBUSTION ENGINES IN GENERAL WITH COMBUSTIBLE MIXTURES OR CONSTITUENTS THEREOF
    • F02M59/00—Pumps specially adapted for fuel-injection and not provided for in groups F02M39/00 -F02M57/00, e.g. rotary cylinder-block type of pumps
    • F02M59/20—Varying fuel delivery in quantity or timing
    • F02M59/24—Varying fuel delivery in quantity or timing with constant-length-stroke pistons having variable effective portion of stroke
    • F02M59/26—Varying fuel delivery in quantity or timing with constant-length-stroke pistons having variable effective portion of stroke caused by movements of pistons relative to their cylinders
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/04—Vegetal fibres
    • D06M2101/06—Vegetal fibres cellulosic
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/04—Vegetal fibres
    • D06M2101/06—Vegetal fibres cellulosic
    • D06M2101/08—Esters or ethers of cellulose
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F02—COMBUSTION ENGINES; HOT-GAS OR COMBUSTION-PRODUCT ENGINE PLANTS
    • F02M—SUPPLYING COMBUSTION ENGINES IN GENERAL WITH COMBUSTIBLE MIXTURES OR CONSTITUENTS THEREOF
    • F02M2700/00—Supplying, feeding or preparing air, fuel, fuel air mixtures or auxiliary fluids for a combustion engine; Use of exhaust gas; Compressors for piston engines
    • F02M2700/13—Special devices for making an explosive mixture; Fuel pumps
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F02—COMBUSTION ENGINES; HOT-GAS OR COMBUSTION-PRODUCT ENGINE PLANTS
    • F02M—SUPPLYING COMBUSTION ENGINES IN GENERAL WITH COMBUSTIBLE MIXTURES OR CONSTITUENTS THEREOF
    • F02M2700/00—Supplying, feeding or preparing air, fuel, fuel air mixtures or auxiliary fluids for a combustion engine; Use of exhaust gas; Compressors for piston engines
    • F02M2700/13—Special devices for making an explosive mixture; Fuel pumps
    • F02M2700/1317—Fuel pumpo for internal combustion engines
    • F02M2700/1388—Fuel pump with control of the piston relative to a fixed cylinder

Definitions

  • threads manufactured from viscose by means of sulphuric acid containing at least about 55 per cent. of H 50 preferably however more than 55 per cent. of H SO for example 70 to 85 per cent. of
  • artificial silkor staple fibre that has a dry tenacity of more than Qgrammes and even more-than 3 grammes per denier, for example 3 or even 3,5 to 4 grammes perdenier'and in some cases even-more than igrammes per denier and a wet tenacity of 1,5 to 2,5 grammesper denier and more.
  • a further advantage of the artificial threads manufactured according to the present processover ordinaryiviscosesilk is their higher resistance to aqueous alkalis and to soa 4 (lhnsidering that, according to the present process, sulphuric acid containing up to 90 and even 95 per cent. of H SO gives excellent results, this discovery is extremely sur- 5 prising for two reasons: First of all, with a view to the well-known fact that strong sulphuric acid, for example such containing 60 per cent.
  • H have an energetic depolymerizing action on cellulose, just the contrary was to be expected, namely that strong sulphuric acid would decompose the coagulated thread during or after coa lation and thus render it weak, brittle an litthan any viscose thread known hitherto.
  • the process is carried out in such a manner that viscose is brought into the form of an artificial material and coa lated by means of sulphuric acid, containing at least per cent, of H 50 for example sulphuric acid containing 55 to 85 per cent. of monov hydrate; Irrmost cases, for instance in manufacturing artificial threads or-filaments, or films, or hands, or plates, this can be effected in such a manner that the viscose is caused to pass through suitably formed openings into sulphuric acid, containing 55 to 98 per cent. of H 50 for instance such of to 85 per cent. strength (calculated on H or into a bath containing 55 to 98 per cent., for instance 65 to per cent. of monohydrate.
  • the strong sulphuric acid may be employed byitself or in admixture with one or more suitable inorganic substances, for example with another strong mineral acld such as hydrochloric acid, nitric acid or phosphoric acid, or with a neutral or acid salt, such as sodiumsulphate, sodium bisulphate, ammonium sulphate, magnesium sulphate, zinc sulphate, sodium bisulphite, sodium sulphite, sodium nitrite, boric acid or the like.
  • a strong mineral acld such as hydrochloric acid, nitric acid or phosphoric acid
  • a neutral or acid salt such as sodiumsulphate, sodium bisulphate, ammonium sulphate, magnesium sulphate, zinc sulphate, sodium bisulphite, sodium sulphite, sodium nitrite, boric acid or the like.
  • organic bodies such as glycerol or a sugar, for ex ample glucose, or alcohol or a salt of an organic base, for example of aniline, or an organic acid, such as acetic acid or formic acid or lactic acid or oxalic acid.
  • a salt is added which is capable of reacting with the strong sulphuric acid under formation of an acid sulphate, or which mutually interacts with the sulphuric acid, the strength of the sulphuric acidshould be so chosen that, after the amount required for the formation of the acid sulphate or for the mutual interaction is used up, the coagulating bath contains tree sulphuric acid of the desired strength, but
  • the strength'of the sulphuric acid depends, ceteris paribus, partly on the. time of maturing given the alkali cellulose, partly on the time or ripening, given the finished viscose and partly on viscosity or amount of cellulose contained in the viscose. which however the invention is not confined,
  • sulphuric acid as viscoses that have not been allowed to mature or have been allowed to mature for a 'short time (forinstance 3 to 48 hours), only and/or have been prepared frdm alkali cellulose that has been not allowed to mature at all or has been allowed to mature for a shorter time than usual, for example for 3 to 48 I .hours, and/or are rich incellulose or viscous respectively.
  • the strength of the sulphuric acid is further, to a certain degree, dependent on'the length of immersion in' the coagulating bath and the tension given the coagulated ma- As a rule, to
  • sulphuric acid or in the bath containing it' may be varied within wide-limits, for examples from 3 to 60 centimetres and even more, for instance 1 to 2 meters.
  • the thread or film or band may be stretched either immediately after its formation, i. e. in the coagulating bath containing, or consisting of, strong -sulphuric acid, or subsequently, i. e. between the coagulating bath and the collecting device, such as bobbin or centrifuge, or both in the coagulating bath and between the coagulating bath and the collecting device.
  • the collecting device such as bobbin or centrifuge
  • the thread or film or band or plate or coated or impregnated material may, after Washing, be heated or steamed before or after drying.
  • any viscose prepared according to any process or any methodknown hitherto may be used in the present process.
  • the process gives excellent results with viscoses that are prepared from alkali cellulose that has been allowed to mature for such a time as it is commonly given the alkali cellulose in the artificial silk or film art and also with viscoses in the manufacture of which alkali cellulose is employed which has been not allowed to mature at all or has been allowed to mature for a shorter time than such as is usual in the artificial silk or'film art, i. e. not Q5 longer than about 48 hours, for example 1 to 24 hours.
  • the present process gives excellent results with such viscoses also as are prepared without making alkali. cellulose, .i. e. by direct mixing the ingredients. 4
  • viscose-silk art there may beadded to the viscose one or more suitable substances known in the viscose-silk art, for example glycerol or glucose or sodium sulphate or sodium sul-' phite or sodium 'bisulphite or. ammonium sulphate or an alkali silicate Oran-alkali aluminate or ammonia.
  • the reacting mixture preferably under stirring (for example in a closed kneading inachine) or agitating (for example in a sulphidizing drum), kept for'several (for example 4 to 8) hours at 16 a 20 o. Thereafter the excess of the carbon bisulphide is removed by driving ofi' orievacuating, and then the su'lphidized mass is dissolved in water or dilute caustic soda solution in such a manner that the viscose contains about 8 to 12 per. cent.
  • the viscose is spun in a known manner into oneof the following precipitatingbaths:
  • the temperature of the coagulating bath is kept at 0 to 16 0., for instance at8 C., or at 4 to s C. 1
  • the length of immersion in the coagulating bath of the threads forming therein may be short, for example 10 centimetres or long, for instance from 30 to 100 centimetres and more. They are then collectedin a known manner on a bobbin or in a spinning centrifuge which may be placed either'by the precipitating bath or at a distance from20 to 120 centimetres from the bath, whereupon the threads are washed anddried.
  • the threads may bestretched in any known manner whilst they are in the coagulating bath, or after they have been removed-from the bath, i. e. between the coagulating bath and the collecting device. This maybe done for example either by choosing a more or less long distance between the bath and the collecting device, or by leading the threads over rods or hooks arranged in the bath or between the bath and the collecting device, or in the bath andbetween the bath and the collecting device.
  • the speed of spinning may be varied within'widelimi-ts.
  • the coagulating bath is used at a temperature below 0 C., for,example at minus 5 6., and if the length of immersion is 60 to 120, for example 80 centimetres, and if the distance between the coagulating bath and the collecting device, for example bobbin, is
  • sults are obtained with a speed'of 18 to 26 meters a minute, or of 30 meters a minute, but also a higher speed, for example of 30 to 40 meters a minute may be employed if desired.
  • a speed up to 40 to 60 meters a minute may be employed.
  • the speed may be up to 50 to 60 meters a minute.
  • the threads Before being washed, the threads may be treated in any known mannerv with a coagulating bath known in the viscose-silk art, for
  • the washed threads may, before orafter dr ing, be heated G- or steamed.
  • Example III (a) to (0) Mode ofoperation as in Example I (a) or I (b) or I (0) or as in Example II (01) or II (6) or II (0), with the exceptionthat the,
  • viscose is not allowed to mature at all or to mature for 12 to 48 hours only, and that as coagulating bath sulphuric acid of 60 to 64 B., for instance sulphuric acid of 62 B. at 6 to 10 C. is used.
  • the viscose solution thus obtained is then filtered in a known manner through cotton wool or a dense cotton fabric or through both and freed from gas bubbles if any; Immediately after, or after it has been allowed to ripen at 16-18 C. for a shorter (for example 12 hours to two days) or a longer (for example four days or seven days) time, the viscose is spun in a known manner of glucose in 190-185 parts by weight of sulphidizing o the soda-cellulose.
  • the viscose being into one of the following precipitating baths (1 Sulphuric acid of 60 B., or (2 Sulphuric acid 06 B., or (3) A solution of 13.3 partsby weight of ammonium-sulphate in 120 parts by weight of sulphuric acid of 55 to B., to which 9 to 10 parts of sulphuric acid of 66 B. have been added, or (4) A solution of 10 to 15 parts by weight phuric acid of 55 to 60 B.
  • the temperature of the coagulatlng bath is kept at 0 to 16 0., for instance at 8 C., drat 4t08 C.
  • the spinning and treating of the threads during and after spinning is done in the same manner as. described. in the foregoing ex- (b).
  • The'mode of operation is as in (a), with the difference that a caustic soda solution of 3 to5 per cent. strength is employed for the, dissolving of the sulphidized soda cellulose. Accordingly, the viscose 1s somewhat more viscous.
  • the mode of operation is as in (a.) or (b) except that 75 to 150 parts by welght of carbon bisul hide are employed for the sul- (d).
  • Themode of operation is as in (a) or (b) or (0), with the difference that the sodacellulose is pressed to 200 parts by weight.
  • the mode. of operation is as in (a) or (b) or (c) or (d), with the diflerence that sulphuric acid of 62 to 64 B. at 8 C. is
  • V (a) to' (e) The method of preparing the viscose differs from that described in IV (a) or (b) or (0) or (d) or (e) in that the soda-cellulose, after pressing and comminuting and before being sulphidized, isallowed to ripen for 3 to 24 hours at 16 to 20 C.
  • the viscose is spun .in a known manner into one of the following coagulating baths:
  • Patent 212,865 for example according to the following examples of said specification: I (a) to (s) or II (a) to (a) or II (a) to c) or IV (a) to (e) or V (a) to, b) or VI a) to (c) or VII or VIII or IX or or XII or XIII.
  • reaction mass is removed from the shredder and dissolved in 920 parts by weight of a caustic 'soda solution of 6,15 per cent, strength, the weight of the sulphidized mass being 330 parts.
  • the final viscose contains 8 per cent. of starting cellulose.
  • a viscose prepared as described in Example I or II or III or IV or V or VI or VII is caused to pass through a suitable hopper or slit in one of the coagulating liquors mentioned in these examples, and after having left the precipitating bath, is washed and dried in any known manner.
  • a cotton fabric is impregnated or filled or coated once or several times .with a viscose prepared according to one ofthe methods described in Example I or II or III or IV or V or VI .or VII, for which purpose any suitable machine, such as a padding machine or a back fillin'g'machine or a spreading machine may be emplo ed.
  • a lling substance for instance talcum or china clay or a colouring matter or a pigment such. as mica, or soot or a mineral colour or the like; or coated material is, without beingdried,
  • nitric acid for example such as contains 6.0
  • sulphuric acid for example of 1,5 to 1,86 specific gravity, or arsenic acid, for example such as contains
  • arsenic acid for example such as contains
  • bleached cotton or cellulose
  • strong sulphuric acid or sulphuric acid containing at least 55 per cent. of sulphuric acid monohydrate means in the description and claims: sulphuric acid of 55 to 98 or 100- per cent. strength.
  • heating in the claims is intended to cover anyknown kind of heating, steaming included.
  • Iclaimr 1 Process for manufacturing artificial materials from vlscose, which comprises bringing a viscose, prepared from an alkali cellulose which has been allowed to mature only from naught to 48 hours, into the form of an artificial material and acting upon it with sulphuric acid containing at least 55 per cent. of sulphuric acid monohydrate.
  • the rocess for manufacturing artificial suitably, formed opening into a bath which contains a mineral acid present in an amount equivalent to at least 55 per cent. sulphuric acid monohydrate.
  • v 7. The process for manufacturing artificial thread of high dry tenacity which comprises causing a viscose, prepared from alkali cellulose which has been allowed to mature only from naught to 48 hours, to pass through a suitably formed opening, thereafter contacting it with a liquid which contains a strong mineral acid present in an amount equivalent to at least per cent. sulphuric acid monohydrate and washing the thread.
  • Process for manufacturing artificial materials from viscose which comprises bringing a viscose, prepared from an alkali cellulose which has been allowed to mature only from naught to 48 hours, into tlge form of an artificial material and acting upon it with a bath which" has a coagulating action on said viscose and a plasticizing action on the coagulated product.
  • Process for manufacturing artificia materials from viscose which comprises causing a viscose, prepared from an alkali cellulose which has been allowed to mature only from naught to 48 hours, to pass through suitably formed openings into a bath of concentrated acid coagulating agent which bath has a plastici'zing action thereupon.
  • threads 0 high dry tenacity which comprises causing a viscose, prepared from alkali cellulose which has been allowed to mature only from naughtto 48 hours, to pass through a

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Combustion & Propulsion (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Artificial Filaments (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)

Description

Patented: Aug. 25,. 1931 PATENT OFFICE I LEON murmur, or vmmu, nus'rum ARTIFICIAL MATERIAL AND PROCESS FOR MAKING em Nolli'awing. Application filed. June 3, 1926, serial- No. 113,582, and in Austria June 20, 1925.
Heretofore strong sulphuric acid has not been used as coagulating bath in the manufacture of artificial materials, such as artificial threads and films from viscose, because, by
; means of. such acid, the formation of a lustrons thread, band, film or the like has been impossible. (See U. S. Patent 836,452.)
Now I have discovered that this holds good with sulphuric acid containing up to about 55. per cent. of H 30 but that sulphuric acid containing about 55 per cent. of H SO,, and preferably sulphuric acid containing more than 55 per cent.,for example 65 to 86 per cent. of H 80 when used as coagulating bath for viscose brought into the form of a thread or film or band or the like, yields threads, films, bands or the like which have a good lustre.
But what is still more important: I have discovered that threads, manufactured from viscose by means of sulphuric acid containing at least about 55 per cent. of H 50 preferably however more than 55 per cent. of H SO for example 70 to 85 per cent. of
H SO with regard to their tensile strength,
surpassany artificial thread known'hitherto and in some cases approach, in some cases equal, and in some cases even surpass even natural fibres, such as cotton or wool or real silk. For example, it ofiers no difiiculty to produce according to the present process, artificial silkor staple fibre that has a dry tenacity of more than Qgrammes and even more-than 3 grammes per denier, for example 3 or even 3,5 to 4 grammes perdenier'and in some cases even-more than igrammes per denier and a wet tenacity of 1,5 to 2,5 grammesper denier and more.
A further advantage of the artificial threads manufactured according to the present processover ordinaryiviscosesilk is their higher resistance to aqueous alkalis and to soa 4 (lhnsidering that, according to the present process, sulphuric acid containing up to 90 and even 95 per cent. of H SO gives excellent results, this discovery is extremely sur- 5 prising for two reasons: First of all, with a view to the well-known fact that strong sulphuric acid, for example such containing 60 per cent. or more of H have an energetic depolymerizing action on cellulose, just the contrary was to be expected, namely that strong sulphuric acid would decompose the coagulated thread during or after coa lation and thus render it weak, brittle an litthan any viscose thread known hitherto.
The second reason why the present invention is surprising is the lustre of the threads,
bands or films, considering that, up to now, it has been believed, that the want of lustre in the threads made by means of somewhat stronger acid had been caused by the fact that not enough water had been present in the coa' lating bath to dissolve the gaseous by-pro acts.
I have further found that it is advantageous to the tensile strength of the artificial materials, particularly threads, manufactured according to the present process, to stretch the threads either in the coagulating bath or between the coagulating bath and the collecting device or in both places.
The process is carried out in such a manner that viscose is brought into the form of an artificial material and coa lated by means of sulphuric acid, containing at least per cent, of H 50 for example sulphuric acid containing 55 to 85 per cent. of monov hydrate; Irrmost cases, for instance in manufacturing artificial threads or-filaments, or films, or hands, or plates, this can be effected in such a manner that the viscose is caused to pass through suitably formed openings into sulphuric acid, containing 55 to 98 per cent. of H 50 for instance such of to 85 per cent. strength (calculated on H or into a bath containing 55 to 98 per cent., for instance 65 to per cent. of monohydrate. The strong sulphuric acid may be employed byitself or in admixture with one or more suitable inorganic substances, for example with another strong mineral acld such as hydrochloric acid, nitric acid or phosphoric acid, or with a neutral or acid salt, such as sodiumsulphate, sodium bisulphate, ammonium sulphate, magnesium sulphate, zinc sulphate, sodium bisulphite, sodium sulphite, sodium nitrite, boric acid or the like. To the strong sulphuric acid or its niixture'with another strong. acid or with one or more of the inorganic substances mentioned above, there may be added one or more organic bodies, such as glycerol or a sugar, for ex ample glucose, or alcohol or a salt of an organic base, for example of aniline, or an organic acid, such as acetic acid or formic acid or lactic acid or oxalic acid. It a salt is added which is capable of reacting with the strong sulphuric acid under formation of an acid sulphate, or which mutually interacts with the sulphuric acid, the strength of the sulphuric acidshould be so chosen that, after the amount required for the formation of the acid sulphate or for the mutual interaction is used up, the coagulating bath contains tree sulphuric acid of the desired strength, but
at any rate not less than 55 parts-by weight of'monohydrate in parts by weight of the precipitating bath.
The strength'of the sulphuric acid depends, ceteris paribus, partly on the. time of maturing given the alkali cellulose, partly on the time or ripening, given the finished viscose and partly on viscosity or amount of cellulose contained in the viscose. which however the invention is not confined,
it may be stated that viscoses which have ma-,
tured for several days and/or viscoses that have been prepared from alkali cellulose that has been allowed to mature for a longer time, for example 2 to 3 days and/or viscoses that are poor incellulose or little viscous respectively, do not support so strong a sulphuric acid as viscoses that have not been allowed to mature or have been allowed to mature for a 'short time (forinstance 3 to 48 hours), only and/or have been prepared frdm alkali cellulose that has been not allowed to mature at all or has been allowed to mature for a shorter time than usual, for example for 3 to 48 I .hours, and/or are rich incellulose or viscous respectively. The strength of the sulphuric acid is further, to a certain degree, dependent on'the length of immersion in' the coagulating bath and the tension given the coagulated ma- As a rule, to
eaaerr.
sulphuric acid or in the bath containing it' may be varied within wide-limits, for examples from 3 to 60 centimetres and even more, for instance 1 to 2 meters.
If desired the thread or film or band may be stretched either immediately after its formation, i. e. in the coagulating bath containing, or consisting of, strong -sulphuric acid, or subsequently, i. e. between the coagulating bath and the collecting device, such as bobbin or centrifuge, or both in the coagulating bath and between the coagulating bath and the collecting device. I
The thread or film or band or plate or coated or impregnated material may, after Washing, be heated or steamed before or after drying.
Any viscose prepared according to any process or any methodknown hitherto may be used in the present process. The process gives excellent results with viscoses that are prepared from alkali cellulose that has been allowed to mature for such a time as it is commonly given the alkali cellulose in the artificial silk or film art and also with viscoses in the manufacture of which alkali cellulose is employed which has been not allowed to mature at all or has been allowed to mature for a shorter time than such as is usual in the artificial silk or'film art, i. e. not Q5 longer than about 48 hours, for example 1 to 24 hours.
The present process gives excellent results with such viscoses also as are prepared without making alkali. cellulose, .i. e. by direct mixing the ingredients. 4
If desired, there may beadded to the viscose one or more suitable substances known in the viscose-silk art, for example glycerol or glucose or sodium sulphate or sodium sul-' phite or sodium 'bisulphite or. ammonium sulphate or an alkali silicate Oran-alkali aluminate or ammonia.-
The processv eing open-to manifold vari ations', it is not intended to confine the invention to the following examples given for the practical carrying out of the process.
iat
parts by weight of a caustic soda solution of 18 per cent. strength at 15 to 18 C., and the mixture allowed to stand for 3 to 24 hours. Then the mass is pressed to '300.t o 400 parts by weight, and the residue comminuted by hand or in a suitable apparatus, for instancein a cooled shredder. The comminuted soda cellulose is then kept for 60 to 72 hours at room temperature, whereafter 30 to .60 parts by weight of carbon bisulphide are added, and
the reacting mixture, preferably under stirring (for example in a closed kneading inachine) or agitating (for example in a sulphidizing drum), kept for'several (for example 4 to 8) hours at 16 a 20 o. Thereafter the excess of the carbon bisulphide is removed by driving ofi' orievacuating, and then the su'lphidized mass is dissolved in water or dilute caustic soda solution in such a manner that the viscose contains about 8 to 12 per. cent.
of cellulose (determined in the known manner by precipitating with'acid, washing and or through both and freed from gas bubbles if any. Immediately after, or after it has been allowed to ripen at 1618 C. for a' shorter (for example 12 hours to two days) or a longer (for example four days to seven days) time, the viscose is spun in a known manner into oneof the following precipitatingbaths:
( l) Sulphuric acid of 50 to 55 B., or
(2) Sulphuric acid of to B., or
(3) A solution of,13,3 parts by weight of ammonium sulphate in 120 parts by weight of sulphuric acid of 50 to B., to which 7 to 9 parts of sulphuric acid of 66 B. have been added, or a (4) A solution "of 10 to 15 parts by weight of glucose in 190-185 parts by weight of S111- phuric acid of 45 to 55 B.
The temperature of the coagulating bath is kept at 0 to 16 0., for instance at8 C., or at 4 to s C. 1
The length of immersion in the coagulating bath of the threads forming therein may be short, for example 10 centimetres or long, for instance from 30 to 100 centimetres and more. They are then collectedin a known manner on a bobbin or in a spinning centrifuge which may be placed either'by the precipitating bath or at a distance from20 to 120 centimetres from the bath, whereupon the threads are washed anddried.
The threads may bestretched in any known manner whilst they are in the coagulating bath, or after they have been removed-from the bath, i. e. between the coagulating bath and the collecting device. This maybe done for example either by choosing a more or less long distance between the bath and the collecting device, or by leading the threads over rods or hooks arranged in the bath or between the bath and the collecting device, or in the bath andbetween the bath and the collecting device. The speed of spinning may be varied within'widelimi-ts. As a'rule to which, however, the invention is not intended to be confined, it may be assumed thatthe upper limit of speed possible Is dependent partly upon the temperature oi the coagulatingv bath, partly upon the length of immersion, partly upon the distance between the coagulating bath and the collecting device, partly u on the degree of stretching given the threa during spinning, and partly upon the quantity of viscose delivered by the pump. The followingexamples to which, however, the process is not intended to be limited, may be adduced for the purpose of illustration.
(1) If. the coagulating bath is used at a temperature below 0 C., for,example at minus 5 6., and if the length of immersion is 60 to 120, for example 80 centimetres, and if the distance between the coagulating bath and the collecting device, for example bobbin, is
'60 to 150 centimetres, for instance 120 centimetres, and if the stretching given the thread between the coagulating bath and the collecting device is comparatively high, and if the pum' delivers about 2 to '3 cubic centimetres 0 viscose a minute, then excellent re-.
sults are obtained with a speed'of 18 to 26 meters a minute, or of 30 meters a minute, but also a higher speed, for example of 30 to 40 meters a minute may be employed if desired.
(2) If all spining conditions remain the same as in (l) except that the pump delivers 4 to 5 cubic centimetres ofviscose a minute,
then if desired a speed up to 40 to 60 meters a minute may be employed.
(3) If the spinning conditions are exactly -as 1n (1) except that the temperature ofthe coagulating bath is plus 4 to plus 25 (1.,
for example 8 (3., if desired the speed may be up to 50 to 60 meters a minute.
It in ('1) the length of immersion or the distance between the coagulating bath and the collecting device or bothare shortened, .it is recommendable not to use too low a speed.
Before being washed, the threads may be treated in any known mannerv witha coagulating bath known in the viscose-silk art, for
example a solution of sodium bisulphate or sodium bisulphite or with dilute sulphuric acid or the like.
1 The washed threads may, before orafter dr ing, be heated G- or steamed.
They may also be treatedwith any des'ulphurating' or bleaching agent known in the viscose art.
(for example at 100110 or (b) with the difierence that the soda-cellulcse is pressed to 200 parts by weight.
I l (a) to (0) Mode of operation as in Example vI (a) or I (b) or I (0), with the difi'erence (1) that the sulphidized mass is dissolved (b). The mode of operation is as in (a), I
in water or dilute caustlc soda solution so as to yield a viscose that contains 5 to 8 per cent. of cellulose, for instance, 6 to 7 per 66 B. have been added, or
(4) A solution of 10 to parts by weight of glucose in 190 to 185 parts by weight ofamples.
sulphuric acid of 55 to 60 B.
III (a) to (0) Mode ofoperation as in Example I (a) or I (b) or I (0) or as in Example II (01) or II (6) or II (0), with the exceptionthat the,
viscose is not allowed to mature at all or to mature for 12 to 48 hours only, and that as coagulating bath sulphuric acid of 60 to 64 B., for instance sulphuric acid of 62 B. at 6 to 10 C. is used.
In using so strong an acid it is preferable to run the spinning at a high spee for example to 60 meters a minute.
I V (a) to (e) (a). 100 parts by weight ofsulphite-pulp or linters are impregnated with 900 to 2000 parts by weight of a caustic soda solution of 18 per cent. strength at 15 to 18 (1., and the mixture allowed to stand for 3 to 24 hours.
Then the mass is. pressed to 300 parts by" weight, and the residue comminuted by hand orin a suitable apparatus, .for instance ina cooled shredder. Immediately or soon (for.
example 1 hour) after the comminution has taken place, 30 to 60 parts by weight of carbon bisulphide are added, and the reacting mixture, preferably under stirring (for example in a closed kneading machine) or agitating (for example in a sulphidizing drum), kept for several (for example 4 to 12) hours vat 16 to 20 C. Thereafter the excess ofthe carbon bisulphide is removed by driving 011' or evacuating, and the sulphidized mass, the' I weight of which generally amounts to from about 330 to 400 parts by; weight, is dis-' solved in 650 to 900 parts by weight of a caustic soda solution of 6.5 to 10 per cent. strength. The viscose solution thus obtained is then filtered in a known manner through cotton wool or a dense cotton fabric or through both and freed from gas bubbles if any; Immediately after, or after it has been allowed to ripen at 16-18 C. for a shorter (for example 12 hours to two days) or a longer (for example four days or seven days) time, the viscose is spun in a known manner of glucose in 190-185 parts by weight of sulphidizing o the soda-cellulose.
.used as coagulating bath, the viscose being into one of the following precipitating baths (1 Sulphuric acid of 60 B., or (2 Sulphuric acid 06 B., or (3) A solution of 13.3 partsby weight of ammonium-sulphate in 120 parts by weight of sulphuric acid of 55 to B., to which 9 to 10 parts of sulphuric acid of 66 B. have been added, or (4) A solution of 10 to 15 parts by weight phuric acid of 55 to 60 B. The temperature of the coagulatlng bath is kept at 0 to 16 0., for instance at 8 C., drat 4t08 C.
The spinning and treating of the threads during and after spinning is done in the same manner as. described. in the foregoing ex- (b). The'mode of operation is as in (a), with the difference that a caustic soda solution of 3 to5 per cent. strength is employed for the, dissolving of the sulphidized soda cellulose. Accordingly, the viscose 1s somewhat more viscous. (c) The mode of operation is as in (a.) or (b) except that 75 to 150 parts by welght of carbon bisul hide are employed for the sul- (d). Themode of operation is as in (a) or (b) or (0), with the difference that the sodacellulose is pressed to 200 parts by weight.
(e) The mode. of operation is as in (a) or (b) or (c) or (d), with the diflerence that sulphuric acid of 62 to 64 B. at 8 C. is
12 to 48 hours'old and the speed of spinning .100 about 45 to 60 meters a minute. g
V (a) to' (e) The method of preparing the viscose differs from that described in IV (a) or (b) or (0) or (d) or (e) in that the soda-cellulose, after pressing and comminuting and before being sulphidized, isallowed to ripen for 3 to 24 hours at 16 to 20 C. The amount and concentration of the caustic soda solution used forthe dissolving of the sulphidlzed mass-maybe equal to those used in Example IV or somewhat lower, for example so as to produce a 10 to 12 per cent viscose (calculated on starting cellulose).
The workingup into threads is efi'ected as IV (a) to (e).
VI (a) to (d) (a). -100 partsby weight of finely-'di- -vided sulphite-pulp or bleached cotton are mixed with 920-900 parts by weight of a caustic soda solution of 8 to 10 per cent. strength. To this mixture 40 to 150 parts by weight of carbon bisulphide are added and the reacting mixture kept at room temperature for 12 to 72 hours, preferably under continual or temporary stirring or kneading. The viscose solution thus obtained is then in filtered in a known manner through cotton wool or a dense cotton fabric or through both and freed from as bubbles if any. Im-.
mediately after, or a ter it has been allowed to ripen at 16-18 G. for a shorter (for example 12 hours to two days) or a longer (for example four to seven days) time, the viscose is spun .in a known manner into one of the following coagulating baths:
1; -Sulphuric acid of 55 to 60 B., or 2 Sulphuric acid of 45m 50 B., or (3) A solution of 13,3 parts by weight of ammonium sulphate in 120 parts by weight of sulphuric acid of 45 to 60 B., to which 7 to 9 parts of sulphuric acid of 66 Be, have.
been added, or
Patent 212,865, for example according to the following examples of said specification: I (a) to (s) or II (a) to (a) or II (a) to c) or IV (a) to (e) or V (a) to, b) or VI a) to (c) or VII or VIII or IX or or XII or XIII. v I v Mode of operation as in (a) or (b), with the exception that, before or after the addition of carbon bisulphide takes lace, a small quantity of a catalyzer is adde to the mixture of the cellulosic body with the caustic alkali solution, for example 0,2 to 1 parts by weight of a soluble chromicsalt or nickel .salt or iron salt; 1
((1) Mode of operation as in (a) or with the diflerence that, before or after the addition of carbon bisulphide takes place, a small quantity of a soluble peroxyde, such as 5 to parts by weight of sodium peroxyde to 100 parts by'weight of starting celluloseare added. 7 i V! I 100 parts by weight of sulphite-pulp are placed in a cooled shredder admitting of bemg hermetically'closed, whereu on 200 parts by weight of a caustic soda solutlon of 12 to 20 per cent. strength are added, preferably in small portions. As soon-as the mass is homogeneous, 40 to parts by weight of carbon bisulphide are added, whereupon the shredder is closed. After 4 to 8 hoursthe reaction mass is removed from the shredder and dissolved in 920 parts by weight of a caustic 'soda solution of 6,15 per cent, strength, the weight of the sulphidized mass being 330 parts. The final viscose contains 8 per cent. of starting cellulose.
The filtering and spinning of this viscose and the treatment of'the threads is doneas in the foregoing examples.
Examples for producing staple fibre follow automatically from the foregoing examples. f
According to the foregoing examples, it is possible to obtain artificial silk or staple fibre which has a considerably higher dry and wet tenacity than silk spun under same spinning conditions, but by means of chemicals customary in the viscose silk-art, for example by using a known precipitating bath. For example: it is not difiicult to produce after the present process artificial silk having a dry tenacity of more than 2 grammes per denier,
1 even more than 3 grammes per denier, for example 3 grammes to 4 grammes per denier and a wet tenacity of 1,5 to 2,5 grammes per denier and more.
' VIII A viscose prepared as described in Example I or II or III or IV or V or VI or VII is caused to pass through a suitable hopper or slit in one of the coagulating liquors mentioned in these examples, and after having left the precipitating bath, is washed and dried in any known manner.
A cotton fabric is impregnated or filled or coated once or several times .with a viscose prepared according to one ofthe methods described in Example I or II or III or IV or V or VI .or VII, for which purpose any suitable machine, such as a padding machine or a back fillin'g'machine or a spreading machine may be emplo ed. To the viscose there may be added a lling substance, for instance talcum or china clay or a colouring matter or a pigment such. as mica, or soot or a mineral colour or the like; or coated material is, without beingdried,
through one of the precipitating baths described in Example whereupon the material'is washed and dried. v
' Instead of strong sulphuric acid there may be used in the foregoing examples a strong halogen hydracid, such as hydrochloric acid,
' for example of 25 to 40 per cent. strength, or
nitric acid, for example such as contains 6.0
from 60 to per cent. of H AsO In the foregoing examples, in the preparation of viscose, instead of wood pulp, there treated in the cold or in the heat with dilute acids, for example hydrochloric or sulphuric acid, in short any'kind of cellulosic bodies employed in, or proposed for the manufacture of viscose.
The impregnated 'optionally in the stretched state,- taken 'to'90 per cent. of I-INOg, or phosphoric acid,
for example of 1,5 to 1,86 specific gravity, or arsenic acid, for example such as contains" may be used bleached cotton, or cellulose The expression strong sulphuric acid or sulphuric acid containing at least 55 per cent. of sulphuric acid monohydrate means in the description and claims: sulphuric acid of 55 to 98 or 100- per cent. strength.
The expression: artificial material in the description and claims is intended to mean:
artificial threads and filaments of any kind,
. for example artificial silk, staple fibre, artificialcotton, artificial wool, artificial hair, films, plates, coatings and fillings of any kind.
The expression heating in the claims is intended to cover anyknown kind of heating, steaming included.
The statements in the description and claims regardingpercentages relate to percentages by Weight.
Iclaimr 1. Process for manufacturing artificial materials from vlscose, which comprises bringing a viscose, prepared from an alkali cellulose which has been allowed to mature only from naught to 48 hours, into the form of an artificial material and acting upon it with sulphuric acid containing at least 55 per cent. of sulphuric acid monohydrate.
2. Process for manufacturing artificial materials from viscose, which comprises calls-- ing a viscose, prepared from an alkali cellulose which has been allowed to mature only from naught to 48 hours, to pass through suitably formed openings into a coagulating bath whlch contains at least 55 per cent. of sulphuric acid monohydrate. I
. '3. Process for manufacturing artificial ma-- terials fromviscose, which comprises causing a viscose, prepared from an alkali cellulosewhich has been allowed to mature only from naught to 48 hours, 'to pass through suitably formed openings into acoagulating bath containing at least 55 per cent. of sulphuric acid monohydrate and keeping the bath at a temperature below room temperature.
4. The process .for manufacturing artificial stron mineral acid of a strength equivalent to at east 55 per cent sulphuric acid monohydrate.
6. The rocess for manufacturing artificial suitably, formed opening into a bath which contains a mineral acid present in an amount equivalent to at least 55 per cent. sulphuric acid monohydrate. v 7. The process for manufacturing artificial thread of high dry tenacity which comprises causing a viscose, prepared from alkali cellulose which has been allowed to mature only from naught to 48 hours, to pass through a suitably formed opening, thereafter contacting it with a liquid which contains a strong mineral acid present in an amount equivalent to at least per cent. sulphuric acid monohydrate and washing the thread.
- 8. The process for manufacturing artificial thread of high dry tenacity which comprises causing a viscose, prepared from alkali cellulose which has been allowed to mature only from naught to 48 hours, to pass through a suitably formed opening, thereafter acting upon it with sulphuric acid containing at least per cent. sulphuric acid'monohydrate and Washing the thread. 5
9. Process for manufacturing artificial materials from viscose, which comprises bringing a viscose, prepared from an alkali cellulose which has been allowed to mature only from naught to 48 hours, into tlge form of an artificial material and acting upon it with a bath which" has a coagulating action on said viscose and a plasticizing action on the coagulated product.
10. Process for manufacturing artificia materials from viscose, which comprises causing a viscose, prepared from an alkali cellulose which has been allowed to mature only from naught to 48 hours, to pass through suitably formed openings into a bath of concentrated acid coagulating agent which bath has a plastici'zing action thereupon.
In testimon whereof I aflix m sigjnature.
R. LEON LILIE F LD.
threads 0 high dry tenacity which comprises causing a viscose, prepared from alkali cellulose which has been allowed to mature only from naughtto 48 hours, to pass through a
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US2536094A (en) * 1949-09-17 1951-01-02 American Viscose Corp Process for spinning artificial fibers
GB709629A (en) * 1950-08-11 1954-06-02 Textile & Chem Res Co Ltd Improvements in or relating to the production of artificial filaments and similar products from cellulose xanthogenates
BE510207A (en) * 1951-04-25
US2935372A (en) * 1955-02-21 1960-05-03 Du Pont Process of producing shaped bodies by combining reactive intermediates, at least one of which intermediates is in the vapor phase
US3084020A (en) * 1956-05-30 1963-04-02 Rene Ruegg Method of treating knitted superpoly-amide textile fabric with an aqueous phenol bath subjected to ultra-sonic waves and fabric produced thereby
US2946650A (en) * 1958-02-17 1960-07-26 Tatsuji Tachikawa Process for the manufacture of viscose rayon staple
US3511591A (en) * 1965-04-09 1970-05-12 Deering Milliken Res Corp Process and product of rendering cellulosic fabrics amenable to molding operations
US3689613A (en) * 1970-11-02 1972-09-05 Anselm Talalay Glove making
FR2175582B1 (en) * 1972-03-14 1974-08-02 Omnium De Prospective Ind Sa
US4196559A (en) * 1973-03-28 1980-04-08 Ljungbo Sven O B Swellable fabrics for ceiling structures
FR2377462A2 (en) * 1977-01-13 1978-08-11 Centre Tech Ind Papier Viscose fibre prepn. - by spinning, coagulating in a volatile gas, partially regenerating and then completely regenerating
DE2720087A1 (en) * 1976-05-07 1977-11-24 Centre Tech Ind Papier PROCESS FOR MANUFACTURING VISCOSE FEMES AND FEMES PRODUCED BY THE PROCESS
FR2372251A1 (en) * 1976-11-26 1978-06-23 Rhone Poulenc Textile NEW PROCESS FOR SPINNING OR SHAPING CELLULOSE SOLUTIONS AND ARTICLES THUS OBTAINED
JPS6027496B2 (en) * 1977-10-19 1985-06-29 南国パルプ工業株式会社 Manufacturing method of cellophane for casing
US5849818A (en) * 1993-06-03 1998-12-15 Walles; Wilhelm E. Skin sulfonated particles in matrices
AT506268B1 (en) 2008-01-11 2014-08-15 Chemiefaser Lenzing Ag MICROFIBRE

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2536093A (en) * 1947-05-28 1951-01-02 American Viscose Corp Method for spinning artificial filaments

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GB281352A (en) 1927-11-30
NL26633C (en)
FR35551E (en) 1930-03-26
GB274690A (en) 1927-07-11
DE542713C (en) 1932-01-27
GB317608A (en) 1929-08-22
FR35751E (en) 1930-03-27
US1989099A (en) 1935-01-29
FR37344E (en) 1930-11-15
US1881742A (en) 1932-10-11
GB319293A (en) 1929-09-11
GB264161A (en) 1928-07-05
DE643543C (en) 1937-04-10
US1989098A (en) 1935-01-29
NL23113C (en)
US2112499A (en) 1938-03-29
GB298548A (en) 1928-10-08
US1683199A (en) 1928-09-04
NL21442C (en)
BE361387A (en)
USRE18170E (en) 1931-08-25
BE334767A (en)
DE593833C (en) 1934-03-07
FR666178A (en) 1929-09-27
GB281351A (en) 1927-11-29
BE342830A (en)
FR37021E (en) 1930-10-08
US1683200A (en) 1928-09-04
GB321679A (en) 1929-11-11
NL23112C (en)
NL23093C (en)
GB274521A (en) 1927-07-11
FR35752E (en) 1930-03-27
NL21473C (en)

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