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US1989098A - Manufacture of artificial threads - Google Patents

Manufacture of artificial threads Download PDF

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Publication number
US1989098A
US1989098A US186575A US18657527A US1989098A US 1989098 A US1989098 A US 1989098A US 186575 A US186575 A US 186575A US 18657527 A US18657527 A US 18657527A US 1989098 A US1989098 A US 1989098A
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Prior art keywords
threads
solution
per cent
shrinking
artificial
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US186575A
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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

  • This invention is a method for eflecting an improvement in or modification of the products described in the aforesaid patents.
  • This result may be attained according to the invention by treating the artificial threads with an agent adapted to cause the threads to shrink, under conditions which permit shrinkage of the thread to occur.
  • mercerizing agents have proved particularly suitable, especially basic mercerizing agents and among them such compounds of alkali metals as contain at least one element of the oxygen group.
  • solutions of alkali hydroxides and more particularly solutions of alkali hydroxides containing not less than 15, preferably not less than 18 per cent. of alkali hydroxide (calculated as NaOH).
  • Useful results are, however, obtained with other mercerizing agents also, for instance, with a strong solution of an alkali sulphide (e. g. a solution of sodium sulphide of at least 15, for example 30 to 58 per cent.
  • the artificial threads may be treated in various ways with the shrinking agent. For example, they may be immersed in, or impregnated with a solution of the agent, or passed through the solution, or passed over rollers which are in contact with the solution; or they may be sprayed with an atomized solution of the agent, or treated with a solution of the agent in a foulard, or by calendering, or coating; in short, by any known method of application, impregnation,.,immerslon or coating.
  • the invention is applicable not only to the treatment of artificial threads as such (e. g. artificial silk), in the form of spun threads, yarn in hanks or cops or in the form of warp or twisted yarn or the like, but also to artificial threads (e. g. artificial silk or staple fibre) in the form of woven fabrics. It is also applicable to threads or fabrics consisting wholly of artificial fibre (e. g. artificial silk, artificial wool, or staple fibre), and to mixed threads or fabrics, that is, to fibres or fabrics eontainingin addition to the artificial threads another fibrous material, for instance natural cotton, silk, wool or the like.
  • the ex pression artificial threads" throughout the application is intended to include, wherever the context permits, artificial threads such as artificial silk, cotton, wool, hair, and so on, in any of the forms hereinbefore mentioned.
  • the success of the process depends upon the fact that the artificial threads, or the-materials consisting of, or containing them, are treated with the shrinking agent in such a manner that the shrinkage remains either at its full extent, this extent depending on the nature and concentration of the shrinkage agent vused, or that at least a part of the shrinkage remains. That is to say, either the material under treatment may be subjected to no tension during or after the treatment or, if tension is applied, it must be subsequently discontinued or reduced.
  • the treatment'according to the invention may be combined into a single operation with a treatment for desulphurizing the threads.
  • a suitable quantity of the shrinking agent such as alkali hydroxide, may be added to the desulphurizing bath. If, however, the desulphurizing bath is a strong solution of an alkali sulphide, it may be unnecessary to add a further shrinking agent.
  • a caustic alkali solution there may be added a suitable quantity of a neutral or alkaline salt, such as sodium chloride or sodium sulphate or sodium silicate or sodium aluminate or sodium zincate or borax or a sodium phosphate or sodium acetate or a monoor polyvalent alcohol, such as ethyl alcohol or glycerine.
  • a neutral or alkaline salt such as sodium chloride or sodium sulphate or sodium silicate or sodium aluminate or sodium zincate or borax or a sodium phosphate or sodium acetate or a monoor polyvalent alcohol, such as ethyl alcohol or glycerine.
  • this invention it is possible to increase the extensibility of the artificial threads by -200 per cent. or more, so that threads of even very low extensibility can be improved so as to attain an extensibility of at least 8 per cent.
  • the present process has, in most cases, a favorable, i. e. increasing effect on the elasticity oi the threads also.
  • Viscose silk made according to the process described in U. S. Patent No. 1,683,199 is introduced, in the finished, dried, but preferably unbleached state, in the form of hanks, without stretching; into' a caustic soda solution of 18-25 per cent. strength at a temperature'ot 15-18 C.
  • the mode of operation is as in Example 1, except that a mixture of 1500 parts of a caustic soda solution of 22.5 per cent. strength with 150 parts of water-glass of 39 Baum is employed as shrinking agent.
  • Example 5 The procedure is as in Example 1, with the exception that a 20 per cent. caustic soda solution containing 8-10 per cent. of glycerine is used as shrinking agent.
  • the mode of operation is as in Example 1, with the diil'erence that a solution of 270 parts of caustic soda and 450 parts of sodium sulphide in 1050 parts of water is employed as shrinking agent.
  • Example 2 The procedure is as in Example 1, with the diiference that a sodium sulphide solution of -58 per cent. strength is used as shrinking agent.
  • the mode of operation is as in Example 1, with the difference that an 18-22 per cent, solution of caustic soda containing 8-10 per cent. of sodium sulphide is used as shrinking agent.
  • the hank is, optionally after being washed with water, introduced for about 5 minutes into sulphuric acid of 5-10 per cent. strength at room temperature or in a solution of ammonium sulphate of 25 per cent. strength at room temperature or at 50 C.
  • the skein is then washed, it desired, bleached and dried without stretching or under moderate tension only.
  • Example 11 The procedure is as in Example 10, with the exception that a mixture of 1500 parts of a caustic soda solution of 22.5 per cent. strength with 150 parts 01 water-glass of 39 Baum is used as shrinking medium.
  • the mode of operation is as in Example 10, except that the skein is not desulphurized, but only washed, and that a solution of 270 parts of caustic soda and 450 parts of sodium sulphide in 1050 parts of water is used as shrinking bath, which, at the same time, acts as desulphurizing agent also.
  • the mode of operation is as in Example 10, with the difierence that the skein is not desulphurized, but only washed, and that a sodium sulphide solution of 58 per cent. strength is employed as shrinking agent, which, at the same time, acts as desulphurizing agent also.
  • Example 14 The procedure is as in Example 10, with the exception that a 30-50 per cent. sodium sulphide solution containing 1-5 per cent. of caustic soda is used as shrinking agent, which, at the same time, acts as desulphurizing agent also.
  • Example 15 The procedure is as in Example 13, with the difierence that an 18-22 percent. caustic soda solution that contains 8-10 per cent. of sodium, sulphide, is used as shrinking agent.
  • the procedure is as in any of the preceding examples, with the exception that the artificial silk is stretched during a part of the process, the stretching being discontinued, or considerably reduced, towards the end of, or after the treatment with the shrinking agent.
  • a fabric consisting of, or containing viscose silk (made according to the process described in U. S. Patent No. 1,683,199, is passed through one of the shrinking baths given in the preceding examples. It is allowed to shrink during or after the treatment with the shrinking agent, and is, if desired, after removal of the excess of the shrinking medium by pressing or centrifuging and/or, if desired, after a short washing, then introduced into dilute sulphuric acid (for example of 5-10 per cent. strength), washed, and dried without stretching, or whilst stretching only moderately.
  • dilute sulphuric acid for example of 5-10 per cent. strength
  • shrinking agents may be used, for instance, instead of caustic soda solution, a solution or another alkali hydroxide,
  • caustic potash of equivalent strength or instead 01' the sodium sulphide another alkali sulphide, for instance potassium sulphide, or sulphuric acid of 47 to 50 Baum specific gravity, or hydrochloric acid of 27 to 30 per cent. strength, or nitric acid of 50 to 60 per cent. strength, or a 40 to per cent. solution of calcium thiocyanate.
  • sodium sulphide another alkali sulphide, for instance potassium sulphide, or sulphuric acid of 47 to 50 Baum specific gravity, or hydrochloric acid of 27 to 30 per cent. strength, or nitric acid of 50 to 60 per cent. strength, or a 40 to per cent. solution of calcium thiocyanate.
  • mercerizing agents means in the description and claims all chemicals known as mercerizing agents in the mercerization art.
  • oxygen group is intended to include the following elements: 0, S, Se and Te.
  • strong. mineral acid means in the description and in the claims: Sulphuric acid of at least 50 per cent. of H2804 and the other mineral acids equivalent in strength, i. e. hydrochloric acid of at least 35 per cent. strength, nitric acid of at least 60 per cent. strength, phosphoric acid of at least 1.5 specific gravity and arsenic acid of at least 75 per cent. of H3ASO4.
  • strong sulphuric acid or sulphuric acid containing at least 50 per cent, of sulphuric acid monohydrate means in the description and claims: Sulphuric acid of 50 to 98 or per cent. strength.
  • Process for increasing the extensibility of artificial threads of high dry tenacity, exceeding 2 grammes per denier, of the kind produced from viscose by means of a coagulating bath consisting of a strong mineral acid which process comprises treating the threads with at least one mercerizing reagent of a concentration capable of mercerizing cotton, and allowing permanent shrinking of the said threads to occur during said treatment.
  • Process for increasing the extensibility of artificial threads of high dry tenacity, exceeding 2 grammes per denier, of the kind produced from viscose by means of a coagulating bath consisting of a strong mineral acid which process comprises treating the threads with a liquid containing an alkali sulphide of at least 15 per cent strength (calculated as NaaS) and allowing permanent shrinking or said threads to occur during said treatment.
  • Process tor increasing the extensibility of artificial threads or high dry tenacity, exceeding 2 grammes per denier, or the kind produced from viscose by means of .a coagulating bath containing a strong mineral acid which process comprises treating the threads with a liquid containing not substantially less than 15% (figured as NaOH and NaaS) of a caustic alkali and an alkali sulphide, and allowing permanent shrinking of said threads to occur during said treatment.
  • artificial threads produced from viscose which threads in the dry state have both a tenacity exceeding 2 grammes per denier and an extensibility of at least 8 per cent, which material has been produced by treating artificial threads produced from viscose and having a dry tenacity exceeding 2 grammes per denier, with a mercerizing reagent having a shrinking action on said threads not substantially less than the shrinking action of a 15% aqueous caustic soda, and allowing permanent shrinkage of the said threads to occur during said treatment.
  • the process of increasing the extensibility of regenerated cellulose threads having a dry tenacity exceeding 2 grammes per denier produced from viscose by means of a setting bath consisting of a strong mineral acid which comprises treating such threads with at least one shrinking agent having a shrinking action equivalent to that of an aqueous caustic soda solution of at least about 15% strength continued for about 1 to 5 minutes, and allowing permanent shrinking of the said threads to occur during the said treatment.
  • the process of increasing the extensibility of Lilienfeld silk which is characterized by having a dry tenacity exceeding 2 grammes per denier, which comprises treating such threads with at least one shrinking agent, said shrinking agent being a basic compound of an alkali metal which contains at least one element of the oxygen group, said shrinking agent having a shrinking action equivalent to that of an aqueous caustic soda solution of at least about 15% strength continued for about 1 to 5 minutes, and allowing a permanent shrinking of said threads to occur during the said treatment.

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

Description

Patented Jan. 2?, 1935 UNITED STATES PATENT OFFICE No Drawing.
Application April 25, 1927, Serial No. 186,575. In Austria June 12, 1926 QCInima.
cases exceeding 3, 4 or 5 grammes per denier,
by a process comprising coagulation of the viscose formed into threads by means of strong mineral acid, particularly strong sulphuric acid of at least 50 to per cent., preferably of at least to per cent. strength. Artificial silk, of this high tenacity, is known in the art as Lilienfeld silk.
This invention is a method for eflecting an improvement in or modification of the products described in the aforesaid patents.
It is desirable in many cases to increase the extensibility of the artificial threads which are obtainable according to the processes of the aforesaid patents (such as artificial silk, staple fibre, or artificial wool), without influencing (or at least without considerably lowering) the strength or lustre of the threads.
This result may be attained according to the invention by treating the artificial threads with an agent adapted to cause the threads to shrink, under conditions which permit shrinkage of the thread to occur.
As agents for the purpose in question, mercerizing agents have proved particularly suitable, especially basic mercerizing agents and among them such compounds of alkali metals as contain at least one element of the oxygen group. Thus, good results are obtained with solutions of alkali hydroxides, and more particularly solutions of alkali hydroxides containing not less than 15, preferably not less than 18 per cent. of alkali hydroxide (calculated as NaOH). Useful results are, however, obtained with other mercerizing agents also, for instance, with a strong solution of an alkali sulphide (e. g. a solution of sodium sulphide of at least 15, for example 30 to 58 per cent. strength), or with a solution of an alkali hydroxide that contains an alkali sulphide, or with a strong mineral acid (e. g. sulphuric acid of 46-60 Baum specific gravity, or phosphoric acid of specific gravity 1.5-1.8, or nitric acid of 50-60 per cent. strength, or hydrochloric acid of 26-32 per cent. strength), or with a solution of zinc chloride, or with a solution of a thiocyanate, for example calcium thiocyanate, or the like. Substances'as set forth in this paragraph will hereinafter be included in the term mercerizing agents".
The artificial threads may be treated in various ways with the shrinking agent. For example, they may be immersed in, or impregnated with a solution of the agent, or passed through the solution, or passed over rollers which are in contact with the solution; or they may be sprayed with an atomized solution of the agent, or treated with a solution of the agent in a foulard, or by calendering, or coating; in short, by any known method of application, impregnation,.,immerslon or coating. I
The invention is applicable not only to the treatment of artificial threads as such (e. g. artificial silk), in the form of spun threads, yarn in hanks or cops or in the form of warp or twisted yarn or the like, but also to artificial threads (e. g. artificial silk or staple fibre) in the form of woven fabrics. It is also applicable to threads or fabrics consisting wholly of artificial fibre (e. g. artificial silk, artificial wool, or staple fibre), and to mixed threads or fabrics, that is, to fibres or fabrics eontainingin addition to the artificial threads another fibrous material, for instance natural cotton, silk, wool or the like. The ex pression artificial threads" throughout the application is intended to include, wherever the context permits, artificial threads such as artificial silk, cotton, wool, hair, and so on, in any of the forms hereinbefore mentioned.
The success of the process depends upon the fact that the artificial threads, or the-materials consisting of, or containing them, are treated with the shrinking agent in such a manner that the shrinkage remains either at its full extent, this extent depending on the nature and concentration of the shrinkage agent vused, or that at least a part of the shrinkage remains. That is to say, either the material under treatment may be subjected to no tension during or after the treatment or, if tension is applied, it must be subsequently discontinued or reduced.
I have referred to the fact that the shrinkage (or at least some of it) remains or persists after the end of the treatment. I accordingly refer to the process as producing "permanent shrinkage, to distinguish from any treatment in which the threads would leave the treatment in a stretched condition, as such a treatment would not accomplish the result of increasing the extensibility. g
It is to be noted that in the treatment according to the invention, it is not necessary to impreg- I nate or coat the artificial threads with any protective agent before they are subjected to the action of the shrinkingagent, since the threads which are treated by the invention differ from threads of artificial silk hitherto known in that they withstand the action of shrinking agents without being materially damaged. However, preliminary treatment with a protective agent is not excluded from the invention for it does not prevent the production of the desired effect.
The treatment'according to the invention may be combined into a single operation with a treatment for desulphurizing the threads. Thus, a suitable quantity of the shrinking agent, such as alkali hydroxide, may be added to the desulphurizing bath. If, however, the desulphurizing bath is a strong solution of an alkali sulphide, it may be unnecessary to add a further shrinking agent.
To the shrinking agent, for example a caustic alkali solution there may be added a suitable quantity of a neutral or alkaline salt, such as sodium chloride or sodium sulphate or sodium silicate or sodium aluminate or sodium zincate or borax or a sodium phosphate or sodium acetate or a monoor polyvalent alcohol, such as ethyl alcohol or glycerine..
By this invention it is possible to increase the extensibility of the artificial threads by -200 per cent. or more, so that threads of even very low extensibility can be improved so as to attain an extensibility of at least 8 per cent. In addition to this, the present process has, in most cases, a favorable, i. e. increasing effect on the elasticity oi the threads also.
The following examples illustrate the invention; the parts being by weight:-
1. Viscose silk made according to the process described in U. S. Patent No. 1,683,199 is introduced, in the finished, dried, but preferably unbleached state, in the form of hanks, without stretching; into' a caustic soda solution of 18-25 per cent. strength at a temperature'ot 15-18 C.
After a period of 1-5 minutes, it is removed and then introduced, if desired, after removal otthe excess caustic soda by centrifuging or pressing,
with the diflference that a solution of 200 parts of sodium chloride in 1500 parts of a caustic soda solutionof 20 per cent. strength is employed as shrinking agent.
3. The procedure is as in Example 1, with the difference that a solution of 88 parts of sodium sulphate in 1500 parts of a caustic soda solution of 20 per cent. strength is used as shrinking agent.
4. The mode of operation is as in Example 1, except that a mixture of 1500 parts of a caustic soda solution of 22.5 per cent. strength with 150 parts of water-glass of 39 Baum is employed as shrinking agent.
5. The procedure is as in Example 1, with the exception that a 20 per cent. caustic soda solution containing 8-10 per cent. of glycerine is used as shrinking agent.
6. The mode of operation is as in Example 1, with the diil'erence that a solution of 270 parts of caustic soda and 450 parts of sodium sulphide in 1050 parts of water is employed as shrinking agent.
'7. The procedure is as in Example 1, with the diiference that a sodium sulphide solution of -58 per cent. strength is used as shrinking agent.
8. The procedure is as in Example 1, except that a 30-50 per. cent. sodium sulphide solution containing i-5 per cent. of caustic soda is used as shrinking agent.
As the strong sodium sulphide solutions act as desulphurizing agents, in Examples 6, 7, and 8 the dry silk need not be desulphurized prior to the treatment according to these examples.
9. The mode of operation is as in Example 1, with the difference that an 18-22 per cent, solution of caustic soda containing 8-10 per cent. of sodium sulphide is used as shrinking agent.
10. Artificial silk is spun on a bobbin according to the process of U. S. Patents Nos. 1,683,199 or 1,683,200, whereupon, preferably after being washed with water for a shorter or longer time, it is twisted and converted into a skein. This skein is then in the wet state desulphurized in a known manner by means of a warm, weak solution of sodium sulphide and, if desired, after being washed again, introduced without tension into a solution of 200 parts of sodium chloride or of 88 parts of sodium sulphate in 1500 parts of a caustic soda solution of 20 per cent. strength where it remains for 1-5 minutes. From this bath the hank is, optionally after being washed with water, introduced for about 5 minutes into sulphuric acid of 5-10 per cent. strength at room temperature or in a solution of ammonium sulphate of 25 per cent. strength at room temperature or at 50 C. The skein is then washed, it desired, bleached and dried without stretching or under moderate tension only.
11. The procedure is as in Example 10, with the exception that a mixture of 1500 parts of a caustic soda solution of 22.5 per cent. strength with 150 parts 01 water-glass of 39 Baum is used as shrinking medium.
12. The mode of operation is as in Example 10, except that the skein is not desulphurized, but only washed, and that a solution of 270 parts of caustic soda and 450 parts of sodium sulphide in 1050 parts of water is used as shrinking bath, which, at the same time, acts as desulphurizing agent also.
13. The mode of operation is as in Example 10, with the difierence that the skein is not desulphurized, but only washed, and that a sodium sulphide solution of 58 per cent. strength is employed as shrinking agent, which, at the same time, acts as desulphurizing agent also.
14. The procedure is as in Example 10, with the exception that a 30-50 per cent. sodium sulphide solution containing 1-5 per cent. of caustic soda is used as shrinking agent, which, at the same time, acts as desulphurizing agent also.
15. The procedure is as in Example 13, with the difierence that an 18-22 percent. caustic soda solution that contains 8-10 per cent. of sodium, sulphide, is used as shrinking agent.
16. The procedure is as in any of the preceding examples, with the exception that the artificial silk is stretched during a part of the process, the stretching being discontinued, or considerably reduced, towards the end of, or after the treatment with the shrinking agent.
17. A fabric consisting of, or containing viscose silk (made according to the process described in U. S. Patent No. 1,683,199, is passed through one of the shrinking baths given in the preceding examples. It is allowed to shrink during or after the treatment with the shrinking agent, and is, if desired, after removal of the excess of the shrinking medium by pressing or centrifuging and/or, if desired, after a short washing, then introduced into dilute sulphuric acid (for example of 5-10 per cent. strength), washed, and dried without stretching, or whilst stretching only moderately.
18. The procedure is as in Example 17, with the exception that the fabric contains cotton in addition to the artificial silk or staple fibre.
19. The procedure is as in any of the preceding examples, with the exception that the artificial silk is in the form of warps.
20. The procedure is as in any of the preceding examples, with the exception that the thread or fabric is impregnated or sized with a solution or gelatine 'or albumen of 23 per cent. strength, or with a solution of starch of 3-4 per cent. strength, before it is treated with the shrinking medium.
In the examples other shrinking agents may be used, for instance, instead of caustic soda solution, a solution or another alkali hydroxide,
for example caustic potash of equivalent strength, or instead 01' the sodium sulphide another alkali sulphide, for instance potassium sulphide, or sulphuric acid of 47 to 50 Baum specific gravity, or hydrochloric acid of 27 to 30 per cent. strength, or nitric acid of 50 to 60 per cent. strength, or a 40 to per cent. solution of calcium thiocyanate.
The artificial threads or-fabrics may be keired or treated at room, or at a raised temperature under atmospheric or increased pressure in any known manner with an alkaline agent, for instance with sodium carbonate or lime, or with a very dilute caustic alkali solution, or with a solution of sodium carbonate and a dilute caustic alkali solution, or with a solution of soap or Turkey red oil or the like.
The expression mercerizing agents means in the description and claims all chemicals known as mercerizing agents in the mercerization art.
The expression oxygen group is intended to include the following elements: 0, S, Se and Te.
The expression strong. mineral acid" means in the description and in the claims: Sulphuric acid of at least 50 per cent. of H2804 and the other mineral acids equivalent in strength, i. e. hydrochloric acid of at least 35 per cent. strength, nitric acid of at least 60 per cent. strength, phosphoric acid of at least 1.5 specific gravity and arsenic acid of at least 75 per cent. of H3ASO4.
The expression strong sulphuric acid" or sulphuric acid containing at least 50 per cent, of sulphuric acid monohydrate means in the description and claims: Sulphuric acid of 50 to 98 or per cent. strength.
The statements in the description and claims regarding percentages relate to percentages by weight.
I claim:
1. Process for increasing the extensibility of artificial threads of high dry tenacity, exceeding 2 grammes per denier, of the kind produced from viscose by means of a coagulating bath consisting of a strong mineral acid, which process comprises treating the threads with at least one mercerizing reagent of a concentration capable of mercerizing cotton, and allowing permanent shrinking of the said threads to occur during said treatment.
2. Process for increasing the extensibility of artificial threads of high dry tenacity, exceeding 2 grammes per denier, of the kind produced from viscose by means of a coagulating bath containing not less than about 55 per cent. of H2804, which process comprises treating the threads with a liquid containing a caustic alkali of not substantially below 15% concentration, calculated as NaOH, and allowing permanent shrinking of said threads to occur during said treatment.
3. Process for increasing the extensibility of artificial threads of high dry tenacity, exceeding 2 grammes per denier, of the kind produced from viscose by means of a coagulating bath consisting of a strong mineral acid, which process comprises treating the threads with a liquid containing an alkali sulphide of at least 15 per cent strength (calculated as NaaS) and allowing permanent shrinking or said threads to occur during said treatment.
4. Process tor increasing the extensibility of artificial threads or high dry tenacity, exceeding 2 grammes per denier, or the kind produced from viscose by means of .a coagulating bath containing a strong mineral acid, which process comprises treating the threads with a liquid containing not substantially less than 15% (figured as NaOH and NaaS) of a caustic alkali and an alkali sulphide, and allowing permanent shrinking of said threads to occur during said treatment.
5. As new products, artificial threads produced from viscose, which threads in the dry state have both a tenacity exceeding 2 grammes per denier and an extensibility of at least 8 per cent, which material has been produced by treating artificial threads produced from viscose and having a dry tenacity exceeding 2 grammes per denier, with a mercerizing reagent having a shrinking action on said threads not substantially less than the shrinking action of a 15% aqueous caustic soda, and allowing permanent shrinkage of the said threads to occur during said treatment.
6. As new products, artificial threads produced from viscose, which threads in the dry state have both a tenacity exceeding 4 grammes per denier and an extensibility of at least 8 per cent... which products have been produced by treating artificial threads produced from viscose and having a dry tenacity exceeding 4 grammes per denier, with a mercerizing reagent having a shrinking action on said threads not substantially less than the shrinking action of a 15% solution of caustic soda, and allowing permanent shrinkage 01 said threads during said treatment. 7. The process of increasing the extensibility of regenerated cellulose threads having a dry tenacity exceeding 2 grammes per denier produced from viscose by means of a setting bath consisting of a strong mineral acid, which comprises treating such threads with at least one shrinking agent having a shrinking action equivalent to that of an aqueous caustic soda solution of at least about 15% strength continued for about 1 to 5 minutes, and allowing permanent shrinking of the said threads to occur during the said treatment.
8. The process of increasing the extensibility of regenerated cellulose threads having a dry tenacity exceeding 2 grammes per denier, which comprises treating such threads with at least one shrinking agent having a shrinking action equivalent to that of an aqueous caustic soda solution of about 15 to 22% strength continued for about 1 to 5 minutes, and allowing a permanent shrinking of the said threads to occur during the said treatment.
9. The process of increasing the extensibility of Lilienfeld silk, which is characterized by having a dry tenacity exceeding 2 grammes per denier, which comprises treating such threads with at least one shrinking agent, said shrinking agent being a basic compound of an alkali metal which contains at least one element of the oxygen group, said shrinking agent having a shrinking action equivalent to that of an aqueous caustic soda solution of at least about 15% strength continued for about 1 to 5 minutes, and allowing a permanent shrinking of said threads to occur during the said treatment.
LEON LILIENFELD.
US186575A 1925-06-20 1927-04-25 Manufacture of artificial threads Expired - Lifetime US1989098A (en)

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US113583A Expired - Lifetime US1683200A (en) 1925-06-20 1926-06-03 Artificial material and process for making same
US113582A Expired - Lifetime US1820811A (en) 1925-06-20 1926-06-03 Artificial material and process for making same
US156751A Expired - Lifetime US1683199A (en) 1925-06-20 1926-12-23 Artificial thread and process for making same
US186575A Expired - Lifetime US1989098A (en) 1925-06-20 1927-04-25 Manufacture of artificial threads
US367149A Expired - Lifetime US1881742A (en) 1925-06-20 1929-05-29 Process for the manufacture of artificial threads
US367148A Expired - Lifetime US1989099A (en) 1925-06-20 1929-05-29 Process of improving artificial threads
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US113582A Expired - Lifetime US1820811A (en) 1925-06-20 1926-06-03 Artificial material and process for making same
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US2497519A (en) * 1946-12-04 1950-02-14 Alrose Chemical Company Art of stabilizing rayon type fabric
US2509549A (en) * 1943-11-06 1950-05-30 Du Pont Process of producing highly extensible regenerated cellulose yarn
US2524113A (en) * 1946-04-24 1950-10-03 Stein Hall & Co Inc Process of stabilizing rayon-containing textile fabrics
US2586795A (en) * 1948-05-11 1952-02-26 Textile & Chem Res Co Ltd Pneumatic tire
US2647036A (en) * 1946-08-17 1953-07-28 Hogg & Mitchell Ltd Curving cellulose collar blanks by differential shrinking with chemical shrinking agents
US2682443A (en) * 1944-12-30 1954-06-29 Bener Christian Hot acid neutralization of regenerated cellulose containing fabrics treated with alkaline swelling agents
US2687447A (en) * 1951-04-25 1954-08-24 Dewey And Almy Chem Comp Battery separator
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
US3511591A (en) * 1965-04-09 1970-05-12 Deering Milliken Res Corp Process and product of rendering cellulosic fabrics amenable to molding operations
US3905763A (en) * 1972-03-14 1975-09-16 Omnium De Prospective Ind Sa Processes for treating polyamides

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DE749264C (en) * 1938-11-09 1944-11-21 Ig Farbenindustrie Ag Process for the production of synthetic fibers or threads from viscose
DE749501C (en) * 1941-05-25 1952-04-17 Spinnfaser A G Process for the production of rayon from viscose
US2515834A (en) * 1942-11-13 1950-07-18 Du Pont Cellulose filaments and method of producing same
DE903208C (en) * 1943-01-23 1954-02-04 Schachenmayr Mann & Cie Process for curling cellulose hydrate cellulose wool or rayon
US2467541A (en) * 1943-07-03 1949-04-19 American Viscose Corp Method and apparatus for spinning artificial filamentous products
US2457350A (en) * 1943-07-07 1948-12-28 American Viscose Corp Method and apparatus for spinning artificial filamentous products
US2517694A (en) * 1943-09-14 1950-08-08 American Viscose Corp Crimped artificial filament
NL61100C (en) * 1944-02-15
US2531513A (en) * 1944-04-20 1950-11-28 Celanese Corp Process for the production of textile materials
US2439039A (en) * 1944-09-26 1948-04-06 American Viscose Corp Process of producing medullated artificial filaments
US2479218A (en) * 1944-12-12 1949-08-16 Int Paper Canada Process for making rayon filaments
US2581835A (en) * 1946-03-22 1952-01-08 Du Pont Method of spinning viscose
FR957246A (en) * 1946-12-14 1950-02-17
BE480557A (en) * 1947-04-14
FR961353A (en) * 1947-04-26 1950-05-11
BE482687A (en) * 1947-05-28
US2512951A (en) * 1947-06-16 1950-06-27 Dixie Mercerizing Company Mercerization
BE488949A (en) * 1948-05-11
US2518753A (en) * 1949-07-14 1950-08-15 Du Pont Crimped yarn production
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
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
US2946650A (en) * 1958-02-17 1960-07-26 Tatsuji Tachikawa Process for the manufacture of viscose rayon staple
US3689613A (en) * 1970-11-02 1972-09-05 Anselm Talalay Glove making
US4196559A (en) * 1973-03-28 1980-04-08 Ljungbo Sven O B Swellable fabrics for ceiling structures
DE2720087A1 (en) * 1976-05-07 1977-11-24 Centre Tech Ind Papier PROCESS FOR MANUFACTURING VISCOSE FEMES AND FEMES PRODUCED BY THE PROCESS
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
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 (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2509549A (en) * 1943-11-06 1950-05-30 Du Pont Process of producing highly extensible regenerated cellulose yarn
US2682443A (en) * 1944-12-30 1954-06-29 Bener Christian Hot acid neutralization of regenerated cellulose containing fabrics treated with alkaline swelling agents
US2524113A (en) * 1946-04-24 1950-10-03 Stein Hall & Co Inc Process of stabilizing rayon-containing textile fabrics
US2647036A (en) * 1946-08-17 1953-07-28 Hogg & Mitchell Ltd Curving cellulose collar blanks by differential shrinking with chemical shrinking agents
US2497519A (en) * 1946-12-04 1950-02-14 Alrose Chemical Company Art of stabilizing rayon type fabric
US2586795A (en) * 1948-05-11 1952-02-26 Textile & Chem Res Co Ltd Pneumatic tire
US2687447A (en) * 1951-04-25 1954-08-24 Dewey And Almy Chem Comp Battery separator
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
US3511591A (en) * 1965-04-09 1970-05-12 Deering Milliken Res Corp Process and product of rendering cellulosic fabrics amenable to molding operations
US3905763A (en) * 1972-03-14 1975-09-16 Omnium De Prospective Ind Sa Processes for treating polyamides

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US1820811A (en) 1931-08-25
GB319293A (en) 1929-09-11
NL21442C (en)
NL21473C (en)
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BE334767A (en)
US2112499A (en) 1938-03-29
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FR35551E (en) 1930-03-26
FR35751E (en) 1930-03-27
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DE542713C (en) 1932-01-27
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US1881742A (en) 1932-10-11
GB321679A (en) 1929-11-11
USRE18170E (en) 1931-08-25
FR37344E (en) 1930-11-15
GB264161A (en) 1928-07-05
FR35752E (en) 1930-03-27
FR666178A (en) 1929-09-27
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NL23112C (en)
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US1989099A (en) 1935-01-29
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GB274690A (en) 1927-07-11

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