Classifications

• • 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
  • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
  • D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
  • D06M13/345—Nitriles
  • D06M13/348—Nitriles unsaturated, e.g. acrylonitrile
• • 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
  • D06M11/13—Ammonium halides or halides of elements of Groups 1 or 11 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
• • 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
  • D06M11/56—Sulfates or thiosulfates other than of elements of Groups 3 or 13 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
  • D06M11/58—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
  • D06M11/65—Salts of oxyacids of nitrogen

Definitions

• This invention relates generally to the production of I improved regenerated cellulose products and more particularly to a process for lowering the degree of swelling of regenerated cellulose products in water, especially viscose rayon fibers and fabrics.
• Another object of this invention is to provide a process for treating regenerated cellulose products to lower their degree of swelling in water.
• Still another object of this invention is to provide a process for producing regenerated cellulose products that absorb less moisture from the atmosphere.
• regenerated cellulose products are first treated with an acqueous hydroxide solution that has a normality not higher than 0.70 and containsat least one salt of an alkali metal hydroxide and an inorganic acid derived from one of the first five anions of the lyotropic series according to Hofmeister (see E. A. Hauser, Collodial Phenomena, page 132, First Edition, 1939). Thereafter, the pro-ducts are treated with an azeotropic mixture of acrylonitrile and where A is the weight of the air dried cellulose pro-duct and B is the weight of the product after it had been soaked in water for two hours and centrifuged for ten minutes.
• the normality of the hydroxide solution is higher than 0.70, the treated products have a cce higher degree of swelling than do the untreated products.
• the normality of the hydroxide solution must be below 0.70.
• the alkaline metal hydroxides that may be'used in the process include lithium hydroxide, sodium hydroxide, potassium hydroxide, rubidium hydroxide, and cesium hydroxide. However, for economy reasons, it is preferred to use sodium hydroxide.
• the salts added to the caustic solution may be lithium salt, sodium salt, potassium salt, rubidium salt, or cesium salt, although, also for economy reasons, it is preferred to use sodium salts.
• the :salts are derived from an alkali metal hydroxide and any one of the following acids: sulfuric acid, hydrofluoric acid, nitric acid, hydrochloric acid, and hydrobr-omic acid. The anions of these acids are the first five members of the lyotropic series according to H-ofmeister.
• sodium sulphate or sodium chloride is added to the caustic solution since these salts are commercially available at a low price.
• the reaction may be accelerated by increasing the amount of salt in the caustic solution, the amount of salt added being dependent on the desired decrease in the degree of swelling in the product treated.
• the temperature at which the treatment with the hydroxide solution is carried out may vary between wide limits. However, higher temperatures are desirable since the wet strength of the product decreases to a lesser extent. Also, the time during which the products are treated with the hydroxide solution preferably should be as short as possible to limit the decrease in the wet strength of the product. If needed, a wetting agent may be added to the hydroxide solution.
• the products After the products have been treated with the hydroxide solution, excess liquid may be removed by centrifuging or pressing.
• the products are then treated with a mixture of acrylonitrile and a small amount of water.
• the temperature of the acrylonitrile mixture i maintained as high as possible in order that the/treatment may be short, thus allowing the process to be carried out in a continuous manner.
• the treatment may be carried out at 70 C. using an azeotropic mixture consisiting of 88% of acrylonitrile and 12% water. If the treatment is carried out under pressure, even higher temperatures may be used.
• a mixture of acrylonitrile and a diluent, such as benzene, toluene, acetone, or chloroform may be used.
• the amount of acrylonitrile reacting with the products may vary within wide limits depending on the decrease in the degree of swelling desired.
• Products treated in accordance with this invention not only have a lower degree of swelling in water, but also absorb less moisture in air.
• the percentage of moisture absorbed from air may be reduced to below 8%. which corresponds to a moisture absorption of about 1 2% for untreated products of regenerated celiulose in air at 20 C. and a relative humidity of 65%.
• Viscose rayon staple fibers having a denier of 1 /2 were separated into several samples and each sample treated with an aqueous sodium hydroxide and salt solution.
• the numberof cyanoethyl groups may Run3 11 to 15 Show that y mcfreaslng the Sodlllm $111 be determined and such determination expressed as the P Content the reactlonls' conslderably accelelatfidweight percent of acryloni-trile bound to the final product. Runs 15 to 19 Show the afflicts Obtained using Sodium After the treatment with acrylonit-rile, the samples were 20 chlfmde, Potasslum Sulfate, Sodium nitrate, and Sodium successively washed with dilute acetic acid and warm wafluoflde as the Salts added 0 h Caustic Soluti n.
• EX MPLE V The conditions and results of runs 1 to 10 are et A fabric having a warp conslsting of 120 denier comforth in Table I. tinuous filament viscose rayon threads and a weft consist- Table I Hydrox- Percent Tempera- Acryloni- Percent Moisture Normal- Percent Temp. ids soluincrease ture acrytrile treatacryloni- Deg.
• 0.1 NSZSOA- 20 90 1 44 70 5 19.1 NaOH 0.1 NaCl- 5 90 1 44 70 5 12.2 Na-OHW 0.1 K1S01 5 90 7 1 45 70 5 13.4 NaOH 0.1 NaNO 5 90 .1 41 70 5 16.6 NaOH 0.1 NaF 5 90 1 38 70 5 20.6 NaOH--- 0. 2 KI 46 90 1 96 70 2% 23.1 NaOH.-- 0.1 Na2HPO4. 25 90 1 44 70 5 0.4 NaOH 0.1 NazSOr--- 5 20 1 44 70 5 16.5
• the table shows that using a sodiurnhydroxide solution having a normality of 0.7 or lower results in a decrease of swelling.
• the untreatedcontrol fibers had a degree of swelling of 75. Fibers treated according to runs 1 to 5 had a degree of swelling of 55, 58, 60,44 and7l,
• the weight of the treated fabric was 124.7% of its original weight.
• the fabric was immersed in water and afterwards centrifuged. It then contained about 63% by weight water.
• EXAMPLE IV A selfsupporting film made from viscose was passed through an aqueous bath maintained at 90 C. containing 1% by weight sodium hydroxide and 5% by weight sodium sulfate. The residence time of the him in the bath was one minute. The film was passed between two rollers thereby removing excess liquid. Thereafter, the film was passed through a bath maintained at 70 C. containing 88% by weight acrylonitrile and 12% by weight water. Residence time in this bath was 1 /2 minutes. The film thus treated was passed between two rollers to remove excess liquid and successively washed with dilute acetic acid and warm water. After drying the film was immersed in water and centrifuged. The increase in weight of the film was only 65% in contrast with untreated film, similarly immersed in water and centrifuged which increased 98% in weight.
• a process for lowering the degree of swelling in water of a dry viscose regenerated cellulose product comprising the steps of treating said product with an aqueous solution of an alkali metal hydroxide having a maximum normality of 0.70 for a suflicient period of time to effect cyanoethylation of the product upon subsequent treatment with acrylonitrile, said solution having present therein in addition to said alkali metal hydroxide a small amount of at least one salt of an alkali metal hydroxide and an acid derived from one of the first five anions of the lyotropic series of Hofmeister, treating the alkali impregnated product with acrylonitrile for a sufiicient period of time to cyanoethylate the product and to reduce the degree of swelling of the product upon contact with water, and thereafter drying the resulting product.
• a process for treating a dry viscose regenerated cellulose product to lower its degree of swelling in water comprising the steps of immersing said product in an aqueous solution of an alkali metal hydroxide having a maximum normality of 0.70 for a sutlicient period of time to eifect cyanoethylation of the product upon subsequent treatment with acrylonitrile, said solution having present therein in addition to said alkali metal hydroxide a small amount of at least one salt of an alkali metal hydroxide and an acid derived from one of the first five anions of the lyotropic series of Hofmeister, immersing the alkali impregnated product in acrylonitrile for a sufficient period of time to bind to the product from about 6.7% to about acrylonitrile, based on the weight of the final cyanoethylated product, and thereafter drying the thustreated product.
• a process for treating a dry viscose regenerated cellulose product to lower its degree of swelling in water comprising the steps of immersing said product for about 70 one minute in an aqueous solution of an alkali metal hydroxide having a maximum normality of 0.50 and a temperature of about 90 (3., said solution having present therein in addition to said alkali metal hydroxide a small amount of at least one salt of an alkali metal hydroxide and an acid selected from the group consisting of sulfuric acid, hydrofluoric acid, nitric acid, hydrochloric acid, and hydrobromic acid, immersing the alkali impregnated product in an azeotropic mixture of acrylonitrile and water for a sufficient period of time to bind to the product from about 6.7% to about 35% acrylonitrile, based on the weight of the final cyanoethylated product, washing the product, and thereafter drying the thus-treated prodnot.
• a process for treating a dry viscose regenerated cellulose product to lower its degree of swelling in water comprising the steps of immersing said product for a maximum of two minutes in an aqueous solution of an alkali metal hydroxide having a maximum normality of 0.70, said solution having present therein in addition to said alkali metal hydroxide 5% by weight of said solution of at least one salt of an alkali metal hydroxide and an acid selected from the group consisting of sulfuric acid, hydrofiuoric acid, nitric acid, hydrochloric acid, and hydrobromic acid, immersing the alkali impregnated product in an azeotropic mixture of acrylonitrile and water main tained at a temperature ranging from 15 C.30 C. for a sufiicient period of time to bind to the product from about 6.7% to about 35% acrylonitrile, based on the weight of the final cyanoethylated product, washing the product, and thereafter drying the thus-treated product.
• alkali metal hydroxide is sodium hydroxide and the salt is a sodium salt.
• a process for treating a dry viscose regenerated cellulose product to lower its degree of swelling in water comprising the steps of immersing said product in an aqueous solution of an alkali metal hydroxide having a maximum normality of 0.70 for a sufficient period of time to increase the weight of the product by at least 38% after centrifuging, said solution having present therein in addition to said alkali metal hydroxide 5% by weight of at least one salt of an alkali metal hydroxide and an acid selected from the group consisting of sulfuric acid, hydrofluoric acid, nitric acid, hydrochloric acid, and h drobromic acid, immersing the alkali impregnated product in an azeotropic mixture of acrylonitrile and water maintained at a temperature of C. for a sufircient period of time to bind to the product from about 6.7% to about 35% acrylonitrile, based on the weight of the final cyanoethylated product, washing the product, and thereafter drying the

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• Engineering & Computer Science (AREA)
• Textile Engineering (AREA)
• Chemical Or Physical Treatment Of Fibers (AREA)
• Polysaccharides And Polysaccharide Derivatives (AREA)
• Treatments Of Macromolecular Shaped Articles (AREA)
• Compositions Of Macromolecular Compounds (AREA)
• Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

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Citations (7)

• 0
  • BE BE622899D patent/BE622899A/xx unknown
  • NL NL270070D patent/NL270070A/xx unknown
• 1962
  • 1962-09-21 CH CH1115062A patent/CH385159A/de unknown
  • 1962-10-03 US US228025A patent/US3199943A/en not_active Expired - Lifetime
  • 1962-10-05 GB GB37749/62A patent/GB955306A/en not_active Expired
  • 1962-10-08 FR FR911530A patent/FR1337579A/fr not_active Expired
  • 1962-10-08 ES ES281360A patent/ES281360A1/es not_active Expired
  • 1962-10-09 DE DEN22192A patent/DE1186617B/de active Pending

Patent Citations (7)

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