US2516083A - Transparentizing regenerated cellulose silk - Google Patents

Transparentizing regenerated cellulose silk Download PDF

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US2516083A
US2516083A US637119A US63711945A US2516083A US 2516083 A US2516083 A US 2516083A US 637119 A US637119 A US 637119A US 63711945 A US63711945 A US 63711945A US 2516083 A US2516083 A US 2516083A
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Weiss Ernst
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Heberlein Patent Corp
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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06Q—DECORATING TEXTILES
    • D06Q1/00—Decorating textiles
    • D06Q1/02—Producing patterns by locally destroying or modifying the fibres of a web by chemical actions, e.g. making translucent
    • 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
    • D06M11/155—Halides of elements of Groups 2 or 12 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
    • D06M11/32—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
    • D06M11/46—Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic Table; Titanates; Zirconates; Stannates; Plumbates
    • 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
    • D06M11/67—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 cyanogen or compounds thereof, e.g. with cyanhydric acid, cyanic acid, isocyanic acid, thiocyanic acid, isothiocyanic acid or their salts, or with cyanamides; with carbamic acid or its 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
    • D06M11/68—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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
    • D06M11/70—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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with oxides of phosphorus; with hypophosphorous, phosphorous or phosphoric acids or their salts

Definitions

  • This invention relates to a process for transparentizing fibers and fabrics of regenerated cellulose.
  • Transparentizing of cotton fabrics by means of sulfuric acid is known and has been used extensively commercially.
  • 'Iransparentizing of artificial silk, namely, regenerated cellulose silk fabrics with swelling agents is known, but due to the ease with which sulfuric acid and other swelling agents proposed attack the regenerated cellulose, it has been difficult to control such processes to produce a transparentization, either in all-over or pattern effect, having the same uniform appearance and high quality obtainable by the process as applied to cotton.
  • Attempts to secure greater uniformity and to lessen the vigorous action of the sulfuric acid have been proposedby combining with the acid substances, such as monovalent or multivalent alcohols, heterocyclic bases, formaldehyde, ammonia salts, urea and their derivative amino compounds. But these processes have not given the desired results to produce a satisfactory commercial transparentized viscose or other regenerated cellulose in transparent-form.
  • the principal object of the invention accordingly is to provide a process for the treatment of regenerated cellulose silk, such as viscose, which may be easily controlled to produce a transparentized, regenerated cellulose of high quality and appearance.
  • caustic soda of a much lower concentration may be used, namely, 6 to less than 12 Baum'. Room temperature is also used. The treatment is followed by washing with boiling water to eliminate the caustic soda.
  • the use of caustic potash and caustic soda in the concentrations mentioned is in accordance with the known solubilities of regenerated cellulose, such as viscose in aqueous solutions of these alkalies.
  • Potassium hydroxide has a far lower dissolving power for regenerated cellulose, dissolving (when about 4.5 N KOI-I is used) only about 6% thereof as compared with for sodium hydroxide (using about 2.5 N NaOI-I) at 0 C.
  • dissolving when about 4.5 N KOI-I is used
  • sodium hydroxide using about 2.5 N NaOI-I
  • the dissolving power decreases as the temperature rises.
  • My process is suitable for the production of both all-over effects and for local transparent effects with the use of water-soluble or waterinsoluble resists and with dyes or pigments a may be desired.
  • the process is applicable to the treatment of all fine fabrics made from regenerated cellulose, such as spun rayon muslin or viscose muslin, or corresponding voiles.
  • .As transparentizing or parchmentizing agents there may be used the well-known cellulose swelling agents such as sulfuric acid (with or without additions) of over 42 Baum', phosphoric acid of over 50 Baum, hydrochloric acid of over 20 Baum, zinc chloride solutions of over 50 Baum, calcium thiocyanate solutions of over 25 Baum, in which connection the requisite concentrations are in :addition dependent also upon the reaction temperature.
  • cellulose swelling agents such as sulfuric acid (with or without additions) of over 42 Baum', phosphoric acid of over 50 Baum, hydrochloric acid of over 20 Baum, zinc chloride solutions of over 50 Baum, calcium thiocyanate solutions of over 25 Baum, in which connection the requisite concentrations are in :addition dependent also upon the reaction temperature.
  • caustic potash solution of about 30 Baum at room temperature may be employed, or caustic soda solution may be used in concentrations of 6 to less than 12 Baum with subsequent rapid removal of the caustic to correct this lack of clarity and non-uniformity.
  • the control of the process is more easily effected by the use of caustic potash.
  • Viscose muslin which has been pre-cleansed by the usual methods and dried under tension is passed in the broad state through sulfuric acid of 48 Baum (measured at 15 0.). The temperature of the acid is kept between l C. and +l C.; the time of action amounts to 11 seconds. Immediately thereafter the acid is washed out with .water at room temperature, and any possible residues of acid are neutralized besides with dilute ammonia. The fabric is now freed from the excess of water by pressing or suction, and in still moist condition is then exposed for 6 seconds to the action of caustic potash solution of 30 Baum, freed from caustic by means of hot water at about 70 C., acidified with sulfuric acid of 1 Baum, and washed. The material can now be either blued or dyed by the usual methods, whereupon it is dried under tension in the directions of warp and weft; expediently it is further stentered before the drying.
  • Viscose muslin that has been imprinted with dyes fast to acid and fast to alkali is exposed for 12 seconds to the action of sulfuric acid cooled to C., whose specific gravity measured at 15 C. amounts to 47 Baum, is then washed neutral and dried under tension. Now the material is immersed for seconds at to C. in caustic potash solution of Baum, freed from caustic .with hot water (about 70 C.), acidified, and washed until a neutral reaction is attained. After pressing-off of the excess water, the material is dried under tension. The drying of the material can be effected on a tension frame.
  • the temperature of the bath is kept at 25 C.
  • the time of action amounts to 16 seconds. Tm mediately thereafter the material is washed cold, and the moist material is then subjected to aftertreatment with caustic potash solution of 28 Baum for 8 seconds at room temperature. After the freeing from caustic and washing with hot water, the material is stentered and dried under tension. Advantageously, the material is finally calendered besides.
  • Spun rayon muslin that has been treated in this manner corresponds in appearance to a highgrade cotton organdy.
  • Viscose spun rayon muslin is, in accordance with the usual methods, singed, desized, boiled, bleached, dried on a tension frame, and imprinted with a resist of the following composition:
  • Viscose voile is parchmentized at 10 C. for 15 seconds with phosphoric acid of 55 Baum (measured at 15 C.), and immediately thereafter is subjected to after-treatment with caustic potash solution as described in Example 4 and dried under tension.
  • Viscose marquisette is pre-cleansed by the well-known methods and dried on a tension frame. Now the material is passed in the open width through 60% sulfuric acid to which per liter 10 cc. of 40% technical concentrated formaldehyde have been added. The temperature of the acid should be 0 C., the time of action 12 seconds. After the washing out of the acid, the material is dried under tension, whereupon it is subjected to after-treatment with caustic soda solution of 8 Baum for 5 seconds, is washed hot, acidified, and thoroughly rinsed. Finally the fabric is tensed in the warp and weft directions and dried.
  • a light weight fabric consisting in warp and weft of cuprammonium silk yarns is precleansed by the well-known methods and dried on a tension frame. Now the material is treated in the open width for 12 seconds with sulfuric acid of 475 Baum at a temperature of 0 C. After washing out the acid the fabric is exposed for 6 seconds to the action of caustic potash solution of 28 Baum, washed with hot water to remove the caustic, :acidulated with sulfuric acid of 1 Baum, washed until a neutral reaction .is attained, stentered and dried under tension.
  • the fabrics obtained in accordance with the above examples have a uniform appearance where an all-over effect is obtained and the same uniformity may be observed in the transparent patterned goods.
  • the goods are of high quality, are relatively soft, and of marketable character.
  • regenerated cellulose material refers to regenerated cellulose in the form of fiber, yarns, and fabrics of such material.
  • a process which comprises treating regenerated cellulose with an aqueous solution selected from the group consisting of sulfuric acid of about 42 to about 48 B., phosphoric acid of about 50 to about 55 B., hydrochloric acid of the order of B., zinc chloride of the order of 50 B and calcium thiocyanate of the order of B. for a period of time of the order of 10 seconds at a temperature in a range of about room temperature and below, whereby an acid parchmentized regenerated cellulose textile material results which lacks clarity and is non-uniform in appearance, and treating such material substantially free from acid at room temperature with an aqueous caustic alkali solution selected from the group consisting of potassium hydroxide of the order of B. and sodium hydroxide at 6 to less than 12 B. for a period of the order of 10 seconds to produce a clear uniform transparent fabric.
  • an aqueous solution selected from the group consisting of sulfuric acid of about 42 to about 48 B., phosphoric acid of about 50 to about 55 B., hydrochlor
  • a process which comprises treating regenerated cellulose with an aqueous solution of sulfuric acid of about 42 to about 48 B. for a period of time of the order of 10- seconds at a temperature in a range of about room temperature and below, whereby an acid parchmentized regenerated cellulose textile material results which lacks clarity and is non-uniform in appearance, and treating such material substantially free from acid at room temperature with an aqueous caustic alkali solution selected from the group consisting of potassium hydroxide of the order of 30 B. and sodium hydroxide at 6 to less than 12 B. for a period of the order of 10 seconds to produce a clear uniform transparent fabric.
  • a process which comprises treating regenerated cellulose with an aqueous solution of phosphoric acid of about 50 to about B. for a period of time of the order of 15 seconds at a temperature in a range of about room temperature and below, whereby an acid parchmentized regenerated cellulose textile material results which lacks clarity and is non-uniform in appearance, and treating such material substantially free from acid at room temperature with an aqueous solution of potassium hydroxide of about 30 B. for a period of the order of 6 seconds to produce a clear uniform transparent fabric.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
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Description

Patented July 18, 1950 TRANSPARENTIZIN G REGENERATED CELLULOSE SILK Ernst Weiss, Wattwil, Switzerland, assignor to Heberlein Patent Corporation, New York, N. Y., a corporation of New York No Drawing. Application December 22, 1945, Se-
rial No. 637,119. In Switzerland December 27,
4 Claims.
, 1 This invention relates to a process for transparentizing fibers and fabrics of regenerated cellulose.
Transparentizing of cotton fabrics by means of sulfuric acid is known and has been used extensively commercially. 'Iransparentizing of artificial silk, namely, regenerated cellulose silk fabrics with swelling agents is known, but due to the ease with which sulfuric acid and other swelling agents proposed attack the regenerated cellulose, it has been difficult to control such processes to produce a transparentization, either in all-over or pattern effect, having the same uniform appearance and high quality obtainable by the process as applied to cotton. Attempts to secure greater uniformity and to lessen the vigorous action of the sulfuric acid have been proposedby combining with the acid substances, such as monovalent or multivalent alcohols, heterocyclic bases, formaldehyde, ammonia salts, urea and their derivative amino compounds. But these processes have not given the desired results to produce a satisfactory commercial transparentized viscose or other regenerated cellulose in transparent-form.
The principal object of the invention accordingly is to provide a process for the treatment of regenerated cellulose silk, such as viscose, which may be easily controlled to produce a transparentized, regenerated cellulose of high quality and appearance.
vI have found, unexpectedly in accordance with my invention, that the above difliculties may be overcome by giving such fibers or fabrics a transparentizing treatment, followed by a treatment which has the result of making the fabric appear more uniform and to give it a high quality both as to strength and appearance. This may be most satisfactorily done by the use of caustic potash used, in accordance with my invention, at a regulated. range of temperature, time and concentration. And I have found also that the caustic solution should be removed as rapidly as possible, for example, by means of hot rinsing. The concentrations of potassium hydroxide which may be employed are preferably quite high, namely, of the order of 30 Baum. Room temperature is preferably used. Instead of caustic potash, caustic soda of a much lower concentration may be used, namely, 6 to less than 12 Baum'. Room temperature is also used. The treatment is followed by washing with boiling water to eliminate the caustic soda. The caustic alkali solutions-are used under .conditi'onsof time, temperature and concentration such that the solutions areincapable of producing a parch- 2 mentizing effect on the original untreated regenerated cellulose. The use of caustic potash and caustic soda in the concentrations mentioned is in accordance with the known solubilities of regenerated cellulose, such as viscose in aqueous solutions of these alkalies. Potassium hydroxide has a far lower dissolving power for regenerated cellulose, dissolving (when about 4.5 N KOI-I is used) only about 6% thereof as compared with for sodium hydroxide (using about 2.5 N NaOI-I) at 0 C. In the case of both caustic potash and caustic soda solution, the dissolving power decreases as the temperature rises. I take advantage of these facts, in accordance with my invention, to avoid the use of either caustic potash or caustic soda in concentrations and at temperatures which will cause any substantial dissolving of regenerated cellulose material. In other words, after applying the sulfuric acid or other transparentizing treatment which in itself constitutes a partial solution of the cellulose I avoid in the after-treatment with the caustic a further dissolving action. Accordingly, I employ these caustic alkalies under conditions such that this second dissolving action is substantially avoided.
As a result I obtain transparentized regenerated cellulose which has a uniform and otherwise pleasant appearance and is of high quality, i. e., it has good wearing qualities and has a relatively soft feel, clue probably to the fact that the second caustic treatment is not a dissolving treatment since it appears that each dissolving treatment tends to stiffen and otherwise impair the material somewhat. By my process only one such dis solving treatment is effected, and accordingly only a limited stiifening occurs.
My process is suitable for the production of both all-over effects and for local transparent effects with the use of water-soluble or waterinsoluble resists and with dyes or pigments a may be desired.
The process is applicable to the treatment of all fine fabrics made from regenerated cellulose, such as spun rayon muslin or viscose muslin, or corresponding voiles.
.As transparentizing or parchmentizing agents there may be used the well-known cellulose swelling agents such as sulfuric acid (with or without additions) of over 42 Baum', phosphoric acid of over 50 Baum, hydrochloric acid of over 20 Baum, zinc chloride solutions of over 50 Baum, calcium thiocyanate solutions of over 25 Baum, in which connection the requisite concentrations are in :addition dependent also upon the reaction temperature. By such transparentizing treatment, a parchmentized regenerated cellulose textile material results which lacks clarity and is non-uniform in appearance.
As above stated, for the subsequent treatment caustic potash solution of about 30 Baum at room temperature may be employed, or caustic soda solution may be used in concentrations of 6 to less than 12 Baum with subsequent rapid removal of the caustic to correct this lack of clarity and non-uniformity. The control of the process is more easily effected by the use of caustic potash.
The following examples are illustrative of the process. It is to be understood that these examples are illustrative and the invention is not restricted thereto except as indicated in the appended claims.
Examples 1. Viscose muslin which has been pre-cleansed by the usual methods and dried under tension is passed in the broad state through sulfuric acid of 48 Baum (measured at 15 0.). The temperature of the acid is kept between l C. and +l C.; the time of action amounts to 11 seconds. Immediately thereafter the acid is washed out with .water at room temperature, and any possible residues of acid are neutralized besides with dilute ammonia. The fabric is now freed from the excess of water by pressing or suction, and in still moist condition is then exposed for 6 seconds to the action of caustic potash solution of 30 Baum, freed from caustic by means of hot water at about 70 C., acidified with sulfuric acid of 1 Baum, and washed. The material can now be either blued or dyed by the usual methods, whereupon it is dried under tension in the directions of warp and weft; expediently it is further stentered before the drying.
In this way one obtains an extensively translucent, comparatively but little stiffened fabric. The clarity and uniformity of the fabric picture are considerably improved in comparison with a material that has only been parchmentized with acid.
2. Viscose muslin that has been imprinted with dyes fast to acid and fast to alkali is exposed for 12 seconds to the action of sulfuric acid cooled to C., whose specific gravity measured at 15 C. amounts to 47 Baum, is then washed neutral and dried under tension. Now the material is immersed for seconds at to C. in caustic potash solution of Baum, freed from caustic .with hot water (about 70 C.), acidified, and washed until a neutral reaction is attained. After pressing-off of the excess water, the material is dried under tension. The drying of the material can be effected on a tension frame.
. After the above treatment sequence, one obtains a variegated fabric with greatly increased transparency; in the imprinted parts a deepening of color takes place.
3. A fabric produced from spun rayon of high wet tenacity, for example, No. 80 Eng, is desized, soaped, bleached, dyed, and dried on a tension frame.
Now one passes it through a parchmentizing bath of the following composition:
Per cent Sulfuric acid calculated as H2804 59.6 Urea 14.8
Water 25.6
.The temperature of the bath is kept at 25 C.;
the time of action amounts to 16 seconds. Tm mediately thereafter the material is washed cold, and the moist material is then subjected to aftertreatment with caustic potash solution of 28 Baum for 8 seconds at room temperature. After the freeing from caustic and washing with hot water, the material is stentered and dried under tension. Advantageously, the material is finally calendered besides.
Spun rayon muslin that has been treated in this manner corresponds in appearance to a highgrade cotton organdy.
4. Viscose spun rayon muslin is, in accordance with the usual methods, singed, desized, boiled, bleached, dried on a tension frame, and imprinted with a resist of the following composition:
Grams Titanium dioxide 260 Acetyl cellulose 40 Acetone 500 Phenol Water 50 Now the material is exposed in the open width for 10 seconds to the action of sulfuric acid of 47 Baum. In this process the temperature of the acid should be kept at 10 C. After the complete washing-out of the acid, the material is subjected to after-treatment with caustic potash solution of 30 Baum for 6 seconds at room temperature, .washed hot, neutralized, and dried under tens1on.
In this way one obtains highly contrasting patterns of white opaque printed areas on a transparent ground.
5. Viscose voile is parchmentized at 10 C. for 15 seconds with phosphoric acid of 55 Baum (measured at 15 C.), and immediately thereafter is subjected to after-treatment with caustic potash solution as described in Example 4 and dried under tension.
There results an extensively transparentiz'ed, moderately stiffened fabric.
6. Viscose marquisette is pre-cleansed by the well-known methods and dried on a tension frame. Now the material is passed in the open width through 60% sulfuric acid to which per liter 10 cc. of 40% technical concentrated formaldehyde have been added. The temperature of the acid should be 0 C., the time of action 12 seconds. After the washing out of the acid, the material is dried under tension, whereupon it is subjected to after-treatment with caustic soda solution of 8 Baum for 5 seconds, is washed hot, acidified, and thoroughly rinsed. Finally the fabric is tensed in the warp and weft directions and dried.
An extensively transparent fabric is obtained.
7. A light weight fabric consisting in warp and weft of cuprammonium silk yarns is precleansed by the well-known methods and dried on a tension frame. Now the material is treated in the open width for 12 seconds with sulfuric acid of 475 Baum at a temperature of 0 C. After washing out the acid the fabric is exposed for 6 seconds to the action of caustic potash solution of 28 Baum, washed with hot water to remove the caustic, :acidulated with sulfuric acid of 1 Baum, washed until a neutral reaction .is attained, stentered and dried under tension.
There results a highly transparent, moderately stiffened fabric.
'8. Spun rayon muslin containing effect yarns or twists of cotton is singed, desized, boiled. bleached and dried on a tension frame. Now it is treated with sulfuric acid of 47 Baum as described in Example 4, and after complete washing out of the acid, exposed to the action of caustic soda solution of Baum for 8 seconds, washed with hot water, acidified and washed until a neutral reaction is attained. Finally the fabric is stentered and dried under tension.
There results a transparent fabric containing nontransparentized effect yarns giving interesting optical contrasts.
The fabrics obtained in accordance with the above examples have a uniform appearance where an all-over effect is obtained and the same uniformity may be observed in the transparent patterned goods. In addition the goods are of high quality, are relatively soft, and of marketable character.
The expression regenerated cellulose material as employed in the claims refers to regenerated cellulose in the form of fiber, yarns, and fabrics of such material.
What I claim is:
1. A process which comprises treating regenerated cellulose with an aqueous solution selected from the group consisting of sulfuric acid of about 42 to about 48 B., phosphoric acid of about 50 to about 55 B., hydrochloric acid of the order of B., zinc chloride of the order of 50 B and calcium thiocyanate of the order of B. for a period of time of the order of 10 seconds at a temperature in a range of about room temperature and below, whereby an acid parchmentized regenerated cellulose textile material results which lacks clarity and is non-uniform in appearance, and treating such material substantially free from acid at room temperature with an aqueous caustic alkali solution selected from the group consisting of potassium hydroxide of the order of B. and sodium hydroxide at 6 to less than 12 B. for a period of the order of 10 seconds to produce a clear uniform transparent fabric.
2. A process which comprises treating regenerated cellulose with an aqueous solution of sulfuric acid of about 42 to about 48 B. for a period of time of the order of 10- seconds at a temperature in a range of about room temperature and below, whereby an acid parchmentized regenerated cellulose textile material results which lacks clarity and is non-uniform in appearance, and treating such material substantially free from acid at room temperature with an aqueous caustic alkali solution selected from the group consisting of potassium hydroxide of the order of 30 B. and sodium hydroxide at 6 to less than 12 B. for a period of the order of 10 seconds to produce a clear uniform transparent fabric.
3. A process which comprises treating regenerated cellulose with an aqueous solution of phosphoric acid of about 50 to about B. for a period of time of the order of 15 seconds at a temperature in a range of about room temperature and below, whereby an acid parchmentized regenerated cellulose textile material results which lacks clarity and is non-uniform in appearance, and treating such material substantially free from acid at room temperature with an aqueous solution of potassium hydroxide of about 30 B. for a period of the order of 6 seconds to produce a clear uniform transparent fabric.
4. A clear, uniform, transparent fabric of regenerated cellulose produced by the process of claim 1.
ERNST WEISS.
REFERENCES CITED The following references are of record in the file of this patent:
UNITED STATES PATENTS Number Name Date 1,558,453 Barrett Oct. 27, 1925 1,812,204 Hall June 30, 1931 1,985,124 Weiss Dec. 18, 1934 1,989,100 Lilienfeld Jan. 29, 1935 1,989,101 Lilienfeld Jan. 29, 1935 1,998,577 Heberlein Apr. 23, 1935 2,085,946 Bodmer et al July 6, 1937 2,174,534 Shipp Oct. 3, 1939 2,200,792 Hefti May 14, 1940 2,202,200 Haller et a1. May 28, 1940 2,215,938 Schonholzer Sept. 24, 1940 2,245,123 Belloc June 10', 1941 FOREIGN PATENTS Number Country Date 464,965 Great Britain Apr. 28, 1937 516,843 Great Britain Jan. 12, 1940

Claims (1)

1. A PROCESS WHICH COMPRISES TREATING REGENERATED CELLULOSE WITH AN AQUEOUS SOLUTION SELECTED FROM THE GROUP CONSISTING OF SULFURIC ACID OF ABOUT 42* TO ABOUT 48*BE''., PHOSPHORIC ACID OF ABOUT 50* TO ABOUT 55*BE''., HYDROCHLORIC ACID OF THE ORDER OF 20*BE''., ZINC CHLORIDE OF THE ORDER OF 50*BE''. AND CALCIUM THIOCYANATE OF THE ORDER OF 25*BE''. FOR A PERIOD OF TIME OF THE ORDER OF 10 SECONDS AT A TEMPERATURE IN A RANGE OF ABOUT ROOM TEMPERATURE AND BELOW, WHEREBY AN ACID PARCHMENTIZED REGENERATED CELLULOSE TEXTILE MATERIAL RESULTS WHBICH LACKS CLARITY AND IS NON-UNIFORM IN APPEARANCE, AND TREATING SUCH MATERIAL SUBSTANTIALLY FREE FROM ACID AT ROOM TEMPERATURE WITH AN AQUEOUS CAUSTIC ALKALI SOLUTION SELECTED FROM THE GROUP CONSISTING OF POTASSIUM HYDROXIDE OF THE ORDER OF 30*BE''. AND SODIUM HYDROXIDE AT 6* TO LESS THAN 12*BE''. FOR A PERIOD OF ORDER OF 10 SECONDS TO PRODUCE A CLEAR UNIFORM TRANSPARENT FABRIC.
US637119A 1944-12-27 1945-12-22 Transparentizing regenerated cellulose silk Expired - Lifetime US2516083A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3313592A (en) * 1963-10-21 1967-04-11 Harshaw Chem Corp Process of parchmentizing cellulose with an aqueous solution of boron trifluoride and a strong acid
US3348904A (en) * 1964-02-12 1967-10-24 Brown Co Paper parchmentized with ortho-phosphoric acid

Citations (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1558453A (en) * 1922-04-13 1925-10-27 Tootal Broadhurst Lee Co Ltd Treatment of cellulosic fibers and fabrics
US1812204A (en) * 1927-07-09 1931-06-30 Silver Springs Bleaching & Dye Process in which viscose silk is surjected to the action of caustic alkalis
US1985124A (en) * 1931-11-23 1934-12-18 Heberlein Patent Corp Process for treating cellulose containing fabrics, threads, and the like, and product therefrom
US1989101A (en) * 1928-06-16 1935-01-29 Lilienfeld Leon Process for improving artificial fibers or fabrics
US1998577A (en) * 1926-01-16 1935-04-23 Heberlein Patent Corp Novel artificial silk effects and process of producing same
GB464965A (en) * 1936-04-20 1937-04-28 Cilander Ag Improvements in or relating to methods of treating linen textiles
US2085946A (en) * 1933-05-22 1937-07-06 Heberlein Patent Corp Patterned effects on crepe fabrics
US2174534A (en) * 1936-04-22 1939-10-03 Du Pont Chemical process
GB516843A (en) * 1937-07-26 1940-01-12 Walter Rotta A process for producing finishing or dressing effects on textiles
US2200792A (en) * 1936-09-11 1940-05-14 Firm Ag Cilander Patterned fabric and method of producing the same
US2202200A (en) * 1937-01-30 1940-05-28 Ciba Products Corp Process of producing pattern effects on textile fabrics
US2215938A (en) * 1937-05-07 1940-09-24 Raduner & Co Ag Method of producing noncurling stiffened woven fabrics and product thereof
US2245123A (en) * 1936-07-31 1941-06-10 Nobel Francaise Soc Fabric printing

Patent Citations (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1558453A (en) * 1922-04-13 1925-10-27 Tootal Broadhurst Lee Co Ltd Treatment of cellulosic fibers and fabrics
US1998577A (en) * 1926-01-16 1935-04-23 Heberlein Patent Corp Novel artificial silk effects and process of producing same
US1812204A (en) * 1927-07-09 1931-06-30 Silver Springs Bleaching & Dye Process in which viscose silk is surjected to the action of caustic alkalis
US1989101A (en) * 1928-06-16 1935-01-29 Lilienfeld Leon Process for improving artificial fibers or fabrics
US1989100A (en) * 1928-06-16 1935-01-29 Lilienfeld Leon Process for improving artificial fibrous material
US1985124A (en) * 1931-11-23 1934-12-18 Heberlein Patent Corp Process for treating cellulose containing fabrics, threads, and the like, and product therefrom
US2085946A (en) * 1933-05-22 1937-07-06 Heberlein Patent Corp Patterned effects on crepe fabrics
GB464965A (en) * 1936-04-20 1937-04-28 Cilander Ag Improvements in or relating to methods of treating linen textiles
US2174534A (en) * 1936-04-22 1939-10-03 Du Pont Chemical process
US2245123A (en) * 1936-07-31 1941-06-10 Nobel Francaise Soc Fabric printing
US2200792A (en) * 1936-09-11 1940-05-14 Firm Ag Cilander Patterned fabric and method of producing the same
US2202200A (en) * 1937-01-30 1940-05-28 Ciba Products Corp Process of producing pattern effects on textile fabrics
US2215938A (en) * 1937-05-07 1940-09-24 Raduner & Co Ag Method of producing noncurling stiffened woven fabrics and product thereof
GB516843A (en) * 1937-07-26 1940-01-12 Walter Rotta A process for producing finishing or dressing effects on textiles

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3313592A (en) * 1963-10-21 1967-04-11 Harshaw Chem Corp Process of parchmentizing cellulose with an aqueous solution of boron trifluoride and a strong acid
US3348904A (en) * 1964-02-12 1967-10-24 Brown Co Paper parchmentized with ortho-phosphoric acid

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DE850292C (en) 1952-12-08
BE461347A (en)

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