US3895907A - Turnbull{3 s blue single bath mineral dyeing process (ferri-zirc) for cellulosic textiles - Google Patents
Turnbull{3 s blue single bath mineral dyeing process (ferri-zirc) for cellulosic textiles Download PDFInfo
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/0076—Dyeing with mineral dye
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- 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
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/58—Material containing hydroxyl groups
- D06P3/60—Natural or regenerated cellulose
Definitions
- This invention relates to mineral dyeing of cellulosic textiles. More specifically, this invention relates to a single-bath textile dyeing process which utilizes a ferric salt, and ammonium sulphite of ammonium oxalate as an inhibited reducing agent, which are combined without reaction with an alkali metal ferricyanide and zirconyl ammonium carbonate to produce a stable single bath solution.
- the solution thus prepared remains clear as long as it remains alkaline due to the presence of ammonium ions.
- Turnbulls Blue coloration is imparted to cellulosic textiles.
- the finished product contains the blue coloration combined with zirconia from heat decomposition of the zirconyl ammonium carbonate, causing the Turnbulls Blue-zirconia deposit to lock onto the cellulosic textile, thus making the blue pigment significantly more resistant to alkalis than it would be if the zirconyl ammonium carbonate were not included in the formulation.
- the main object of this invention is to provide a single-bath system for dyeing Turnbulls Blue color shades by a simple pad (wetting and squeezing out excess bath), dry and cure procedure, followed by wash and dry to remove byproducts.
- a second object of this invention is to provide an attractive and appealing color shade for the textile dyer, by shorter processing and requiring less mill equipment.
- a third object of this invention is to provide a singlebath system for Turnbulls Blue mineral dyeing that can be finished with a paraffin-ammonium stearate wax, requiring no after-rinse with aluminum formo-acetate to neutralize the residual stearic acid.
- the hydrous zirconia in the invention dyeing reacts with and neutralizes the stearic acid, without an added step.
- the utility of this invention is obviously in the field of mineral dyeings of cellulosic textiles to obtain attractive and specific blue color shades in finished goods such as curtains, umbrellas, tents, sails, awnings, canvas shoes, upholstery, etc.
- the present invention provides a unique single-bath system where a ferric salt and ammonia inhibited reducing agents; i.e., ammonium. oxalate and ammonium sulfite, are combined together without reaction-with an alkali metal ferricyanide and zirconyl ammonium carbonate-to produce a stable single bath, clear, system as long as it remains alkaline from the presence of ammonium ions. In this state it may be applied to cellulosic textiles. When the wet impregnated textile is heated up to about from l50 to 160C.
- the ammonium salts are decomposed, ammonia leaves the system, and the oxalate and sulfite ions remaining, are capable of reducing the ferric salt to the ferrous state, when it reacts with the ferricyanide in the cellulosic textile, to produce ferrous ferricyanide (Turnbulls Blue).
- the zirconyl ammonium carbonate decomposes to liberate ammonia and carbon dioxide and produce hydrous zirconia, which is deposited as a lake with the Turnbulls Blue dye pigment.
- Beautiful pure blue mineral dyeings are produced in the cellulose by simply wetting and heating the wetted cellulosic to develop the dye.
- the present invention can best be described as a plurality of mineral dye baths as well as a mineral dyeing process for cellulosic textiles.
- One of the preferred embodiments would be described as a dye bath for imparting to cellulosic textiles a durable-to-waterwashing Turnbulls Blue coloration, the said dye bath containing.
- zirconyl ammonium carbonate solution aqueous 10 percent ZI'OQ
- Another of the preferred embodiments of this invention would be described as a mineral dyeing process to impart durable-to-water-washing Turnbulls Blue coloration to cellulosic textiles, the process comprising.
- zirconyl ammonium carbonate solution (aqeuous 10 percent 02);
- EXAMPLE 1 5 Grams of potassium ferricyanide, grams of water and 2 grams of ferric sulphate were dissolved together in 43 grams of water (distilled). To this was added 10 grams of ammonium sulphite (monohydrate) crystals. Upon stirring, a clear brown colored bath resulted. No Turnbulls Blue precipitated, and the sulfite reducer was inhibited by the ammonium (alkaline) ion. This bath was capable of dyeing a pure blue by heat (150C.) decomposition on a cellulosic.
- EXAMPLE 4 The following formulation utilizes both ammonium oxalate and ammonium sulfite for increased bath alka- 5 linity and stability:
- EXAMPLE 5 The incorporation of zirconyl ammonium carbonate (10 percent ZrO into Example 6, produces a brighter pure blue color shade through lake" formation of the Turnbulls Blue with zirconia.
- the following formation variations were prepared and successfully evaluated:
- EXAMPLE 8 The following bath formulation gave excellent color shades, on duck, and showed a bath stability of 10 hours: (6519-82) 3.00 grams Potassium Ferricyanide Crystals 70.00 grams Water 3.00 grams Ammonium oxalate 3.00 grams Ferric Sulphate 10.00 grams Zirconyl Ammonium Carbonate Solution (10% ZrO 9.00 grams Ammonium Sulfite (monohydrate) 2.00 grams monoethanolamine EXAMPLE 9 Samples of scoured duck were wetted with the bath 5 from Example 8 and oven dried at C. for 2 minutes, followed by oven curing at 150C. for 2 minutes. Excellent results were obtained. Other samples were dried at C. for 1 minute, followed by oven curing at 155C. for 1 minute. Excellent results were again ob tained. Evaluations indicate that predrying produces a uniform deposit ofbath solids and reaching a temperature of 150C. or higher is only required to effect decomposition of all ammonium salts.
- a mineral dyeing process for imparting a Turnbulls Blue coloration to cellulosic textiles consisting of impregnating a cellulosic textile with an aqueous solution containing an inhibited reducing agent, ferric salt, and alkali metal ferricyanide, and zirconyl ammonium carbonate, then curing the impregnated cellulosic textile.
- a mineral dyeing process to impart durable-towater washing Turnbulls Blue coloration to cellulosic textiles comprising.
- zirconyl ammonium carbonate solution aqueous 10 percent Z
- a mineral dyeing process to impart durable towater washing Turnbulls Blue coloration to cellulosic textiles comprising.
- zirconyl ammonium carbonate solution aqueous 10 percent ZrO b. removing the excess solution to obtain a wet pickup of about 70-80 percent
- a dye bath for imparting to cellulosic textiles a durable-to-water-washing Turnbulls Blue coloration the said dye bath containing.
- zirconyl ammonium carbonate solution aqueous 10 percent ZrO and about from 60 to 85 parts by weight of water.
- a dye bath for imparting to cellulosic textiles a durable'to-water-washing Turnbulls Blue coloration the said dye bath containing.
- a dye bath for imparting to cellulosic textiles a late monohydrate, Turnbulls Blue coloration the dye bath containing. about from 1 to 5 parts by weight of ferric sulphate, about from 5 to parts by weight of ammonium sul- 1 part b i h f potassium fe i id Phite monohydrate, 5 1 part by weight of ferric sulphate, about from 1 to 5 parts by weight of monoethanol- 1 part by weight of ammonium oxalate, and
- amme 27 parts by weight of water to give a greenish-- about from 5 to 10 parts by weight of zirconyl ammonium carbonate solution (aqueous 10 percent ZrO and about from 60 to 85 parts by weight of water. 6.
- a dye bath for imparting to cellulosic textiles a Tumbulls Blue coloration the dye bath containing.
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Abstract
Certain inhibited reducing agents are combined in a single bath with a ferric salt and an alkali metal ferricyanide, which is activated by heat decomposition of the inhibited reducers, to cause reduction of the ferric salt to the ferrous state on the cellulosic, in contact with the ferricyanide, thereby producing Turnbull''s Blue in the cellulosic textile. A zirconium salt is used in the bath to lock the dye to the cellulosic. The resulting uniform pure blue mineral dyeing of cellulose by this single bath process has been defined as the FERRI-ZIRC BLUE PROCESS.
Description
United States Patent [191 Conner 1 TURNBULLS BLUE SINGLE BATH MINERAL DYEING PROCESS (FERRl-ZIRC) FOR CELLULOSIC TEXTILES [75] Inventor: Charles James Conner, New
Orleans, La.
[73] Assignee: The United States of America as represented by the Secretary of Agriculture, Washington, DC.
[22] Filed: Oct. 10, 1973 [21] Appl. No.: 404,974
[52] US. Cl 8/52; 8/17 [51] Int. Cl D06p 3/60 [58] Field of Search 8/52, 17, 3O
[56] References Cited UNITED STATES PATENTS 1,661,606 3/1928 Escaich 8/52 1,686,540 10/1928 White 8/52 2,214,845 9/1940 Wells 8/52 2,923,592 2/1960 Crosland 8/52 3,671,178 6/1972 Conner 8/52 3,702,753 11/1972 Conner.... 8/52 3,705,004 12/1972 C0nner.... 8/52 3,768,965 10/1973 Conner.... 8/52 3,779,702 12/1973 Conner 8/52 July 22, 1975 Conner 8/52 2/1974 2/1974 Conner OTHER PUBLICATIONS American Dyestuff Reporter, March 1974, pp. 37-45. Textile Research Journal, April 1964, pp. 347-357. Textile Research Journal, February 1967, pp. 94-102. One-Bath Zirchrome Chloride Fungicide and Dye by C. J. Conner, et al.
Primary ExaminerBenjamin R. Padgett Assistant ExaminerD. P. Walsh Attorney, Agent, or FirmM. Howard Silverstein; Max D. Hensley [57] ABSTRACT Certain inhibited reducing agents are combined in a single bath with a ferric salt and an alkali metal ferri- 8 Claims, No Drawings TURNBULLS BLUE SINGLE BATH MINERAL DYEING PROCESS (FERRI-ZIRC) FOR CELLULOSIC TEXTILES A non-exclusive, irrevocable, royalty-free license in the invention herein described throughout the worid for all purposes of the United States Government, with the power to grant sublicenses for such purposes, is hereby granted to the Government of the United States of America.
This invention relates to mineral dyeing of cellulosic textiles. More specifically, this invention relates to a single-bath textile dyeing process which utilizes a ferric salt, and ammonium sulphite of ammonium oxalate as an inhibited reducing agent, which are combined without reaction with an alkali metal ferricyanide and zirconyl ammonium carbonate to produce a stable single bath solution. The solution thus prepared remains clear as long as it remains alkaline due to the presence of ammonium ions. When the prescribed conditions are adhered to a Turnbulls Blue coloration is imparted to cellulosic textiles. The finished product contains the blue coloration combined with zirconia from heat decomposition of the zirconyl ammonium carbonate, causing the Turnbulls Blue-zirconia deposit to lock onto the cellulosic textile, thus making the blue pigment significantly more resistant to alkalis than it would be if the zirconyl ammonium carbonate were not included in the formulation.
The main object of this invention is to provide a single-bath system for dyeing Turnbulls Blue color shades by a simple pad (wetting and squeezing out excess bath), dry and cure procedure, followed by wash and dry to remove byproducts.
A second object of this invention is to provide an attractive and appealing color shade for the textile dyer, by shorter processing and requiring less mill equipment.
A third object of this invention is to provide a singlebath system for Turnbulls Blue mineral dyeing that can be finished with a paraffin-ammonium stearate wax, requiring no after-rinse with aluminum formo-acetate to neutralize the residual stearic acid. The hydrous zirconia in the invention dyeing reacts with and neutralizes the stearic acid, without an added step.
The utility of this invention, therefore, is obviously in the field of mineral dyeings of cellulosic textiles to obtain attractive and specific blue color shades in finished goods such as curtains, umbrellas, tents, sails, awnings, canvas shoes, upholstery, etc.
The prior art teaches that water-soluble ferrous salts react with water soluble alkali metal ferricyanides to produce an insoluble blue dye pigment of ferrous ferricyanide known as Turnbulls Blue. It has also been known from the prior art that cellulosics can be wetted with a ferrous salt, and then with a solution of alkali metal ferricyanide, using two separate baths, to produce ferrous ferricyanide by double decomposition.
Now, this writer has unexpectedly discovered what is disclosed in the process of this invention. The present invention provides a unique single-bath system where a ferric salt and ammonia inhibited reducing agents; i.e., ammonium. oxalate and ammonium sulfite, are combined together without reaction-with an alkali metal ferricyanide and zirconyl ammonium carbonate-to produce a stable single bath, clear, system as long as it remains alkaline from the presence of ammonium ions. In this state it may be applied to cellulosic textiles. When the wet impregnated textile is heated up to about from l50 to 160C. the ammonium salts are decomposed, ammonia leaves the system, and the oxalate and sulfite ions remaining, are capable of reducing the ferric salt to the ferrous state, when it reacts with the ferricyanide in the cellulosic textile, to produce ferrous ferricyanide (Turnbulls Blue). During the same heat cure the zirconyl ammonium carbonate decomposes to liberate ammonia and carbon dioxide and produce hydrous zirconia, which is deposited as a lake with the Turnbulls Blue dye pigment. Beautiful pure blue mineral dyeings are produced in the cellulose by simply wetting and heating the wetted cellulosic to develop the dye.
EQUATIONS PERTINENT TO THIS INVENTION ferrous ferricyanide Blue *R represents either sodium or potassium.
Fe; [Fe(CN) .ZrO .2H O Turnbulls Blue-zirconia mineral dye SUMMARY OF THE INVENTION In brief the present invention can best be described as a plurality of mineral dye baths as well as a mineral dyeing process for cellulosic textiles. One of the preferred embodiments would be described as a dye bath for imparting to cellulosic textiles a durable-to-waterwashing Turnbulls Blue coloration, the said dye bath containing.
about from 1 to 5 parts by weight of sodium or potassium ferricyanide,
about from 2 to 5 parts by weight of ammonium oxalate monohydrate,
about from 1 to 5 parts by weight of ferric sulphate,
about from 5 to 10 parts by weight of zirconyl ammonium carbonate solution (aqueous 10 percent ZI'OQ), and
about 60 to parts by weight of water.
Another of the preferred embodiments of this invention would be described as a mineral dyeing process to impart durable-to-water-washing Turnbulls Blue coloration to cellulosic textiles, the process comprising.
a. impregnating a cellulosic textile with an aqueous solution containing. about from 1 to 5 parts by weight of potassium ferricyanide, about from 2 to 5 parts by weight of ammonium oxalate monohydrate, about from 1 to 5 parts by weight of ferric sulphate,
about from to parts by weight of ammonium sulphite monohydrate,
about from 1 to 5 parts by weight of monoethanolamine, and
about from 5 to 10 parts by weight of zirconyl ammonium carbonate solution (aqeuous 10 percent 02);
b. removing the excess solution to obtain a wet pickup of about 70-80 percent,
c. drying. the wet impregnated textile for about 2 minutes at about 120 to 130C., and
d. curing the textile for about 2 minutes at about from 150 to 155C.
The following examples are provided to illustrate the preferred embodiments of the invention, and should not be construed as limiting the invention in any manner whatever. The various formulations and techniques were employed with paper, wood, and other textiles having partial quantities of cellulose.
EXAMPLE 1 5 Grams of potassium ferricyanide, grams of water and 2 grams of ferric sulphate were dissolved together in 43 grams of water (distilled). To this was added 10 grams of ammonium sulphite (monohydrate) crystals. Upon stirring, a clear brown colored bath resulted. No Turnbulls Blue precipitated, and the sulfite reducer was inhibited by the ammonium (alkaline) ion. This bath was capable of dyeing a pure blue by heat (150C.) decomposition on a cellulosic.
EXAMPLE 4 The following formulation utilizes both ammonium oxalate and ammonium sulfite for increased bath alka- 5 linity and stability:
grams distilled water grams distilled water grams ferric sulphate grams ammonium oxalate grams ammonium sulfite (monohydrate) grams monoethanolamine grams Clear Greenish-Black Bath 2 PPPPP!" 0 000000 The addition of a small amount of monoethanolamine gives an increased alkaline stability and bath stability.
EXAMPLE 5 EXAMPLE 6 The incorporation of zirconyl ammonium carbonate (10 percent ZrO into Example 6, produces a brighter pure blue color shade through lake" formation of the Turnbulls Blue with zirconia. The following formation variations were prepared and successfully evaluated:
to 5.00 grams Sodium or Potassium Ferricyanide Crystals to 85.00 grams Water (distilled or soft) to 5.00 grams Ammonium Oxalate Crystals (monohydrate) to 5.00 grams Ferric Sulphate (Fe (SO.,) H O) to 1000 grams Zirconyl Ammonium Carbonate Solution (10% ZrO to 10.00 grams Ammonium Sulfite Crystals (monohydrate) to 5.00 grams Monoethanolamine EXAMPLE 2 EXAMPLE 3 One gram of potassium ferricyanide, 1 gram of ferric sulphate, and 1 gram of ammonium oxalate were dissolved together in 27 grams of distilled water. A greenish-yellow single bath resulted, all ingredients being solgrams of Clear Greenish-Black Single Bath (Ferri-Zirc) uble. On wetting a piece of scoured duck (2X4 inches) with the bath and then heating it to 150C. for 2 minutes, a deposit of Turnbulls Blue was produced, dyeing the fabric pure deep Turnbulls Blue, and showing ammonium oxalate to be a suitable inhibited reducer in the bath. Due to lack of sufficient ammonium ion alkalinity, the bath stability was poor, and some blue precipitations occurred in the bath after 10 minutes. (5993-121) EXAMPLE 7 All of the above bath variations could be used successfully to produce single bath Turnbulls Blue color shades with heat curings at l50-155C for l to 3 minutes, using scoured duck or paper.
EXAMPLE 8 The following bath formulation gave excellent color shades, on duck, and showed a bath stability of 10 hours: (6519-82) 3.00 grams Potassium Ferricyanide Crystals 70.00 grams Water 3.00 grams Ammonium oxalate 3.00 grams Ferric Sulphate 10.00 grams Zirconyl Ammonium Carbonate Solution (10% ZrO 9.00 grams Ammonium Sulfite (monohydrate) 2.00 grams monoethanolamine EXAMPLE 9 Samples of scoured duck were wetted with the bath 5 from Example 8 and oven dried at C. for 2 minutes, followed by oven curing at 150C. for 2 minutes. Excellent results were obtained. Other samples were dried at C. for 1 minute, followed by oven curing at 155C. for 1 minute. Excellent results were again ob tained. Evaluations indicate that predrying produces a uniform deposit ofbath solids and reaching a temperature of 150C. or higher is only required to effect decomposition of all ammonium salts.
EXAMPLE l The amount of monoethanolamine in Example 8, was
varied'up to 5 grams, and the bath stability observed.
With 5 grams of this amine stabilizer, the life of the bath was increased to 48 hours.
EX MPLE 1 1 The incorporation of zirconyl ammonium carbonate in the dye also results in a Turnbulls Blue zirconia dyeing on cellulosics, which is much more resistant to alka line water washing than dyeing from the dye bath with out zirconyl ammonium carbonate. Two baths were prepared as follows:
gram Potassium or Sodium Ferricyanide gram Water (soft or distilled) grams Ammonium Oxalate grams Ferric Sulphate grams Zirconyl Ammonium Carbonate ZrO grams ammonium Sulphite grams Monocthanolamine grams Bath A (with Zr) gram Potassium or Sodium Ferryanide gram Water (soft or distilled) gram Ammonium Oxalate gram Ferric Sulphate gram Amminium Sulphate gram Monocthanolamine gram Bath 8 (No Zr) EXAMPLE 12 The fabric sample A from Example 1 l after cure and wash, was wetted with a 7 percent paraffin emulsion (paraffimammonium stearate type), squeezed free of excess liquid, and oven dried at ll C. for 2 minutes, followed by raising the temperature to 150C. for 1 minute. The cooled paraffin finished sample was deep blue in color, and water repellent (spray rated 90-100).
1 claim:
1. A mineral dyeing process for imparting a Turnbulls Blue coloration to cellulosic textiles, the process consisting of impregnating a cellulosic textile with an aqueous solution containing an inhibited reducing agent, ferric salt, and alkali metal ferricyanide, and zirconyl ammonium carbonate, then curing the impregnated cellulosic textile.
2. A mineral dyeing process to impart durable-towater washing Turnbulls Blue coloration to cellulosic textiles, the process comprising.
a. impregnating a cellulosic textile with an aqueous solution containing.
about from 1 to 5 parts by weight of sodium ferricyanide,
about from 2 to 5 parts by weight of ammonium oxalate monohydrate,
about from 1 to 5 parts by weight of ferric sulphate,
about from 1 to 10 parts by weight of ammonium sulphite monohydrate,
about from 1 to 5 parts by weight of monoethanol' amine, and
about from 5 to 10 parts by weight of zirconyl ammonium carbonate solution (aqueous 10 percent Z);
b. removing the excess solution to obtain a wet pickup of about -80 percent,
c. drying the wet impregnated textile for about 2 minutes at about to C, and
d. curing the textile for about 2 minutes at about from to C.
3. A mineral dyeing process to impart durable towater washing Turnbulls Blue coloration to cellulosic textiles, the process comprising.
a. impregnating a cellulosic textile with an aqueous solution containing.
about from l to 5 parts by weight of potassium ferricyanide,
about from 2 to 5 parts by weight of ammonium oxalate monohydrate,
about from 1 to 5 parts by weight of ferric sulphate,
about from 5 to 10 parts by weight of ammonium sulphite monohydrate,
about from 1 to 5 parts by weight of monoethanolamine, and
about from 5 to 10 parts by weight of zirconyl ammonium carbonate solution (aqueous 10 percent ZrO b. removing the excess solution to obtain a wet pickup of about 70-80 percent,
c. drying the wet impregnated textile for about 2 minutes at about 120 to 130C, and
d. curing the textile for about 2 minutes at about from 150 to 155C.
4. A dye bath for imparting to cellulosic textiles a durable-to-water-washing Turnbulls Blue coloration, the said dye bath containing.
about from 1 to 5 parts by weight of sodium ferricyanide,
about from 2 to 5 parts by weight of ammonium oxalate monohydrate,
about from 1 to 5 parts by weight of ferric sulphate,
about from 5 to 10 parts by weight of ammonium sulphite monohydrate,
about from 1 to 5 parts by weight of monoethanolamine,
about from 50 to 10 parts by weight of zirconyl ammonium carbonate solution (aqueous 10 percent ZrO and about from 60 to 85 parts by weight of water.
5. A dye bath for imparting to cellulosic textiles a durable'to-water-washing Turnbulls Blue coloration, the said dye bath containing.
about from 1 to 5 parts by weight of potassium ferricyanide,
7 8 about from 2 to parts by weight of ammonium oxa- 7. A dye bath for imparting to cellulosic textiles a late monohydrate, Turnbulls Blue coloration, the dye bath containing. about from 1 to 5 parts by weight of ferric sulphate, about from 5 to parts by weight of ammonium sul- 1 part b i h f potassium fe i id Phite monohydrate, 5 1 part by weight of ferric sulphate, about from 1 to 5 parts by weight of monoethanol- 1 part by weight of ammonium oxalate, and
amme 27 parts by weight of water to give a greenish-- about from 5 to 10 parts by weight of zirconyl ammonium carbonate solution (aqueous 10 percent ZrO and about from 60 to 85 parts by weight of water. 6. A dye bath for imparting to cellulosic textiles a Turnbulls Blue coloration, the dye bath containing.
yellow solution. 8. A dye bath for imparting to cellulosic textiles a Tumbulls Blue coloration, the dye bath containing.
3 parts by weight of sodium ferricyanide, 3 parts by weight of ferric sulphate, 3 parts by weight of ammonium oxalate,
5 parts by weight of potassium ferricyanide, 2 parts by weight of ferric sulphate, 9 parts by weight of ammonium sulfite monohydrate, 10 parts by weight of ammonium sulphite monohy- 2 Parts y weight of monoethaflolamine, and
d w, d 80 parts by weight of water to give a clear greenparts by weight of water to give a clear brown ish-black solution.
solution. 20
Claims (8)
1. A MINERAL DYEING PROCESS FOR IMPARTING A TURNBULLS BLUE COLORATION TO CELLULOSIC TEXTILES THE PROCESS CONSISTING OF IMPREGNATING A CELLULOSIC TEXTILE WITH AN AQUEOUS SOLUTION CONTAINING AN INHIBITED REDUCING AGENT FERRIC SALT AND ALKALI METAL FERRICYANIDE AND ZIRCONYL AMMONIUM CARBONATE THEN CURING THE IMPREGNATED CELLULOSIC TEXTILE.
2. A mineral dyeing process to impart durable-to-water washing Turnbull''s Blue coloration to cellulosic textiles, the process comprising. . . a. impregnating a cellulosic textile with an aqueous solution containing. . . about from 1 to 5 parts by weight of sodium ferricyanide, about from 2 to 5 parts by weight of ammonium oxalate monohydrate, about from 1 to 5 parts by weight of ferric sulphate, about from 1 to 10 parts by weight of ammonium sulphite monohydrate, about from 1 to 5 parts by weight of monoethanolamine, and about from 5 to 10 parts by weight of zirconyl ammonium carbonate solution (aqueous 10 percent ZrO2); b. removing the excess solution to obtain a wet pickup of about 70-80 percent, c. drying the wet impregnated textile for about 2 minutes at about 120* to 130*C., and d. curing the textile for about 2 minutes at about from 150* to 155*C.
3. A mineral dyeing process to impart durable-to-water washing Turnbull''s Blue coloration to cellulosic textiles, the process comprising. . . a. impregnating a cellulosic textile with an aqueous solution containing. . . about from 1 to 5 parts by weight of potassium ferricyanide, about from 2 to 5 parts by weight of ammonium oxalate monohydrate, about from 1 to 5 parts by weight of ferric sulphate, about from 5 to 10 parts by weight of ammonium sulphite monohydrate, about from 1 to 5 parts by weight of monoethanolamine, and about from 5 to 10 parts by weight of zirconyl ammonium carbonate solution (aqueous 10 percent ZrO2); b. removing the excess solution to obtain a wet pickup of about 70-80 percent, c. drying the wet impregnated textile for about 2 minutes at about 120* to 130*C., and d. curing the textile for about 2 minutes at about from 150* to 155*C.
4. A dye bath for imparting to cellulosic textiles a durable-to-water-washing Turnbull''s Blue coloration, the said dye bath containing. . . about from 1 to 5 parts by weight of sodium ferricyanide, about from 2 to 5 parts by weight of ammonium oxalate monohydrate, about from 1 to 5 parts by weight of ferric sulphate, about from 5 to 10 parts by weight of ammonium sulphite monohydrate, about from 1 to 5 parts by weight of monoethanolamine, about from 50 to 10 parts by weight of zirconyl ammonium carbonate solution (aqueous 10 percent ZrO2), and about from 60 to 85 parts by weight of water.
5. A dye bath for imparting to cellulosic textiles a durable-to-water-washing Turnbull''s Blue coloration, the said dye bath containing. . . about from 1 to 5 parts by weight of potassium ferricyanide, about from 2 to 5 parts by weight of ammonium oxalate monohydrate, about from 1 to 5 parts by weight of ferric sulphate, about from 5 to 10 parts by weight of ammonium sulphite monohydrate, about from 1 to 5 parts by weight of monoethanolamine, about from 5 to 10 parts by weight of zirconyl ammonium carbonate solution (aqueous 10 percent ZrO2), and about from 60 to 85 parts by weight of water.
6. A dye bath for imparting to cellulosic textiles a Turnbull''s Blue coloration, the dye bath containing. . . 5 parts by weight of potassium ferricyanide, 2 parts by weight of ferric sulphate, 10 parts by weight of ammonium sulphite monohydrate, and 20 parts by weight of water . . . to give a clear brown solution.
7. A dye bath for imparting to cellulosic textiles a Turnbull''s Blue coloration, the dye bath containing. . . 1 part by weight of potassium ferricyanide, 1 part by weight of ferric sulphate, 1 part by weight of ammonium oxalate, and 27 parts by weight of water . . . to give a greenish-yellow solution.
8. A dye bath for imparting to cellulosic textiles a Turnbull''s Blue coloration, the dye bath containing. . . 3 parts by weight of sodium ferricyanide, 3 parts by weight of ferric sulphate, 3 parts by weight of ammonium oxalate, 9 parts by weight of ammonium sulfite monohydrate, 2 parts by weight of monoethanolamine, and 80 parts by weight of water . . . to give a clear greenish-black solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US404974A US3895907A (en) | 1973-10-10 | 1973-10-10 | Turnbull{3 s blue single bath mineral dyeing process (ferri-zirc) for cellulosic textiles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US404974A US3895907A (en) | 1973-10-10 | 1973-10-10 | Turnbull{3 s blue single bath mineral dyeing process (ferri-zirc) for cellulosic textiles |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US3895907A true US3895907A (en) | 1975-07-22 |
Family
ID=23601797
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US404974A Expired - Lifetime US3895907A (en) | 1973-10-10 | 1973-10-10 | Turnbull{3 s blue single bath mineral dyeing process (ferri-zirc) for cellulosic textiles |
Country Status (1)
| Country | Link |
|---|---|
| US (1) | US3895907A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101509205B (en) * | 2009-03-05 | 2011-02-02 | 苏州大学 | Dyeing and functionally finishing integrated processing method for textile |
| WO2011105689A1 (en) * | 2010-02-26 | 2011-09-01 | Korea University Research And Business Foundation | Agents for improving dye fastness |
| CN102953293A (en) * | 2012-11-14 | 2013-03-06 | 安徽山鹰纸业股份有限公司 | Combined dyeing process of regenerative lined box paperboards |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1661606A (en) * | 1922-11-25 | 1928-03-06 | Escaich Auguste | Dyeing process |
| US1686540A (en) * | 1926-12-23 | 1928-10-09 | Vivatex Processes Inc | Mineral dyeing |
| US2214845A (en) * | 1939-05-06 | 1940-09-17 | Dow Chemical Co | Improving color of iron stained material |
| US2923592A (en) * | 1954-12-01 | 1960-02-02 | Crosland Percy Field | Processes of dyeing cellulosic materials with inorganic metallic compounds |
| US3671178A (en) * | 1970-05-19 | 1972-06-20 | Us Agriculture | Single bath process for orange to brown mineral dyeings,with and without fungicide,using iron,manganese,and zirconium (zirc-ox process) |
| US3702753A (en) * | 1970-05-19 | 1972-11-14 | Us Agriculture | Pad bath formulation of iron salt,ammonium oxalate and zirconyl ammonium carbonate |
| US3705004A (en) * | 1970-05-19 | 1972-12-05 | Us Agriculture | Pad bath formulation of iron salt,potassium permanganate,ammonium oxalate and zirconyl ammonium carbonate |
| US3768965A (en) * | 1971-08-31 | 1973-10-30 | Us Agriculture | Activated single bath pearl gray chrome green mineral dyeing and composition therefor |
| US3779702A (en) * | 1972-05-05 | 1973-12-18 | Us Agriculture | Bright pink, lavender and blue mineral dyeing single bath process for cellulosics |
| US3791786A (en) * | 1972-04-05 | 1974-02-12 | Agriculture | Process for brown mineral dyeings of cellulosics without oxidative degradation (tendering), from a single bath |
| US3794466A (en) * | 1972-04-27 | 1974-02-26 | Us Agriculture | Single bath chromic chloride mineral dyeing process for cellulosics |
-
1973
- 1973-10-10 US US404974A patent/US3895907A/en not_active Expired - Lifetime
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1661606A (en) * | 1922-11-25 | 1928-03-06 | Escaich Auguste | Dyeing process |
| US1686540A (en) * | 1926-12-23 | 1928-10-09 | Vivatex Processes Inc | Mineral dyeing |
| US2214845A (en) * | 1939-05-06 | 1940-09-17 | Dow Chemical Co | Improving color of iron stained material |
| US2923592A (en) * | 1954-12-01 | 1960-02-02 | Crosland Percy Field | Processes of dyeing cellulosic materials with inorganic metallic compounds |
| US3671178A (en) * | 1970-05-19 | 1972-06-20 | Us Agriculture | Single bath process for orange to brown mineral dyeings,with and without fungicide,using iron,manganese,and zirconium (zirc-ox process) |
| US3702753A (en) * | 1970-05-19 | 1972-11-14 | Us Agriculture | Pad bath formulation of iron salt,ammonium oxalate and zirconyl ammonium carbonate |
| US3705004A (en) * | 1970-05-19 | 1972-12-05 | Us Agriculture | Pad bath formulation of iron salt,potassium permanganate,ammonium oxalate and zirconyl ammonium carbonate |
| US3768965A (en) * | 1971-08-31 | 1973-10-30 | Us Agriculture | Activated single bath pearl gray chrome green mineral dyeing and composition therefor |
| US3791786A (en) * | 1972-04-05 | 1974-02-12 | Agriculture | Process for brown mineral dyeings of cellulosics without oxidative degradation (tendering), from a single bath |
| US3794466A (en) * | 1972-04-27 | 1974-02-26 | Us Agriculture | Single bath chromic chloride mineral dyeing process for cellulosics |
| US3779702A (en) * | 1972-05-05 | 1973-12-18 | Us Agriculture | Bright pink, lavender and blue mineral dyeing single bath process for cellulosics |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101509205B (en) * | 2009-03-05 | 2011-02-02 | 苏州大学 | Dyeing and functionally finishing integrated processing method for textile |
| WO2011105689A1 (en) * | 2010-02-26 | 2011-09-01 | Korea University Research And Business Foundation | Agents for improving dye fastness |
| US20110209294A1 (en) * | 2010-02-26 | 2011-09-01 | Korea University Research And Business Foundation | Agents for improving dye fastness |
| US8900330B2 (en) | 2010-02-26 | 2014-12-02 | Korea University Research And Business Foundation | Agents for improving dye fastness |
| CN102953293A (en) * | 2012-11-14 | 2013-03-06 | 安徽山鹰纸业股份有限公司 | Combined dyeing process of regenerative lined box paperboards |
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