US2592852A - Process of producing dyed lustrous printed pattern effects using acidcuring resins and free leuco bases of vat dyes - Google Patents

Process of producing dyed lustrous printed pattern effects using acidcuring resins and free leuco bases of vat dyes Download PDF

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Publication number
US2592852A
US2592852A US20114A US2011448A US2592852A US 2592852 A US2592852 A US 2592852A US 20114 A US20114 A US 20114A US 2011448 A US2011448 A US 2011448A US 2592852 A US2592852 A US 2592852A
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United States
Prior art keywords
fabric
printing
lustrous
paste
printed
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Expired - Lifetime
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US20114A
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English (en)
Inventor
Jr George Alan Billingsley
William P Hall
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Joseph Bancroft and Sons Co
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Joseph Bancroft and Sons Co
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Priority to US20114A priority Critical patent/US2592852A/en
Priority to DEP29463D priority patent/DE845337C/de
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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
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06Q—DECORATING TEXTILES
    • D06Q1/00—Decorating textiles
    • D06Q1/08—Decorating textiles by fixation of mechanical effects, e.g. calendering, embossing or Chintz effects, using chemical means
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S8/00—Bleaching and dyeing; fluid treatment and chemical modification of textiles and fibers
    • Y10S8/916—Natural fiber dyeing
    • Y10S8/918—Cellulose textile

Definitions

  • This invention relates to. dyed durable lustrous printed, pattern effects for cellulose textile fabrics.
  • the primary object of the present invention is to provide a process whereby vat dyes may be incorporated in the resinous printing paste and sharp, distinct, colored, lustrous mechanical finished patterns may be obtained having excel lent light and wash fastness and without smearing and mark-oil? of the pattern on the unprinted portion of the cloth.
  • vat type of dye it is especially valuable to be able to use a vat type of dye since this type allows a complete and full range of colors of a high degree of durability to light and washing, and exceptionally good and durable results are obtained with, the better grades of anthraquinone and thio-indigo types which are recommended for this process.
  • dyes come on the market in pigment form, i. e., they are in particle form, each particle containing thousands of dye molecules.
  • the dyestufl has no aflinity for the cellulose fibers and if printed upon the fabric, will mark-01f in the glazer and bleed and wash oif during subsequent washing.
  • vat dye or dyes are first treated in an alkaline solution containing a reducing agent, usually caustic soda and sodium hydrosulfite which will reduce the dyestuff" into what is called the leuco form underwhich conditions the dyestuff is obtained in the solution in the molecular or semi-molecular form as the sodium salt of the leuco base of the dyestuff.
  • a reducing agent usually caustic soda and sodium hydrosulfite
  • Dispersing agents such as- Blancol (sodium naphthalene sulfonate-formaldehyde) may also be added to aid the dispersion.
  • the solution containing the leuco base is now mixed into the printing paste containing the usual type of printing gum or mixtures of printing gums such as, for example, starch, converted starch, gum tragacanth, karaya gum, locust bean gum, kelgin gums, methyl cellulose polymerized styrene gum, and acrylate gum.
  • printing gums such as, for example, starch, converted starch, gum tragacanth, karaya gum, locust bean gum, kelgin gums, methyl cellulose polymerized styrene gum, and acrylate gum.
  • Any well known printing gum may be used provided it does not undesirably alter the state of the dyestuif nor interfere with the setting of the resinous material used.
  • Theprinting paste also contains the thermosetting resin forming ingredients which may be, for example, melamine-formaldehyde, phenolformaldehyde, urea-formaldehyde, dicyandiamide-formaldehyde, urea-glyoxal, and mixtures of melamine-formaldehyde, and urea-formaldehyde.
  • thermosetting resin forming ingredients may be, for example, melamine-formaldehyde, phenolformaldehyde, urea-formaldehyde, dicyandiamide-formaldehyde, urea-glyoxal, and mixtures of melamine-formaldehyde, and urea-formaldehyde.
  • thermo-setting resin serve as the printing gum by using, for example, polyvinyl alcohol-formaldehyde, methyl celluloseglyoxal, or starch-formaldehyde thermo-sctting materials. These products while serving as the resin forming material also have enough viscosity in solution to serve as the printing gum. Usually, under these conditions, a stiffer print is obtained and this is somewhat desirable.
  • a catalyst may be dispensed with, but usually it is found advantageous to add a catalyst to speed the setting of the thermo-setting materials.
  • the usual type of catalysts such as, for example, diammonium phosphate, ammonium 'thiocyanate, di-monoethanolamine phosphate, ammonium sulfate, and di-propanolamine phosphate, may be employed. Catalysts should preferably not be used which would precipitate the dyestuif.
  • Similar printing pastes as the ones described above may be prepared using the leuco ester type of vat dyes sold on the market under the commercial names of Algosol and Indigosol. Since these leuco ester compounds of the vat dyestuff form molecular dispersions when added to water, it is possible to add these directly to the printing gum containing the thermosetting resin catalyst and lubricant together with an acid such as lactic, acetic, and sulphuric, and a mild oxidizing agent such as sodium nitrite; these latter serving to change the leuco ester dyestuff into a molecular or semi-molecular dispersion of the vat dyestuff during the processing which is identical with the procedure already described for the regular type of vat dyestuff.
  • an acid such as lactic, acetic, and sulphuric
  • a mild oxidizing agent such as sodium nitrite
  • the printing paste may also contain a lubricant to prevent the sticking and chewing of the cloth when passing through the mechanical equipment. This addition becomes necessary when large printed patterns are glazed as these would not go through the glazer without some lubrication.
  • Sulfonated vegetable, petroleum, and animal oil may be used but care should be taken that these products do not flocculate or coagulate the leuco base vat dye dispersion when added to the printing paste as this will be detrimental.
  • Lubricants of a permanent character which have a tendency to remain in the print after the final washing may also be used; these will act as softeners in the finished fabric and may also impart water resistance which is sometimes desirable when the fabric is subsequently to be overdyed as will be further explained.
  • durable lubricants we may mention cation-active softeners, such as, for example, Triton K-GO (tetra alkyl quaternary ammonium chloride), Amonyx T (trialkylbenzyl ammonium chloride), stearamidomethylpyridinium chloride, and stearyloxymethylpyridinium chloride. The last two products will also impart water resistance to the finished printed pattern.
  • the fabric is printed in a customary manner, the number of printing rolls employed corresponding to the number of different colors in the pattern.
  • the printing may also be done by means of the system known as screen printing instead of on one of the regular types of printing machines.
  • the cloth After printing, the cloth is carefully dried until the printed portion of the fabric Preferably contains from 5% to 15% moisture by weight of the fabric above that of the normal moisture content of the fabric. After the cloth has been dried, it may be advantageously cooled by passing it either through a cooling chamber or over cooling cans.
  • the printed portion containing the thermo-setting material will, after curing, be durable to the subsequent washing treatment and the mechanical finish will remain, resulting in a two-tone effect between the printed and the unprinted portion, showing a high glossy print against a durable background.
  • the heated bowls on the friction calender are operated between 300 F. and 400 F., polymerization will occur on the calender, and if a sufiicient number of runs are given, the polymerization of the resinous material may actually be completed thereon. In case the polymerization is not completed on the calender, it is advantageous to give the fabric a short cure at elevated temperature to complete the setting.
  • the heated steel bowl has the higher surface speed.
  • calenders imparting mechanical finishes to textile fabrics may also be used.
  • the chase and flat nip calenders we prefer to operate at a temperature of from approximately 200 F. to 300 F. on heated bowls.
  • the schreiner and embossing calenders we prefer to operate between the temperatures of approximately 200 F. to 400 F.
  • the curing of the resin depends to some extent upon the previous treatment the cloth has received. As stated above, it is possible to completely cure the fabric by multiple runs on a calender operating at high temperatures. When operating at the lower temperatures using two or perhaps three runs, it is preferable to cure the fabric in an oven at a temperature ranging from 250 F. to 400 F., and a period of time rangin from 10 minutes to 1 minute. In the case of the chaser and the fiat nip calender, we prefer to cure the fabric in an oven at a temperature ranging from about 250 F. to about 400 F., for a period of time ranging from about 15 minutes to about 2 minutes.
  • Thatthe pattern does not mark off even when using a hot friction calender, we attribute to. the fact that the d'yestuifis. present inthe printing paste primarily in a molecular or semi-molecular form rather than in large pigment particle form, so that when printed and partly dried, the. dyestuif penetrates and adheres to the fabric. and stays there during the calendering rather than sticking on the hot bowl and then marking off on the cloth.
  • the same dyestufi as sold in pigment form is added to the same printing paste, printed; dried, and calendered, it will. be found to smear and mark-on" within a few yards.
  • vat dyestufi after printing and before calenderingsince such treatment would smear the pattern.
  • the usual steam aging method of developing vat prints cannot be used prior to calendering since the steam aging sets up the resinous material, resulting in a non-durable mechanical finish.
  • To develop the dyestufi after calendering and curing is also impractical since the strong chemical treatments at elevated temperatures necessary to develop the dyes will either destroy or seriously reduce the mechanical finish.
  • the cured fabric may be run through an oxidizing solution to insure complete conversion of the leuco dyestuff to. the. keto. or insoluble. form.
  • an oxidizing solution for example, hydrogen peroxide, sodium perborate, and potassium dichromate may be used. This step, however, is not necessary since ithas. been found that the contact with the air during printing, drying, and curing, has for all practical purposes already converted the dyestuif to the keto or insoluble form.
  • caustic soda and sodium. hydrosulphite to reduce and disperse the vat. dyestufi
  • the caustic soda may be substituted by potassium hydroxide, trisodium phosphate, soda ash, triethanolamine, and other strong alkalies.
  • the hydrosulphite maybe substituted by sodium sulfoxylate formaldehyde, sodium ibisulphi-te, sodium hydrosulphite formaldehyde, and others.
  • sodium liydrosulphite and caustic soda are used in proportions which vary according to dyestulf but which are well known in the art.
  • thermo-setting material in the printing may be varied between wide limits, depending upon the degree of stillnessv desired in the printed. portion.
  • the latter may vary between a softflexible print. approaching the unprinted part of the cloth. in hand to a firm stifi pattern imposed upon a soft flexible background of unprinted cloth.
  • we. operate. between 6% thermosetting materialin the printin gum to 25% by weight of the paste.
  • the percentage of dyestuir' may also be varied. It is, of course, rather difiicult: to give a: lower limit since. the printing; paste may be applied: in the tinted form, in. which case. only a very small quantity of dyestuif is used, say .l% by weight of the paste.
  • the upper limit on the percentage of dyestuif varies, depending upon the ease with which a dyestuif will. mark. ofi during the mechanical processing and. also upon many other factors, such as percentage of moisture in the printybefore the; mechanical: treatmenitis; applied. type of gum, lubricant, and other ingredients.
  • the patterns. represent approximately 80% coverage
  • no difficulty is encountered in passing the fabric through the friction calender.
  • the friction calender if the coverage is substantially less, than 80%, then it is desirable, in order to prevent chewing of the fabric, to size the fabric before printing with a sizing producing. substantially the. same coefiicient of friction as the printed areas after printing.
  • the sizing solution should contain a small percentage of the lubricants mentioned previously, usually about 10% by weight, and may in addition also contain a small percentage of some stiffening agent such as, for example, dextrin, casein, glucose, and starch.
  • the fabric after curing or after washing and drying may be subjected to further auxiliary textile treatments to produce new and novel effects.
  • a sheer lawn having the lustrous colored patterns applied may be subjected to cellulose swelling treatments such as, for example, treatments with cuprammonium solutions and caustic sodium zincate solutions to produce organdy effects, the final results. being alustrous colored pattern on a sheer organdy fabric.
  • Example I The printing paste was made by first preparing the molecular or the very fine dispersion of the vat" dye-stuff. The following formula was used to prepare this dispersion:
  • a 40", 48/48, 3.50, cotton fabric which had previously been purified through the regular bleaching process was printed by passing it through a regular textile printing machine followed by careful drying, so that approximately 10% moisture above the normal moisture remained in the printed portion of the cloth.
  • the cloth was then taken to a conventional friction calender having a friction ratio of 3:1, a total pressure of 40 tons, and a temperature of the upper steel bowl of approximately 350 F. The cloth was given three runs through this calender and during this procedure, no mark-off, smearing, or staining of the unprinted portion of the cloth took place.
  • Example If A dispersion of reduced vat dyestuff was prepared as described in Example I, except that Ponsol Violet BN Paste (C. I. 1163) was used as the dyestuff.
  • the printing paste used in'this case had the following composition:
  • a 40", 46/40, 3.50, spun rayon fabric was presized by padding it through a solution containing dextrine and /2% sulphonated tallow by weight and then framing to width.
  • the cloth so prepared was printed in the regular printing machine, using the conventional methods of printing and using the printing pastes described above.
  • the cloth after printing was carefully dried until approximately 10% of residual moisture above the normal moisture remained in the printed portions of the fabric.
  • This fabric was then passed once through a 5-bowl heavyweight chasing calender, using a temperature of 300 F. on the heated bowls and a total pressure of 30 tons on the machine.
  • the cloth was then washed through a warm solution containing a small quantity of detergent and alkaline material, followed by a thorough washing in warm water.
  • the fabric was then extracted and frame dried.
  • the resulting cloth had a mellow, deep-seated lustrous, colored pattern imposed upon a dull white background of unprinted cloth. This eifect was durable to drycleaning, soaping, treatments, and light.
  • Example III Dispersion of the leuco base was prepared as previously described, using the following formulation:
  • a printing paste having the following composition was prepared:
  • Example IV A four-color lustrous printed pattern on a dull dyed fabric was obtained.
  • Example V A printing paste of the following composition was made up:
  • Algosol Green lBW Paste (C. I. 1101) 75 Carbowax 1500 1000 Lactic acid (85%) 100 Ammonium thiocyanate 120 Aerotex M-3 2000 Sodium nitrite 150 Supertex T-125 4000 Water 2400 Color was pasted with small amount of water, added to Supertex T125, and mixed thoroughly. Sodium nitrite, Aerotex M-3, and Carbowax 1500, put into solution and added in order. Finally, the lactic acid (85%) and ammonium thiocyanate in water solution were added and the total mixture was strained. Printing and processing was carried out as described in Example I.
  • An aqueous printing paste for use in producing durable mechanical colored lustrous pattern effects on cellulose textile fabrics which tern efiects on cellulose textile fabrics, which consists essentially of Water, printing gum, vat dyestuff in free leuco base form, thermosetting acid-curing resin-forming materials, an acidic catalyst, and a softener.
  • a printing paste according to claim 5 in which a textile lubricant is employed in addition to a textile softener.

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  • Textile Engineering (AREA)
  • Coloring (AREA)
US20114A 1948-04-09 1948-04-09 Process of producing dyed lustrous printed pattern effects using acidcuring resins and free leuco bases of vat dyes Expired - Lifetime US2592852A (en)

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US20114A US2592852A (en) 1948-04-09 1948-04-09 Process of producing dyed lustrous printed pattern effects using acidcuring resins and free leuco bases of vat dyes
DEP29463D DE845337C (de) 1948-04-09 1949-01-01 Waessrige Druckpaste fuer die Herstellung farbiger glaenzender Muster-effekte auf Stoffen aus pflanzlichen Fasern und Verfahren zur Erzeugung von Mustereffekten hiermit

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US20114A US2592852A (en) 1948-04-09 1948-04-09 Process of producing dyed lustrous printed pattern effects using acidcuring resins and free leuco bases of vat dyes

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2722489A (en) * 1952-08-16 1955-11-01 Gen Aniline & Film Corp Process of coloring glass fabrics with vat dyes
US2882280A (en) * 1955-02-14 1959-04-14 Pittsburgh Coke & Chemical Co Dibenzanthrone vat dyestuffs
FR2014360A1 (de) * 1968-06-28 1970-04-17 Sandoz Sa

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE937583C (de) * 1952-06-04 1956-01-12 Cassella Farbwerke Mainkur Ag Fuer Textildruck geeignete Kuepenfarbstoff-Praeparate
DE1045365B (de) * 1956-11-13 1958-12-04 Basf Ag Viskose farbstoff- oder pigmenthaltige Druckpasten vom OEl-in-Wasser-Typ

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1909221A (en) * 1930-10-20 1933-05-16 Gen Aniline Works Inc Printing colors and process of preparing them
US2123153A (en) * 1935-04-04 1938-07-05 Celanese Corp Printing and other textile treatments
US2169546A (en) * 1936-09-17 1939-08-15 Soc Of Chemical Ind Fixing dyestuffs on substrata
US2267609A (en) * 1939-01-28 1941-12-23 Nat Aniline & Chem Co Inc Vat dye composition

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1909221A (en) * 1930-10-20 1933-05-16 Gen Aniline Works Inc Printing colors and process of preparing them
US2123153A (en) * 1935-04-04 1938-07-05 Celanese Corp Printing and other textile treatments
US2169546A (en) * 1936-09-17 1939-08-15 Soc Of Chemical Ind Fixing dyestuffs on substrata
US2267609A (en) * 1939-01-28 1941-12-23 Nat Aniline & Chem Co Inc Vat dye composition

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2722489A (en) * 1952-08-16 1955-11-01 Gen Aniline & Film Corp Process of coloring glass fabrics with vat dyes
US2882280A (en) * 1955-02-14 1959-04-14 Pittsburgh Coke & Chemical Co Dibenzanthrone vat dyestuffs
FR2014360A1 (de) * 1968-06-28 1970-04-17 Sandoz Sa

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DE845337C (de) 1952-07-31

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