US 2248128 A
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Patented July 8, 1941 PBOEUCTION OF PATTERN EFFECTS ON TEXTILE MATERIALS George W. Seymour and Victor Sluyty Salvin,
Cumberland, Md., assignors to Celanese Corporation of America, a corporation of Delaware No Drawing. Application May 10, 1939,
Serial No. 272,806
6 Claims. (Cl. 8-64) This invention relates to the treatment of textile and other materials, and relates more particularly to a process for discharging colorations on textile materials for the purpose of producing pattern effects thereon.
An object of this invention is to apply the means of discharging compositions containing as the discharging agent an oxidation product of thiourea, such as thiourea dioxide, or a derivative of such oxidation product. By the use of For the production of pattern efiects on textile materials, the materials are commonly colored with a ground color, and then printed or otherwise locally treated with a composition which will discharge the ground color in the printed areas. As an alternative, the textile material may first be printed with the discharge composition and then colored with the ground color in which case 'the printed areas remain uncolored. In both cases colored pattern effects upon a colored background may be obtained by'incorporating in the discharge composition a dyestuif having an aflinity for the material or capable of being fixed thereon, and which is resistant to the discharging agent. yAfter the application of the discharge composition, the materials are submitted to steaming or ageing or equivalent treatment in order to eflect or complete the action of the discharging agent and also to fix properly the coloring matter in the discharge composition and/or the ground color. In general, a short steaming only is necessary to cause the discharging agent to act but a relatively longer steaming is neces sary for the fixation of the color on the ma- -terial.
Examples of substances which have heretofore.
since they do not discharge all of the color com-- ponents thus failing to yield clear white discharges andior destroy the coloring matter in the discharge composition with the result that poor illumination effects are obtained. It has now been found that highly desirable pattern effects can be produced on textile materials by these reducing discharging agents improved-results are obtained in white discharges and also in colored discharges.
By way of example this invention will be described as applied to textile materials made-of or containing cellulose acetate but this process is also applicable to textile materials made of or containing other organic derivatives of cellulose such as cellulose esters and celluloseethers. Examples of cellulose esters, other than cellulose acetate, are cellulose formate, cellulose propionate and cellulose butyrate, while examples of cellulose ethers are methyl cellulose, ethyl cellulose and benzyl cellulose. This invention is also applicable to textile materials generally Whether the same may be made of or contain silk, cotton, wool or artificial silk of the reconstituted cellulose type. v
According to the present invention, therefore, clear white discharges and illuminated charge effects are produced on textile materials made of or containing cellulose acetate by means of dis= charge preparations containing thiourea dioxide, or a derivative thereof in which alkyl, aralkyl and/or aryl groups are substituted on the nitrogen, or a calcium, zinc or sodium salt of thiourea dioxide or alkyl, aralkyl or aryl derivative of thiourea dioxide. Such compositions may be represented by the formula NRR CSO:
contain a suitable thickening agent such as gum;
tragacanth or gum arabic.
It is preferred, however, to employ as the discharging agent thiourea dioxide, which compound is prepared in the following manner:
To 600 cubic centimeters of 14% hydrogen peroxide 76 grams (lmol) of powdered thiourea are added slowly. Since the reaction is exothermic it is necessary to employ external cooling and to add the thiourea slowly in order to maintain the temperature below 20 C. of the theoretical yield (54 grams) will separate from the solution on standing. The thiourea dioxide thus prepared is a white crystalline powder containing 24 to 26% nitrogen (theoretical, 25.8%) and has a reduction value of SO: against iodine of 1175-122. The thiourea dioxide is slightly soluble in water and soluble in dilute alkali.
,Preferably a penetrating agent or a mixture of penetrating agents, such as calcium thiocyanate, sodium thiocyanate, potassium thiocyanate, glycerol monoacetin, glycerol formal, Glyezine A, etc., is added to the discharge preparation. Where illuminated discharge eflects are desired coloring matter is of course added to the discharge preparation. Bufier compounds may be added to the discharge preparation to control the pH value thereof, salts such as sodium acetate or sodium salts of other fatty acids being employed where a pH of between 7 and 10 is desired, and acids such as acetic acid, citric acid and tartaric acid being employed to discharge at a pH of lessthan 7.
The proportions in which the ingredients are incorporated in the discharge preparation for use in obtaining clear white discharges vary with textile material and the coloring matter to be discharged. However, a general formula for the application of the discharge compounds of this invention to a dischargeable material is as follows:
v Per cent by weight Oxidation product of thiourea or derivative thereof 10-15 Thickening agent 25-50 Penetrating agent 5-10 Bufier compound 5-10 Where illuminated discharge efiects are desired a suitable amount of the desired coloring matter is added to the discharge preparation.
Suitable coloringv matters which may be added to the discharge preparation for the production of illuminated efiects may be any desired unre-. duced coloring matters of the anthraquinone series, especially such coloring matters as contain a single anthraquinone nucleus. For instance, there may be used mono-, di or polyaminoanthraquinones whether unsubstituted or substituted in the nucleus or in an amino group or both, for example, amino-methyl anthraquinones,
-acidyl-amino-anthraquinones, -alkylamino anthraquinones, and substituted -alkyl-amino anthraquinones, e. g. oxy-alkylamino-anthraquinone., Moreover, hydroxylor mercapto anthraquinones or their ethers or" other substitution products may be employed. Sulphonated anthraquinone color matters having amnity for cellulose ester or ether materials may likewise be employed for producing illuminated eflects on materials containing cellulose esters or ethers. Cotton vat dyes such as the Indanthrene dyes, which are pyranthrones, may also beused as coloring matters in accordance with this invention. Using vat dyestuffs, which have been reduced to their leuco form, it is possible to discharge print and illuminate mixed fabrics such as cellulose acetate and cotton, 'cellulose acetate and regenerated cellulose, cellulose acetate and silk, etc. 3
If desired the discharge agents of this invention may be employed in combination withother reducing agents. Thus, for example, thiourea dioxide may be employed to replace a part of other reducing discharging agents such as sodium Iormaldehydesulphoxylate or zinc formaldehyde sulphoxylate.
One of the important advantages of the use of the discharging agents of this invention over those heretofore employed is that the former are absorbed in the fibers of the textile material, particularly when the fibers are made of or contain cellulose acetate, where their strong reducing action may be utilized more completely.
The fabric may be previously dyed with a ground color containing any suitable dischargeable dyestufi, examples of which are:
Setacyl Direct Discharge Blue G Setacyl Direct Yellow 5G Setacyl Direct Orange GI-I Setacyl Direct Red GN Celliton Discharge Yellow 3GN Celliton Discharge Blue 5G Celliton Discharge Yellow RL Celliton Discharge Red BDL SRA Red VIII SRA Navy Base VI SRA Navy Developer I A fabric consisting wholly of cellulose acetate yarn and which has been dyed blue with 2,4-dinitro -6 -chlorbenzeneazo 2- dihydroxy-ethylamino-4-acetylamino-anisole has applied locally thereto by means of engraved rollers a discharge paste of the following formula Per cent Thiourea dioxide 15 Monoacetin l0 Disodium phosphate l0 Gum tragacanth (7 oz. per gal.) 30 Water 35 The fabric, after printing, is passed through an ager where it is exposed for five to twenty minutes to steam at 211-212 F., and is then washed in an open soaper, in which the reduction products of the dyestufi are removed.
A design of white discharge o a bl b k. ground is produced.
Example II The process of Example I is carried out, with the exception that the following discharge paste is employed:
. alkali, then scoured with neutral soap or Gardinol to remove the reduction products of the.
Per cent Thiourea dioxide 15 Monoacetin 1 0 Vat dyestufi (20% Indan-threne Scarlet B I in water) 20 Disodium phnsphafn I 10 Gum tragacanth (7 oz. per gal). 30 Water 15 This fabric is steamed as in Example I. It is then washed in an open soaper, as follows:
The fabric is subjected to water to remove dyestufi, and then oxidized in the known mannet. It is preferable to remove these reduction products prior to oxidation to preclude the possibility of the formation of dyes oi the type of Bismarck Brown and Aniline Black.
A fabric having a design in scarlet red color on a background ofblue is produced.
It is to be understood that the foregoing detailed description is given merely by way of illustration and that many variations may be made therein without departing from the spirit of our invention.
Having described our invention, what we desire to secure by Letters Patent is:
1. Process for the production of discharge effeets upon materials having a basis ofan organic derivative of cellulose and colored with a dischargeable ground color having an'afiin-ity for said organic derivative of cellulose materials, which comprises applying to the materials a discharge composition of a pH less than '7 containing 25 to 50% by weight of a thickening agent, to by weight of a penetrating agent, 5 to 10% by weight of a buffer compound and from 10 to by weight of a reducing agent of the formula.
1ilvherein R or R is hydrogen, alkyl, aryl or aral- 2 Process for the production of discharge effects upon materials having a basis of cellulose acetate and colored with a dischargeable ground- 3. Process for the production of discharge effects upon materials having a basis of anorganic derivative of cellulose and colored with a dischargeable ground color having an afiinity for said organic derivative of cellulose materials,
which comprises applying to the materials a discharge composition of a pH less than 7 containing from 10 to 15% by weigh-t of thiourea dioxide, as to by weight of a. thickening agent, 5 to 10% by weight of a penetrating agent-and 5 to 10% by weight of a buffer compound.
4. Process for the production of discharge effects upon materials having a basis of cellulose acetate and colored with a dischargeable ground color having an affinity for said cellulose acetate materials, which comprises applying to the materials a discharge composition of a pH less than 7 containing from 10' to-15% by weight of thinurea dioxide, 25 to 50% by weight of a thickening agent, 5 to 10% by weight of a penetrating agent and 5 to 10% by weight of a buffer compound.
5. Process for the production of discharge effects upon materials having a basis of an organic derivative of cellulose and colored with a dischargeable ground color having an affinity for said organic derivative of cellulose materials, which comprisesapplying to the materials a discharge composition of a pH less than 7 containing 15% by weight of thiourea dioxide, 10%
by weight of monoacetin, 10% by weight of disodium phosphate, 30% by weight of gum traga canth and 35% by weight of water. I
6. Process for the production of discharge effects upon materials having a basis of cellulose acetate and colored with a disch-argeable ground color having an aflinity for said cellulose acetate materials, which comprises applying to the materials a discharge composition of a pH less than '7 containing 15% by weight of thiourea dioxide,
10% by weight of monoacetin, 10% by weight of disodium phosphate, 30% by weight of gum tragacanth and 35% by weight of water. I Y
GEORGE w. SEYMOUR. VICTOR SLUYTY sat-VIN.