Part 50

In textile dyeing and printing, substances called mordants are largely used, either to fix or to develop the color on the fiber. Substances of mineral origin, such as salts of aluminum, chromium, iron, copper, antimony, and tin, principally, and many others to a less extent and of organic origin, like acetic, oxalic, citric, tartaric, and lactic acid, sulphonated oils, and tannins are employed as mordants.

Iron liquor, known as black liquor or pyrolignite of iron, is made by dissolving scrap iron in pyroligneous acid. It is used as a mordant in dyeing silks and cotton and in calico printing.

Red liquor is a solution of aluminum acetate in acetic acid, and is produced by acting on calcium or lead acetate solutions with aluminum sulphate or the double alums, the supernatant liquid forming the red liquor. The red liquor of the trade is often the sulpho-acetate of alumina resulting when the quantity of calcium or lead acetate is insufficient to completely decompose the aluminum salt. Ordinarily the solutions have a dark-brown color and a strong pyroligneous odor. It is called red liquor because it was first used in dyeing reds. It is employed as a mordant by the cotton dyer and largely by the printer.

«Non-Poisonous Textile and Egg Dyes for Household Use.»—The preparation of non-poisonous colors for dyeing fabrics and eggs at home constitutes a separate department in the manufacture of dyestuffs.

Certain classes of aniline dyes may be properly said to form the materials. The essence of this color preparation consists chiefly in diluting or weakening the coal-tar dyes, made in the aniline factories, and bringing them down to a certain desired shade by the addition of certain chemicals suited to their varying characteristics, which, though weakening the color, act at the same time as the so-called mordants.

The anilines are divided with reference to their characteristic reactions into groups of basic, acid, moderately acid, as well as dyes that are insoluble in water.

In cases where combinations of one or more colors are needed, only dyes of similar reaction can be combined, that is, basic with basic, and acid with acid.

For the purpose of reducing the original intensity of the colors, and also as mordants, dextrin, Glauber’s salt, alum, or aluminum sulphate is pressed into service. Where Glauber’s salt is used, the neutral salt is exclusively employed, which can be had cheaply and in immense quantities in the chemical industry. Since it is customary to pack the color mixtures in two paper boxes, one stuck into the other, and moreover since certain coal-tar dyes are only used in large crystals, it is only reasonable that the mordants should be calcined and not put up in the shape of crystallized salts, particularly since these latter are prone to absorb the moisture from the air, and when thus wet likely to form a compact mass very difficult to dissolve. This inconvenience often occurs with the large crystals of fuchsine and methyl violet. Because these two colors are mostly used in combination with dextrin to color eggs, and since dextrin is also very hygroscopic, it is better in these individual cases to employ calcined Glauber’s salt. In the manufacture of egg colors the alkaline coloring coal-tar dyes are mostly used, and they are to be found in a great variety of shades.

Of the non-poisonous egg dyes, there are some ten or a dozen numbers, new red, carmine, scarlet, pink, violet, blue, yellow, orange, green, brown, black, heliotrope, etc., which when mixed will {276} enable the operator to form shades almost without number.

The manufacture of the egg dyes as carried on in the factory consists in a mechanical mixing of basic coal-tar dyestuffs, also some direct coloring benzidine dyestuffs, with dextrin in the ratio of about 1 part of aniline dye to 8 parts of dextrin; under certain circumstances, according to the concentrated state of the dyes, the reducing quantity of the dextrin may be greatly increased. As reducing agents for these colors insoluble substances may also be employed. A part also of the egg dyes are treated with the neutral sulphate; for instance, light brilliant green, because of its rubbing off, is made with dextrin and Glauber’s salt in the proportion of 1:3:3.

For the dyeing of eggs such color mixtures are preferably employed as contain along with the dye proper a fixing agent (dextrin) as well as a medium for the superficial mordanting of the eggshell. The colors will then be very brilliant.

Here are some recipes:

Parts Color Dyestuff by Cit. Dextrin Weight Acid Blue Marine blue B. N. 3.5 35.0 60.0 Brown Vesuvin S. 30.0 37.5 30.0 Green Brilliant green O. 13.5 18.0 67.5 Orange Orange II. 9.0 18.0 75.0 Red Diamond fuchsine I. 3.5 18.0 75.0 Pink Eosin A. 4.5 — 90.0 Violet Methyl violet 6 B. 3.6 18.0 75.0 Yellow Naphthol yellow S. 13.5 36.0 67.5

Very little of these mixtures suffices for dyeing five eggs. The coloring matter is dissolved in 600 parts by weight of boiling water, while the eggs to be dyed are boiled hard, whereupon they are placed in the dye solution until they seem sufficiently colored. The dyes should be put up in waxed paper.

«Fast Stamping Color.»—Rub up separately, 20 parts of cupric sulphate and 20 parts of anilic hydrochlorate, then mix carefully together, after adding 10 parts of dextrin. The mixture is next ground with 5 parts of glycerine and sufficient water until a thick, uniform, paste-like mass results, adapted for use by means of stencil and bristle-brush. Aniline black is formed thereby in and upon the fiber, which is not destroyed by boiling.

«New Mordanting Process.»—The ordinary method of mordanting wool with a bichromate and a reducing agent always makes the fiber more or less tender, and Amend proposed to substitute the use of a solution of chromic acid containing 1 to 2 per cent of the weight of the wool, at a temperature not exceeding 148° F., and to treat it afterwards with a solution of sodium bisulphite. According to a recent French patent, better results are obtained with neutral or slightly basic chromium sulphocyanide. This salt, if neutral or only slightly basic, will mordant wool at 148° F. The double sulphocyanide of chromium and ammonium, got by dissolving chromic oxide in ammonium sulphocyanide, can also be used. Nevertheless, in order to precipitate chromium chromate on the fiber, it is advisable to have a soluble chromate and a nitrate present, as well as a soluble copper salt and a free acid. One example of the process is as follows: Make the bath with 2 to 3 per cent of ammonio-chromium sulphocyanide, one-half of 1 per cent sodium bichromate, one-third of 1 per cent sodium nitrite, one-third of 1 per cent sulphate of copper, and 1.5 per cent sulphuric acid—percentages based on the weight of the wool. Enter cold and slowly heat to about 140° to 150° F. Then work for half an hour, lift and rinse. The bath does not exhaust and can be reinforced and used again.

«Process for Dyeing in Khaki Colors.»—Bichromate of potash or of soda, chloride of manganese, and a solution of acetate of soda or formiate of soda (15° Bé.) are dissolved successively in equal quantities.

The solution thus composed of these three salts is afterwards diluted at will, according to the color desired, constituting a range from a dark brown to a light olive green shade. The proportions of the three salts may be increased or diminished, in order to obtain shades more or less bister.

Cotton freed from its impurities by the usual methods, then fulled as ordinarily, is immersed in the bath. After a period, varying according to the results desired, the cotton, threads, or fabrics of cotton, are washed thoroughly and plunged, still wet, into an alkaline solution, of which the concentration ought never to be less than 14° Bé. This degree of concentration is necessary to take hold of the fiber when the cotton comes in contact with the alkaline bath, and by the contraction which takes place the oxides of chrome and of manganese remain fixed in the fibers.

This second operation is followed by washing in plenty of water, and then the cotton is dried in the open air. If the color is judged to be too pale, the threads or fabrics are immersed again in the initial bath, left the necessary time for obtaining the desired shade, and then {277} washed, but without passing them through an alkaline bath. This process furnishes a series of khaki colors, solid to light, to fulling and to chlorine.

«LAKES:»

Scarlet Lake.—In a vat holding 120 gallons provided with good agitating apparatus, dissolve 8 pounds potash alum in 10 gallons hot water and add 50 gallons cold water. Prepare a solution of 2 pounds ammonia soda and add slowly to the alum solution, stirring all the time. In a second vessel dissolve 5 pounds of brilliant scarlet aniline, by first making it into a paste with cold water and afterwards pouring boiling water over it; now let out steam into the vat until a temperature of 150° to 165° F. is obtained. Next dissolve 10 pounds barium chloride in 10 gallons hot water in a separate vessel, add this very slowly, stir at least 3 hours, keeping up temperature to the same figures. Fill up vat with cold water and leave the preparation for the night. Next morning the liquor (which should be of a bright red color) is drawn off, and cold water again added. Wash by decantation 3 times, filter, press gently, and make into pulp.

It is very important to precipitate the aluminum cold, and heat up before adding the dyestuff. The chemicals used for precipitating must be added very slowly and while constantly stirring. The quantity used for the three washings is required each time to be double the quantity originally used.

I.—Madder Lakes.—Prepare from the root 1 pound best madder, alum water (1 pound alum with 1 1⁠/⁠2 gallons of water), saturated solution of carbonate of potash (3⁠/⁠4 pound carbonate of potash to 1⁠/⁠2 gallon of water).

The madder root is inclosed in a linen bag of fine texture, and bruised with a pestle in a large mortar with 2 gallons of water (free from lime) added in small quantities at a time, until all the coloring matter is extracted. Make this liquor boil, and gradually pour into the boiling water solution. Add the carbonate of potash solution gradually, stirring all the time. Let the mixture stand for 12 hours and drop and dry as required.

II.—Garancine Process.—This is the method usually employed in preference to that from the root. Garancine is prepared by steeping madder root in sulphate of soda and washing.

Garancine 2 pounds Alum (dissolved in a little water) 2 pounds Chloride of tin 1⁠/⁠2 ounce Sufficient carbonate of potash or soda to precipitate the alum.

Boil the garancine in 4 gallons of pure water; add the alum, and continue boiling from 1 to 2 hours. Allow the product to partially settle and filter through flannel before cooling. Add to the filtrate the chloride of tin, and sufficient of the potash or soda solution to precipitate the alum; filter through flannel and wash well. The first filtrate may be used for lake of an inferior quality, and the garancine originally employed may also be treated as above, when a lake slightly inferior to the first may be obtained.

Maroon Lake.—Take of a mixture made of:

2⁠/⁠3 Sapan wood, 1⁠/⁠3 Lima wood 56 parts Soda crystals 42 parts Alum 56 parts

Extract the color from the woods as for rose pink, and next boil the soda and alum together and add to the woods solution cold. This must be washed clean before adding to the wood liquor.

Carnation Lake.—

Water 42 gallons Cochineal 12 pounds Salts of tartar 1 1⁠/⁠2 pounds Potash alum 3⁠/⁠4 pound Nitrous acid, nitromuriate of tin 44 pounds Muriatic acid, nitromuriate of tin 60 pounds Pure block tin, nitromuriate of tin 22 pounds

Should give specific gravity 1.310.

Boil the water with close steam, taking care that _no iron_ touches it; add the cochineal and boil for not more than five minutes; then turn off the steam and add salts of tartar and afterwards carefully add the alum. If it should not rise, put on steam until it does, pass through a 120-mesh sieve into a settling vat, and let it stand for 48 hours (not for precipitation). Add gradually nitromuriate of tin until the test on blotting paper (given below) shows that the separation is complete. Draw off clear water after it has settled, and filter. To test, rub a little of the paste on blotting paper, then dry on steam chest or on the hand, and if on bending it cracks, too much tin has been used.

To Test the Color to See if it is Precipitating.—Put a drop of color on white blotting paper, and if the color spreads, it is not precipitating. If there is a {278} colorless ring around the spot of color it shows that precipitation is taking place; if the white ring is too strong, too much has been used.

«BLACK LAKES FOR WALL-PAPER MANUFACTURE:»

Bluish-Black Lake.—Boil well 220 parts of Domingo logwood in 1,000 parts of water to which 2 parts of ammonia soda have been added; to the boiling logwood add next 25 parts of green vitriol and then 3.5 parts of sodium bichromate. The precipitated logwood lake is washed out well twice and then filtered.

Black Lake AI.—Logwood extract, Sanford, 120 parts; green vitriol, 30 parts; acetic acid, 7° Bé., 10 parts; sodium bichromate, 16 parts; powdered alum, 20 parts. The logwood extract is first dissolved in boiling water and brought to 25° Bé. by the addition of cold water. Then the remaining ingredients are added in rotation, the salts in substance, finely powdered, with constant stirring. After the precipitation, wash twice and filter.

Aniline Black Lake.—In the precipitating vat filled with 200 parts of cold water enter with constant stirring in the order mentioned the following solutions kept in readiness: Forty parts of alum dissolved in 800 parts of water; 10 parts of calcined soda dissolved in 100 parts of water; 30 parts of azo black dissolved in 1,500 parts of water; 0.6 parts of “brilliant green” dissolved in 100 parts of water; 0.24 parts of new fuchsine dissolved in 60 parts of water; 65 parts of barium chloride dissolved in 1,250 parts of water. Allow to settle for 24 hours, wash the lake three times and filter it.

«Carmine Lake for Wall Paper and Colored Papers.»—Ammonia soda (98 per cent), 57.5 parts by weight; spirits (96 per cent), 40 parts by weight; corallin (dark), 10 parts by weight; corallin (pale), 5 parts by weight; spirit of sal ammoniac (16° Bé.), 8 parts by weight; sodium phosphate, 30 parts by weight; stannic chloride, 5 parts by weight; barium chloride, 75 parts by weight. Dissolve the corallin in the spirit, and filter the solution carefully into eight bottles, each containing 1 part of the above quantity of spirit of sal ammoniac, and let stand. The soda should meanwhile be dissolved in hot water and the solution run into the stirring vat, in which there is cold water to the height of 17 inches. Add the sodium phosphate, which has been dissolved in a copper vessel, then the corallin solution, and next the stannic chloride diluted with 3 pailfuls of cold water. Lastly the barium chloride solution is added. The day previous barium chloride is dissolved in a cask in as little boiling water as possible, and the receptacle is filled entirely with cold water. On the day following, allow the same to run in slowly during a period of three-fourths of an hour, stir till evening, allow to settle for 2 days, draw off and filter.

«English Pink.»—

Quercitron bark 200 parts Lime 10 parts Alum 10 parts Terra alba 300 parts Whiting 200 parts Sugar of lead 7 parts

Put the bark into a tub, slake lime in another tub, and add the clear limewater to wash the bark; repeat this 3 times, letting the bark stand in each water 24 hours. Run liquor into the tub below and add the terra alba and whiting; wash well in the top tub and run into liquor below through a hair sieve, stirring well.

Dissolve the sugar of lead in warm water and pour gently into the tub, stirring all the time; then dissolve the alum and run in while stirring; press slightly, drop, and dry as required.

«Dutch Pink.»—

I.—Quercitron bark 200 parts Lime 20 parts Alum 20 parts Whiting 100 parts Terra alba 200 parts White sugar of lead 10 parts

II.—Quercitron bark 300 parts Lime 10 parts Alum 10 parts Terra alba 400 parts Whiting 100 parts Sugar of lead 7 parts

Put the bark into a tub with cold water, slake 28 pounds of lime, and add the limewater to the bark. (This draws all the color out of the wood.) Dissolve alum in water and run it into bark liquor. The alum solution must be just warm. Dissolve sugar of lead and add it to above, and afterwards add the terra alba and whiting. The product should now be in a pulp, and must be dropped and dried as required.

«Rose Pink.»—I.—Light.

Sapan wood 100 parts Lima 100 parts Paris white 200 parts Alum 210 parts {279}

II.—Deep. Sapan wood 300 parts Lima 300 parts Terra alba 400 parts Paris white 120 parts Lime 12 parts Alum 200 parts

III.—Sapan wood 200 parts Alum 104 parts Whiting 124 parts

Boil the woods together in 4 waters and let the products stand until cold; wash in the whiting and terra alba through a hair sieve, and afterwards run in the alum. If a deep color is required slake 12 pounds lime and run it in at the last through a hair sieve. Let the alum be just warm or it will show in the pink.

«DYES, COLORS, ETC., FOR TEXTILE GOODS:»

«Aniline Black.»—This black is produced by carefully oxidizing aniline hydrochloride. The exact stage of oxidation must be carefully regulated or the product will be a different body (quinone). There are several suitable oxidizing agents, such as chromic acid, potassic bichromate, ferrocyanide of potassium, etc., but one of the easiest to manipulate is potassic chlorate, which by reacting on copper sulphate produces potassic sulphate and copper chlorate. This is easily decomposed, its solution giving off gases at 60° F. which consist essentially of chloride anhydrate. But one of the most useful agents for the production of aniline black is vanadate of ammonia, 1 part of which will do the work of 4,000 parts of copper. Many other salts besides copper may be used for producing aniline black, but the following method is one of the best to follow in making this dye:

Aniline hydrochloride 40 parts Potassic chlorate 20 parts Copper sulphate 40 parts Chloride of ammonia (sal ammoniac) 16 parts Warm water at 60° F 500 parts

After warming a few minutes the mass froths up. The vapor should not be inhaled. Then set aside, and if the mass is not totally black in a few hours, again heat to 60° F., and expose to the air for a few days, and finally wash away all the soluble salts and the black is fit for use.

«Aniline Black Substitutes.»—I.—Make a solution of

Aniline (fluid measure) 30 parts Toluidine (by weight) 10 parts Pure hydrochloric acid, B. P. (fluid measure) 60 parts Soluble gum arabic (fluid measure) 60 parts

Dissolve the toluidine in the aniline and add the acid, and finally the mucilage.

II.—Mix together at gentle heat:

Starch paste 13 quarts Potassic chlorate 350 scruples Sulphate of copper 300 scruples Sal ammoniac 300 scruples Aniline hydrochloride 800 scruples

Add 5 per cent of alizarine oil, and then steep it for 2 hours in the dye bath of red liquor of 2 1⁠/⁠2° Tw. Dye in a bath made up of 1⁠/⁠2 ounce of rose bengal and 1 1⁠/⁠2 ounces of red liquor to every 70 ounces of cotton fabric dyed, first entering the fabric at 112° F., and raising it to 140° F., working for 1 hour, or until the desirable shade is obtained; then rinse and dry.

«Blush Pink on Cotton Textile.»—Rose bengal or fast pink will give this shade. The mordant to use is a 5 per cent solution of stannate of soda and another 5 per cent solution of alum.

Dissolve in a vessel (_a_) 8 1⁠/⁠2 parts of chloride of copper in 30 parts of water, and then add 10 parts chloride of sodium and 9 1⁠/⁠2 parts liquid ammonia.

In a second vessel dissolve (_b_) 30 parts aniline hydrochlorate in 20 parts of water, and add 20 parts of a solution of gum arabic prepared by dissolving 1 part of gum in 2 parts of water.

Finally mix 1 part of _a_ with 4 parts of _b_; expose the mixture to the air for a few days to develop from a greenish to a black color. Dilute for use, or else dry the thick compound to a powder.

If new liquor is used as the mordant, mix 1 part of this with 4 parts of water, and after working the fabric for 1 to 2 hours in the cold liquor, wring or squeeze it out and dry; before working it in the dye liquor, thoroughly wet the fabric by rinsing it in hot water at a spring boil; then cool by washing in the dye bath until the shade desired is attained, and again rinse and dry.

The red liquor or acetate of aluminum may be made by dissolving 13 ounces of alum in 69 ounces of water and mixing this with a solution made by dissolving 7 1⁠/⁠2 ounces of acetate of lime, also dissolved in 69 ounces of water. Stir well, allow it to settle, and filter or decanter {280} off the clear fluid for use, and use this mixture 2 1⁠/⁠2° Tw.

The fabric is first put into the stannate of soda mordant for a few minutes, then wrung out and put into the alum mordant for about the same time; then it is again wrung out and entered in the dye bath at 120° F. and dyed to shade desired, and afterwards rinsed in cold water and dried.

The dye bath is made of 1⁠/⁠4 ounce of rose bengal per gallon of water. If fast pink is the dye used, the mordant used would be Turkey red oil and red liquor. Use 8 ounces of Turkey red oil per gallon of water. Put the fabric into this, then wring out the textile and work in red liquor of 7° Tw. for about 2 hours, then wring out and dye in a separate bath made up of eosine, or fast pink, in water in which a little alum has been dissolved.

«To Dye Woolen Yarns, etc., Various Shades of Magenta.»—To prepare the dye bath dissolve 1 pound of roseine in 15 gallons of water. For a concentrated solution use only 10 gallons of water, while if a very much concentrated color is needed, dissolve the dye in methylated spirit of wine, and dilute this spirituous tincture with an equal quantity of water.

No mordant is required in using this color in dyeing woolen goods. The dyeing operation consists simply in putting the goods into the dye bath at 190° F. and working them therein until the desired shade is obtained, then rinsing in cold water and drying.

If the water used in preparing the dye is at all alkaline, make use of the acid roseine dissolved in water in which a little sulphuric acid has been mixed, and work, gradually raising to the boiling point, and keep up the temperature for 30 minutes, or according to the shade desired. Put about 20 per cent sulphate of soda into the dye bath.