so. СО (a) Sodium Antkraquinone-2-tulfonate (“Silver Salt”) To 125 grains of oleum containing 18 per cent S03 is added, with stirring, 100 grams of anthraquinone of highest purity. The mixture is heated gradually to 135°C., while being stirred slowly, and held at this temperature for 3 hours. The mixture is then allowed to cool to […]
Архивы рубрики ‘DYE CHEMISTRY’
1-Nitro-2-methylanthraquinone
In a round-bottomed flask equipped with a stirrer, 100 grams of 2- methylanthraquinone is dissolved in 900 grams of 66° Вё sulfuric acid. The solution is cooled in an ice-salt bath to 0°C. and 50 grams of finely powdered potassium nitrate is added slowly with vigorous stirring. The temperature should be held as near 0° […]
COMPOUNDS OF THE ANTHRAQUINONE SERIES
21. Anthraquinone Method It Oxidation of Anthracene73 CH CO CH CO Anthracene Anthraquinone Impure anthracene should not be used in the preparation of anthraquinone, since too much chromic acid is required. The product now produced by coal tar distillation varies in purity from 80 to 92 per cent, the value for any given sample being […]
Naphthalenetetracarboxylic Acid
In a three-necked flask, provided with calcium chloride tube, dropping funnel, and thermometer, the 130 grams of chlorination product from above is stirred with 2400 grams of 20 per cent oleum for 1 hour at 100°C. The mixture is then cooled to 70°, 1300 grams of concentrated sulfuric acid is added, and the solution is […]
Tetrachloropyrene
In a moisture-tight, three-necked flask provided with stirrer, thermometer, and reflux condenser, 101 grams (0.5 mole) of pyrene is dissolved at 130°C. in 1500 grams of dry trichlorobenzene (or dichloro — benzerie). A stream of dry chlorine is introduced with vigorous stirring until the increase in weight reaches 65 grams. Toward the end of the […]
L-Aminonaphthalene-4,8-disulfomc Acid, 2-Amino — naphthaleiie-4,8-disulfonic Acid, and
l — Aminonaphthalene-3,8-disulfonic Acid To 900 grams of 100 per cent sulfuric acid, cooled to 5°C., is added, over a period of 15 minutes with good stirring, 384 grams of pure powdered naphthalene. Stirring is continued for 30 minutes and then 900 grams of oleum (64 per cent S03) is added slowly, not allowing the […]
L-Amino-8-naphlhol-3,6-di»ulfonic Acid (H Acid)
Alkali fusion of l-naphthylamine-3,6,8-trisulfonic acid yields H acid, the most important member of this series of intermediates in the dye industry. The preparation of H acid is a typical example of fusion reactions. In order to obtain H acid in good yields, the temperature of fusion must not exceed 190°C. and the caustic soda must […]
From Є Acid and 2,8-Uihydroxynaphthalene-6*tulfonic Acid
G acid is subjected to fusion with NaOH and a small amount of water at 200° in an open vessel to yield 2,8-dihydroxynaphthalene-6-sulfonic acid. This product is not isolated, but is treated directly with ammonium sulfate, neutralizing part of the free alkali with sulfuric acid. This process gives a very satisfactory product and has the […]
From 2-fiaphthol-6,8-disulfonic Acid
G salt is converted to amino-G acid by heating with 25 per cent ammonia and ammonium sulfite at 140°C. (pressure, 20 atmospheres). The procedure involves nothing of special interest. A yield of 92 per cent of the theoretical amount is easily attained, and after blowing off the ammonia, the whole reaction mass is fused with […]
(a) 2,6,8’ and 2J5,7-Naphthylaminedimlfonic Acid* from. fl-Naphthyiamine
To 800 grams of 15 per cent oleum is added, over a period of 10 minutes, 192 grams (1.0 mole) of finely powdered /3-naphthylamine sulfate which has been intimately mixed with 1 gram of anhydrous carbonate. The temperature should not be allowed to rise above 50°C. The reaction mixture is now tested for complete solubility […]