806
T H E JOCRNAL OF IiVDCSTRIAL A N D E Y G I S E E R I S G C H E M I S T R Y
Yol. ;. No. 9
I
NOTES AND CORRESPONDENCE ON MANUFACTURE O F TURKEY-RED OILS FROM FATTY ACIDS Editor of Journul of Industrial and Engineering Chemistry: In an article in Chemical Abstracts, 9 (191j), 1400-1401, entitled “Manufacture of Turkey-red Oils from Fatty Acids,” F. Erban mentions the results of three experiments as “low degree,” “medium degree,” and “high degree” of sulfonation; each of these produced an unsatisfactory product, inasmuch as neither one was wholly soluble and this indeed is the property sought. The writer has read and heard of a great number of experiments made on the production of a soluble sulfonated oil, some of which were attended by explosions, while others produced dark brown and only partly soluble products. The cause of these failures he attributes to the fact that too much attention is paid to the proportion of oil and acid used and entirely too little attention to the mode and manner of mixing. 1-The temperature of the mixture must not be allowed to rise above 40’ C. This is best controlled by surrounding the vessel by water. 2-And one of the most important points of all, the acid should be allowed t o run into the oil very, very slowly and the mixture constantly stirred. When manufacturing in fair-sized quantities, this should be a matter of hours. In laboratory experiments the acid should be in a burette and allowed to run in very slowly, drop by drop, while the mixture is stirred constantly. The grade of the product produced depends to a very great extent upon the care exercised in this stage of the process. 3-The product should be washed thoroughly, three or four times, a t least, with a saturated solution of common salt. This will wash away the free sulfuric acid. If the mixture is not constantly and thoroughly stirred the product will be darker and not wholly soluble; practically the same effect is caused by an incomplete washing. The finished product has an acid reaction. I t can be used in this state, made neutral, or slightly alkaline as desired. The slightly acid product is best when employed for treating animal fibers, as i t preserves the luster of the fiber and a t the same time produces a silk-like handle. For vegetable fibers the slightly alkaline product is preferable as i t is a very good cleansing agent and also produces a wonderfully soft handle. I n the writer’s experiments and manufacture on a small scale of Turkey-red oil, four parts by weight of castor oil were used to one part by weight of sulfuric acid, sp. gr. 1.84. The writer hopes this information may be a help to other chemists. WM. J. SCHEPP Chief Chemist and Textile Expert r\-ATIONAL C L O A K & S U I T C O .
XEW YORKCITY, May 29, 1915
A NEW NATIVE DYE WOOD The yellow Locust tree, Robinia pseudocacia I,., grcws abundantly in the Middle States, Virginia and iYorth and South Carolina, and is highly valued as a strong, even-grained, permanent timber. It is also much used for the manufacture of small, hard wood objects. I n a factory working this wood, i t appeared desirable to discover some better disposal for the sawdust and chips than of their use as fuel. Upon extracting the sawdust by prolonged digestion with hot water, a brown liquor is obtained which affords decided colors with the common mordants.
Through the kindness of Messrs. Jno. H. Heald & Company, manufacturers of tanning extracts, Lynchburg, Ya., a test of this sawdust has been made. This report states that the “amount of soluble is only about one-third that of black oak bark, so that the yield of dye extract would be low. The dyeing power of this is, however, quite strong, as, using the same amount of the iocust sawdust as black oak bark, the locust gives the deeper color.”. . . .The colors afforded with mordants are similar to those obtained from black oak, or Quercitron bark. ’\s’ith manganese a strong umber-brown is obtained, and with alum, a bright, strong, yellow, khaki color. As locust wood is so very hard, it would not prove profitable to chip it for this purpose, but when a supply of sawdust or chips from turning is available, i t may prove of advantage to employ it for dyeing in place of Quercitron bark. F. P. DUNXINGTOX UNIVERSITY OF VIRGINIA June 14, 1915
NOTE ON THE DETERMINATION OF ALUMINUM OXID E AND TOTAL ALUMINUM IN STEEL It has long been known that aluminum oxide when freshly precipitated is readily soluble in acids and when strongly ignited is very difficultly soluble in acids. When metallic aluminum is added to steel while casting, its tendency is to unite a t once with the oxygen existing in the steel, both as metallic oxides and as CO gas. The products of this reaction are -41203,the metals of the oxides reduced, and carbon. Since in regular practice there is only sufficient aluminum added to “quiet the steel,” the aluminum added is nearly all converted to the oxide -41203. This aluminum oxide is, during the operation, heated to the temperature of pouring steel, about 1600 t o 1650’ C. (2912 to 3 0 0 0 ~F,), whereby it is rendered almost entirely insoluble in dilute hydrochloric acid. I n order to test the effect of high temperature on the solubility of A1203 the following experiment was carried out: I O grams metallic aluminum were dissolved in hydrochloric acid, boiled low and replaced three times with nitric acid. This solution of aluminum nitrate was evaporated to dryness to drive off acid fumes; the residue was transferred to a platinum dish and placed into a muffle furnace where the temperature was gradually raised to a high heat, taking out a portiou a t iutervals, and noting the temperature each time with a Scimatco optical pyrometer. Portions of aluminum oxide were removed a t 8 1 j , 900, 980, 106j and 1150’ C. Solubility tests were made by taking I gram of each portion and digesting for one hour with IOO cc. hydrochloric acid ( I : I ) , filtering, and determining A1203 in the filtrate. Portion heated t o . , , . Gram solubleA120a. , .
C.
815’ 0.931,
900° C 0.3962
980’ C . 0,2337
1065’ C . 0,0472
l150° C . 0.0390
The increase in temperature was a t the rate of 8 to IO minutes between observations. i\nother portion of the same -41203 prepared above, was placed in a boat in the silica tube of a n electric furnace and held for one hour a t a temperature of 1000’ C . ; I gram of, this was treated as above with I : I hydrochloric acid and showed o.on8j gram soluble Al2O:i. One gram alundum, 1 2 0 mesh, was treated with hydrochloric acid as above and showed a mere trace of soluble & 0 3 . The solubility diminishes with increase of temperature and ’length of time to which the A1203had been exposed to the heat. If A1203exposed to 1000’ C. will yield 2.85 per cent of its .%os content, and alupdum exposed to a little over 2000’ C. yields a trace, it is safe t o assume that the A1203 formed in molten steel would yield only I or z per cent of its content on treatment
