LIME SAPONIFICATION.
The saponification in an autoclave is usually carried out by introducing the fats into the autoclave with a percentage of lime, magnesia or zinc oxide, together with water. If the fats contain any great amount of impurities, it is first necessary to purify them either by a treatment with weak sulfuric acid, as described under the Twitchell process, or by boiling them up with brine and settling out the impurities from the hot fat.
To charge the autoclave a partial vacuum is created therein by condensation of steam just before running the purified oil in from an elevated tank. The required quantity of unslaked lime, 2 to 4 per cent. of the weight of the fat, is run in with the molten fat, together with 30 per cent. to 50 per cent. of water. While 8.7 per cent. lime is theoretically required, practice has shown that 2 per cent. to 4 per cent. is sufficient. The digestor, having been charged and adjusted, steam is turned on and a pressure of 8 to 10 atmospheres maintained thereon for a period of six to ten hours. Samples of the fat are taken at various intervals and the percentage of free fatty acids determined. When the saponification is completed the contents of the autoclave are removed, usually by blowing out the digestor into a wooden settling tank, or by first running off the glycerine water and then blowing out the lime, soap and fatty acids. The mass discharged from the digestor separates into two layers, the upper consisting of a mixture of lime soap or "rock" and fatty acids, and the lower layer contains the glycerine or "sweet" water. The glycerine water is first run off through a clearing tank or oil separator, if this has not been done directly from the autoclave, and the mass remaining washed once or twice more with water to remove any glycerine still retained by the lime soap. The calculated amount of sulfuric acid to decompose the lime "rock" is then added, and the mass agitated until the fatty acids contained therein are entirely set free. Another small wash is then given and the wash water added to the glycerine water already run off. The glycerine water is neutralized with lime, filtered and concentrated as in the Twitchell process.
Due to the difficulties of working the autoclave saponification with lime, decomposing the large amount of lime soap obtained and dealing with much gypsum formed thereby which collects as a sediment and necessitates cleaning the tanks, other substances are used to replace lime. Magnesia, about 2 per cent. of the weight of the fat, is used and gives better results than lime. One-half to 1 per cent. of zinc oxide of the weight of the fat is even better adapted and is now being extensively employed for this purpose. In using zinc oxide it is possible to recover the zinc salts and use them over again in the digestor, which makes the process as cheap to work as with lime, with far more satisfactory results.