Salt removal ammonia extraction process

Preparation. The mother liquors from strychnine manufacture are concentrated and the alkaloids precipitated as neutral oxalates. The precipitate is dried and extracted with dry alcohol in which the strychnine salt is the more soluble. The less soluble salt dissolved in water is decolorised with charcoal, the alkaloid regenerated with ammonia and purified by crystallisation as the sulphate. According to Saunders, pure brucine may be obtained by slow crystallisation from a solution of the pure hydrochloride in alcoholic ammonia. A method of separation depending on the greater solubility in water of strychnine hydriodide was employed by Shenstone, whilst others have made use of the sparing solubility of strychnine chromate for the removal of small quantities of this alkaloid from brucine. For a large scale process see Schwyzer. ... 

Codeine may be isolated from opium by the Gregory process [9], in which the concentrated aqueous opium extract is treated with a concentrated solution of calcium chloride, when calcium meconate, lactate, and sulphate are precipitated and removed, when the filtrate on concentration deposits the Gregory salt , a mixture of the hydrochlorides of morphine and codeine. This is purified, dissolved in water, and the morphine precipitated by ammonia, when the codeine remains in solution from which it is extracted by benzene, or the solution concentrated to the point at which a mixture of codeine hydrochloride and ammonium chloride separates. Other procedures for the isolation of codeine are available [7, 8, 10-22 inc.], critical summaries of which are given by Kanewskaja [23] and Barbier [24], Codeine may be separated from neopine (see Chap. VII) through the sulphate [25] and from morphine by chromatography [26-29]. Most of the codeine used commercially is prepared by the methylation of morphine (see below). 

Cuprous ammonium acetate extraction. Butadiene is purified by aqueous CAA extraction in a liquid-gas countercurrent process developed by Exxon (67-69). The cuprous salt forms a soluble addition complex with butadiene, which is decomposed by heat thus the process is adaptable to countercurrent multistage equipment. Typically, the C4 hydrocarbon mixture with a butadiene content of 30-40% contacts the CAA solution in a countercurrent fashion in a series of mixer-settlers. Cooling to ca -15°C is required to promote complex formation. The more saturated hydrocarbons, butanes, and butenes are first removed by distillation. Butadiene is released from the complex by further heating to 80° C. After ammonia is removed by washing with water, distillation produces butadiene that is 98-99% pure. Acetylenes and allenes are extracted with the butadiene but must... 

To remove chlorate and other salts, the 50 percent diaphragm cell caustic may be extracted with liquid ammonia in a pressurized system. The ammonia fraction then is processed through a stripper to remove and recycle the ammonia. The alkaline stripper bottoms are useful in neutralizing acidic waste streams. The purified caustic is evaporated further, and then fed to an anhydrous concentrator, typically an Inconel falling film evaporator, heated with molten salt. The anhydrous caustic, containing at least 97.5 percent NaOH, is marketed as one solid mass in drums, as flake caustic, or more desirably as beads or prills. The last are marketed in bulk or bags. 

---