Salt extract

Add 4 4 g. of recrystaUised -phenylhydroxylamine to a mixture of 20 ml. of concentrated sulphuric acid and 60 g. of ice contained in a 1 litre beaker cooled in a freezing mixture. Dilute the solution with 400 ml. of water, and boil until a sample, tested with dichromate solution, gives the smell of quinone and not of nitrosobenzene or nitrobenzene (ca. 10-15 minutes). Neutralise the cold reaction mixture with sodium bicarbonate, saturate with salt, extract twice with ether, and dry the ethereal extract with anhydrous magnesium or sodium sulphate. Distil off the ether p-aminophenol, m.p. 186°, remains. The yield is 4-3 g. 

Dissolve the solid in 700 ml. of water in a 1500 ml. round-bottomed flask, and add a solution of 88 ml. of concentrated sulphuric acid in about 200 ml. of water until the liquid has a distinct odour of sulphur dioxide sufficient heat will be liberated in the neutralisation to cause the solution to boil. Immediately steam distil the liquid (Fig. II, 40, 1 it is better to use the apparatus shown in Fig. II, 41, 3) until a sample of the distillate gives only a slight precipitate with bromine water. About 700 ml. of distillate should be collected. Saturate the steam distillate with salt, extract the dl with ether, dry the extract with a little anhydrous magnesium or calcium sulphate, distil oflF the ether (compare Fig. II, 13, 4, but with a 50 ml. Claisen flask replacing the distilling flask) and distil the residue under diminished pressure. Collect the p-cresol at 95-96°/15 mm. the colourless liquid solidifies to a white crystalline solid, m.p. 31°. The yield is 24 g. 

Salt extraction Salt flotation Salt index... 

Seawater. Salt extraction from seawater is done by most countries having coastlines and weather conducive to evaporation. Seawater is evaporated in a series of concentration ponds until it is saturated with sodium chloride. At this point over 90% of the water has been removed, and some impurities, CaSO and CaCO, have been crystallized. This brine, now saturated in NaCl, is transferred to crystallizer ponds where salt precipitates on the floor of the pond as more water evaporates. Brine left over from the salt crystallizers is called bitterns because of its bitter taste. Bitterns is high in MgCl2, MgSO, and KCl. In some isolated cases, eg, India and China, magnesium and potassium compounds have been commercially extracted, but these represent only a small fraction of total world production. 

Hydrochloric acid-water Maximum boiling azeotrope Sulfuric acid Alternative to salt extractive... 

TABLE 13-19 Examples of Extractive Distillation/ Salt Extractive Distillation... 

One problem limiting the consideration of salt extractive distillation is the fact that the performance and solubility of a salt in a particiilar system is difficult to predict without experimental data. Some recent advances have been made in modeling the X T.E behavior of organic-aqueous-salt solutions using modified UNIFAC, NRTL, UNIQUAC, and other approaches [Kumar, Sep. Sci. Tech., 28(1), 799 (1993)]. 

Coiicin E (from E.coli) [11032-88-5], Purified by salt extraction of extracellular-bound colicin followed by salt fractionation and ion-exchange chromatography on a DEAE-Sephadex column, and then by CM-Sephadex column chromatography [Schwartz and Helinski J Biol Chem 246 6318 1971],... 

Jacobsen subsequently reported a practical and efficient method for promoting the highly enantioselective addition of TMSN3 to meso-epoxides (Scheme 7.3) [4]. The chiral (salen)Cl-Cl catalyst 2 is available commercially and is bench-stable. Other practical advantages of the system include the mild reaction conditions, tolerance of some Lewis basic functional groups, catalyst recyclability (up to 10 times at 1 mol% with no loss in activity or enantioselectivity), and amenability to use under solvent-free conditions. Song later demonstrated that the reaction could be performed in room temperature ionic liquids, such as l-butyl-3-methylimidazo-lium salts. Extraction of the product mixture with hexane allowed catalyst recycling and product isolation without recourse to distillation (Scheme 7.4) [5]. 

Figure 3 shows a flowsheet for plutonium processing at Rocky Flats. Impure plutonium metal is sent through a molten salt extraction (MSE) process to remove americium. The purified plutonium metal is sent to the foundry. Plutonium metal that does not meet foundry requirements is processed further, either through an aqueous or electrorefining process. The waste chloride salt from MSE is dissolved then the actinides are precipitated with carbonate and redissolved in 7f1 HN03 and finally, the plutonium is recovered by an anion exchange process. 

An overview is presented of plutonium process chemistry at Rocky Flats and of research in progress to improve plutonium processing operations or to develop new processes. Both pyrochemical and aqueous methods are used to process plutonium metal scrap, oxide, and other residues. The pyrochemical processes currently in production include electrorefining, fluorination, hydriding, molten salt extraction, calcination, and reduction operations. Aqueous processing and waste treatment methods involve nitric acid dissolution, ion exchange, solvent extraction, and precipitation techniques. 

Molten Salt Extraction. MSE has been used very successfully at Pocky Flats si nee 1967 to remove americium from plutonium ( 1, 2). 

Molten salt extraction residues are processed to recover plutonium by an aqueous precipitation process. The residues are dissolved in dilute HC1, the actinides are precipitated with potassium carbonate, and the precipitate redissolved in nitric acid (7M) to convert from a chloride to a nitrate system. The plutonium is then recovered from the 7M HNO3 by anion exchange and the effluent sent to waste or americium recovery. We are studying actinide (III) carbonate chemistry and looking at new... 

R. C. "Molten Salt Extraction of Americium from Molten Plutonium Metal," U.S. ERDA Rept. RFP-2365, Dow Chemical Co., Golden, Colorado, March 12, 1976. 

The following pages will describe several examples of pyrochemical processing as applied to the recycle of plutonium, and will briefly review the fundamental chemistry of these processes. We shall review the conversion of plutonium oxide to plutonium metal by the direct oxide reduction process (DOR),the removal of americium from metallic plutonium by molten salt extraction (MSE), and the purification of metallic... 

Figure 10 shows in graphic form the utility of molten salt extractions for americium removal in one, two, and three stage extractions for various salt-to-metal extraction feeds. This graph demonstrates the impressive power of molten salt extraction systems for purification of plutonium from americium and related rare earth elements. 

The very chemically reactive plutonium hydride is usually decomposed in a vacuum-tight furnace capable of attaining a temperature of 700°C. Plutonium hydride that is decomposed under vacuum at temperatures below 400°C forms a very fine (<20y) metallic powder above 500°C the powder begins to sinter into a porous frit which melts at 640°C to form a consolidated metal ingot. This metal typically contains significant oxide slag but is suitable for feed to either molten salt extraction or electrorefining. 

Long, J.L. Perry, C.C. "The Molten Salt Extraction of Americium from Plutonium Metal", Nuc. Metal 15 p. 385 (1969). 

Knighton, J.B. Auge, R.G. Berry, J.W. "Molten Salt Extraction of Americium from Molten Plutonium Metal", Rocky Flats Plant report RFP-2365 (1976). 

Molten Salt Extraction. The metal from DOR and PuF4 reduction is impure and proceeds to the next step in the process sequence... 

Molten Salt Extraction (MSE) - Salt Recovery. The salt residue from the americium extraction process is made up of NaCl, KC1, MgCl2, PuCl3, and AmCl3. A typical residue weighs approximately 2.0 kg and contains 200 g plutonium, 10-20 g americium, 50 g MgCl3 with the remaining equimolar NaCl-KCl. 

Molten Salt Extraction Salts Plutonium and Americium Recovery. We have demonstrated the ability to successfully strip the plutonium from the MSE salts. The resulting metal product now contains as much as 10% americium and as a result cannot be fed directly into the metal processing sequence. To use the plutonium we must remove the americium. 

Molten Salt Extraction and Electrorefining Salt Recycle. 

Chloride slagging process—See Molten salt extraction... 

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