Metals vacuum distillation

Vacuum distillation of the atmospheric residue complements primary distillation, enabli r.ecoyery of heavy distillate cuts from atmospheric residue that will un r o further conversion or will serve as lube oil bases. The vacuum residue containing most of the crude contaminants (metals, salts, sediments, sulfur, nitrogen, asphaltenes, Conradson carbon, etc.) is used in asphalt manufacture, for heavy fuel-oil, or for feed for others conversion processes. 

It occurs chiefly as cinnabar, the red sulphide HgS, from which it is readily extracted either by roasting (to give the metal and sulphur dioxide) or by heating with calcium oxide the metal distils off and can be purified by vacuum distillation. 

Safety goggles should always be worn over the eyes when carrying out potentially dangerous operations, e,g. vacuum distillations, distillation of large volumes of inflammable liquids and experiments employing large quantities of metallic sodium. 

In 1986 Britannia Refined Metals (Northfleet, U.K.) introduced technology for the treatment of Parkes cmst, a triple alloy of Ag, Zn, Pb, which by 1992 had been adopted by seven lead refineries (22). The technology consists of a three-stage process in which the silver-rich cmst is first Hquated to reduce its lead content, then placed in a sealed furnace where the 2inc is removed by vacuum distillation and, finally, the silver—lead metal is treated in a bottom blown oxygen cupel (BBOC) to produce a Htharge slag and dorn metal. 

Volatilization. In this simplest separation process, the impurity or the base metal is removed as a gas. Lead containing small amounts of zinc is refined by batch vacuum distillation of the zinc. Most of the zinc produced by smelting processes contains lead and cadmium. Cmde zinc is refined by a two-step fractional distillation. In the first column, zinc and cadmium are volatilized from the lead residue, and in the second column cadmium is removed from the zinc (see Zinc and zinc alloys). 

Fused-salt electrolysis of K2NbFy is not an economically feasible process because of the low current efficiency (31). However, electrowinning has been used to obtain niobium from molten alkaU haUde electrolytes (32). The oxide is dissolved in molten alkaU haUde and is deposited in a molten metal cathode, either cadmium or zinc. The reaction is carried out in a ceramic or glass container using a carbon anode the niobium alloys with the cathode metal, from which it is freed by vacuum distillation, and the niobium powder is left behind. 

Selenium and precious metals can be removed selectively from the chlorination Hquor by reduction with sulfur dioxide. However, conditions of acidity, temperature, and a rate of reduction must be carefliUy controlled to avoid the formation of selenium monochloride, which reacts with elemental selenium already generated to form a tar-like substance. This tar gradually hardens to form an intractable mass which must be chipped from the reactor. Under proper conditions of precipitation, a selenium/precious metals product substantially free of other impurities can be obtained. Selenium can be recovered in a pure state by vacuum distillation, leaving behind a precious metals residue. 

It will be recalled that is 100% abundant and is the heaviest stable nuclide of any element (p. 550), but it is essential to use very high purity Bi to prevent unwanted nuclear side-reactions which would contaminate the product Po in particular Sc, Ag, As, Sb and Te must be <0.1 ppm and Fe <10ppm. Polonium can be obtained directly in milligram amounts by fractional vacuum distillation from the metallic bismuth. Alternatively, it can be deposited spontaneously by electrochemical replacement onto the surface of a less electropositive metal... 

Vacuum distillation of the americium away from the plutonium has been demonstrated by Berry and Knighton.12 In this work the goal was to recover pure americium metal. They demonstrated the ability to recover >50 g batches of americium (>99% pure) in a two-stage distillation. 

The chloride is mixed on a laboratory scale with xs Ca (powder or chips) in an Fe tube in a high-T glass distillation vessel. The Fe tube protects the glass from corrosive attack by the alkali-metal vapors. The vessel is inclined and evacuated while slowly heating to 700-800°C. The liberated Rb or Cs distills onto the cooler upper walls of the vessel and runs into integral glass ampules, which are sealed under vacuum for storage. Further purification is achieved by repeated. vacuum distillation at 300°C. Yields arc theoretical. 

Ultra-high-purity Mg has been prepared by either zone refining or vacuum distillation. Zone refining " is a difficult process because of the high volatility and reactivity of the metal. Nevertheless, the process can be carried out in SOj atmospheres where protective films of MgS04 and MgO are formed " ", or in ultra-pure Ar atmospheres "". Zone refining removes a number of major impurities, includ-... 

Multiple reciystallizations (three or more) from the molten metal give specimens free of the other alkaline-earth metals and a final assay of 99.9999% Combined vacuum distillation and zone melting (five passes at 880-900°C under He) reduces the alkaline-earth metal impurity levels below the detection limits. ... 

Metallic Sr (Ba) can also be produced by vacuum distillation of Sr (Ba) amalgams. The amalgams are obtained by electrolysis of saturated aqueous solutions of SrClj (BaCl2) using a Hg cathode and a Pt anode. ... 

Atmospheric sensitivity renders the preparation of ultrapure samples difficult. Nevertheless, vacuum distillation ", ultra-high-vacuum reactive distillation " and crystal growth purification methods " are described zone-refining methods have been applied on a limited scale only - , presumably because of the high volatility of the metals and the unfavorable distribution coefficients. 

Crystallization from the liquid metal has been assessed theoretically and experimentally as a purification method for both Sr and Ba After five recrystallizations, metals of 99.9999% purity can be produced. The purification of Ba by zone refining is inefficient, many passes being required for the removal of the other alkaline-earth metals. The application of combined methods (i.e., vacuum distillation plus crystal growthor vacuum distillation plus zone refining ) to the purification of both metals has also been described. 

Figure 4.23 Vacuum distillation assembly for separation of zirconium/titanium metals from reduction products.

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