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Oct. 22, 1957 R. C. KRK 2,810,636 METHOD FOR PRODUCING SODIUM Filed June 4, 1956 Charge tAeac for Waco, 7-2C-2Wa CO Wa Vooor 7 CO Gas Mo/fern Wa Gornoeraser Guerch Mo/fer? Wa 7. Aea/ O/ro SS Af xcharger Aeser/or Mo/fer? Wa WoOh+WaCOf c. Ma INVENTOR. - Aoy CAar/es kirA BY A77OAAWEYS 2,810,636 United States Patent Office Patented Oct. 22, 1957 1. 2 Some dross is inevitably formed during this condensa tion operation and is separated from the molten sodium 2,810,636 by fluxing with sodium hydroxide. It has been discovered that the carbon monoxide which METHOD FOR PRODUCING SODUM is obtained as a by-product from the reaction of carbon with sodium carbonate will react with the sodium hy Roy.Chemical Charles Company,Kirk, Midland, Midland, Michassignor Mich., a corporation to The Dow of droxide in the flux at temperatures of at least 318 C. Delaware (at which temperature the sodium hydroxide is fluid or molten) to produce sodium carbonate. The thus treated Application June 4, 1956, Serial No. 589,198 0 flux may then be fed into the reactor with added carbon 7 Claims. (C. 75-66) to produce more sodium, since the higher melting sodium carbonate does not attack the graphite lining of the re actor. In this manner a cyclical process is obtained which recovers almost 100 percent of the sodium values present. This invention relates to a process for producing So 5 Since the sodium values in the dross are almost entirely dium and is particularly directed to an improved cyclical recovered, economical modifications of the sodium car method of making sodium by the carbothermic reduction bonate reduction process which previously could not be of sodium carbonate. employed because of increased dross formation can now The carbothermic process of producing sodium by re be effected. For example, the substitution of a sodium ducing sodium carbonate with carbon in a high fempera quench for a lead quench, with the accompanying elimi ture reactor is known and is described, for example, in nation of distillation operations, may be economically United States Patent No. 2,391,728, patented December employed in spite of substantial increases in the amount 25, 1945. In general, this process comprises charging of dross formed. sodium carbonate and carbon, to a high temperature In describing the present invention in detail, reference reactor in which the carbon reduces the sodium carbonate 25 is made to the accompanying drawing which comprises to sodium vapor, and carbon monoxide is produced as a flow sheet illustrating the present process. A charge a by-product. These gases are then passed through a is made up for the reactor by combining pitch, coke and condenser in which they are directly contacted with a Sodium carbonate in the form of briquettes. While coke quench metal so as to rapidly chill the sodium vapor and is a preferred source of carbon, some pitch is desired for prevent reaction with the carbon monoxide. In the 30 use as a binder in the briquetting operation. By com process of condensing the sodium vapor, some dross is bining the carbon and sodium carbonate in intimate mix formed and must be separated from the molten sodium. ture in briquettes, the sodium carbonate preferentially This can be accomplished by fluxing the dross from the reacts with the carbon rather than the graphite liner in mixture of molten sodium and dross by adding thereto so the reactor. Also, briquetting provides the added func dium hydroxide, but the amount of sodium hydroxide 35 tion of reducing the fines which contribute materially to required for this fluxing, operation is such that approxi the amount of dross formed in the condenser. The mately 0.575 mole of sodium (in the form of the hy briquetted charge is then fed into the reactor by a droxide) must be added for each mole of sodium re suitable conveyor, such as a screw conveyor. In this covered. Thus, allowing also for reversion, this process specific example, the reactor is an electric arc furnace can never exceed a maximum of about fifty percent 40 having a graphite lining and operating at a temperature efficiency, unless the sodium values in the flux are re between 850 and 1300° C. Preferably the temperature covered. This flux - can not be fed directly back into in the reactor is at least 1200° C. The pressure within the high temperature reactor, however, because the high the reactor must exceed that in the condenser in order sodium hydroxide content thereof would react with the to force Sodium vapor from the reactor into the con graphite lining of the reactor and destroy it within a 45 denser. Reactor pressures in excess of one atmosphere relatively short period of time. are not generally employed, and it is preferable to main It is an object of this invention, therefore, to provide tain the pressure at about 0.5 atmosphere. a cyclical process for producing sodium wherein sub The sodium vapor and carbon monoxide gas produced stantially all of the sodium values are recovered from the in the reactor are forced out of the reactor through an flux in the high temperature thermal production of so 50 orifice into a condenser which is maintained at a pres dium. Another object of this invention is to provide a Sure lower than that of the reactor, preferably about cyclical process for producing sodium by the carbothermic 0.03 atmosphere. The temperature of the quench metal reduction of sodium carbonate wherein the by-products of in the condenser is preferably maintained at approxi the carbothermic reaction are so combined that they mately 300° C., although it may range from as low as provide additional charge materials for the high tempera 55 290 C. up to as high as 500° C. The condenser may ture carbothermic reaction. Other objects of this inven be constructed in various ways, and one form which has tion will become apparent from the following detailed been found Satisfactory comprises a series of curtains of description thereof when read in conjunction with the molten quench metal which intimately contact the sodium accompanying drawing, which represents a flow sheet ill vapor to rapidly chill and condense it. The quench lustrating the present invention. 60 metal may be sodium, lead or mixtures of the two metals, In practicing the process of the present invention in although in this particular illustration sodium is employed. the manner described above in connection with Patent The carbon monoxide is not condensed by the sodium No. 2,391,728, sodium carbonate is reduced with car quench and is vented from the condenser in the gaseous bon in a high temperature reactor. The charge of sodium state into a reservoir, or is used directly by passing it carbonate and Some suitable form of carbon such as 65 through valve 13 as hereinafter set forth. There is a coke is fed to the reactor in which the pressure and tem certain amount of reversion of the sodium vapor and carbon monoxide gas to produce sodium carbonate. perature are so regulated as to produce sodium vapor This carbonate along with carbon, oxides, and unreacted and carbon monoxide. The sodium vapor and carbon charge becomes intermixed with the molten sodium to monoxide are forced out of the reactor and into a con 70 produce dross. This dross passes with the molten sodium denser into intimate contact with a quench metal such into a reservoir where flake sodium hydroxide is added as inciten lead, molten sodium or a mixture thereof. to flux the dross from the sodium. The temperature 2,810,636 3 4. of the sodium in the reservoir must be within the range producing sodium in which almost all of the sodium of 290 C. to 500 C. in order to prevent reaction with values are recovered. A primary advantage of this proc the sodium hydroxide. Preferred temperatures of the ess resides in the use of fluid flux while still molten and reservoir metal range from 360° C. to 380° C. The freed the hot moisture-free carbon monoxide gas to produce sodium is then drawn off at a predetermined rate, part of 5 sodium carbonate. Under the conditions of the present it being recirculated through a heat exchanger for use as invention, this reaction is highly economical and com a quenching medium and the remainder being separated bines two waste byproducts to provide a charge material as the end product. The hot fluid flux, which consists that can be directly introduced into the single reactor principally of sodium hydroxide and sodium carbonate, employed. along with some unreacted carbon and occluded sodium, O What is claimed is: is drawn off from the bottom of the reservoir. 1. In a process for producing sodium which comprises Up to this point the flow sheet process is quite similar reducing sodium carbonate with carbon in a high tem to that disclosed in Patent 2,391,728. The primary dis perature reactor to produce sodium vapor and carbon tinction resides in the use of a sodium quench rather monoxide, condensing the sodium vapor to produce than the lead quench disclosed in the patent, which re molten sodium and a dross consisting principally of so quires a still for recovering the molten sodium from the dium carbonate and carbon, fluxing the dross from the molten lead. Of course, the lead quench can be used in molten sodium with sodium hydroxide and separating the the present process, although one of the advantages of flux from said molten sodium, the improvement which the instant process is that a sodium quench, which pro comprises the steps of contacting the flux with carbon duces more dross than the lead quench, can be economi monoxide gas at a temperature of at least 318 C.