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6A/.444/ Patented Apr April 13, 1937. B. MILLER ET AL 2,076,909 ELECTROLYTIC IRON MANUFACTURE Filed Sept. 21, 1931 77 fe C4HO Solution 3vvuevitovs aaraaaaaaaa-Pavarara Pararapaya Yavarara PP- Pararasaatar 2aey 26 Colin 6 Ain A and Benjamin Miller 53 their elitotley6A/.444/ Patented Apr. 13, 1937 2,078,909 UNITED STAT E. 2,66,909 ELECTRoLYTIC RON MANUEFACTURE Benjamin Miller and Colin G. Fink, New York, N. Y., assignors to Patents Corporation of America, Jersey City, N. J., a corporation of Delaware Application September 21, 1931, serial No. 563,954 Y 15 Claims. (C. 204-1) This invention relates to the manufacture of A still further object of the invention is to pro electrolytic iron, particularly in the form of pipes wide a process for making electrolytic iron in or tubes. which various important factors are so controlled The production of electrolytic iron has been a that iron tubes may be produced on a commer subject of investigation for many years, but up cial scale at a cost comparabie with that for pros to the present time no commercial process has ducing steel tubes. been Sufficiently successful to establish and main Another object of the invention is the provision tain itself as an industry. In the few processes of a cell for the electro-deposition of iron which which have been tried on any substantial scale, includes a specially controlled acid electrolyte. O the high consumption of electrical energy, the OW and an anode laving Special properties. O rate of iron deposit and the high investment cost With these and other objects in view the process have made operation unprofitable. : Many at of the present invention for the manufacture of tempts have been made to correct these difficul electrolytic iron tubes or sheets comprises one ties by various changes in operative procedure of in which the anode. composition, the electrolyte 5 such as the use of various iron salts, the use composition, temperature and acidity, the circu 5 of organic addition agents in the electrolyte, by lation of the electrolyte, the spacing of the elec the use of highly concentrated or dilute solutions, trodes and other factors are accurately controlled. by changes in temperature of the electrolyte, by Further objects and advantages of the process the use of oxidizing agents and by Variously node will be apparent to those sixiled in the art from fying other steps and factors involved in the the fosswing detailed description taken in cona 20 20 process. Such changes while apparently in nection with the accompanying dirawing, in proving the process in some respects have not Which:- materially aided in reducing the cost of pro Fig. is a diagranatic showing of appara duction. tus suitable for carrying out the process of the The primary object of the present invention is invention; 25 therefore to overcome the difficulties previously Fig. 2 is a longitudinal view party in Vertical encountered and produce electrolytic iron tubes or section of one of the cells shown in Fig. ii; otherforms by a profitable commercial operation. Fig. 3 is a cross-section taken on the line 3 A further object of the present invention is to of Fig. 2, and 30 provide a commercial process for the manufac Fig. 4 is a cross-section of the cell shown in 30 ture of electrolytic iron tubes or sheets, by which Fig. 2 taken on the line 4-3. a consistent Smooth deposit of iron may be ob Referring to Fig. 1 of the drawing, the general tained in an economical manner. features of the process will be described in con A further object of the invention is the produc nection with the elements of the apparatus tion of electrolytic iron sheets or tubes having a shown. In accordance with the present inven 35 thickness suitable for present and future com tion the iron to be deposited electrolytically as Emerica uses, The greatest known thickness for tubes or sheets, is deposited from an acid solu tubes or sheets made by previously tried processes tion of ferrous chloride also containing sodium is only about 0.2 inch, while usually they were only fluoride. In starting the process the ferrous 40 0.1 inch in thickness. Tubes of such thickness chloride solution, hydrochloric acid and sodium 40 would not fulfil the requirements of modern fluoride are introduced into a sump 2, from which toiler or oil still practice, or be suitable for high the solution mixture is withdrawn through a pressure gas and oil pipe lines. By the process of pipe 6 and passed by a pump 8, pipe and the present invention heavy walled tubes of any waived pipes 2 into a plurality of heating and 45 desired thickness may be made. storage tanks 4, 6 and 8. (Any suitable num 45 A further object of the invention is to provide per may be used.) In these tanks the Solution is a process whereby ores may be exploited where heated to a suitable temperature by means of their content of phosphorus or of sulfur or both direct steam introduced from a steam main 20 nakes it impractical to use them in present fer through submerged tubes 22 mounted in each 50 rous metal production processes. Experiments tank. The solution in tanks 6, 6 and 8 may 50 have show that an anode having a relatively also be heated electrically or by steam coils 26 high content of phosphorus or sulfur, or both, which may be connected through valved pipes has no effect on the cell voltage, and that such With the stean nain. 20. The storage tanks are an anode gives a cathode deposit well within the also used as settling chambers for the removal of 55 commercia imits for these substances. any suspended solid matter which gay be pres 55 2,076,909 ent in the electrolyte. Such deposits as may set ously tried processes was largely due to the neces tle out in the tanks are withdrawn through valved sary use of high cell voltage and relatively low drain pipes 26. current density. One process for example used In carrying out the process electrolyte is usu a voltage of 5 in order to obtain a current density 5 ally supplied to only two (or less than all) of . of 60 amps. per square foot. In this connection the tanks at any one time, and the heated elec it has been discovered that an iron anode Sub trolyte is continuously withdrawn from these stantially free from carbon, silicon and man tanks through valved discharge lines 28 and con ganese gives a much lower cell voltage than other ducted by means of conduit 30 to a series of cells fron. Furthermore, the presence of sulfur and lO 32, 34, etc. The electrolyte is introduced into phosphorus in the iron has no adverse effect. On 10 each cell from the line 30 through a valved the cell. The iron for the process therefore may connection 36. While electrolyte is continuously contain such quantities of sulfur and phosphorus introduced into each cell it is also continuously as to be entirely unsuited for the manufacture of withdrawn therefrom through drain pipes 38 into Steel. l5 a pipe 40 which leads to the sump 2. During the In preparing the anode pieces for the cells, a operation of the process the electrolyte is circu blast furnace iron which may be highi in phos lated at a very rapid rate through the cells and phorus, is subjected to a modified Bessemer treat back to the heating tanks in order to prevent ment in that the iron is thoroughly blown with any sediment settling out in the cells and to air to remove any carbon, silicon and manganese 20 maintain the temperature and composition of the present. Then instead of recarburizing the iron electrolyte in the cells substantially constant. as in the usual. Bessemer process the iron is Any convenient number of cells may be used in drawn at the end of the air blow and cast into connection with the lines 30 and 40, only two anode pieces in substantially the form shown in being shown in Fig. 1 for purpose of illustration. Fig. 4. The cathode may comprise an Ordinary 25 A more detailed showing of the cells 32, 34, steel tube having suitable mounting flanges sub- : etc., is given in Fig. 2 to Fig. 4, from which it will stantially as shown in Fig. 2. be seen that the electrolyte is introduced at the In starting up the apparatus a substantially bottom and near the middle of each cell and clean solution of the desired composition is made Withdrawn from both ends thereof. Each cell up preferably in the Sump 2 and then pumped 30 comprises an anode composed of a pair of pref into tanks 4, 6 and 8. The preferred solution erably semicylindrical cast iron pieces 42 suitably comprises ferrous iron in a concentration equal Supported and insulated from the remainder of to from 350 to 450 grams per liter of ferrous the cell as shown in the drawing. Within these chloride tetrahydrate together with 10 to 20 semicylindrical anode elements is mounted a grams per liter of sodium fluoride which prob 35 rotatable cathode 44, supported by blocks 46 out ably acts as a buffer. The solution is made 3.5 side the cell casing proper. The cathode may be acid by the addition of hydrochloric, hydrofluoric rotated at any suitable speed by means of a or other acid until the solution has a pH value motor 48. of from about 4 to 6, for example 5.
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