US1238604A - Process of winning metals. - Google Patents

Process of winning metals. Download PDF

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US1238604A
US1238604A US85800114A US1914858001A US1238604A US 1238604 A US1238604 A US 1238604A US 85800114 A US85800114 A US 85800114A US 1914858001 A US1914858001 A US 1914858001A US 1238604 A US1238604 A US 1238604A
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aluminum
chlorid
silicon
halogen
chlorin
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Victor M Weaver
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Priority to US1559A priority patent/US1297946A/en
Priority to US2234A priority patent/US1241796A/en
Priority to US44517A priority patent/US1296575A/en
Priority to US44518A priority patent/US1269236A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/02Silicon
    • C01B33/021Preparation
    • C01B33/027Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
    • C01B33/029Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition of monosilane

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  • Wj/bmssas fnlvcn/wr W4 Y, V/YZEZOFM Wcovcar 2'10 $9M I I; I 1-1 [I I 9 V. M. WEAVER.
  • ZSHEETSSHEET 7- fins-566s Invenfior Q Tliaivfi M. Weave/ I Atbfys UNITED sTATEs PATENTOFFICE.
  • My invention relates to processes of winning metals and is concerned particularly with a process of securing metals from their oxide.
  • the chlorin I charge the aluminum chlorid into an electrolyzing vat preferably containing melted sodium chlorid and the consequent electrolysis separates the aluminum from the chlorin so that the former may be tapped away from the sodium chlorid while the latter may he conducted to a storage tank for further use.
  • I may point out, that my process'is continuous in the sense that it permits of the constant feeding of clay at one point in the process with the corresponding production of aluminum and silicon at other points in the process and the reacting agents may be used and reused and may require replenishing only because of any unavoidable leaks which may occur in the system.
  • the silicon tetrachlorid is fed into a chamber containing molten aluminum and by reason of the greater aflinity of the chlorin for chlorid, like the aluminum chlorid obtained,
  • condenser elements may be subjected to electrolysis, as above described, in order to free the chlorin and secure the aluminum therefrom.
  • FIG. 2 is a vertical sectional View of the chlorinizing furnace
  • Fig. 3 is a hOI'lZOIltiLl sectional view of the chlorinizing furnace taken on the plane of the line 3-3 of Fig. 2 and looking in the direction indicated by the arrows;
  • Fig. 4 is a sectional view, taken on a horizontal plane, of the electrolyzing vat
  • Fig. 5 is a vertical sectional view taken on the'plane of the line 55 of Fig. 4 and looking in the direction indicated by the ar rows;
  • Fig. 6 is a sectional view drawn on a larger scale, taken on the plane of the line 66 of Fig. 4 and looking in the direction indicated by the arrows;
  • Fig. 7 is a sectional view, taken on a horizontal plane, of the second furnace which is employed.
  • Fig. l the chlorinizing furnace is shown at 9, and by reference to Figs. 2 and 3 it will be seen that this chlorinizing furnace is of the closed type and provides for a bed of coke 10, in which a plurality of electrodes 1111, extending inwardly through the circular housing as illustrated in Fig. 3, are lodged.
  • Each of the carbon electrodes 11 is firmly mounted in a terra cotta pipe 12, which in turn is mounted in the fire brick housing 13.
  • An electric conductor 14 is provided for each of the carbon electrodes and this conductor is in the form of a pipe which is connected with the electrode at 15 and which is supported in position by means of a union 16 packed at 17.
  • the pipe 14 is kept cool by a flow of water introduced through the entry pipe 18, and, after circulation, passed through the return pipe 19.
  • the usual insulated electric conductor 20 may be attached to the end of the pipe 14, as illustrated, and at this distance from the furnace housin the conductor and its insulation will not be injuriously affected by the heat.
  • the reference character 21 indicates a clean-out door which may be provided, and a peep hole arrangement 22 may also be provided.
  • the charge is indicated at 26 and the bed is preferably so arrangedthat the coke exposed in the middle is surrounded by packed clay, as illustrated at.27, 27.
  • the char e may be any clay but I have found that t e higher grades of clay, such as kaolin, of the formula AlASiO (the moisture being driven therefrom) is especially desirable.
  • the furnace has only the outlet 28 and it will be nbted as this description. proceeds that'the entire-system is closed as this furnace is.
  • a graphite pipe 29 extends through the fire brick housing of the furnace and terminates in the heart of the coke bed. This pipe 29 is fed through a pipe 30 (Fig. 1)
  • This condenser is in the form of a double closed chamber providing the compartment 34 and the compartment 35 separated by a partition 36.
  • the compartment 34 is provided with a system of cooling pipes 37, 37, which extend downwardly through and from the top of the chamber and which are distributed throughout the entire space of this particular compartment in order to get complete temperature control.
  • the pipes 37, 37 are joined at the upper ends outside of the chamber by means of the header pipe 38 and circulation is secured in any desirable manner.
  • the system of pipes is connected to a cold water supply and the result is that as the three gases which have been referred to enter and pass through the.
  • the first condenser element 34 is devoted to the condensation of the aluminum chlorid and the white powder to .which it is reduced is removed fromthe pipes upon which it is deposited by means of the scrapers 39, 39, which by means of pulley cords 40 passing over suitable pulleys 41, 41 on the outside of the condenser are drawn up and down on the pipes to scrapethem, in an obvious manner.
  • the condenser element 35 is provided with a. system of cooling pipes 50 like the pipes 37, these pipes having the outside header 51 and being provided with the scrapers 52, 52 hung fromthe pulley cords 53, 53, pass ing over the pulleys 54, 54.
  • the cooling pipes 50 are supplied with a freezing mixture of ice Water and salt, and the temperature in the condenser element 35 is therefore considerably lower than the temperature in the condenser element 34.
  • the lower temperature is sufiicient to condense the silicon tetrachlorid which comes down as a colorless liquid, except for any impurities which may discolor it.
  • This liquid silicon tetrachlorid passes down the sloping bottom of the condenser element 35 and passes through the outlet 55, controlled by 'the valve 56 which leads to the tank 57.
  • the condenser element 35 is provided with scrapers as the condenser element 34 is, because condenser element are operated during all the time that the system is being worked.
  • the condense-r element 35 is provided wit a conveyer 58.
  • the carbon monoxid passes out of the son I denser element 35 through a pipe 59, past a valve 60 and to a closed gas pump 61, and is then carried to a scrubber 62 by means of a pipe 63, this scrubber being in the form of a tank containing lime water and having an outletpipe 63" leading therefrom.
  • This outlet pipe is provided with a valve 64 and leads to a telescoping gas tank 65 so that pressure may be kept upon the carbon monoxid which finds its way to this tank and so that the carbon monoxid may be fed by way of a pipe 66 to any number of burners 67, 68 and 69, which are used for heating purposes in certain other steps in the process which will hereinafter'be referred to.
  • the lining of the furnace provides a closed cavity 76 for the molten metal which is formed between and around tubular casing parts 77, 77, within which the magnetic circuit frame and the primary coils 78 and 79, respectively, are disposed.
  • the details of this furnace per 80 do not constitute part of my present invention, but I refer to them because it is a type of furnace well adapted for use as part of my system.
  • the valve 71 is opened and the liquid aluminum chlorid is fed into this bath of molten aluminum near the bottom thereof, the aluminum chlorid is immediately reconverted into a gas due to the release of pressure and heat of bath, and passes up through the molten aluminum. Due to the greater affinity of the chlorin for thealuminum than for the iron, or other im-' purity for that matter, the chlorin releases the iron and takes on the'proper share of aluminum. The result is that the refined aluminum chlorid will vleave the bath of aluminum and will pass out of the furnace through the pipe 81. It will be noted that the pipe 81 divides into the pipes 82 and 83, which are provided with valves 84 and 85,
  • valve 84 is kept closed and the valve 85 is opened, so that the aluminum-chlorid gas may pass up the pipe 83 and be passed back into the condenser element 34 for condensation purposes, and in its refined state it will be recharged into the Rodenhauserfurnace, as has been described, and this process may be repeated until the required degree of purityhas been attained.
  • the valve 85 is closed and the valve 8 1 is opened, so that the substantially pure aluminum chlorid may be passed into what may be termed condenser #2, as indicated.
  • This condenser is of the same structure as the condenser element 34, and the condensed aluminum chlorid in the formof a white powder is brought down into the tank 86.
  • the aluminum chlorid may be put under pressure by Way of the pipe 87 leading from the compressedair tank' 48, and may also be subjected to heat from afiame at the burner 69, preferably confined within fire-walls. This again melts-the aluminum chlorid, which may then be conducted to a storage tank 88 through a pipe 89controlled by a valve 90, the pure aluminum chlorid being heated by a carbon monoxid flame at the burner 68 so as to be kept in a liquid condition.
  • the liquid aluminum chlorid is conducted through a valve 91 and a pipe 92 to the electrolytic vat, which is also sealed.
  • the electrolytic vat is illustrated in detail in Figs. 4, 5 and 6, and it will be seen that it comprises a graphite hearth 93 and fire-brick surround ing walls 94, 94:, with magnesite linings 95, 95, the entire vat being surrounded by sustaining plates 96.
  • Each of the anodes is provided with a collar 112, which is engaged by a loose collar 113 'which may be tops of the electrode stems 110, and in this way the current is conveyed to the bath, the
  • the liquid aluminum chlorid is kept at a high temperature, about 200 centlgrade, and at about a pressure of two and a half atmospheres.
  • the electrolyte is a bath of melted sodium chlorid at a high temperature which is primarily induced by external means, but which is maintained by the application'of the current, the heat being due to the resistance of the bath.
  • the aluminum chlorid is fed to the bath at such a rate'as to keep the bath saturated.
  • the action which takes place inthe electrolytic vat separates the aluminum from the chlorin and leaves the sodium chlorid.
  • the free silicon is tapped from the Rodenhauser furnace my way of the spout 127, and the aluminum-chlorid gas is passed either to the condenser element 34, if it is to be further refined, or to the condenser #2, if it is to be immediately condensed and passed on to the electrolytic vat to be split up into the elements aluminum and chlorin.
  • the Rodenhauser furnace has the double function of displacing the iron or other impurities in the impure aluminum chlorid with aluminum, in which case the impurities are cleaned out of the furnace chlorinizing furnace, while the carbon mon-' oxid which is formed by the oxygen liberated from theclay and the coke which is 1ntroduced is used for burner purposes. It is important .that the system be a closed sys-. term, as described, to exclude the moisture and to protect the active chlorids, particularly the aluminum chlorid.
  • anoxygen compound is speci-' fied it is assumed that it may or may not be separated from both halogen or chlorin compounds, it being preferable, however, to do so, as is the case in the specific description above..
  • the essential thing is that the or chlorin compounds are separated.
  • the hearth is the cathode and the graphite blocks constitute the anode
  • I may also state that, sofar as I have been able to, observe, the action of the vat is a reduction process.
  • the aluminum forms globules varying in size from more specks to considerably larger particles.
  • the chlorin is liberated and streams away with great rapidity.
  • the aluminum which is thus formed is heavier and settles to the bottom, and the particles of aluminum as formed above the bottom frequently join to form Where, in the winning of other metals; for instance, zinc can be secured from zinc chlorid by this process.
  • Theprocess of securing a metal from a substance containing1 it and silicon which comprises treating t e substance with a halogen to-form a compound of the metal and the halogen and a compound of silicon and the halogen, then separating the two halogen compounds, and then separating the metal from the halogen.
  • the process of securinglaluminum and silicon from clay which comprises treating the clay with chlorin in the presence of a reducing agent inert toward chlorin to form i aluminum chlorid, silicon tetrachlorid and a compound formed by the reducing agent and oxygen released from the clay, then separating the two chlorids, and then separatmg each of the desired elements from the chlorin.

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Electrolytic Production Of Metals (AREA)

Description

V. M. WEAVER.
PROCESS OF WINNING METALS.
APPLICATION FILED AUG-22. 1914.
1,238,604. Patented Aug. 28,1917.
[SHEETS-SHEET 1- 62 CONDENSER *8 'Wz'Jbn/esses: Inventor U W Victor M Wwvez y Wm V. M. WEAVER.
PROCESS OF WINNING METALS.
. APPLICATION FILED AUG-22,1914. 1,23 04, PatentedAug. 28,1917.
7 SHEETS-SHEET 2.
Wj/bmssas: fnlvcn/wr W4 Y, V/YZEZOFM Wcovcar 2'10 $9M I I; I 1-1 [I I 9 V. M. WEAVER.
PROCESS OF WINNING METALS.
APPLlCATlON FILED AUG-22,1914.
1,288,604. Patented Aug. 28,1917.
ZSHEETS-SHEET 3.
51157165665 2 .ZTLUiT/OT %4? y W W V. M. WEAVER.
PROCESS OF WINNING METALS.
APPLICATION FILED AUG-22. 1914.
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v. M. WEAVER.
PROCESS OF WINNING METALS.
APPLICATION FILED AUG-22, 19H.
1,238,604. v Patenfed Au 28,1917.
7 SHEETSSHEET 5- W/ ixbnaes I 8- '7 17122621102 yictormwmr B. V r
V. M. WEAVER.
PROCESS OFWINNKNG METALS. APPLICATION FILED AUG-22. 1914.
Patented Aug. 28, 1917.
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V. M. WEAVER.
PROCESS OF WINNING METALS,' APPLICATION FILED AUG-22, 1914.
1,238,604. Patented Aug. 28,1917.
ZSHEETSSHEET 7- fins-566s: Invenfior Q Tliaivfi M. Weave/ I Atbfys UNITED sTATEs PATENTOFFICE.
vIoTon M. WEAVER, oEHAEEIsBUEo, :eEnnsYLvAmA, Assrcnon ro WEAVER com- IPANY, A CORPORATION or WISCONSIN.
rEooEss-oE wmmnc METALS.
Application filed August 22, 1914. Serial No. 858,001.
ary 11, 1915, Serial No. 2234, filed January To all whom z't may concern:
Be it known that I, VICTOR M. WEAVER, a
. citizen of the United States, residing at Harrisburg, in the county of Dauphin and State of Pennsylvania, have invented a certain new and useful Improvement in Processes of. Winning Metals, of which the following is a full, clear, concise, and eXact description, reference being had to the accompanying-drawings, forming a part of this specification.
My invention relates to processes of winning metals and is concerned particularly with a process of securing metals from their oxide.
It will. appear to those skilled in the art that my invention may be variously employed in order to secure various metals from their various compounds and that certain steps in the process of my invention and certain parts of the apparatus-which l employ may be usefully engaged in various pursuits, and while I shall define the metes and bounds of my invention by the appended claims I shall refer specifically in this disclosure to a certain process and to certain apparatus for the recovery of aluminum and silicon, respectively, from clay, time being the embodiment of: my in- .vention with which I have experimented I most thoroughly and which I regard as ot special importance. This description 01 my process as utilized to secure'aluminuin and silicon in their respective elemental states from clay will enable those skilled in the art to understand and appreciate my invention, and it will be understood that the process and ap'oaratus'whioh 1 herein set forth is an example of the carrying out and use of my invention so that those skilled in the art maybe duly advised. In my process of securing aluminum and silicon from clay I have devised numerous refinements which are peculiarly adapted to this particular embodimentof my invention and I make these refinements the subject matter of the more limited oi the appended claims. It Wlll appear' also that there is novelty not only in the combination of steps which I employ in my process but that the steps per 86 are novel, the steps per se being claimed in my co pending applications, Serial No. 919, filed January 7 1915, Serial No. 1559, filed Janu- 191'5, Serial No. 44,518, filed August 9, 5.
I shall now proceed with a' specific description of my invention as embodied in my process of and apparatus for recovering aluminum and silicon fromclay, and I shall refer to and describe the various parts of the apparatus and the various steps in the process in detail in order to instruct those skilled in the art.
In the treatment of clay I break up the compound by the use of chlorin gas so as to produce aluminum chlorid and silicon .tetrahlorid, this action being carried on under special restrictions and conditions, as will later be more fully described. I then subject the chlorids which are thus formed to condensing temperatures and the process here divides into two branches, one of which is concerned with theproduction of aluminum in its elemental state and the other of which is directed toward the production of silicon in its elemental state. In order to separate the aluminum time the chlorin I charge the aluminum chlorid into an electrolyzing vat preferably containing melted sodium chlorid and the consequent electrolysis separates the aluminum from the chlorin so that the former may be tapped away from the sodium chlorid while the latter may he conducted to a storage tank for further use. In this connection I may point out, that my process'is continuous in the sense that it permits of the constant feeding of clay at one point in the process with the corresponding production of aluminum and silicon at other points in the process and the reacting agents may be used and reused and may require replenishing only because of any unavoidable leaks which may occur in the system.
, The silicon tetrachlorid is fed into a chamber containing molten aluminum and by reason of the greater aflinity of the chlorin for chlorid, like the aluminum chlorid obtained,
from the condenser elements, may be subjected to electrolysis, as above described, in order to free the chlorin and secure the aluminum therefrom.
I My invention will be more readily understood by reference to the accompanying Fig. 2 is a vertical sectional View of the chlorinizing furnace;
Fig. 3 is a hOI'lZOIltiLl sectional view of the chlorinizing furnace taken on the plane of the line 3-3 of Fig. 2 and looking in the direction indicated by the arrows;
Fig. 4 is a sectional view, taken on a horizontal plane, of the electrolyzing vat;
Fig. 5 is a vertical sectional view taken on the'plane of the line 55 of Fig. 4 and looking in the direction indicated by the ar rows;
Fig. 6 is a sectional view drawn on a larger scale, taken on the plane of the line 66 of Fig. 4 and looking in the direction indicated by the arrows;
Fig. 7 is a sectional view, taken on a horizontal plane, of the second furnace which is employed; and
Fig. 8.1s a sectional view taken on the plane of the line 88, Fig. 7, and looking in the direction indicated by the arrows.
Referring first to Fig. l, itwill be seen that the chlorinizing furnace is shown at 9, and by reference to Figs. 2 and 3 it will be seen that this chlorinizing furnace is of the closed type and provides for a bed of coke 10, in which a plurality of electrodes 1111, extending inwardly through the circular housing as illustrated in Fig. 3, are lodged. Each of the carbon electrodes 11 is firmly mounted in a terra cotta pipe 12, which in turn is mounted in the fire brick housing 13. An electric conductor 14 is provided for each of the carbon electrodes and this conductor is in the form of a pipe which is connected with the electrode at 15 and which is supported in position by means of a union 16 packed at 17. The pipe 14; is kept cool by a flow of water introduced through the entry pipe 18, and, after circulation, passed through the return pipe 19. The usual insulated electric conductor 20 may be attached to the end of the pipe 14, as illustrated, and at this distance from the furnace housin the conductor and its insulation will not be injuriously affected by the heat. The reference character 21 indicates a clean-out door which may be provided, and a peep hole arrangement 22 may also be provided.
The charge isintroduced into the chlorinizing furnace by way of a screw conveyer, indicated at 23 at the bottom of a hopper bin 24, this screw conveyer leadin the charge to the passage 25,-through which'the charge may drop on to the bed of coke which has already been referred to.
The charge is indicated at 26 and the bed is preferably so arrangedthat the coke exposed in the middle is surrounded by packed clay, as illustrated at.27, 27. The char e may be any clay but I have found that t e higher grades of clay, such as kaolin, of the formula AlASiO (the moisture being driven therefrom) is especially desirable. It will be noted that the furnace has only the outlet 28 and it will be nbted as this description. proceeds that'the entire-system is closed as this furnace is. It will be noted that a graphite pipe 29 extends through the fire brick housing of the furnace and terminates in the heart of the coke bed. This pipe 29 is fed through a pipe 30 (Fig. 1)
from a storage tank 31, the connection being controlled by a valve 32. It will now be noted that with the chlorin properly fed to the graphite pipe and with the current properly applied to the electrodes the activity of the chlorin gas and the heat immediately effects the disintegration of the kaolin, the formation of aluminum chlorid and silicon tetrachlorid, and, by the combination of the carbon and the oxygen liberated from the kaolin, the formation of carbon monoxid. So'far. as the degree of heat is concerned, thoseskilled in the art will, of course, be guided by the fact that such a degree of heat as effects reaction between the chlorin and the aluminum and silicon is required, the effective temperatures being well known in the art. I might add, for what further assistance it may give, that I have found that temperatures between 900 and 1200 centigrade are most efiicient.
The reaction is as follows:
, The three gases thus formed naturally rise and pass out of the outlet opening 28, and, as illustrated in Fig. 1', are conducted to the condenser 33. This condenser is in the form of a double closed chamber providing the compartment 34 and the compartment 35 separated by a partition 36. The compartment 34 is provided with a system of cooling pipes 37, 37, which extend downwardly through and from the top of the chamber and which are distributed throughout the entire space of this particular compartment in order to get complete temperature control. The pipes 37, 37 are joined at the upper ends outside of the chamber by means of the header pipe 38 and circulation is secured in any desirable manner. In this particular condenser element the system of pipes is connected to a cold water supply and the result is that as the three gases which have been referred to enter and pass through the.
which these respective gases condense are, of course, well known in the art. It might be mentioned here that it is possible that chlorid which plays any considerable part.
Since the temperature which is produced by the circulation of mere cold water in the cooling pipes 37, 37 is not sufliciently low to condense silicon tetrachlorid, this gas, together with the carbon monoxid, passes on to the neXt compartment-35 of the condenser. Thus the first condenser element 34 is devoted to the condensation of the aluminum chlorid and the white powder to .which it is reduced is removed fromthe pipes upon which it is deposited by means of the scrapers 39, 39, which by means of pulley cords 40 passing over suitable pulleys 41, 41 on the outside of the condenser are drawn up and down on the pipes to scrapethem, in an obvious manner. The powder is thus thrown down on to the conveyer 42, the upper run of which passes in the direction of the arrow 43, and thus the condensed aluminum chlorid is brought to the end of the condenser element where the outlet 44 leading to a tank 45 is provided. This outlet may be controlled by a valve 46. It will be noted that this tank is connected by means of a pipe 47 with :acompressed air tank 48, which is fed through the air compressor 49. It is important, as before indicated, that the system be a closed system and that various actions be carried on under pressure, and I speak of it particularly at this time because of the fact that the aluminum chlorid to which I have just referred is extremely deliquescent and must be kept free from moisture in order to avoid decomposition and the formation of hydrochloric acid. When the system is closed, however. such a result is not possible, and the pressure has a purpose to be referred to later.
Leaving the aluminum chlorid, which has been deposited in the'tank 45, for the present, I shall follow the course of the silicon tetrachlorid gas and the carbon monoxid through the second element of the condenser. The condenser element 35 is provided with a. system of cooling pipes 50 like the pipes 37, these pipes having the outside header 51 and being provided with the scrapers 52, 52 hung fromthe pulley cords 53, 53, pass ing over the pulleys 54, 54. Instead of being supplied with mere cold water, however, the cooling pipes 50 are supplied with a freezing mixture of ice Water and salt, and the temperature in the condenser element 35 is therefore considerably lower than the temperature in the condenser element 34. The lower temperature is sufiicient to condense the silicon tetrachlorid which comes down as a colorless liquid, except for any impurities which may discolor it. This liquid silicon tetrachlorid passes down the sloping bottom of the condenser element 35 and passes through the outlet 55, controlled by 'the valve 56 which leads to the tank 57. The condenser element 35 is provided with scrapers as the condenser element 34 is, because condenser element are operated during all the time that the system is being worked. The condense-r element 35 is provided wit a conveyer 58.
The carbon monoxid passes out of the son I denser element 35 through a pipe 59, past a valve 60 and to a closed gas pump 61, and is then carried to a scrubber 62 by means of a pipe 63, this scrubber being in the form of a tank containing lime water and having an outletpipe 63" leading therefrom. This outlet pipe is provided with a valve 64 and leads to a telescoping gas tank 65 so that pressure may be kept upon the carbon monoxid which finds its way to this tank and so that the carbon monoxid may be fed by way of a pipe 66 to any number of burners 67, 68 and 69, which are used for heating purposes in certain other steps in the process which will hereinafter'be referred to.
powder in the tank 45 (this powder being,
white unless discolored by impurities), it will be noted that l have placed the burner 67 under this tank, and I may mention here that I surround the tank in practice with a suitable fire wall so that I can subject the tank to a high degree of heat. With the valve 46 closed, the material in the tank 45 can be placed under high pressure from the tank 48, and this pressure, together with the heat from the carbon monoxid burner, melts the aluminum chlorid, after which step the aluminum chlorid is much more stable and much more easily handled, due to its physical condition, and desirably so in view of the steps which are to follow and which will presently be described. I desire to state, however, that it is entirely feasible to conduct the aluminum chlorid to the farther later.
mounted in a correspondingly shaped base 7 5, the idea being that when the connecting pipes are temporarily detached, the, furnace can be tilted in order to tap off molten metal, as will be pointed out a little later. The lining of the furnace provides a closed cavity 76 for the molten metal which is formed between and around tubular casing parts 77, 77, within which the magnetic circuit frame and the primary coils 78 and 79, respectively, are disposed. The details of this furnace per 80 do not constitute part of my present invention, but I refer to them because it is a type of furnace well adapted for use as part of my system. For the purposes of the pres.- ent description, I shall assume that the valve 80 is closed, and I shall refer to this valve With this assumption, it will be seen that when the valve 71 is opened, the liquid aluminum chlorid'is conducted to the working chamber of the Rodenhauser furnace. The reason for this step in the process is as follows:
In the first condensation of the aluminum chlorid in the condenser element 34,. there are likely to be impurities, principally iron, and it is the object of the step in the process now under description to eliminate this iron and to secure pure aluminum chlorid. Therefore, preliminarily, the Rodenhauser furnace is charged with aluminum, and the molten bath, as illustrated, is formed, when,
as beforestated, the valve 71 is opened and the liquid aluminum chlorid is fed into this bath of molten aluminum near the bottom thereof, the aluminum chlorid is immediately reconverted into a gas due to the release of pressure and heat of bath, and passes up through the molten aluminum. Due to the greater affinity of the chlorin for thealuminum than for the iron, or other im-' purity for that matter, the chlorin releases the iron and takes on the'proper share of aluminum. The result is that the refined aluminum chlorid will vleave the bath of aluminum and will pass out of the furnace through the pipe 81. It will be noted that the pipe 81 divides into the pipes 82 and 83, which are provided with valves 84 and 85,
respectively. If the refined aluminum chlorid is to be further purified, the valve 84 is kept closed and the valve 85 is opened, so that the aluminum-chlorid gas may pass up the pipe 83 and be passed back into the condenser element 34 for condensation purposes, and in its refined state it will be recharged into the Rodenhauserfurnace, as has been described, and this process may be repeated until the required degree of purityhas been attained. At this point, the valve 85 is closed and the valve 8 1 is opened, so that the substantially pure aluminum chlorid may be passed into what may be termed condenser #2, as indicated. This condenser is of the same structure as the condenser element 34, and the condensed aluminum chlorid in the formof a white powder is brought down into the tank 86. In this tank 86 the aluminum chlorid may be put under pressure by Way of the pipe 87 leading from the compressedair tank' 48, and may also be subjected to heat from afiame at the burner 69, preferably confined within fire-walls. This again melts-the aluminum chlorid, which may then be conducted to a storage tank 88 through a pipe 89controlled by a valve 90, the pure aluminum chlorid being heated by a carbon monoxid flame at the burner 68 so as to be kept in a liquid condition.
. From this storage tank 88 the liquid aluminum chlorid is conducted through a valve 91 and a pipe 92 to the electrolytic vat, which is also sealed. The electrolytic vat is illustrated in detail in Figs. 4, 5 and 6, and it will be seen that it comprises a graphite hearth 93 and fire-brick surround ing walls 94, 94:, with magnesite linings 95, 95, the entire vat being surrounded by sustaining plates 96. Along opposite sides of the vat are access openings 97, 97, which are normally sealed by means of covers 98, 98, and a tap hole 99 is provided for a purpose .that will be referred to presently, this tap .nected by means of a pipe 102, in which there is a valve 103,with a chlorin compressor 104, which in turn is connected by a pipe 105 with a chlorin cooler 106, these two elements being merely diagrammatically shown. The cooler 106 is connected. by means of a pipe 107 with the liquid chlorin tank 31, which has already been referred to, and the connecting pipe 107 is provided with a valve 108 Returning to the detailed showing of the electrolytic vat, it will be seen, from Figs. 5 and 6 particularly, that the'anodes are in the form of graphite blocks 109, to each of which three stems 110, 110 are secured, the
stems-being firmly lodged in a reinforcedfire-brick seal cover 111. Each of the anodes is provided with a collar 112, which is engaged by a loose collar 113 'which may be tops of the electrode stems 110, and in this way the current is conveyed to the bath, the
graphite hearth acting as the opposite electrode. The center one of each set of three anode stems is drilled axially, as indicated 20 a storage tank is transmitted through hot-oil at 119, and this bore, is connected to distributing-passageways 120, 12.0 in the corresponding graphite block. Each of. these bores is connected by means of a pipe .121 with the suppl pipe 92, which has been hereinbefore re erred to, and a valve 122 is disposed in each pipe 121 and is intermittentlyoperated for feeding purposes by a traveler 123 which is mounted upon a rotating shaft 124 Thus, when the various r0- tating shafts 124 are put into operation, and, as before stated, the valve 91 is opened to permit the passage of the liquid aluminum chlorid, a constant feed is afforded down through the passageways 119 and into the vat. 1
The liquid aluminum chlorid is kept at a high temperature, about 200 centlgrade, and at about a pressure of two and a half atmospheres. The heated material from the baths in pipes 125 which surround the supply pipes 92, and thus it is insured that the aluminum chlorid be fed'into the vat at the proper temperature. The electrolyte is a bath of melted sodium chlorid at a high temperature which is primarily induced by external means, but which is maintained by the application'of the current, the heat being due to the resistance of the bath. The aluminum chlorid is fed to the bath at such a rate'as to keep the bath saturated. The action which takes place inthe electrolytic vat separates the aluminum from the chlorin and leaves the sodium chlorid. Due to the difference in specific gravity between the pure aluminum which is thus obtained and the melted sodium chlorid, it is a simple matter to. tap off the molten aluminum by removing the plug 100, and in this way the first ultimate ob ect of my process is obtainedthe securing of aluminum in its elemental state from clay. Since the action is secured leaving sodium chlorid, the electrolyte may go on indefinitely. The chlorin which is freed is passed to the chlorin compressor 104, then to the cooler, and then to the storage tank, where is is drawn from to supply the chlorinizing furnace 9, all as hereinberore described.
-Returning now to the silicon chlorid which has been collected in the tank 57 in liquid'condition, it will be seenthat the pipe 126 leads to the valve 80, which has hereinbefore been referred, to, and at the time when the silicon chlorid is to be split up the immediately 'begun, due to the greater affinity of the chlorin for'the aluminum than for the silicon. In this way the aluminum displaces the silicon in the chlorid and free silicon and aluminum-chlorid gas are formed. The free silicon is tapped from the Rodenhauser furnace my way of the spout 127, and the aluminum-chlorid gas is passed either to the condenser element 34, if it is to be further refined, or to the condenser #2, if it is to be immediately condensed and passed on to the electrolytic vat to be split up into the elements aluminum and chlorin.
Thus the Rodenhauser furnace has the double function of displacing the iron or other impurities in the impure aluminum chlorid with aluminum, in which case the impurities are cleaned out of the furnace chlorinizing furnace, while the carbon mon-' oxid which is formed by the oxygen liberated from theclay and the coke which is 1ntroduced is used for burner purposes. It is important .that the system be a closed sys-. term, as described, to exclude the moisture and to protect the active chlorids, particularly the aluminum chlorid.
An important feature in the matter of the operation of my system is found in the feeding of the melted aluminum chlorid to the electrolytic vat. It is an important feature of my invention that the electrolytic bath is fed with the melted aluminum chlorid insuch a' way as to keep it saturated.
It-will be apparent to those skilled in the art that various modifications might be made in this system without departing from the spirit or scope thereof. For instance, one might use fused zinc, instead of fused aluminum, forthe breaking up of the silicon chlorid, or one might use a diflerent electrolyte; so far as structure is concerned, it will be seen that any kind of furnace might be used, but I have attempted to refer to those which are particularly adaptable, and, so
far as certain refinements are concerned,
necessary. In heatin the ip es which maintain the aluminum ch orid 1n 1ts melted condition while being fed to the electrolytic bath, it might be better practice in some instances to use electric heating coils than to use an oil bath, and it might be well to heat the aluminum-chlorid containers in a manner other than by the carbon monoxid flame. With the closed system-which has vantage that there is no electrode consumption, and therefore when the electrodes are halogen adjusted they will remain adjusted, and economic service is secured.
In charging the chlorinizing furnace, it is good practice to mix calcined clay and coke breeze to the right proportions before feeding it into the furnace, and to drop the mixture through the roof. I also use a deep fire and run the pile at a white heat. I contemplate the use of other reducin agents than that specifically mentione and I have taken care of this in some of the appended claims. claims, I speak of a reducing agent inert toward the reagent, I mean, of course, inert under the circumstances of the process set forth. For instance carbon, which I mention specifically, does react with chlorin under certain circumstances, but not under the conditions of theprocess described. I may state here, for what further assistance it may give, that carbon monoxid is a perfectly feasible reducing agent for use in my process. In the appended claims where the formation of anoxygen compound is speci-' fied it is assumed that it may or may not be separated from both halogen or chlorin compounds, it being preferable, however, to do so, as is the case in the specific description above.. The essential thing is that the or chlorin compounds are separated. I desire to call attention to the fact that it is possible to treat the clay with chlorin in some other way than to feed the chlorin described. I contemplate the use of comto the chlorinizing furnace, as has been pounds of chlorin to secure reactions, in order to produce the chlorids. For instance I might use carbon tetrachlorid and fee this carbon tetrachlorid, which is a colorless mobile liquid, into the chlorinizing furnace with the clay and. carbon, or into the mixture of clay and carbon already fedinto the furnace.
Referring to the electrolytic vat, I may mention here that the hearth is the cathode and the graphite blocks constitute the anode, and I may also state that, sofar as I have been able to, observe, the action of the vat is a reduction process. The aluminum forms globules varying in size from more specks to considerably larger particles. The chlorin is liberated and streams away with great rapidity. The aluminum which is thus formed is heavier and settles to the bottom, and the particles of aluminum as formed above the bottom frequently join to form Where, in the winning of other metals; for instance, zinc can be secured from zinc chlorid by this process. Although I have entitled my invention Process of winning metals it will be understood that it is not necessarily limited strictly to metals but includes other substances which partake of the nature of metals in the reactions entailed. For instance, I secure silicon and, while strictly speaking, it is not a metahits response in the process is analogous to that of a metal.
While I have already referred to the fact that-the broad conception of my invention has to do with the winning of any adaptable metal from anyadaptable compound, I desire to point out that my process is particularly useful in the winningof metals from compounds containing those metals and ox gen and in this respect I have particular y in mind bauxite, which, so far as some of the broader features of my invention are concerned, would be regarded as the e u-ivalent of clay. However, I have directe my at: tention merely tothe treatment Ofl clay, and
the more specific aspects of my invention will be seen to be directed to this end. I
. The various suggestions of changes and the suggestions as to explanations of the action. are presented in closin this descri tion so that those skilled in t 0 art may e as fully advised as possible, and so that it may be clear that my inven ion is to be measured in its broader aspects as set forth in the broader of the appended claims, and in its more limited aspects as set forth in the more specific claims.
I claim as new and desire to secure by Letters Patent: 3
1. Theprocess of securing a metal from a substance containing1 it and silicon, which comprises treating t e substance with a halogen to-form a compound of the metal and the halogen and a compound of silicon and the halogen, then separating the two halogen compounds, and then separating the metal from the halogen.
2. The process of securing a metal from a substance containing it and silicon and oxygen, which comprises treating the 'substance with a halogen inthe presence of a reducing agent inert toward the halogen to form a compound of the metal and the halogen, a compound of silicon and the halogen and a compound of oxygen and the regen compounds, metal from. the halogen.
3. The process of securing aluminum from" a substance containing it and silicon, which 'comprises treating the substance with a halogen to form a compound of aluminum and the halogen and a compound of silicon and the halogen, then se' aratingthe two halo gen compounds, an then separating the aluminum from the halogen, all the steps treating fresh charges of clay.
5. The process of securing aluminum from a substance containing it and silicon, which comprises treating the substance with a halogen to form a compound of aluminum and the halogen and a compond of silicon and the halogen, then separating the halogen compounds, and then separating the aluminum from the halogen. v
6. The process of securing aluminum from a substance containing it and silicon and oxygen which comprises treating the substance with a halogen. in the presence ofa reducing agent inert toward thehalogen to form, a compound of aluminum and the halogen, a compound of silicon and the halogen and a compound of oxygen and the reducing agent, then separating the two halogen compounds, and then separating the aluminum from the halogen.
7 Theprocess of securing aluminum and silicon from clay which comprises treating the claywith a halogen in the presence of a reducing agent inert toward the halogen to form a compound of aluminum and the halogen, a compound of silicon and the halogen and a com ound of oxygen and the reducing agent, t en separating the two halogen compounds, and then separating the desired elements from the halogens.
8. The process of securing aluminum from a substance containing'it and silicon, which comprises treating the substance with chlorin, to form aluminum chlorid and silicon tetra-chlorid, then-separating the two chlo-v rids, and 'then separating the aluminum from the chlorin. I 9. The process of securing aluminum from a substance containing it and silicon and oxygen, which. comprises treating the substance with chlorin in the presence of a reducing agent inert toward chlorin to form aluminum chlorid, and silicon tetrachlorid, then separating the two chlorids, and then separating the aluminum from the chlorin.
' 10. The process of securing aluminum from a substance containing it and-silicon,
which comprises treating the substance with chlorin to form aluminum chlorid and sili- *con tetra-chlorid, then se arating the two chlorids, and then separating the aluminum from the chlorin, all the steps being performed ,in a moisture free atmosphere.
11. The process of securing aluminum p from clay which comprises treating the clay with chlorin in the presence of carbon to form aluminum chlorid, silicon tetrachlorid and carbon monoxid, then separating the two chlorids and the carbon monoxid, and
then separating the aluminum from the chlorin.
12. The process of securing aluminum and rid and silicon tetrachlorid, then separat-- ing the two chlorids, and then separating eachof the desired elements from the chlor1n. Y
14:. The process of securing aluminum and silicon ,from a substance containing them and oxygen, which comprises treating the substance with chlorin in the presence of a reducing agent inert toward chlorin'to form aluminum chlorid and silcon tetrachlorid, then separating the two chlorids, and then separating each of the desired elements from the chlorin.
15. The process of securinglaluminum and silicon from clay which comprises treating the clay with chlorin in the presence of a reducing agent inert toward chlorin to form i aluminum chlorid, silicon tetrachlorid and a compound formed by the reducing agent and oxygen released from the clay, then separating the two chlorids, and then separatmg each of the desired elements from the chlorin.
- 16. The process of securing aluminum arid silicon from a substance containing them, which comprises treating the substance with chlorin to formaluminum chlorid and silicon tetrachlorid, then separating the two clorids and then separating each of the desired elements from the chlorin, all the steps being performed in a moisture free atmosphere.
17. The process of securing silicon from a substance containin it and a metal, which gen to form a compound of silicon and the halogen and a compound of. the metal and the halogen, then so arating the two halogen compounds, an then separating the silicon from the halogen.
, 18. The process of securing a metal from a substance containing it and oxygen and another material, which com rises treating the substance with a halogen 1n the resence of, a reducing agent inert toward t e halo gen to form a compound of the metal and the halogen, 'a compound of oxygen and the reducing agent and a compound of the other material and the halogen, then separating the two halogen compounds, and then separating the metal from the halogen.
19. The process of securing aluminum from a substance containing it and another material, which comprises treating'the substance with a halogen to form a compound of aluminum and the halogen and a compound of the other material and the halogen, then separating the two halogen compounds, and then separating the aluminum from the halogen. I
20. The process of securing aluminum from asubstance containing it and oxygen and another material, which comprises treating the substance with a halogenin the separating the two halogen compounds, and
then separating the aluminum from the halogen.
In witnem whereof, I hereunto subscribe my name this 17th day of August, A. D.
VICTOR M. WEAVER.
Witnesses NOAH I. HEIsEY, EDWARD J. DUNLAP.
US85800114A 1914-08-22 1914-08-22 Process of winning metals. Expired - Lifetime US1238604A (en)

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US85800114A US1238604A (en) 1914-08-22 1914-08-22 Process of winning metals.
US919A US1300205A (en) 1914-08-22 1915-01-07 Process of producing and separating certain substances.
US1559A US1297946A (en) 1914-08-22 1915-01-11 Process for securing metals from their compounds.
US2234A US1241796A (en) 1914-08-22 1915-01-14 Process of securing elements from their compounds.
US44517A US1296575A (en) 1914-08-22 1915-08-09 Apparatus for carrying out processes of winning metals.
US44518A US1269236A (en) 1914-08-22 1915-08-09 Process of purification.

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2648715A (en) * 1950-06-06 1953-08-11 Lindberg Eng Co Furnace for molten metal
FR2493340A1 (en) * 1980-11-06 1982-05-07 Samim Spa PROCESS FOR THE EXPLOITATION OF ROCKS CONTAINING LEUCITE

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2648715A (en) * 1950-06-06 1953-08-11 Lindberg Eng Co Furnace for molten metal
FR2493340A1 (en) * 1980-11-06 1982-05-07 Samim Spa PROCESS FOR THE EXPLOITATION OF ROCKS CONTAINING LEUCITE

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