US1329315A - Electrolytic apparatus - Google Patents

Description

V. M. WEAVER.

ELECTROLYTIC APPAR ATUS. APPLICATION HLED my 9.191s.

1,329,315, Patented Jan. 27,1920.-

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Victor M. Weaver By W M v. M. WEAVER.

ELECTROLYHC APPARATUS. APPLICATION FILED JULY 9- I915- Patented Jan. 27, 1920.

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V. M. WEAVER.

ELECTROLYTIC APPARATUS.

APPLICATION FILED JULY 9.1915.

Patented Jan. 27, 1920.

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umrnn STATES PATEN OFFICE.

VICTOR M. WEAVER, OF HARRISBURG,"PENNSYLVANIA, ASSIGNOR T0 WEAVER I COMPANY, A CORPORATION OF WISCONSIN.

ELECTROLYTIC APPARATUS.

Specification of Letters Patent.

Original application filed Auguste, 1914, Serial No. 858,001. Divided and application filed January 11,

1915, Serial No. 286. Divided and this application filed To all whom it may concern Be it known that I, VICTOR M. WEAVER, a citizen of the United States, residing at arrisburg, in the county of Dauphin and State of Pennsylvania,

trolytic Apparatus,.of which the following is a' full, clear concise, and exact description, reference eing had to the fccompanying drawings, forming a part 0 this specification.

My invention relates to apparatus for car rying out electrolytic processes and steps in processes and contemplates a generally SlIIlplified and eflicient structure wherein the action may effectively be carried on. One important feature of my invention lies in the means for feeding the material to be treated and the arrangement of the elements. A

further feature of my invention lies in the sealed construction which I provide fon-pur- It will be clear to art that my invention will admit of broader application than the; specific uses which I shall describe as an instance of its employment. In order to simplify this description I shall describe'my apparatus as employed in carrying out a process of securing aluminum from aluminum chlorid.

This application is divisional from m co-pending application, Serial No. 286 filed .January 11, 1915, which in turn is divisional from my co-pending application, Serial No. 858,001, filed August 22, 1914,'which is concerned with a process and apparatus for winning metals and which, in its'more specific aspects, relates to the treatment of clay in order to secure the aluminum and the silicon therefrom.

In order to instruct those skilled in the art, I shall now proceed with a specific description of my invention as utilized in my process of securing aluminum and silicon have invented a certain new and useful Improvement in Elec- July 9,1915. Serial N 38,858.

from clay, and shall refer to and describe the various parts of the apparatus and the various stages in the process in detail, in order that I may make a complete and intelligent disclosure.

In the treatment of clay, I break up the compound by the use of chlorin gas so as to produce aluminum chlorid and silicon tetrachlorid, this action being carried on under specialrestrictions and conditions, as will later be more fully described. With the aluminum'chlorid thus produced, the next step, so far as this particular part of the process is concerned, is to secure the by electrolysis under certain conditions and restrictions calculated to effect an advantageous and continuous process. I charge the aluminum chlorid into an electrolyzing bath preferably containing melted sodium chlorid, and the consequent electrolysis separates the aluminum from the chlorin, so thatthe former may be tapped away from the sodium chlorid, while the latter may be conducted to astorage tank for further use. It is important in this connection that in carrying out my process I keep the electrolytic bath saturated by steady, regulated additions of aluminum chlorid, and this proves to be a feature of distinct advantage and paramount im portance. I

My invention will be more readily understood by reference to the accompanying drawings, in which:

Figure 1 is a more or less diagrammatic representation of the entire system of apparatus.

Fig. 2 is a sectional view, taken on a horizontal plane, of the electrolyzing vat.

Figs. 3 and 4 are/other sectional views.

Referring first to" Fig. 1, it will be seen that the ChIOI'lIIlZ lIIQf furnace is shown at 9. The details of this furnace are unimportant in connection with the present application and it suffices to say that a charge is, introduced into the chlorinizing furnfie. which is preferably heated 'by electrical means. A pipe 30, which comesfrom a storage tank 31. is led intothe chlorinizing furnace, as indicated in' the drawing, and

Patented Jan. 27, 1920.

aluminum therefrom and this carry out higher grades of'clay,

in this way the charge in the furnace is mediately effects the disintegration of the kaolin, the

. the three gases which at a higher temperature formation of aluminum chlorid and silicon tetrachlorid, and, by the combination of the carbon andthe oxygen liberated' from the kaolin, the formation of carbon monoxid.

The three gases thus formed naturally arise and pass out of the chlorinizing fur nace 9 and are conducted to a 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 tributed throughout the entire space of this particular compartment in order to get a complete temperature control. The pipes 37, 37 are joined at the upper end, 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-v water supply and the result is that as have been referred to enter and pass through the compartment 34 the aluminum chlorid gas, which condenses than'the silicon tetrachlorid gas, is condensed and deposits itself as a white powder upon the pipes Since the temperature which is produced by the circulation of mere cold water in the cooling pipes 37, 37, is not sufiiciently 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 1 chlorid, and the white powder to which it is reduced is removed from the pipes upon which it is deposited by means of the scrapers 39, 39. The powder is thus thrown down on to the conve'yer 42 and carried to a tank 45, the connection to which is controlled by a valve 46. It will be seen that this tank is connected by means of a pipe 47,

- with a compressed air tank 48, which is fed through the air compressor 49. It is important, as before indicated, that the system be afclosed 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 tetrachlorid gas of the chamber and which are disv may be arranged to separate and the inclosure is effective in condensing and keeping condensed this volatile substance. 7

Leaving the aluminum chlorid, which has been deposited in the tank 45, for the prescut, I shall follow the-course of the silicon 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 scrapers 52, 52. Instead of being supplied with mere cold water,

however, the cooling pipes 50 are supplied with a freezing mixture ofice 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 tank 57 has an outlet pipe 57. r

The carbon monoxid passes out'of the con denser element 35 through a pipe 59,- past a valve 60, into a closed gas pump 61, and'is 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 of the process which will hereinafter be referred to.

Where additional chlorids are formed in the chlorinizing furnace, which condense 'at other temperatures, as is the case when iron or titanium is present in clay, the condenser these from the aluminum and silicon chlorids and from each other if desired, by increasing the number of elements maintained at different temperatures required to separately deposit the substances.

Returning now to the aluminum chlorid which has been deposited in the form of a powder in the tank 45 be noted that 1 have placed the burner 67 under this tank, and I may mention here (this powder being white unless discolored by impurities) it will that I surround the tank with a suitable fire I can subject the tank to a high wall so that degree of heat. With thevalve 46 closed, the material in the tank 45 can be placed under high pressure from this pressure prevents the aluminum chlorid, melted by heat from the carbon monoxid burner, from vaporizing. Once in-this c0ndition the aluminum chlorid is much more stable and much more easily handled, due to its physical condition, anddesirably 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 parts of the system in its dry, infusedstate, and I therefore do not wish to be limited to the inclusion of .this step of melting the aluminum chlorid.

A pipe leads from the tank 45 to avalve 71, which in turn is connected with a pipe 72 leading .into a furnace, preferably of the Rodenhauser three-phase type. This furnace comprises a' a heavy outer housing which is provided with a round bottom 74 mounted in a correspondingly shaped base 75, the ideabeing that when the connecting pipes are temporarily detached, the furnace can be tilted in order 'to ta off molten metal, as will bepointed out a little later.

he lining ofthe furnace provides a cavity for the molten metal which is formed between and around tubular casing parts within which the magnetic circuit frame and the primary coils are'disnosed. The details of this furnace 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. 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 proc ess is as follows: Y

In the first condensation of the aluminum chlorid in the condenser element 34, there are likely to be" impurities, iron, and it is the object of process now under description to eliminate this iron and to secure pure aluminum chlorid. Therefore, preliminaril Rodenhauser furnace is charged with aluminum, and the molten bath, as illustrated, is formed when as before stated, 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 ailinity of the chlorin for the aluminum than for the iron,'or other impurity for that matter, the chlorinreleases the iron and takes on the proper share of aluminum.

. The result is the tank 48, and.

84 is kept closed andthe principally the step'in the.

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that the refined aluminum chlorid will leave the bath of aluminum and will pass out of the furnace throu h the pipe 81. It will 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 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 Rodenha-user furnace, as has been described, and this process may be repeated until the required degree of purity has been obtained. At this point the valve 85 is closed and the valve 84 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 form of a white powder is brought down into the tank 86.

In this tank 86the aluminum chlorid mayv be put under pressure by way of the pipe 87 leading from the compressed-air tank 48, and may also be subjected to heat from a flame at the burner 69, preferably confined within fire Walls. his again melts the aluminum chlorid, which may then be conducted to a storage tank 88 through a pipe 89 controlled by a valve 90, the pure aluminum chlorid being kept under the pressure transmitted from the tank 86 and being heated by a carbonmonoxid flame at kept in a liquid This liquid condition is malntained by the heat which is developed by the electrolytic be noted that the pipe action. The electrolytic vat'is illustrated i indetail in Figs. 2, 3' and 4 and it will be seen that it comprises a graphite hearth 93' and firebrick surrounding walls 94, 94, with magnesite linings 95, 95, the entire being surounded 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 hole be ing normally closed by means ofthe plug 100. A chlorin exit 101 ,is provided, and, as indicated in Fig. 1, this exit is connected by means. of a pipe 102, in which there is a valve 103, with .a chlorin compressor 104,

with a chlorin cooler 106, t ese two elements being merely diagrammatically 30 eration, and, as

shown. The cooler 106 is connected by means of a pipe 107 with theliquid 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. 3 and 4 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 reinforced firebrick seal cover 111. 'Each of the anodes is provided with a collar 112, which is engaged by a loose collar 113 which may be moved up and down by means of nuts 111'on bolt rods 115 extending upwardly from .a packing-box cover 116, which surrounds the electrode stem and packs it at 117. By this arrangement the anode stems may be adjusted vertically so that the proper over-all adjustment may be secured within the vat. Copper bus bars 118, 118 connect the 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 at 110, and this bore is connected to distributing passageways 120, 120 in the corresponding graphite block. Each of these bores is connected by means of a pipe 121 with the supply pipe 92, which has been hereinbefore referred to, and a valve 122 is disposed in each pipe 121 and is intermittently operated for feeding purposes by a traveler 123 which is mounted upon a rotating shaft 124. Thus, whenv the various rotating shafts 124. are put into opbefore stated, the valve '91 is opened to permit the passage of the liquid aluminum chlorid, a constant feed per unit of time is afforded down through the passageways 119 and into the vat.

The liquid aluminum chlorid is kept at a high temperature, about 200 degrees centigrade, and at about a pressure of two and a half atmospheres. The heating of the storage tank is transmitted to hot-oil 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. Thealuminum chlorid is fed to the bath at such a rate as to keep the bath saturated. The

action which takes place in the 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 sim- 6b ple. matter to tap off the molten aluminum It will be seen that the process is uniquely continuous, and that the chlorin which is freed in the electrolytic vat may be used over and over again in the chlorinizing furnace, while the carbon monoxid which is formed by the oxygen liberated from the clay and the coke which is introduced is used for burner purposes. 'It is importantthat the system be a closed system, as described, to exclude the moisture and to protect the active chloride, particularly the aluminum chlorid. r i 1 An important feature in the matter of the operation of my system is found in the feeding ofthe melted aluminum'chlorid, or aluminum chlorid in powdered condition for that matter, to the electrolytic vat. It is of importance that the electrolytic bath is fed with the aluminum chlorid in such a way as to keep the bath saturated.

It will be apparent to those skilled in theart that various modifications might be made in this system without departing fromthe spirit or scope thereof. For instance, one' might use a different electrolyte. In heating the pipes which maintain the aluminum chlorid in its melted conditionwhile being fed to the electrolytic bath, it might be better practice insome 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 been described, I have the particular advantagethat there is no electrode consumption, and therefore when the electrodes are adjusted they will remain adjusted, and economic service is secured.

Referring to the electrolytic vat, I may mention here that the hearth is the cathode and the graphite blocks constitute the anode. The aluminum forms'globules varying in size from mere specks to considerably larger particles, and they occur near the bottom and finally rest upon the bottom. The chlorin is liberated and streams away with great rapidity. The aluminum which is thus formed is heavier and settles tothe bottom, and the particles of aluminum as formed above the bottom frequently join to form which, as described, is tapped out from the .vertical y into said chamber,

vat. It is'convenient to retain suflicient moltenaluminum in the vat to keep the carbon cathode constantly covered.

It will appear that changes and modifications in the apparatus of my invention will be possible Without departing from the spirit and scope of my invention. I have already referred to the fact that the apparatus of my invention has much wider appllcation than for carrying out merely the process which I have cited as an instance of use, and it is to be understood that I contemplate any use to which my apparatus may be put. I desire, therefore, that the metes' and bounds of my invention shall be determined by the appended claims, which I have drawn variously so as to tions which, of their use,

I claim:

1. Apparatus for treating chlorid which of themselves, and regardless are new.

comprises a closed chamber for containing an electrolyte having a graphite interior bottom as one electrode and a graphite block depending from a sealed coveras the opposite electrode, and means for feeding material into said electrolyte at a definite and controllable rate ofspeed.

2. Apparatus for treating chlorid which comprises a closed chamber for containin an electrolyte, having a graphite interior bottom as one electrode anda graphite block depending from a sealed cover as the opposite electrode, and means for feeding material into said electrolyte through abore insaid block at a definite and controllable rate of speed.

3. In combination, a chamber having a common electrode at the bottom thereof, a plurality of electrode mem-bers extending and a plurality of horizontal electrode members each common to a bers and connected thereto at the bottom thereof in horizontal position, being spaced properly away fromsaid first-named electrode.

4. In combination, a chamber having a graphite bottomfor one electrode and adapted to contain an electrolyte, a cover sealing said chamber, an electrode passing through said cover, and means for adjusting the vertical position of said electrode, said elecbring out the combina-,

to be. treated to said chamber plurality of said first-named mem-- members and connected thereto at the bot tom thereof in horizontal position, being spaced properly away from said first-named electrode, said electrode members having passageways therethrough whereby said chamber may be fed with material to be treated.

6. In combination, a chamber electrodeblock in the bottom thereof, a plurality; of, horizontal opposing electrode mem e-rs disposed in said chamber, substantially parallel to said block, a plurality of vertical electrodes extending upwardly from each ofsaid horizontal electrodes, one of each of said plurality of vertical electrodes having a passageway therethrough, each said passageway being supplemented by diverging branches in the corresponding horizontal member.

7. Apparatus for treating chlorid which g ,comprises a closed chamber adapted to contain an electrolyte having a conducting interior bottom as one electrode and a c0nducting block depending from a sealed cover mechanically feeding non-gaseous material into said electrolyte at a definite and controllable rate of speed.

8. In combination,'a chamber adapted to contain an electrolyte, electrodes therein, and means for feeding non-gaseous material by a plurality of paths to distribute the feed uniformly throughout the electrolyte.

9. In combination, a chamber adapted to contain an electrolyte, electrodes therein,

and means for feeding non-gaseous material to be treated to said chamber by a plurality of paths in substantially uniform relation to the electrodes.

witness whereof, I my name this 2nd day of July, A. D. 1915.

VICTOR M. WEAVER.

having an as the opposite electrode, and means for hereunto subscribe

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