[1]Patented June 3, 1924. 19496,440 UNITED STATES PATENT OFFICE. VICTOR X. WEAVER, OF THOROLD, ONTARIO, CANADA, ASSIGNOR TO WEAVER COXPANY, OF MILWAUKEF,, WISCONSIN, A CORPORATION OF WISCONSIN. ELECTRIC PURNACE. Application filed March 11, 1918, Serial No. 221,630. Renewed Tanuary 21, 1921. Serial No. 439,049. l'o all it,lioii?, it qiiay coi?,Ceiln: ]3e, it kno%Nn that 1, VICTOIZ AAI. WFAVEIZ, ',t citizen of tlieUnited St,,ites, residing at Tliorold, Oiit,,ti-io, Canada, h,,tve invented ,t certaii-i new and useful Improvement in Electric Fiii-iiaces, of @wliieh the folloiving is,,i full, clear, concise, and exact description, refei-ence bping liad t.o the, acconip,,tnying dr,,iwings, forinilig a part of this specificvlio tion. My invention i-elates to ttie, art of foi-ming desired chemical combinations and has to do particularly witli processes wberein it is necessary to maintain a reducing atinospliere 15 for the purposes of decoiiiposition preliminai@y to coiiibination. I aiyi coiieerned partictilai-ly N@,ith tlip, foriiiatioilof li-,ilides I)ytheti,eatnientof acharge, stic,li ,is an ore, -,vl@ich contains considerable 20 oxvgen, ivitli a balogen gas and it, is ii-ly ptii-pose, to provide for a mode of ot)era-tion whicli at all tinies instit-es the formation of .i inonoxide gas instead of a dioxide gas. It will be clear to those skillpd in the art 25 that my inveiition is applicable, iii itsbroader sense, to any procedure wherein it is necessary or desirable to secure a monoxide gas rather than a dioxide gas and it will be noted that the broader of the appended claims are 30 accordinlyly drawd. More specifically, I "' I iitility and charact@eristic adaptfind specia abilit.y of this broad idea to the formation of balides, still more partictil,,irly chlorides, in which cases new functiong ai,e performed. 35 Accordingly it will be seen that I also make more specific clainis drawn to these more particular features which, in actual practice, I have found to be extremely important. As a specific instance of the desirabl-I.ity 40 of instiring a inonoxide gas instead of ,t dioxide gas, for certain purposes, I make ref ei,ence to my Uiiited States Letters Patent 1,238,604, issued '@tigust 28th 1917, wherein a process of winning metals is described. 45 There the teaching is to, secure a monoxide gas and iny present inventioii contemplates a iiew, effective and "atitomatic" way of insuring it. In a, specific process described in that pat50 ent aluminiim chloride, silieon tetrachloride and carbon monoxide are formed by the action of clilorine gas upon ka6lin, in the presence of carbion, in 9, euitable fumace. I sbill iise this spwific process is aii ex,.tinple in this description for instl-uction to - those 65 skilled in the art. If the aniotint of carbon were sufficiently limited, so that carbon dioxide -%votild be formed instead of carbon monoxide, -,t different restilt, t-he production of c,,trbonyl ebloi-ide, (I) Iiosgelie) 60 rould result. This is qll clearly set folth in ilay copending ,ipplicatioii, Serial No. 210,609, filed January 7, 1918. When, liowever, carbon monoxide is to be formed instead of carbon dioxide, as taught in my 65 patent above refei-red tc,, it is obviously necess@'ry to pro@i(le an excess ratliei- than t deficiency of c,,ti-bon, ind iiiy pi-eseiit invention, as before stated, is directed to this end. My inventioii contemp!ates ,L carbon lined 70 furnace, the cai@I)on linin@,lr coiiipi,isiii- all inside part coiiiposed of clos(@ly linite(fcai,- bon in slabs oi- bricks oi- one large iece of closely united cai-bon foi-iiied and baked iii place, and an outside oi- siii-i-otiiidiiig pae,@ t6 composed of cru,held or finely divided carbon not cementi-d togetliei-. Such t lining has th- properties of beiiig infitsible and of fi-eely distributing the heat over the inside, pait of the lining and of preventing 80 the loss of beat from the, furnace thr6ugithe outside part of the lining, and also provide s at all tiir@es car'Don in contact with the gases after they t@ . bave passed tl-irou(Yti the charge. It is also has the property of 85 bein g inert with respect to the balides. Owing to the carbon being ineit with respec t to the halides, I mty use carbon grate bars whic - h are placed in stich positio'n -,vith relati on to the heating zone that tliey will 90 be niaintained at a re.( heat. A carbon hearth of crushed colke or the like, is provided over the grate bars to support the chargp, and as a'resistor for the elect ric curi-ent, thereby c,ausing a heating 95 effe ct beneath the charge and in the path of the incoming gases. To prevent excessive erosion of the inner carb on wall at the portions touched by the char ge, provision is made for f umishing ad- 100 ditio nal carbon in the form of coal or coke in the side.chuies, which has, tl@e effect of main taining a supply of c,,trbon around the walls , and thereby protects them from the erosi on above referred to. 105 In the specific process above referred to
[2]the charge, such as kaolin, is fed into the furnace with an adequate @harge of carbon, whereupon chlori-ne gas is admitted and the action, under heat, proceeds. It, is proposed th-,tt the same procedure shall folloiv with the tise of rny present furnace, but it will be seen that as my pi-esent furiiace is constructed the adequate charge of carbon is alwa3,s iiisured. If, perchance, the io amoiint of loose c,,irbon introduced with the kaolin sboiild be insufficient to form carbon monoxide the c,,trbon parts of the furnace -themselves -will be attacked so as to insure the foi-niation of the monoxide-an oiianii5 present safety device to avoid upsetting the intended chemical procedure. So f ar as the process phase of my present invention is conceriied, it consists oT insurina an excess of reducer by the constant 20 presetice of a redhot reducer element, in addition to the calculated charge ind @referably in differe,.it pbysical forin. It is con'ceivable that it may also differ chemicalll-. So far as the apparatus phase 0. my in25 vention is concerned, it lies in the construction of the furnace, providing, broadly, inherent carbon elements and, specifically, carboji lining, hearth and grate bars, or any of them. 30 1 'shall -,iow refe-r to t-lic accor.,ipanying dra-vv,ings, in whichFigui-e I - illustro,tes diagrg,minatically the appara,tus by means of which the proc@ess is ca,riied out; 35 Figure 2 is a vertical longitudinal section partly diagrammatic of the furnace en-iployea for carrying out the inventioii; Figure 3 is a plan view of the same on a reduced scale; 40 Figure'4 is a vertical. longittidinal section of the ebarging hopper - Figure 5 is a sectional detail view s owing th,e covers for the coal chutes; Figur@ 6 is an elevational view, pai,tly @n 45 section, showing the electrodes, the adjusting mechanism for the same and the electrode clamps; Figur@ 7 is a side elevation on a larger scale of a modified form of electrode clamp; 50 and Figure 8 is an e-,ld elevation of the same. Figure 1, which is a d'iagrammatic ofitlay of a.system foicarryinp-, out the process of my invpntion, shows @]7e chlorinizing fur55 nace at 9. This furnace, in which the reac-@ion between the clay and carho of the with the chlorine occurs, is of the =typo. The structure of the furnace and its elee60 trodeg is shown in Figures @ to 8 ineltisive. The furnace ' 0-om rises an outer shell or casin:g of sheet meta?10 geherally cvlindrical i@ form having a smaller cylindrical shell of sheet metal of considerably less 65 cliameter, a-s shown at 11, attached to the 1,490,440 lower en.d where the chlorine is introduced at one of the nozzles 12. The top -of the casing 10 is covered by a reinforced sheet metal top oi- cover 13 whicli lias the braces of angle and channel iron 14-15 for stiffening and 7o supporting the same. The interior of the ftii-nace con-ipi-ises a central boi-e 16, commilnicatiilq at its upper end wi-th a cliarging 'noppe@'17'aiid liaving i side otitlet 18 for diseliarging the 75 gtseoiis products of the cheinical combination carried on within the fitriiace. The diseliai@ge opeiiing 18 leads out by way of ti flanged iiozzle 19 whicli coiiiintinic,ates by v,7ay of tlie, discharge pipe 20 with the double Si) chanibei- 33, to be i-eferred to later. The entil,e iikner faciiig of tl).e ftii-iiace is coinposed of carbon. The ",all or sheft of @the fiti,ntee is const i@ticted of carbon bricks or blt)cks laid i,,i cotit-ses from bottom to near 85 tile top OF the furillce. The lieartit 2@o i's coniposed of a bed of coke, or otlii-,,,@ poi-ous mass of carbon supporteil on the carbon- grqte bars 1.25. The, chtti,ge 126 wbieli'in this case comprises'-kao- go, ]in and criislied coke, both freed of moisture, rests upon the hearth 23. Electrodes 22 project into the boi-e of tlie, f til@nacc@ i sli,)i-t distance abc)ve the gi-ate 1),t i-S 125. Tbe, hearth 23 forms a resistoi- be- 95 tween said electrocles 22 and is niaintaiiied at a i-ed --vteat by the passage of current betwe@n the electrodes. The chirge 126 is thus suppoi-ted iipon a hot miss of carbon directly in the path of the incoming gases. 100 Above the liearth of the furnace 23 a plurality of coal feeding chtites 24 are formed in the carboii wal,ls 25. These ebtites comprise ,t lo-,vel' diagonil I)oi-tioji coiivei-gliig into the main bore 16 -,ind upper vei-tical por- 105 tions 26 communic,,iting at, tlieii- tippei, ends with the fillinz openino,,s 27 formed iii the cover plate 13 of the f urnace. These cover plates may be, left f ree to lift and act as relief valve-s in case of gas explosions. 110 The upper end of the mii-n bore 16 is reduced @by Ineans of the tipper coiirses of carbon blocks or bricks 'iO which extend inward to pro-i,ide an opeiiing suitable. for the discharge opening of the charging hopper 116 117' The space between the carbon blocks or bricks and the metallic or sheet metal shell 10 is filled with crushed carboh. The central -carbon lining is thus heat-instilated at the sides, top and bottoiyi. 120 The top plate 17 is pro%,ided with a niiinber of charging openings 2i in line, -with the vertical charging chutes 26. These charging openings 27 are normally closed by a cov6r plate 2 seated iipon anntilar rings 73, 125 as illiistrated in detail in Figure 5. . The closure between the cover 72 ana th'e rip-gs 73 is m-,ide by a lead gasket or other suitable niaterial. The ring 73 Is suitably --Fastene,d as by means of rivets 76 to the Cover plate 330
[3]1,496,440 13. In tlie- particular enibodiiiient' that I have illustrated, six of these charging openings and six of the chargiiig chutes ar6 employed. The six electrodes 22 pass into r) the hearth of the furnace being supporte(I upon the sheet.iron body 10 by the meelianism shown in Figure 6. wliieli will be clescribed in detail later. Tiiese eleetro(les ,iii(I the cliargi'ng cliiites are-sp@eed e(iualiv al)otit 10 the eircuinference of the furiiace. While the ftirnace -,is sho-wn provides for bringing in the electric current by ilieans of horizontal grapl-iite, or plain carbon electrodes I conten-iplate the use of vei-ticil or 15 inclined electrodes in cases wliere this is deemed more desirable. The charging hopper l' coinprisos an upper i,ee,eiviiig sp,6iit 77 whic,h is a(lapted to receive the miterial of the ebarge. ,ind 26 which is closed by a hopper bottom 78 genorall@ conical or funnel-shaped in contour, and liaving its bottom opening nori-fially closed by means of the charging bell 89. The upper bell 79 is apertured at tlie, centey 25 to permit the passage therethrougli of i pipe 81 and is threaded to receive @tlie, en(i of the larger pipe 82, wliicli pipe 82 is tlie. stem of the bell 79. The stem 82 is sectire0i to a flange member 83 wbich flange ineiii3( ber is in turn connected by suitable opei-,,iting meeltanism for raising and lowering tlie, bell 79 to open the hopper bottqin 78, ,)r to close the same. A c@lindrical barrel portion 84 is sectired to the flange 85 of ti-ie 35 hopper bottoin 78 and extends downw,,iid to engage the flange 86 of the secoiicl hopper bottom 87, wliieh is of Vne general contoiir of the hopper bottom 78 ' previously de,scribed. A bell 89 close the hopl)er 1.)ottoiii 40 87, this bell liaving as a stem tlie i)ipe, @,l Nvbieli extends tlirougli ijid above the pip(@ 82 that forins the stei-n of the bell 79. At its i,tpper end the pipe 81 lias -, @ft,@rge 90, to wlilch siiitable opei,,,iti.iig cables are, con4 r) nected fol, manipulat,ing the bell 8@),The hopper bottom 87 pi,ovicl-,@s a ",ater cooled vELIve seat for the I)E@ll 189 as Iliese, parts face the interior of the Tll@, liopper bottom 87 rests iil)oii -,i-riiig 91 s(,,clired to the top 17 of ilie fiii,ii,,ic-1. An enlai,(,oi-nent is fornierl in tlte boppe,,, liott,)m it thi; portion to provide the'iiecess,,ti,-v se,,itiiig surface for the i-ing 91 and also to pi7ovicle rclom for the pipe 92 to be imbeddeci iii thp, 55 -walls of the hopper bottorn -which forii-is the valve seat. The pipe 92 which exteiicls outside bf the valve'seat, as sliown in Figure 3, is adap@ed to be connectecl to a sotirce of cooling water or otber mecliuin. This 60 pipe is imbedded in the v,,ilve seat bl,7 c@tstino, the metal Lbout the same. J'he @Range of the hopper bottom 87 is connected by a short cylindrical section 93 with the 'Lop plate 13 to foriii a tiglit joint between tliese Of parts, A soitnding or feeliiig i,od 94 passes (lovn ii tlirotigli the pipe 81 an(I tlirough 'be valve iiieiiit)er 89, li,,tving a l@iiob 95 ,it its lower eiid for protecting the end of th(,' rocl and for closiii(y off -tlie liole iii the bell iiiemler 70 8( ,). 'I'o this eiid,tlil, 'Lop of tlie, li@iiob 95 is iliade COTlical and is ,idipted @o seat aro-,incl the coiiieil edge of tlie, liole foriiied [Iiiotigli tli(@, b(@ll so as to closp, otf iiiv leal@iage art)und the i-od This rod 94 is (@on'iiectc@d to 75 sitittil )le lowei,ing ,incl raising iiiecliaiiisiii so that the i-od in,,iy be let clowli to feel th-8 lioigl it of tlio cli,.irge in tlle ftii-iiice. Tli p, bottoiii seelion 11 of the -Iiii-iiace, is I)iovi(led ivitli a pair of iii-,iailiolcs 96 ai,id 9-f. 80 The,e iiiadlioles are of a siiit@,i,ble, size to periilit cleaning of the ftirnicc, ,ifter i viin or for idali:iiig i-epairs, or inspe,,@tioi, or tlio, like. Th e elect-i,ocles 2--@ tti-e jii-,tde of,@4i-,il)lilte ,iii(i are provided @it their otiter end witli iiietll '35 caps 98 -whiel-i in tui-,-l are connected I)y mea ns of aii icliustinry rod @)9 'Lhreqclecl @it the outer end for -I'eecling the elLe'Ll@ocle as bv me,,ins of the liin(l-lvlieel 100. '.riie, det,,iils of this coiistriietion are slioivii. in Fig- 90 tire 6. A cast, iiictal flftiige or 101 is secti re(I al)oiit tlie, ol)eiiino- iii the slielli 10 tlilollgli N@-lileli lii(@ electi-6@le 21-1 fling ed sleei,e -1 02 @liade of insiilatl(,@l I)referibly vitr:fi(,fl 1)1-1)e surrolincls the electl,o(le 22 95 sei@ves L,o in,-,ulate if fi-oliai tlie, si@iell ar,(l liiiing of the 'itirn,,ice. @'V -vqtc-i- coole-d miicling plate 103 is supporttct on btit iiisult,,terl from tlie. ring 101 an(-l serves to g,,ii(le, the elect rode 21-) into the insulating sl,-Pvls 101-). 100 A layet, ol siiltable ins-illatioll IC)-! is inlei@ I)osed I)etween -illie flanfe oi' thp@,iii(lillfr 10,@') ancl Llie @;ilpporting 3-in'" 101. I)olts 10,@-) @vlii(,Ii seciii@e tli.-se I)tii@t,s toffetlier ii-e (@,ii,eftilly iiisiilitecl b@7 Tiieain,, )i' - -xasliet,s loi aiid coll@irs of insiilttioii 106. 'rhe f,@tiidiiiplate is cored otit is shoiv-ii ,it 110' to ,)rovi(:I e )ia'tei, cooli@@i,,z space for ivitgr-c-oolin,, the (,,over 1-)Iate aii(I the [)ox 108 a@.tapt,ed to recei.vt, is pro-N@idecl in the cytildi-t-,-r iite 103 fin(I ,,Iie el @, p st,i.if fin(t box gl,,in(I io9 coo @vl @ii -ilie, @'4ti lning I)ox to ii)aintaiii a uigh@L, Pqc,17ing it)out the electi,o,-Ie 22. aci ' jiisting iiieellaiii,,@iyi Poin- 215 I)i,]- "eq tl-.e thre@ide(I hand an(! tiie tlii@ eacletl stein 99 permits the be fe(I ipto the flirnice a-@ lire Plop-. sumecl. The lian(i -oilieel 100 i,; 'moiil-iti@cl in a stiitable 1)edeqtal 110 m-lDiiiit,,-d )i, a -loiin,,Ia- 120 tioii 111, ivlii(@l-i iii,,iv in t@is c@- ,@se be I f'ioor or gallei,y aboiit the, The electrodes 22 are connect@CL to tlae electric cables ivhicli suT)@)!-,r tie necef,,siry curi,en-,, by eltinl)s siieh a,9 S'ilovn a,. 11,@l. 125 1'1)ese clanips pi--afei-ably (!Oiiipi@ise tv@-o seiiiieirc@ilar parts -'Ll@l, subst@,ilitialiv sii-@iiiitiii all i@esD-acts, tlipso semi - 1)"Irts beillo,7 adapti-.d to be clampt-,O,- ,ipon@op-oo--i-te sides of '.he el,-CL@rocles :@,9@ 1)v m,,a'@ns oi' the 120 sliiffing packi,.ifr 110
[4]1,4962440 bolts 115. The ititerior of eacli lialf of the - now ttiriied on aiid that the clilol-iiie gas is clanip i,@; cored olit to provide water jacket space and the two halves are put iiito comiiiunic,ttioii ivith etcli otliei- by means of t flexible, iiietallic! liose 116, Avliieli is preferably beilt iiito U-sliape-as shown in Figiire S. A suitable ililet and otitlet pipe 117 and 118 ire I)i@oN-icled at the bottom of the balves 10 of the claiiip. The electi-ical coiiductors III-) are I)referably (-Iaiiiped b), meaiis of bolts @r stiids to the metallic si@le walls of the clamp members, I)eiii(@- t'liei-eby ptit iiito direct metallic Id contact -with the saiiie' Suitable-rido,@es 119 and 120, provided - %Vith -,crew sockets 121 and 122 may be provided to facilitate% suell attachmeiit of the electrical condtictors. Ile operatioii of the furnace iii connec20 tioll -@vitli the other apparatus will now be desci,il)ed. The bore of the furnace is, fii@st cliar,red AA,itli loose cqrbon, preferabl in the t@ y foi-m of coke to stibstantially the heiolit of the heai-tli. The cliai,(re of material-in thiq 25 ease, clay, referably in the form of kaolin p of the appi-oxiiiiate foi-ii-iiila, Al,(SiO,) '@ 'is fll,-;t(riven a preliminary lieatiiig to arive of! all of tile iiioisture, beiii,(,r lieatel for this piii-po.,@e to a Iiiah -ten-lpei@atiire. The hot 10 ]@,ioliii is tli(-@ii iiiixed Aiith dried carboii s@iieli ,is (,i,iislied (,olie and conN-c.@ ed in dtimp e,,irs to the ditnipiii, sl)otit @7 A@iiei-e it is received in the hopper 78, from tlleiiec discharged by wtv of the ])ell iii the liol)per bottom ii-ito 35 the iiitei,l,)t- of the bopl)er 17. The bell 79 is then closed aiid tlle bell 89 is,opened to diseliai@ge the cl,-,y into the bore of the ftirnace. The co@il chutes ai@e cliarged 'ivi-th ertislied ii-i'ubi@acite coal bv opening the cover 40 I)Iate '42 ttid filliii- the chtites substaiitial@-y ftill of loo,@,e (-oal iii stieli position that i6 ivill tend to settle down iiito the bore oz@ lie,arth Of tl]C flli-ntee as space is n-lade there,for There3'sthiis,,icompos itemassofkaolin 45 all(! co,,il or carbon depositecl oii the heartli ,)f the ftii,iiice. The kaolin an(I coal or cokp- ai-e charged iiito the fiirnace iii. proper proportions, so that the oxvgen of the charge will l@a t@.tken 50 tip I)v -tlie coa,l ind co'k-e thl'is int-odaced; blit ilie cp@rl)on in 1,@lie coal chtites is - niovide(i to pi-otect 11-Iiie side walls in contact -%Yi-tll the (,Iiailge i-,-i case all of the o7r-ygen in these pa-fts of - the (,hc@i-ce is not 'Lakep. Lip by oal or coke r,,rcvided as ,,r'- of 'he 55 the c a p@ cliartye. 'll'iie -rozzles 12 are coii.-Lic-cted b3@-,va.17 of i pipe 3() wi'c-li a, siiitable soutee or chlori-re gas Ls. i nokicated by the -L'anIK 3 i- the aclaiis60 sion of et,@'llorilie beiiio- controlled by JL-, 0 valve 32. clilorine gas is adapted to enter by -,va,,- c.-f the lower sectien 11 f,--i-d p,,tss up tlii,oti@,,It the loose bed of col@e iiito the zoiie of activi@y,@it 'che liearth 'when 4-,he furilace is 65 operati@no,. Ass-aming that the currep-t is diseliared iiito tl-ie active zone the clisintegration of the kaolin with the formation of aliimintiiii chloride and silicon tetrachloride i.,@ accomplished. This is dtie to the - heat, 70 the carboii, and the chlorine, wllich effect the reaction. The oxygen liberated from the 1,.aolin unites witli the excess of ca'rbon to form cai-bon monoxide. So far as the degree of lieat is concerned, those sl,-illed in 75 the ai-t will, of course, be g-w'ded by the fadt fliat sticli a degree of heat as effects reaction between the cliloritle ai-id the aluminum aiid silicon -is required, the effective temperatures being well linown in the art. 80 1 migllt add, for -what fili@Clier assistance it niay give, that I, have,,f6tind that teiyiperatures betiveeh 9000 ai-id 1200' centigrade are most efficieiit. Tlle reactioii is as follows: 85 Al,(SiO,),+12C+24CI= 4AICI,+3sicl,+12CO The three gases tlius foriiied natlirally -rise and pass out of the outlet opening 18, 00 ai@d, as illustrated iii Figtire I are condticte(I to the condenser 33. Tllis coiidenser is III, the fo-.r,m of a dotil)le closed chainber providiiig @tlie compartineiit 34 aiid the coii)l)artiiient, 35 sep,,ti-ated I)y ,i. pii-tition 36. The 95 cor-,ipai@tinent 34 is pi-o-,,ide(i witli t. svsteni of cooliiig pipes 37, 37 wliieli extend aownNvardly thi-ough aiid froin the top of th6 cliambei, and whicli ,ire disti-ibiited throtigliotit the entir@ space of this partictilar - coin- 100 p-,ti@tiyient in order to get coniplete teinpei-ature. coiiti-ol. The, pipes 37, 37 are, joined at blie uppei- ends otitside of the cliaiiibei- 1) inc,,@,ins of the, header pipe 38 and eircttl,,itioll is secured in in@, desii-able iiiannei-. In - tills 105 p,-.rticulpr coiidensei- elenient the s_)-steiii of @pipes is coiln(leted to a. cold water stil)p@@! f,@nd the i-esult is tllat as the tliree, cra,-,(,S whicli hive-been referred to eiitei- and pass thi-ou(yh the compai@trnent 34 the all imilillill 110 c loride gas, ivhich cojideiises it t Iiig@ier t-.Mpei,atiire than the silicon teti-achloride. cas, is condensed aiid del)osits itself as a, ;hite po-,icler tip,oii tlie, I)il)es 3'i, 37. Tiie t@,niperatui-es at whieb these i-espective - gases 115 condense are,, of colirse, ii-ell known iii the art. It iyiight be niejitioned liet@e that it is ioossible that iii tlie action iii the chloriiiizing 'urnaep- some otlier chloride of silicon might id-cidentally be foriiied. a @liloride siieli as 120 lite--z-achlori,,ie (Si,Cl,), biit I fiiid that coiiCli-@-ions are-stieli tli,,It it is 01113- the silicon tetrae..hioride,wli:lch plays Iiiy -considerable part,. V",Iaere tile ci,,,y cojitains oxide of titaiiitim 12,5 or othei- inetals, the process of chloridization will nialse tlie, cliloi-ides (if titanilini and other metals azid carl)oii i-noiioxide. Since '6he teinperature whicli is,.produced by the circulation of mere cold water in the 130
[5]1,496,44o cooling pipes 37, 3t is not sufficiently 16w to condeiise silicon tetrachloride tllis gas, togetlier witli the carbon monoxide, on to the iiext compaitiiient 35 of tli6 colidenser-. Thus the first coiideii'ser element 31 is devoted ti) the condensittioii of the aluminiiiii cliloride- and the white po-%Nder to whicli it is reduced is removed froiii the pipes upon whicli it is deposited by illeaiis of the 10 scrapers 39, 3'9 whi@li by in6ans -of pulley coi-ds 40 passing over stiitable pulleyg 41, 41 on the outside of tlie, condeiiser, are dmwn up and down on the pipes to scrape, them ,I in an obvious manner. The powder is thus 15 throivn down on the eonveyor 42, the upper run of whieh passes in the direction of tli(@ .arrow 43, and thus thecondensed aluminun-i chloride is brought to,the end Gf the condenser element where i@e outlet 44 lee@ding 2f) 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 iiieans of a, pipe 47 with a, conipressed aii- iank 48, whiel-L @s fed throtigh the air cqmpressor 49. It is 25 important, as before indicated, that the @ystem be a, closed system and that various actions be carried on under pressure, and I speak of it pal-ticul@rlv at this time because of the fact that the @luminuni chloride to 30 wliieh I liave just refeited is extremely deliquescent @nd iniist be Icept fi-ee, froni iiioisture in order to avoid decoi-nposition and the formgtion of hydroehloric acid. When the system is, closed, liowever, su6li t reslilt 35 is inot possible, and the piessure has -,t purpose to be referred to.later. Le,,tving the aliiminfiin clilorid, whicli has been deposited in the tank 45, for the present, I shall follow the course of the silicon tetra40 chlorid gas and the carbon monoxid through tiie second element of the condenser. The condenser element 3.5 is provided with a s@istem of cooling pipes r)o like the pipes 37, iese pipes hai,ing. thp, outside header 51 and 45 being provided with the scrapers 52, 52 hung from the pulley cords 53, 53, passing over the puII63,s 5,4, . 54. Iiistead of being supplied witli iiiei-e cold wa-ter, however, thB, cooliiig @ipes 50 are supplied witli k freez@50 ing mixture of ice w,,iter and salt, a-nd the e pera re in the condenser element 35 is t m tu therefore considerably lower than the temperature in the condenser element 34. The lower temperature is sufficient to condense 55. the silicon tetrachlorid which comes down as a cle&r liquid, exce]?t for any impurities which may cliscolor it. This liquid silicon 'tetrachlorid pisms down the sloping bottom of the condenser element 35 and'passes 60 throug@ 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 @lement 34 is, because it is possible that the aluminum chlorid not en@. tirely condensed.in its passage through the condenser eleiiieiit 34. i@iay condense upoil the pipes 50 of the condeilser eleiiieiit 35, and it is tlierefoi-e desii,able periodically to operate the scrapers 62@iii order to this condensatioii. Tlle scrapei-s 39 ;,zi the 70 othe r coiidenser element are operated dtiring all the tiiiie that the svsteni is beiilg worked. The condenser cleiiient 35 is pi-ovided with a conveyor 58. The carbon inonoxide passes otit of tlie, 7 5 cond enser element 35 througli a pipe 59, past a valve 60 and to a closed gas puiiip 61, and ins of is then carried to a scrubber 62 by nie, a pipe 63, this scrubber being in the form o ,t tank c()ntaining lime wate@ and having an 60 outle t pipe 63' leading therefrom. This outlet pipe is provided with t valve 64 and leads to a, telescoping gas tard-, 65 so tli,,tt pressure ma,y be kept upon the carbon monoxide whic h finds its way to this tink and so that 85, the carhon morioxide ii-ity'be fed I)y -way of a pipe 66 to a I)ul@nex wbigli iiiay be iised for heat, ,lg. It will now be seen that there ivill always be an excess of carboii to insure the forma- 90 tion of c,,trbon'monoxide, ratlier than carbon dioxide, as aboi,e pointed out, it being clesr that sliould the looge carbon introduced prov e insufficient, the carbon eleiiients of the f tirnace itself will respond., Beyo.nd t.Iiis the 95 @act that clrbon is used for the purpose speeified is importantbecaiise of the chaiiacteristies of ciii-bon already pointed out. As before indicated, my furnace and process ma;y 1* employed, in broader sense, in 100 conn ection witli the @roduction in any halide from oxygen bearing ores, co-nipounds or mixt ures; and, in fact, in ,t still broader sens e, is applicable to any process wlierein a redu cing atmosphere, particularly an exces- 105 sive one, must be maintained. I
