US957754A - Process of making aluminum fluorid and other aluminum compounds. - Google Patents

Description

P. A. EMANUEL. PROCESS OF MAKING ALUMINUM FLUORID AND OTHER ALUMINUM COMPOUNDS.

APPLICATION IILE D MAY 29, 1909.

Patel lted May 10, 1910.

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v I U P ABMANUEL. PROGESS OF MAKING ALUMINUM FLUOBID AND OTHER ALUMINUM COMPOUNDS.

APPLIG'ATION IILEID MAY 29, N09. 957,754. Patented May 10,1910

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4 PHILIP A. EQFANUEC I 'AIKEN, SOUTH CAROLINA.

PROCESS OF MAKING ,FLUORID AND OTfiEfiALUMINUM COMPOUNDS.

exact descr'i will enable it apperteiu s'lto (My invention "making elumin miuu 'n eom ordinary el all their" through th 4, uniting thelw 7 I 'repr'esen .neetingihe retort i1 2, fen" zari ends 'of exazizftly he furnace mrtion;

is composed eft a "i; hating nt, each shelled The'pe :3

at both ends, ut having inwerdly. to embrace the orlees sffiabmcefion amma Patent 7 3'9 ieest Eerie No.,499,,2o2,.

Patented May 10, 1910'.

'4,fthe ends of which are secured Lions-1n the plate 8, secured to op and bottom the retort is provided: with 'cu- '1 -ved :doors 9, hinged thereto, and with twolpip-e's 10, each provided with aj eojek, such as 11, 'scre'wed into'the eover. Eeeh of the d'o'orsis mounted on a rod 12, iii "l$ l3, projecting from' the body of the alt mm retort are mounted swing- I 14, adaptedtos wing down behind tions "15 on the cover,.thus firmly locke c-ove'rsfl in position. Any desired eweirer, maybe adopted for fastenyers'to the retort. The top and ers arefpreeisely similar. ayer oi asbestos; or simiplaeed over the outer d'n the covers, and netting 115 .the site-the co er por- Ods 12 by having pped around it, as

so the .eenter, and us run shafts 17,

. b he rods 17 When-it is desi move retort; theglpwerhalfo n' is remfived' i To ol the! p as ,A,:--,.B bound toget s'e th movedQI ro de We St0 tending brackets a l offlie outside of thef ets are firmly'fasteI-i. pitta-3 by be bolted'thereto, er made-integral therewith, and have-f theirupper: parts-bent nut-- Wardly for eiigag'ementiwlth the-'ileteheshereinaftermentioned. With each of the braek; ets 22 a pivoted latch lis' adhpted to'enga r ge two of these la tchee being jpi-votally mounted on the part B, and two on the part C; Each latelr23 hes-it's end thickened, "as shown at 24, to own around the. oer-responding basket 22, so that when .thehitches .are=in 1. m, termina ing arts A, B

-.o the parts B and O are p I 5; ,injthejus'ualmanner, which'areadapted to on tracks 26,, so thetfihywh we co sisting of the we posltioli show i 01}virhereby when the latchesflflei'ethrown up, the parts B andizG may beseparated thereof. I 5% o we rddutsbf passe thro. h h

from theretort whex'geupoli .the letter may bfi roteiged-lh meaneof pow app ed toitl e ded with a latsih 29;

e form of serve to the; ohimn thickened, '.as' I shjcw at 32;; igm'id thickened end haying a groove' the in iior the d bf the. retort"- which-i; eopeh endof-the pm isle apted retortA;lea ingth1etter' ,'ejtorotete,

The ifdplatibn is; as f'oflowsb The appa rati s; be ng in the positionfshownj in Fig'. 1;

if itis deslred-to nieke gas, .cbk'eg end ag geto teleseo e.I'; This errengemenfli's. edapted so that t e parts Bggnd L G may be ,mov'ed g t e t ee Qu fb mg f m a w h ee torfiarbon, for" example, the upper door I of the retort is .opened,ia.nd va' suitable" charge obsofl; eoalvintroduced into theint'ei'ior 01E 7':

' fsai'dretort ilito-jthe space between the pipes and oonneetlonsmadeibetwe en the ,'scharg'e pipes lq efiythe top ofthe retort leading t'o,

'the ge'soh -eter, or tofiany place whereiga sfi-is 111 the retort A, the gases passing pumhrou h thediigcharge pipes 10 After. this operm tionha's-beencontinued fofaefiffieienttime,

ere diseng ez'fed from thebracktsQQ, andhe of e fltact-Wibh theretort A. All th'jeocks {we idieeon ectedo .flie pipes di gto 5 disconnected rfrom'f the'rgab 4- both the. uppeifindilp opened. By means go .jron'mdg, tweenthe 111-116 7 is-iol eed-downgfqe soft coal and heat the Sam lop-and bottom doofr's' to be useij- Afilf'is then. startedinthe furii Ina ce B; and-,the hot productfs offc'ombustion pass through theotubes 7 distilling the coal thb plie fIhe parts and Cferethenhrbught back-131i; qo nnection-w ith v theglfetorp epdv 1110M down into, theiposltion e then connected .to-thef gas den e h ksr her The disti hition process isih' v its close, and at hhe'end' th 11 Y a lowe do r v ng' h pipes. 77, tithe wholefinterior oi-"the ret rt- 'fww laxer f e e e b F e sfactythatifthe Lew'renvlayer-o tain this-.beirbijn, -1 ch or any desired kind of f iel' in bhe f" ma A5 theretort A becomes heatedup the gases from. the fqel pass outof -the upper' pip 10in the, usualfman'n'er, Ho en,-which 1, 9 1' 1'1 d vto run -ai'llo'th future consumptio A-descr'ib i niihe eserip tioh of th ap e o ks n collected. and

gafioinet er; and by means, f POW?r up 't-Qf-the pulle 18, theretort' is rotated pa.'reti1s,- th'e 'i'etoxtgi's-"revolved one 01; .more' times during-"the dis ti11 ation' process; .1

so that the dep'ositrof gas carbon withinthe retortI-fion the' filbes an dwallsjthereofimay be: substantially-uniform j'There is left the retort;eokev and-wile sit-of .gas carbon.

Th former may be 13m ired by opening. the

:carbonon the tubes and on the inside of 3 the z q f fid pushing out the coke from between the horif 1 zontel flu'es 7, leaving the deposit":of g'zi' 1 This retort maybe then used when) it stands" or conveyed awa to another portion of-'the' the three parts A,' B and r easing-the hearing ground plant. by lal tchiil together and 1-5 the rodsor Shafts f 17.5

process is v frimerily designedt'ohtreet (31L Q in the clay, I mix with one part of clay six same;

- treatment of these clays) consist of the following parts chemically"combined ri o esio en ogrr o 5 that isto say, one molecule of (ma-f alumina, two molecules of silica, two molecules of water, and-1 to 3' per cent. of ferrous or ferricoxids or both, approximately stated. After determining the amount of alumina I tiines the amount of. lei-sulfate of sodium, as

compared with the alumina in the clay, basing the weights used upon the atomlc weights of the alumina and the bi-sulfate- .015 sodium; so that the latter salt may fur- "nish enough sulfuric acid to give up 3 mole-Q cules'of'said acid to the .alumina'.' In place I of clay, I may, of course, use other ores of alumina, such as bauxite or coruhdu-mw The do quantity of bi-sulfate of sodium used should,

a k or course -be sufficient to furnish whatever iron ispresent w1th a sufiiclent amount, of sulfur cjacid, as well as the alumma, based uponthermolecular weights of the o'iiids of 5 iron and he-bii-sultate of sodium. This mixture i hen heated in one .of 'myaretorts-producing a double sulfate of aluminum and sodium represented by the formula -.Al (SO ,3Na SO ierric alum sulfate of soda, and free silica, according. to the follow- 7 ing reaction n shone :be mentio'ned that the retort should onlyfl be charged so that it isfabout tort-it isseparated from the" furnace B and fchimney connecting -portion- C and revolved,

T thus thoroughly 1 inixi'ng' ;-th'e materials jtogetheri" Thenfthe th'ree"parts AQJfB and C are reunited, as shown inFig. 1 and-there; tort is'heated by the =f1' 1rnace B. Sulfuric acid is set free fromfthebi and attacks the} Gay; mass 1;be'come s f of a a; dark/ blue color and" boils rapidlyg an there: is a rapid ein-unmet steam, Ferric alum is 'formediand alsoa new compound consisting of a double sulfate of aluminum and sodium, but haVingIB' molecules of sul-v fate of sodacombined with '1- molecule of sulfate of aluminum. During the same reaction sillca 1s also formed 1n an anhydrous condition, and when the reaction is.ended,' the mass assumes-a dirty yellow-ishwhite "the fOllOwl atmNa FAL-ea sulfate 0fsodium 1 dens'ed' in the usual The upper and lower.

the contents of the retort. Thefdoublei sul f fates aredissolved out of'the'fused'm-asg. c

leaving the silica in an insoluble forms" The mass of material obtained byw -ashi ng out. I

the retorts is tllGI-L filtered, sepamtingthe silica, which is washed again, if necessit and is then in a fine -whiteconditioralai f.-

mirably suited formaking glass and other;

purposes for which silica is'co'minenly used.

If clay is fused with acidrscdium sulfate,

NaHSO the iron in solution is precipitated with sodium prussiate. -The precipitated ferric prussiat-e is treated withcaustic soda,

and the prussiate of sodium recovered to be used over and overagain.

It will be noted that by myprocess the sulfate of alumina is united chemically with 3 molecule-sot sulfate of soda instead of with 1 molecule, as in ordinary-alum, and by making use of'thi 'new double-sulfate, I have/devised an improved soda process.- This double sulfat fusedinone-of my retorts with cry'ol' i muse ent in the re'tor ofaluminum -isproduced,- which is-"insoluble?" Sulfate of soda is also pro-- duced, which is allowed to partially cool and while stillihot' is lixiviated and the fluorid of "aluminum;separated from the solution of the sulfate of soda by filtration. The fiuorid' is; soluble;

offalilminum, after'being allowed to dry,

is heated to about "redness and showered down upon melted metallic sodium, whereupon-the following reaction takes place:

This reaction results-in the production of metallic 'aluininuin and cryolite. At the- 1 sameti-me a slag is formed which maybe au'sed to fuse with the product obtained from claysaftr'iiusingthem with bi-siilfat-e of idium, as mentioned, above.

portions'indicated by" T carbon being p-resr The mixture I obtain "metallic 'sbdium as follows": The sulfate of soda already obtained isaplac'ed in oneofthe retorts 'A,; tvhich"hasbeen-lined w t f m a Pr v ou y d s ri e Qoke',;iinely pulverized; niayf-thenbe a'd de'd, 1f necessary, and the retort is then heated,

whereupon sulfidof soda is produced, there i :still being an excess 'of carbon left in there tort. Caustic lime is then added and there-' tortheated to about 800 (3., when-metallic sodium commences to distil overand-is conmanner, the reaction be",

ing as follows: p GNafi-l-GCaO-l-6C:6Na +6CaS-{-6CQ:. In other words, I produce inetallic sodium indirectly from the sulfate of sodium or di-' rectly from the sulfid. I .use' lime to take the sulfur from the sodium, forming sodium, oxid,'which is immediately reduced tdmetallic sodium by the carbon present in the retort. I also manufacture aluminate of soda,

Al O 3Na O, in a, similar manner; that is,

I place the double sulfate of soda and alumina already obtained in one of my carbon lined retorts, and heat it until the sulfate of alumina is decomposed, forming the "oxid. Sulfurous acid gas is driven ofi,-passes over carbon monoxidand dioxid into a discharge pipe, which leads into a sulfuric acid chamher, where the, usual treatment for making sulfuric acid takes place. There is left in the retort alumina either mixed or chemically combiner! with 3 moleculesof sulfid of sodium, Al,O 3Na' S. I then add caustic lime in suflicient quantities to take up the sulfur, whereupon the following reaction.

' "I The aluminate of soda thus produced is nate of sodathroun'ha lead pipe. The .following reaction'takes place: al o sn oiiain y vThe hydrofluoric" acid is rapidly condensed andartifieial cryolite is precipitated. Carbonate of soda may also be produced as follows:, Carbonate of lime is heated in oneof my retorts and the carbonic acid pro- "dueed is led away and stored up for use.

- 'Aluminate of soda in solution is then treated with this. gas, whereupon the hydrate of aluminais precipitated, while carbonate of soda IBIIIELHIS in solution, *Whenever icarbonates orcaustic alkalies are heated at a red heat, the difiiculty has been to keep the carbon, which is lighter than the material treated, always in contact with the entire mass of the melted materiaL;

In my retort, the gas. carbon. is fixed around the time andonter ortion' of the retort and held thereimlnova .ly,'-ac cording of alumina soda, ferric alum, and free silica may bmproduced, as well as .fluomd to the reactions already set, forth. According to my method, a new double sulfate of aluminium, sulfate of soda, metallic alumi The mass is allowed to cool and treat:

aluminate of soda, besides various others.

7 num, artificial cryolite, metallic sodium,

"Ina complete plant I design" to useone series or battery of my retorts without distilling coal in them at all, and in another series, where' it 1s desirable to use a carbon lined retort, coal 1s d1st1lled, forming gas and a fresh lining of graphite or fresh carbon at every. dlstillation, taking care in every distillin operation to tip the retort over, so that t e "bottom door is on the top and vice versa. The retort, is preferably suspended from above by hangingsupports, the bottom half; bearings being lifted up to the shaft by bolts and screws, as shown in the-drawing. The retort is detachably fixed' to the furnace and chimne connecting portions by .means of cylin fitting into circular grooves, and these-with the. latches support the retort A when it is releasedfrom its bearings, so that the whole structure; consisting ,ofthe three parts A, B and G'may berolled away to "another part of the plant.

ing' ores containing alumina, silica and iron,

theste which consists in heating them in. a close retort wlth an excess of bi-sulfate of soda, producing thereby a double sulfate of alumina and soda, containing three molecules of sulfate of soda'to one molecule of sulfateof alumina, a ferric alum and free silica, substantially as described.

' 2. In the herein described process, the step 1. In the herein described processof treatrical proj ections which consists inheating clays in. a closed retort with, an excess of bi-sulfate of soda,

producing a double sulfate of soda andalumina, having three molecules of sulfate of soda to one molecule of sulfate of alumina,andjfree silica, and separating said double sulfate from said silica, substantially as described. i v

3.' The herein described process of making aluminum fluorid, which consists in heating clay in a closed retort with an excessof bisulfate of soda, forming a double sulfate of alumina and soda, having three molecules of sulfateof soda to one molecule of sulfate of alumina, separating out *said double sulfate, ,7

' heating it in a carbbndined retort, heating g the resulting product with lime, dissolving out aluminate of soda from the product and leading into'the solution thus formed a stream of" hydrofluoric acid gas,- substantially as"described. w

In testimony whereof, I aflix my signa ture, in presence offiwo witnesses.

' rHILIP A. EMANUEL. Witnesses: 7 I S. SonosKr,

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