May 19, 1925. 1,538,837 A. J. MOXHAM, WANUPACTURE OP ALUMINUM SULPHATE Filed July 25, 1022 ‘Mineral containing AL2 Os and 1 other metalic ingredients. 3 (1250s leach producing potash tum in soluion. + Cite) 2 ‘Aad Potash iFnecessary. crystolize Polash Mura crystals Drive off water ‘Dissohe KaS0e in strong He 508 By fs an Lalasf ip10 26 20 40 Patented May 19, 1925. UNITED STATES 1,538,837 PATENT OFFICE. ARTHUR J. MOXHAM, OF GREAT NECK, NEW YORK, ASSIGNOR, BY MESNE ASSIGN- ‘MENTS, TO J. P. LAPFEY, TRUSTEE, OF WILMINGTON, DELAWARE. ‘MANUFACTURE OF ALUMINUM SULPHATE, ‘Application flea July 25, 1982. To all whom. ét may concern: Be it known that I, Anrmun J. Moxstant, a subject of the King’of Great Britain, and a resident of Great Neck, in the county of Nassau and Stato of New York, have in- vented certain new and useful Tmprove- ments, in the Manufacture of Aluminum Sulphate, of whieh the following is a speci- fication ‘My invention relates to the treatment of minerals containing alumina. Such miner- als contain jron oxide and ‘other, metallic oxides or salts. My process is adapted to the economical separation and commercial production of alumina from ores, such, for ‘example, as many low grade iron ores which heretofore have ordinarily not been treated atall for any of their metallic contents, or if thus treated the alumina contents have been wholly lost. An example of such a mineral or iron ore which exists in large quantities and which has heretofore been almost wholly unworked is green sand or glaucon- ite, “Another example of a mineral from which Tam able to economically obtain alu- mina by my process is the Oriskany iron ore of the Southern States. By my process Tam also able to economically’ separate and re- cover any potash which the mineral con- tains. In accordance with my process I convert the alumina in the mineral into sulphate of alumina and combine, the sulphate of alu- mina with sulphate of potash and water to produce potash alum, which has the formula Ai(80),-£K,S0,2411,0. "The potash ‘him separates from the other ingredients of the ore or mineral by crystallization, and the sulphate of alumina is thereafter obtained therefrom as a pure salt by treat- ing the potash alum erystals with strong sulphuric acid which dissolves the sulphate of potash, leaving the sulphate of aluminum undissolved as a white powder. The sul- phate of aluminum is readily convertible in- to alumina with tho recovery of the SO, gas as fuming sulphuric acid. ‘The potash heeded in my process is in the case of some minerals, as, for example, green sand, pres- en, in large quantity in the mineral, in which case the potash is separately recoy- erablo as a valuablo commeretal product. | If not present, however, in sufficient. quantity, 2 potash salt or other potash bearing ma- terial may be added to the material to be Serial No, 577,452, treated in sufficient quantity to permit the entire alumina contents of the mineral to be made a constituent of potash alum, My process may be practiced without sub; stantial loss of any of the reagents employed and with small expenditure for heat and for labor. Moreover, some of the steps of my process effect reactions which are involved in processes for the production of iron and other metals, and this adds to the efficiency and ccnnomy of the proces, he drawing accompanying this 5 cation is a flow sheet showing specific steps constituting one spec bodiment, of my. process. Istart at 1 with the mineral to be treated, which, as before stated, may be green sand oF glauconite or any other mineral contain- Ing alumina and lange emount of potash with other metallic and non-metallic ingre: nts, or it may he material such as an Oriskany iron ore which contains no sub- stantial amount of potash. ‘The mineral is, preferably crushed so that it may be more readily leached with sulphuric acid, If the mineral has insufficient potash con- tents to enable the alumina contents of the mineral to combine with the potash to form potash alum, then in the next step, 2, Tadd sufficient potash to enable this resulé to be produced. This potash may be added as salt, preferably in the form of sulphate or suflicient potash bearing vaw material may be added. Although the potash sult is rela tively expensive, it is not prohibitive to en ploy it in the process, bectuse, as will pre ently appear, it is recovered Inter with ney Tigible loss, and it nay be used over nnd over again, If desired, the sulpliate of po- Tater ‘recovered may be sold as such. ‘The potash thus added to the mineral should be added to the mineral before or durin leaching. On the other hand, if the potash, contained in the material is in excess, ma- terial containing alumina may be added in suitable quantity to enable all the excess of potash to be recovered. I next, as indicatod in 3, Teach the min- eral (with or without additional potash or alumina, as already explained) with sul- phuric acid under conditions that will cause the metallic ingredients of the mineral to bbe dissolved and which will cause the alu- mina to combine with potash and water to form potash alum. ‘To obtain the most ef- fc 6 8 9% 100 no10 20 25 30 0 60 ficient, and quickest results, the sulphuric acid should be dilute enough to contain the necessary quantity of water to supply the 24 molecules of water for the potash alm, ‘An excess of rater is not harshfuny because it ls preferable that the leaching is carried on af of near the boiling pois, and any feocnabil oes f yar driven of by Treat during the leaching operation. "The Hight auouse of water in he each ean be closely regulated, If too much is can be driven off by the heat ot by adding fuming. gulphurie acid to the leach or DY both, “Ef too litte ip present, water can be directly added to the leach T have found that a suficiently dita sul- antic acid to effet a reasonably rapid pro- Uuetion of the potash alum is’ of suitable strength for digolving the. other motallie ingredients of minerals, sueh, for example, as tho iron contents, ‘The defails of such Texching process for the recovery of iron from jron ores ig set forth in » ponding ap- Dlleation of | A.W. Davidson, Ser Bares, fled iy 1, 1990. ‘At the end of step 3, therefore, the bath contains the silica ingredients of the min- ral og solid, undissolved matter, mainly ag Dre silica, and in solution the potash alum, Ferg oulphato and sulphates ef any other retals that ave ordinarily found im such minerals T next separate the undissolved. ingre- dients from this solution as by the filtering sp, faking care fo thoroy ash the sold thatter fo aveid waste of the dissolved sulphates. "Phe next step, indiented at 5 is to cool the solution and thereby cause the potash alam to crystallize therefrom, Tes possible to produce these potash aun crystals feom the mineral or te mineral mixed "with additional potash by "v. cokd process if desined, In thi ease, the material fo te treated is allowed to stand in strong slpharie acid-—that i, suiphuric acid cate ‘ying less than the proper emount of water ‘After many days, enough water will bo ab: sorbed from tite atmosphere to secute the heeded balance and the: potash alum crys: {als will then gredually form. ‘These ean bo removed. from time to. time until the erp conse to form. “Whe next step of the process, indicated at 6, is to remove the crystals and to. wash 1,588,887 Qh in ol wdc ‘This washing soul lone as quickly as in a centrifuge, or with suction, as the crystals dissolve slowly in cold water. Although a small amount of potash alum will be this dissolved in the ‘washing, this Involves no wasto us the wash ‘ater may be used over again and the pot- ash slum therefore finally recovered from it. Tnext,as indicated at, subject the potash alum ergstals to heat to drive off the water and render the sulphate of aluminum anhy- Grous. "The erystals melt at 845° Cand Imost of the water is driven off at 190° C., the lest molecule being driven off at about 300° C. "It is not necessary to drive off all the waier by beat.” ‘The bull of the ‘water may be driven off and concentrated. sul- phiasie acid an then be added to take out the last of it ‘This acid, if ndded in the proper quantity, will dissolee the sulphate of potash and hs separate from the an- hydrous sulphate of alumina whieh reina’ undissolved in the form of white powd "The sulphate of alumina is then, 2s caied at 9, removed as hy decanting. is desired to sell this sulphate of altonina, Which is a valuable, marketable product, 1¢ is quickly washed in cold water to remove Uholadherig sulphuric act and his water is used over again Zor washing or diluting the acid. . “To earry the process further to obtain pure alumina, the sulphate of alumina is, 45 indicated at 10, enleined at, say, 800° to 900°C, and the $0, gas and adhering sulphurie teid are driven off and condensed for reuse or for sale as concentrated acid. ‘The potassium sulphate solution. is. in proper form to bo uscd over again for the treatment of further material or it may be separately treated and sold as potash, if it isimore profitable to do so. Having thus described my invention, what T claim and desire to protect hy Tat” ters Patent ist "The process of treating potash-alum whiel consists infest. driving of the wat and then separating the sulphates bya solving’ the potasium alphas dn song sulphutie acid and then separating tho shu: minum sulphate residue from the solution In testimony whereof, I have signed my name to this specification. ARTHUR J. MOXHAM. o %0 os