,Tr JOHN EKELEEY AND WILLIAM‘ B. STODDALRID, OF BOULDER, COLORADO. PROCESS OF OBTAINING- TUNGS'I‘ATES.

~ Speci?cation of Letters Patent. - lh?ddnldd. I Patented net. , for, No Drawing. Application ?led June as, 1916. Serial naioaeae. To all whom it may concern: _ ground ore is then roasted in any ‘suitable Be it known that we, JOHN B. EKELEY and furnace so as to drive off the sulfur and WILLIAM B. STonoARo, of Boulder, ‘in the arsenic contained in the ore‘as far as this county of Boulder, and in the State of Colo is possible. The roasted ore is then mixed 60 rado, have invented a certain new and use with sodium chlorid, sodium carbonate, and ful Improvement in Processes of Obtaining if found desirable, some silica. An amount Tungstates, and do hereby‘ declare that the of sodium chlorid is added, preferably from following is a full, clear, and exact descrip two-?fths to the same in-weight as the~ tion thereof. ~ - weight of theore. An amount of the sodium 65 10 Our invention relates particularly to the carbonate is added su?icient to combine with _ treatment of ores containing heavy acid all of the tungstic acid and leave in addition formingelements but particularly , an excess of the sodium carbonate. Su? ‘so as to separate the impurities from the cient silica is ordinarily added to combine same and obtain the ‘tungsten in the form of with the excessof sodium carbonate” so as to it a salt of tungstic acid. It relates however‘ produce an insoluble silicate preferably con also in a similar way to- the treatment of taining sodium oxid and silicon dioxid in ores containing chromium, molybdenum, the proportions of'one to four. Some ores, vanadium, or uranium, which are also heavy however‘, do not require the addition of any acid-forming, elements. silica for this purpose, and in working with 75 20 The object of our invention is to obtain such ores the silica is omitted. If desired, tungstic acid or a salt thereof, or a similar . sodium- nitrate or sodium chlorate may be compound of any of the other heavy acid added to the mixture which provide oxidiz ' forming elements, by the treatment of vari ing agents in the bath'when fused. Instead ‘ ous ores containing the same in such a man of sodium chlorid, we -may - use sodium 80 25 ner as to separate out in a very complete ?uorid or calcium chlorid , or ?uorid. manner the impurities contained in the ores The charge is thenv fused in a suitable and so as to obtain a compound of such ele furnace. After the- bath of fused mate ment, as for example, a salt of tungstic acid, rials has'been allowed to cool, it will be . in a very pure form. A further object is to found that the solid materialsiwill have be 85 30 carry out this process by. the aid of fusion come separated into a water soluble portion in such a manner that the impurities con and a water insoluble portion, the tungstic . tained in the ore will become separated from acid being contained in the form of sodium the compound of' the heavy acid-forming tungstate in the water soluble portion. The element by sharp lines of‘ demarcation in solid mass, is crushed and then extracted with 35 the fused bath and in: the resulting solid water and ?ltered. The ?ltrate is a clear obtained by‘ the cooling of the fused mate solution of sodium tungstate which is pre~= rials. Further objects of our invention will cipitated as calcium tungstate by the addi- - ‘ appear from the detailed description thereof tion of calcium chlorid in a sufficient quan appearing hereinafter. ' tity to replace all of the sodium by calcium 95 40 ' ile) our invention is capable of being 'in the sodium tungstate contained in the L

carried out in many di?'erent Ways, for the solution. . v _ y . purpose of illustration we ‘shall describe The sodium chloridperforms the function only one example of the several ways in of producing sharp‘ lines of demarcation be which our invention may be followed. tween the two portions contained in the 10% As one example of the way in which our .fused bath and :in the resulting solid when invention may‘ be carried out we mayv pro cooled, the said two portions comprising a ceed as\follows: A tungsten ore, as for ex water soluble portion ‘ containing sodium ample, , hiibnerite,‘ , tungstate, sodium carbonate and sodium , , etc., is crushed, sampled, chlorid, and a water insoluble portion com 101 50 and ground while dry‘in any suitableman prising silicates and other materials derived . ‘her, by any one of the well-known methods, from the gangue of themes treated. vThe ' to a suitable degree of ?neness. The degree ‘sodium chlorid, furthermore, acts to/dis, of ?neness may vary to some extent with integrate and dissolve the tungsten ore with the nature of the ore, as for example, the remarkable rapidity. The sodium‘ chlorid 11a 55 facilitywith which it subjects itself to the also acts as a solvent and diluent for the succeeding treatments in the process The sodium carbonate It also plays a p in 1,255,144

almost entirely preventing the formation of tungsten ore ina bath containing an alkali soluble silicates, phosphates, etc. The and a compound of an alkali-forming ele sodium chlorid also produces a crystalline ment, that is a solvent of the alkali when structure with marked to the water fused. soluble portion of the melt when solidi?ed 2. The process which comprises fusing a 65 so that it is very friable and very easily tungsten ore in a bath containing sodium crushed. When sodium chlorid is used, the carbonate and a compound of an alkali portion of the melt containing the sodium forming element, that is a solvent of the tungstate, carries comparatively little un-/ ' sodium carbonate when fused. 10 decomposed sodium carbonate, but ‘large 3. The process which comprises fusing a 70 quantities of sodium chlorid, which makes tungsten ore in a bath containing a halid it very easy to dissolve the water soluble por of an alkali-forming metal, and a basic tion in water as compared with a corre compound of an alkali-forming metal. sponding melt made with sodium carbo 4. The process which comprises fusing a 15 nate alone. Furthermore, the. presence of tungsten ore in a bath containing chlorid 75 sodium chlorid and sodium carbonate per of sodium, and a basic compound of an mits the mass to be more readily melted alkali-forming metal. ' than when the sodium chlorid is omitted, 5. The process which comprises fusing a and the melted mass has a low viscosity so tungsten ore in a bath'containing a halid 20 that the reacting ?uid comes into contact of an alkali-forming metal and'sodium car 80 with the particles of ore very readily. The bonate. extreme ?uidity of the sodium carbonate 6. The process which comprises fusing a and sodium chlorid when fused together tungsten ore in a bath containing chlorid renders it possible also to use less of the of sodium and sodium carbonate. 25 sodium carbonate than when the sodium 7. The process which comprises fusing a 85 chlorid is omitted. For the same reason tungsten ore in a bath containing a halid it is possible to treat a coarser material in of an alkali forming metal and an alkali a shorter time than if the sodium chlorid and silica. ' were omitted. . The sodium carbonate is pro 8. The process which comprises fusing a -30 vided for combining with the tungstic acid tungsten ore in a bath containing chlorid 90 so as to produce sodium tungstate, and. of sodium, an alkali and silica. in the presence of the sodium chlorid the 9. The process which comprises fusing sodium carbonate also exerts a selective a tungsten ore in a bath containing a halid action on the tungstic acid in the ore by of an alkali forming metal, sodium car 85 causing the sodium oxid contained in the bonate and silica. . same to combine with the tungstic acid in 10. The process which com-prises fusing preference to the silica or phosphorus pen a tungsten ore in a bath containing chlorid toxid, or other acid ingredients of the ore. of sodium, sodium carbonate and silica. Instead of treating a tungsten ore as above, 11. The process which comprises fusing 40 an ore of another heavy acid-forming ele a tungsten ore in a bath'containing a halid 100 ment may be similarly treated, as for ex of an alkali-forming metal, an alkali and ample, an ore of chromium, molybdenum, an oxidizing salt. ‘ ' vanadium or uranium, as for example, 12. The process which comprises fusing chromite, molybdenite or carnotite. a tungsten ore in a bath containing a halid 45 By the term “fusing” herein, and in the of an alkali-forming metal, an alkali and 105 claims, we mean maintaining in a state of sodium nitrate. _ , fusion and not necessarily passing from the 13. The process which comprises grinding solid to the liquid state. In other words, and roasting a tungsten ore, fusing the by the term “fusing” in the claims, we mean tungsten ore in a bath containing a halid of 50 fusing one or more of the ingredients sepa an alkali-forming metal, an alkali and an rately and mixing them together while oxidizing salt. 110 fused or heating all of the'ingredients to 14. The process which comprises grind gether until fused.‘ ing and roasting a tungsten ore, fusing the jWhile we have described our invention tungsten ore in a bath containing a halid 55 above in detail,-we wish it to be understood of an alkali-forming metal, an alkali and 115 that many changes may be made therein sodium nitrate. without departing from the spirit of our In testimony that we claim the foregoing invention. we have hereunto set our hands. We claim: JOHN B. EKELEY. 60 1. The process which comprises fusing a WILLIAM B. STODDARD.