US957756A - Process of treating ores. - Google Patents

Description

P. A. EMANUEL.

PROCESS OF TREATING ORES.

APPLIOATION rum) SEPT. 29, 1909.

57,756. Patented May 10, 1910.

2 SHEETS-SHEET 1.

nn Qnnnnn P. A. EMANUEL. PROCESS OF TREATING ORES. APPLICATION I'ILEDSBP'T. 29, 1909. 957,756. Patented May 10, 1910.

2 SHEETS-SHEET 2.

P A. EMANUEL, OF AIKEN, SOUTH CAROLINA.

PROCESS .OF TREATIKQ OBES.

names.

Specification of letters Patent.

Patented m 1o, 19m.

Original application med May 28, 1909, Serial No. 499,202. Divided and this appllcation flled September 29,

- 1909. Serial No. 880,21

I South Carolina, have invented certain new and useful Improvements in Processes of- Treating Ores; and I do hereby declare the following to be a full, clear, and exact description of the invention, such as will enable others skilled in the art to which it appertains to make and use the same.

My invention relates to processes of treating ores and is designed to treat ordinary clays in such a manner as to save all their valuable constituents and at the same time make use of the by-products. It is also applicable to the treatment of bauxite and corundu-m for the making of soda, a double sulfate of sodium and aluminum, silica, aluminum fluorid, sodium sulfate, metallic sodium, and aluminate of sodium, this application being a division of my former application, Serlal No. 499,202, filed May 29, 1909.

I carry out my rocess by an apparatus a part of which is s ow-n in the accompanying drawings, and in which-- Figure 1 is a side elevation showing my invention. Fig. 2 is ahorizonta-l cross section thereof. Fig. 3 is a cross section through the retort. Fi 4 is a side elevation on a larger scale, s owing part of the rctort'and part of the furnace, and Fig. 5

is a partial section showing part of the retort and the manner of securing the wire netting thereon.

Referrin to the drawings, A represents the retort, the furnace portion, and C the portion connecting the retort with the smoke stack.

The retort is composed of a cylindrical bodyedportion 1,.having at each end an extend portion 2,.forming a flange on which the portion 3 is bolted. The part 3 is cylindrical, and open at both ends, but having one end bent inwardly to embrace the portion 2, both ends of the retort being exactly similar.

4 represents a perforated 'plate fitting tightly against the end of the retort, a suitable packing 5 of asbestos or similar material being used if desired. Bolts 6 pass through the bent-in end of the part 3 in cars 13, projecting from the bod mentioned.

through the part 2 and through the plate 4, uniting the whole firmly together.

7 re "resents tubes which ass through the end p ates 4, the ends of w iich are secured in perforations in the plate 8, secured to the plate 4.

At the top and bottom the retort is prov1ded with curved doors 9, hinged thereto, and with two pipes 10, each provided with a cock, such as 11, screwed into the cover. Each of the doors is mounted on a rod 12, of the retort, and on the retort are mountcr "swinging bolts 14, adapted to swin down behind projections 15 on the cover, thus firmly looking the covers in position. 'ihny desired means, however, may be adopted for fastening the covers to the retort. The top and bottom covers are precisely similar.

14 represents a layer of asbestos, or similar refractory material, placed over the outer side of the retort, including the covers,

and held in place by the wire netting 15,

angular frame 19, by means of depending are firmly fastened to the parts 3 by beingbolted thereto, or made integral therewith, and have their upper parts bent outwardly for engagement with the latches hereinafter With each of the brackets 22 a pivoted latch is adapted to engage, two of these latches being pivotally mounted on the part B, and two on the art C. Each latch 23 has its end thickene as shown at 24, to pass down around the corresponding bracket 22, so that when the latches are in the position shown in Fig. 1, the parts A, B-and are prevented from longitudinal movement, except as a whole, bein firmly locked together, with the ends of the parts 3 fitting into corresponding grooves 111 the parts B and C. To the parts B and C are attached wheels 25, in the usual manner, which are adapted to run on tracks 26, so that .the whole apparatus, consisting of the parts A, B and 0 may be moved as a whole from one part of theplant to another, the latches being in the position shown in Flg. 1, or whereby when the latches 23 are thrown up, the parts B and C may be separated from the retort A, whereupon the latter may be rotated by means of power applied to,

the pulley 18 for a purpose hereinafter described. The part B is the furnace portion, and is provided with a grate 26', pipe 27 for the admission of aseous or liquid fuel, and door 28, provide? with a latch 29. Of course, any desired form of fuel could be used in the part B. J

.The rear end of the part B is closed by a erforated plate 30, the perforations being lbcated 0 )posite the tubes 7 in the retort A. Around tins perforated plate, the rear open end of the part B is thickened, as shown at 31, and is provided with a circular groove, into which groove the part 3carried by the retort is adapted to fit.

The part C simply serves to carry the waste products of combustion after they have passed through the tubes 7 of the retort into the chimney. It consists of a flue, preferably cylindrlcal in form, havin one end thickened, as shown at 32, said thickened end having a groove therein for the reception of the part 3 on one end of the retort A.

33 represents a chimney, and 34 the flue thereof.

35 represents a cylindrical o ening, into which the open aid of the part is adapted to telescope. This arrangement is adopted so that the parts B and C may be moved along the track out of engagement with the retort A, leaving the latter free to rotate.

The operation is as follows :The apparatus being in the position shown in Fig. 1, if it is desired to make as, coke, and gas retort carbon, for examp e, the upper door of the retort is opened and a suitable charge of soft coal introduced into the interior of said retort into thespace between the pipes 7. The upper door is then firmly closed,

and connections made between the discharge pipes 10 at the top of the retort leading to the gasometer, or to any place where gas is to be used. A fire is then started in the furnace B, and the hot prodnets of combustion pass through the tubes 7,

distilling the coal in the retort A, the gases passing out through the discharge pipes 10.

After this operation has been continued for a sufficient time to distill about half of the coal, the latches 23 are disengaged from the brackets 22, and the parts B and C moved along the track 20 out of contact with the retort A. All the cocks in the pipes 10 being closed, the upper pipes are disconnected from the pi es leading to the gaso nieter, and by means 0 power applied to the pulley 18, the retort is rotated 180. The parts B and C are then brought back into connection with the retort A, and the latches 23 moved down into the position shown in Fig. 1. The pipes at the top of the retort are then connected to the gas delive pipes, and the cooks therein 0 ened. The istillation process is then carried on to its close, and at the end the upper pipes are disconnected from the gas delivery pipes, and both the upper and ower doors are "opened. By means of iron rods, the coke between the pipe 7' is forced down, out through the lower door, leaving the ipes 7, and in fact the whole interior of tlie retort, coated with an even layer of gas carbon.

The fact that the whole interior of the retort, including the pi s, is coated with an even layer of gas car on, makes the retort highly useful in the production of sodium, for example, in which it is. necessary that the substances under treatment should be subjected to the action of carbon under heat, and in which it is desirable that the retort should be frequently rotated. These retorts ma be used either with or without carbon an are arranged in sets so that they can be moved from one part of the plant to another.

For some of the reactions hereinafter mentioned, it is necessary to have a certain amount of carbon in the retort and for other reactions there must be no carbon. To obtain this carbon, I charge the retort with soft coal and'heat the same, up to the distillation point, b burning gas, coke, coal, or any desired klnd of fuel in the furnace B. As the retort A becomes heated up, the gases from the fuel pass out of the upper pipes 10 in the usual manner, the cooks 11 being open, which gases are collected and either used to run another retort or stored for future consumption.

As described in the description of the apparatus, the retort isrevolved 180 one or more times during the distillation process, so that the deposit of gas carbon within the retort on the tubes and walls thereof may be substantially uniform. There is left in the retort coke and a deposit of gas carbon. The former may be removed by opening the top and bottom doors 9 of the retort and pushing out the coke from between the horizontal flues 7, leaving the deposit of gas carbon on the tubes and on the inside of the end plates and on the walls of the retort. This ee'mse,

IL 1 'retor l may be then used where itstands'or conve ed awa. to'anot-her portion of the plant by latchin the three parts A, B and C together and r easing the bearing around the rods or shafts 17. 1

The- South Carolina clays, which my process is primarily ,designed to treat (although it 18 by no means restricted to the treatment of these clays) consist of the following arts chemically combined-A1 0 2810,, 2%,0, XFe O that is to say, one

' molecule of oxid of aluminum, two molecules of silica, two molecules of water, and 1 to 3 per cent. of ferrous or'fer'ric oxids or both, approximately stated.

After determining the amount-of alumina in the clay, I mix with one art of cla six times the amount of bi-sul ate of so ium, as compared with the alumina in the clay, basing the weights used'upon the molecular weights of the alumina and'the bi-sulfate of sodium, so that the latter. salt may furnish enough sulfuric acid. to give up 3 molecules of said acid to the alumina. Insplace of clay, I may, of course, use other ores of aluminum, such as bauxite or corundum,

The uantity of acid bi-sulfate of sodium used s ould, of course, be sufiicient to furnish whatever iron is present with a sufficient amount of sulfuric acid, as well as the alumina, based uponthe atomic weights of the oxids of iron and the bi-sulfate of sodium.

This mixture is then heated in one of my retorts, producing adouble sulfate of aluminum and sodium re resented by the formulaAl (S0 dNa,,S ferric alum, sulfate of sodium, and free silica, according to the following reaction al o esio en xr o GNaHSO,

It should be mentioned that the a'etort should only be charged so that it is about two-thirds full and before heating the retort "it is separated from the furnace B and chimcombined with 1 molecule of sulfate,of aluminum. During the same reaction silica is also formed inan anhydrous condition, and when the reaction is ended, the mass assumes a dirty yellowish white color. As soon as the reaction is ended, the' lower bearings of the retort A areremoved and the whole approcess.

also produced which paratus beingthen' free to move is rolled off the track to another portions-of the plant. The upper and lower pipes in the retort are then opened and steam. or hot waterv is passed in through the pipes at the top and -1s dis charged through the pipes at the bottom, carrying out with it the'contents of the retort. The double-sulfates are dissolved out 1 of the fused "mass, leaving the silica in an insoluble form. The mass of material obtained by washingout the retorts'is then' filtered, separating the silica, which is washed again, if necessary, and is then in a finev white condition, admirably" suited for making glass and other purposes for which silica is commonly used.

It will be noted that sulfate of aluminum is united chemically with 3 molecules of sulfate of sodium instead of with 1 molecule, as in ordinary aluifi, and'by making useof thisnew double sulfate, I have devised an im roved sodium This double sulfate is fused in one of my retorts with cr .olite in the proportions indicated by the ollowing react-ion, no carbon being present in the retorts: .t

by my process the Fluorid of aluminum is produced, which insoluble, Sulfate of sodium is soluble. The mixture is allowed to partially cool and while; still hot is lixivi'atedand the fiuorid of aluminum separated from the solution of the sulfate of sodium by filtration.. The fluorid of aluminum, after being. allowed to dry,-is heated to about rednessand showered down upon,melted metallic sodium, whereuponthe following reaction takes place:

This reaction results in the production.

of metallic aluminum and cryolite. A't the same time a slag is'formedqwhich may be used to fuse with the product obtained from clays after fusing them with bi-sulfate sodium, as mentioned above.

I obtain metallic sodium as follows: Thesulfate of sodium already obtained is placed in one of the retorts A, which has beenlined with gas -carbon,-as previously described.

Coke, finely pulverized, may then be added,

if necessary, and the retort is then heated, whereupon sulfid. of sodium is produced, there still being an excessof carbon left in the retort. Caustic lime is then added and the retort heated to about 800 CL, when metallic sodium commences to distilover and is condensed in the usual manner, the

reaction being as. follows cNa s+6cao+ec=cna +eqas+eod other words, I produce metallic sodium indirectlyv from the sulfate of sodium or directly from the sulfidfi I use lime to take the sulfur from the sodium, formin sodium oxid, which is immediately reducedto metallic sodium by the carbon present in the retort. I also manufacture aluminate of sodium, Al O' ,3Na O, in a similar manner; that is, I place the ,double'sulfate of sodium and aluminum already obtained in one of my carbon lined retorts, and heat it until thesulfate of aluminum is decomposed, forming the oxid. Sulfurous acid gas is driven off, passes over carbon monoxid and dioxid into a discharge pipe, which leads into a sulfuric'acid chamber, where the usuaL treatment for makingsulfuric acid takes place.- There isleft in the retort alumina either mixed or chemically" combined with 3 molecules of'sulfid of sodium, Al Q 3Na S, I

I then add caustic lime in sufficient quan- 'tities to take up the sulfur, whereupon the following reaction takes place:

A1 0 ,3Na S+3CaO=Al;O 3Na O-l3CaS.

The aluminate of sodium thus produced is soluble while the sulfid of calcium is insoluble. The mass is allowed to cool and treated with water, whereupon the aluminate of sodium dissolves and the sulfid of calcium canbe. separated from the solution byfiltration or decantation.

Artificial cryolite can also be made from "the aluminate of sodium so obtained by treating fluorid of calcium (fluorspar)-in a" lead tank with sulfuric acid, whereupon hydro-fluoric acid is formed, in the usual manner, which acid is led into a solution of aluminate of sodium through a lead pipe.

The following reaction takes place:

Al O ,3 Na O+ 12HF=Al F,,6NaF+6H O. The hydro fluoric acid is rapidly condensed and artificial cryolite is precipitated.

Carbonate of sodium may also be produced as follows: Carbonate of lime is heated in one of my retorts and the carbonic acid produced is led away and stored up for use: Aluminate of sodium in solution is then treated with this gas, whereupon the hydrate of aluminum is precipitated, while carbonate of sodium remains in solution. Whenevercarbonates or caustic alkalies. are heatedat a red heat, the difliculty 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 fines and outer portion of the re-. tort and held there immovably, according to the reactions already set forth. According and chimney to my method, anew double sulfate of alusilica may be produced, as ell as fluorid of aluminum, -su fate of sodium, metallic aluminum, artificial cryolite, metallic sodium, aluminate of sodium, besides various others.

In a complete plant I design to use-one series or batter of my retorts without distilling coal in t cm at all, and in another series, where it is desirable to, use a carbon lined retort, coal is distilled, forming gas and a fresh lining of graphite or fresh carbonat every distillation, taking care in every distilling operation to tip the getort over, so that the bottom door is on the top and vice versa} ,The retort is preferably suspended from above by hangin supports, 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 connecting portions by means of cylindrical projections fitting into circular grooves, and these with the latches support the retort A when it is released from its bearings, so that the whole structure, consisting of the three parts A, B and C may be rolled away to another part of the plant.

From the sodium aluminate made as above described, metallic sodium may be produced in the following manner :.Sodium aluminate is placed in one of my carbon lined retorts'which is then heated and anhydrous sodium carbonate constantly added. At 800 C. the alumina displaces the carbonic acid gas, and the carbon set free immediately reduces the sodium oxid as follows The reactions are set forth below: Al O Na,O+2Na CO +2G= 1. The hereindescribed process. of mak- -105 ing sodium, 'whichconsists in heating in a closed vessel sodium aluminate in the presence of a sodium compound and carbon, substantially as described.

2."The herein described process of mak- 110 ing sodium, which consists in heating in a closed vessel sodium aluminate in the ,pres-' ence of sodium carbonate and gas carbon, substantially as described.

In testimony whereof, I aflix my signature, 115 in presence of two witnesses.

' PHILIP A. EMANUEL.

Witnesses:

T. A. WITHERsPoo R. M. PARKER.

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