US877261A - Method of producing stannic chlorid. - Google Patents

Description

1510.87 261] PATENTED JAN. 21, 1908 G. P. TOWNSEND.

METHOD OF PRODUCING STANNIG GHLORID. APFLIOATION FILED DEC. 6. 1904.

2 51mm Mann-1 PATENTED JAN. 21. 1908.

0. B; TOWNSEND. METHOD OF PRODUCING STANNIG OHLORID.

APPLICATION FILED DEC. 6. 1904 2 BHEBTS-SHEET 2.

UNITED STATES IPA-TENT. 1 OFFICE.

CLINTON PAULTOWNSEND, OF WASHINGTON, DISTRICT OF COLU BIA, ASSIGNOR, BY- MESNE ASSIGNMENTS, TO AMERICAN CAN COMPANY, A CORPORATION OF EW JERSEY m'rrion or PnonucINGs'raN m CHLORIID.

Patented Jan. 21, 1908.

To all whom it may concern? Be itknown that-I, CLINTON PAUL TOWN- SEND, a citizen of the United States, residing at Washington, in the District of Columbia, have invented certain-new and useful InigIOVGlXlGDtS in Method 'of Producing-Stannic hlorid, of which the'following is a specificatiOIl. i

This invention: is. a' method of producing and recovering stannic chlorid from' metallic tin, or from-any materialwhich contains tin in form capable of yielding achlorid of tin by reaction with chlorin. The method is adapted to the recovery -of stannic' chlorid from the product resulting from the detinn-ing of tin-- scra or cuttings, and will be described as alpe.

plie to such product by way of examp his productas commonly obtained as a powder containing from80 to 95 per cent. of tin, largely' as metal, and relatlvely small proportions; of lead and ironor their com pounds; 'Tin in this form can be refined and rendered marketable only at considerable cost, but is well adapted to the production of stannic chlorid according to the present method. k

For a full understanding of the invention .reference is made to the accompanying drawin s',- wherein,,'

igure 1 is a plan view of one form of ap-- aratus for carrying out the vmethod; Fig. 2 is-a side elevationotthe same; and Figs. 3 and 4 are details. I

Referring to the figures, reference numerals 1-10 represent a series of vessels or retorts of which any desired or suitable number. may be employed: These retorts are prefer-v ably arranged in a continuous series with a number of interposed condensers. torts shown constitute a series and are closely grouped, suitable means being rovided for the application of heat as, for instance,

by embedding all rntortsin sand or other,

medium contained in a pan indicated in out line by'dotted lines 18, Figs. 1 and 2: Heat is 'ap lied tothispan in any suitable way, as by t 1e contact of line gases or the application of steam under suitable pressure. retorts may, of course, be separately heated by any convenient means.

The retorts are indicated as consisting of acid \proof stoneware. Each retort is pro-.

videdaivith a central aperture having a cover 19, this aperture serving for charging. the retort an 'scharging the residuum; and two densers may as illustrate The re- The lateral a ertures. 20, 21' for the passage of gases an vaporized reaction products. The

vessel or retort 1 communicates directly withing retortsof a series communicate only through inter osed condensers. These conbe of any desired form, thoseillustrated comprising the pipes 22,-23 and the collecting vessels. '1117. It will be understood that in the production of'stannic .chloridcondensation occurs also in the exit pipe from the retort, and means for with drawing the liquid from this pipe may be used instead of the collecting vessels "shown; 24 is a cock shown in detail in Figs. 3, 4.

"Chlorin isintroduced through inlet 25, and is. directed into either .of the pipes 26 or 27 in accordance with thewqlosition of the opening 28 in the cap 29.. enthe cock is turn'e in Fig. 3 the chlorin-introduced retort 2, and retort 9 with 10,but the remain-j at 25 will pass through pipe 26 into thevessel 1, thence in. succession through the severalretorts and interposed condensers, returning throu h pi e 27' to the-cock and being directe by tlie tube 30, carried'by the cap 29, to the outlet 31 for'waste gases. When the cock is revolved into the position indicated in dotted lines in Fig. 3 the direction of flow throu h the retorts andcondensers is reverse the inlet and outlet remaining unchanged. Any convenientmeans for controlling and reversing the flow of chlorin may be substituted." The pipes and collecting chambers constitutin the condensers may, if desired be provide with a heat insulating cover. The collecting chambers are convenientlyof glass, or other means are provided for watching the progress of the operation.

The don'denser'pi es may advantageously extend for a consl erable distance into the retorts, as indicated lay-dotted lines in Fig. 2, whereby the current of gas is directed toward the surface of the charge.

In using the above described apparatus the operation is conducted substantially as fol-v lows: The retoi'ts 2 9 are charged with the tin-bearing material, preferabl as a layer of relatively slight depth,.and ch orin is admit.- ted to the series, thechlorin being preferably admitted faster than it can be absorbed by the tin in a-single retort. The retorts are maintained during the distillation period at a suitable temperature above the vaporizing point of stannic, chlorid (114.C.), and the vaporized and entrained 'stannic chlorid tofrom a gas containing chlorin.

gether with the excess of chlorin passes into the condensing and collecting apparatus 22, 11, 23, the unconclcnsed portlons )assing thence to the retort S where a further absorption or condensation occurs. At this stage of the operation the distillation will proceed mostrapidly in retort 2, and the number of retorts in series will be so related;

to the rate of supply of chlorin that the first retort will cease to yield stannic chlorid before the distillation has begun in the last retort of the series.

For a clear understanding of the purpose of the series arrangement of retorts and interposed condensing means it should be understood that in order to insure a rapid production and distillation of stannic chlorid it is necessary that an excess of chlorin be brought into presence of the tin; and that it is extremely difficult to secure a complete condensation of stannic chlorid, particularly It is, clear, therefore, 'that if it be attempted to produce stannic chlorid in a single retort followed by a condensing system, there will result a loss of chlorin representing the excess used, and a loss of stannic chlorid representing the uncondensed portion. -According to this in- 'vention such excess of chlorin as is desirable for rapid and economical production and distillation ofstannic chlorid is used, and no particular necessity exists for providing the complex apparatus which would be necessary for securing an approximately complete condensation of the stannic chlorid. The

: gases passing from the first condenser to the second retort ordinarily contain both chlorin and stannic ehlorid, both of which are uickly absorbed or condensed in presence of t e tin in the second and following retorts. As each retort in succession ceases to absorb chlorin and stannic chlorid it will begin the delivery of stannic'chlorid to its condenser and the succeeding retorts. Before the last retort in series has ceased absorbing, one or more of the retorts first in series will have ceased distilling and should then be recharged.

In the particular form of apparatus shown it is advisable at this stage to reverse the direction of flow of chlorin through the-retorts by rotating the cap 29 of the cock 24, permitting the chlorin to enter the retorts through pipe 27 and the waste gases to esca e through pipe 26. .The retorts 9, 8, 7, 6

"wi lthen yield stannic chlorid and the freshly pendent upon the total quantity of chlorin wvliicli'has been introduced beforereversing the flow. V

The ap aratus may be so arranged as to obviate t e necessity for reversing the flow moisture it should be dried, or, preferably,

a part or all of 'the contained moisture should be converted into hydrochloric acid. This is very conveniently ell'ected as follows: The vessels 1 and 10 are intended to contain portions of the residue which remains in the retorts 2-9 after the completionof the distillation. This residue contains a consider able proportion of ferric chlorid, which, upon contact with ,wet chlorin at a suitable temperature, reacts with the contained moisture to produce hydrochloric acid as follows;

X01, 3H,o+ 219601, x01 mo 61-101.

This is advantageous because the reaction is accelerated. by the presence of hydrochloric acid, and also because that portion of the chlorin which would otherwise be lost as ferric chlorid is recovered as stannic chlorid It is, of course, not essential that the vessels 110 for treating the moist chlorin should be grouped with the distilling retorts.

Instead of stoneware. retorts, retorts of lead or of iron lined with lead, or such ves sels as are employed as generators for chlorin by the manganese dioxid method may be used.

It the chlorin bc-substantially undiluted a wide range of temperatures above the vaporizing point of stannic chlorid is applicable;

if, however, the chlorin be diluted with a a "tion pipe introduced into the central aper ture of the retort. The heat developed by the reaction between fresh bodies of tin and chlorin is frequently sufficient to melt the tin, whereby the retortsare endangered: these may be protected byapr -"ing to the interior surface a layer of a Suita. a material such as asbestos aper, cement, etc, indicated at 32 in Fig. 2. n case the retorts are independently heated heat will preferably be applied only is e condensed vapor into presence of tin-bearing rid, which material, substantially as described.

2. The method of producing stannic chlorid,- which consists in subjecting a tin-bear-- ing material to the. action of an excess of chlorinand vaporizing stannic chlorid, condensing stannic chlorid from the vapor, and bringing the uricondense'd. vapor into" resence of tin-bearing material, substantialYy as described. 3. The method of producing'stannic chloconsists in subjecting a tin hearing material to the action of chlorin and vaporizing stannic chlorid, condensing stannic chlorid from the vapor, and bringing the uncondensed vapor into presence oftin-bearmg material at a temperature sufficient to vaporize stannic chlorid, substantially as described.

' 4:. The method of producing stannic chlorid, which consists insubjecting a tin-bearing material to the action of an excess of chlorin and vaporizing stannic chlorid, condensing stannic chlorid from the vapor, and bringing the uncondensed vapor into presence of tin-bearing material ata temperature sufiicient to vaporize stannic chlorid, sub-v stantially as described 5; The method of producing stannic chlorid, which consists in subjecting a tin-bearing material to the action of an excess of chlorin and-vaporizing stannic chlorid, con- (lensing stannic chlorid from the vapor, bringing the uncondensed vapor into presence of tin-bearingmaterial at a'temperaturesuffi- ,absorb'e 6. The method ofproducing stannicchlo-- 171d, which-consists in'subjecting a tin-bearcient to vaporize stannic chlorid, and repeat-- mg the process until the excess of chlorin is substantially as described.

material to the action of chlorin and hydrochloric acid and vaporizing stannic chlorid, condensing stannic chlorid from the vapor, and, bringing the uncondensed vapor' into presence of tin-bearing material, substantially as described.

7. The method'oi producing stannic chlorid, which consists in passing a stream con-'- taining separate bodies of a tin-bearing material, and shifting the point of sup ly of chlorin when the tin in any one of said bodies is substantiallyexhausted, substantially as described.

8. The method of producing stannic chlorid, which consists in alternately passing a stream containing chlorin in contact with separate bodies of a tin-bearing materialand condensing stannic chlorid from said stream, substantially as described.

9. The method of producing stannic chlo rid, which consists in alternately passing a, stream containing chlorin in contact with separate bodies of a tin-bearing material and condensing stannic chloridfrom said stream, and shifting the point of supply of chlorin when the tin in any one of said bodies is substantially exhausted, substantially as described.

10. The method of producing stannic chlcrid which consists in continuously supplying chlorin to a body of metallic tin-bearing ma terial in the presence of anhydrous stannic chlorid.

11. The method of producing stannic chlorid, which consists in reacting on tin-bearing material with chlorin in presence of anhydrous stannic chlorid at a temperature above I the vaporizing point of anhydrous stannic chlorid, maintaining the reaction b supplying chlorin to the reacting mass, an recovering anhydrous stannic chlorid. I

12. Themethod of producing stannic chicrid which consists incontinuously supplying chlorin to a body-of metallic tin-bearing inaterial in the presence of anhydrous stannic chlorid,. and controlling the temperature of the reaction.

In testimonywhereof, I afiix my signature in presence of two Witnesses. CLINTUN, PAUL TOWNSEND. Witnesses:

EUGENE A. Brnnns, JULIA B; HILL.

so chlorin successively in contact with

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