- No Drawing.
Patented Dec. 16, 1939 UNITED STATES PATENT OFFICE HANSON MONROE, OF PAINESVILLE, OHIO, ASSIGNOR, BY MESNE ASSIGNMENTS, TO THE GRASSELLI CHEMICAL COMPANY, OIE CLEVELAND, OHIO, A. CORPORATION or. DELAWARE- PBOCESS OF PRODUCING METALLIC CfkDMIUM FROM CADMIUM-CONTAINING MATERIAL This invention relates to a processwhereby -metallic cadmium is recoveredin a high both, associated with. other substances, and
the process consists substantially in submitting such material to a caustic fusion under reducing conditions. i I Materials of this kind are obtainedinvarious metallurgical processesfor the treatment of zinc and cadmium ores, and the process; I criticalbutit isusually preferable to use at least fi've molecular proportions of NaOH figured on the zinc content of the material.
of the present invention allows of an economical and efficient working up of same.
Flue dusts of high cadmium content as produced in smelting, refining, or distilling zinc and cadmium bearing materials, are one type of industrial by-products which are well suited for the recovery of .cadmium therefrom by my novel process. They are usually highly oxidized and contain, besides metallic cadmium and cadmium oxide, zinc, arsenic, lead, and other metals.
Cadmium sponge is another material from which it has been diflicult to recover directly metallic cadmium in reasonably pure form. It is produced by suspending zinc slabs in a solution of crude zinc salts containing cadmium. The precipitated cadmium sponge is usually heavily contaminated with other metals, and contains, in addition, substantial amounts of zinc originating-partly at.
least from the suspended zinc 'slabs which disintegrate during their dissolution- Such cadmium sponge, when submitted to my novel reducing caustic fusion, will also yield metallic cadmium containing only small amounts of impurities.
- Other similar zinc and cadmium containing materials can be similarly treatedby my process with recovery of metallic cadmium.
My novel process comprises mixing the usually powdered cadmium and zinc bearing material with a ground caustic alkali and a ground carbonaceous fuel material, and heating this mixture slowly to a temperature around 400 to 500 C. The cadmium separates in molten-form whereas the impurie ties dissolve in the molten caustic. The cadmium can be separated directly as such from the slag. It is also possible to leach the soalkali.
Application filed ma 18, 1928. Serial No. 278,912.
lidified melt with water,'and in this manner separate the cadmium metal from the other impurities which will be found associated with the caustic alkali. For economical reasons I prefer to use caustic soda as the I, further found that the addition of a borate to fusions' high in zinc content will materially assist in the separation of this zinc from thehadmium.
The amount of-caustic soda used is not very As the reducing agent I prefer to use a carbonaceous material of low ash'content, as, for
instance, petroleum coke. The amount added should be suflicient to completely reduce such cadmium oxide as may be present in the materials Theaction of the carbonaceous agent does not seem to be limited to the reduction of the oxides present, but has other beneficial eifects inasmuch as I found the recovered cadmium to be of higher purity than can be obtained by a mere caustic fusion and with a practically quantitative yield.
The following examples are given to illustrate my novel process; the parts given therein are by weight, and it is understood that my invention is not limited to the particular materials, nor to the specific reacting conditions, mentioned in these examples.
(1) My novel process was applied to a roasted cadmium residue preparing as a yellow powder and containing:
Per cent Cadmium 45. 72 Zinc 16.00 Arsenic 21.26 Iron ..42 Lead .88 Total sulfur 1.85 Copper Traces One part of this residue was mixed with 2 parts ground caustic soda and 1 part ground coke, and slowly heated to about 420 C. Metallic cadmium collected at the bottom of the crucible and was drawn off. A practicallyquantitative yield of a cadmium of over 98% purity was obtained.
(2) In this example an unroasted, black cadmium residue in powder form, was used. It contained:
Percent Cadmium 47. 01 Zinc 13.05 Arsenic 23. 36' Iron 82 Lead 82 Total sulfur c 1.78 Copper Traces This was submitted to the same fusion as in Example 1. Again a practically quantitative yield of metallic cadmium of .a purity above 98% was obtained.
(3) The cadmium sponge used in this example contained:
Per cent Cadmium 65. 8 Zinc 8. 5 Lead .56
Per cent Cadmium 96. 6 Zinc 1.15 Lead 5 (4) Twenty-five parts of the same cadmium sponge as used in Example 3 were mixed with 5 parts 200 mesh petroleum coke and 30 parts of a mixed fiuxing agent consisting of 90% caustic soda and 10% borax. The
) mixture was slowly heated to about 450 to 500 C., at which temperature the slag be came sufficiently fluid. The metal was drawn olf and an excellent recovery of cadmium was obtained which analyzed;
' Per cent Cadmium 99.09 Lead .92 Zinc 02 The addition of borax in this example materially improved the separation of the zinc.
(5) This fusion was made similar to that of Example 4, using a mixed caustic soda and bor'ax flux, with the exception of adding more caustic soda toward the end so as to improve the fluidity of the slag. The recovered metal analyzed:
Per cent Cadmium 98.86 Lead .95 05 Zinc I Lead smelting, refining, ordistillin (6) Another, purer, cadmium sponge was used in this example. It contained:
Per cent Cadmium 51. Lead .05 Zinc 1.02 This was mixed with part ground coke and part caustic soda; heated until the slag became plastic and kept at this temperature for about hour part of caustic soda was then added and heated until the slag became well fluid; separation was then effected, and a high yield of metallic cadmium was recovered which anal zed y Per cent Cadmium 99. 4
. 06 Zinc Traces I claim:
1. The process of recovering metallic cadmium from zinc and cadmium bearing material, which comprises submitting said material to the action of a molten caustic alkali in the presence of a carbonaceous reducing agent.
2. The process of recovering metallic cadmium from zinc and cadmium bearing material, which comprises mixing said material with a caustic alkali and a ground carbonaceous material, heating until a liquid melt is obtained, and separating the metal from the slag.
3. The process of recovering metallic cadmium from zinc and cadmium bearing material, which comprises mixing said material with caustic soda and apowdered carbonaceous fuel, heating to a temperature above 4100" C., and separating the metal from the s a f The process of reoovering metallic cadmium from a cadmium containing material obtained in metallurgical processes for the of zinc and cadmium, which comprises mixing said material with a caustic alkali and a powerful carbonaceous fuel, heating to effect fusion, and separating the metal from the slag.
5. The process of recovering metallic cadmium from a cadmium bearing material ob- .115 tained in metallurgical processes for the treatment of cadmium and zinc ores, which comprises submitting said material to the action of a molten caustic alkali in the presence of a carbonaceous reducing agent.
6. The process of recovering metallic cadmium from a cadmium containing material obtained in metallurgical processes for the smelting, refining, or distilling of zinc and cadmium, which comprises mixing said material with caustic soda and powdered petroleum coke and heating to a temperature between 400 and 500 C.
7 The process of recovering metallic cadmium from a cadmium containing material 130 obtained in metallurgical processes for the smelting, refining, or distilling of zinc and cadmium, which comprises fusing said material with a flux comprising caustic alkali and an alkali metal borate, and a powdered carbonaceous fuel.
8. 'Theprocess of recovering metallic cadmium from a cadmium containing material obtained in metallurgical processes for the smelting, refining, or distillingiof zinc and cadmium, which comprises mlxing said material with caustic soda, borax and powdered coke, heating to about 400 to 500 (1., and separating the metallic cadmium from the slag.
9. The process of recovering metallic cadmium from cadmium sponge, which comprises fusing the sponge with caustic soda and powdered carbonaceous fuel, and separating the metallic cadmium from the slag.
In testimony 'whereof, I afiix my signature.
HANSON H. MONROE.