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US3288561A - Chlorination of electrolytic copper refinery slimes in a molten salt bath - Google Patents

Chlorination of electrolytic copper refinery slimes in a molten salt bath Download PDF

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US3288561A
US3288561A US36516464A US3288561A US 3288561 A US3288561 A US 3288561A US 36516464 A US36516464 A US 36516464A US 3288561 A US3288561 A US 3288561A
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slimes
bath
chlorides
electrolytic copper
tellurium
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Mellgren Svante
William R Opie
Lamar D Coffin
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Cyprus Amax Minerals Co
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American Metal Climax Inc
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G30/00—Compounds of antimony
    • C01G30/006—Halides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B19/00—Selenium; Tellurium; Compounds thereof
    • C01B19/005—Halides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G1/00—Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general
    • C01G1/06—Halides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G28/00—Compounds of arsenic
    • C01G28/007—Halides
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B5/00—General methods of reducing to metals
    • C22B5/02—Dry methods smelting of sulfides or formation of mattes
    • C22B5/16—Dry methods smelting of sulfides or formation of mattes with volatilisation or condensation of the metal being produced
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/001—Dry processes
    • C22B7/002—Dry processes by treating with halogens, sulfur or compounds thereof; by carburising, by treating with hydrogen (hydriding)
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • the present invention is directed to a process for treating electrolytic copper refinery slimes.
  • Slimes usually contain gold, silver, platinum group metals, copper, lead, tin, antimony, selenium, tellurium, arsenic, etc., and minor amounts of all other metals dependent upon the source.
  • the present invention contemplates the chlorination of slimes in a molten salt environment at elevated temperatures to convert selenium and tellurium found in the slimes to the respective chlorides and recovering said chlorides as volatile products.
  • Slimes as collected periodically from the copper refinery tanks, are usually screened to remove large particles of metallic copper. They are then usually decopperized as, for example, by subjecting the material to 'an acid leach preliminary to further treatment.
  • the decopperized slimes are added to a molten salt bath and treated with gaseous chlorine, to form the chlorides of selenium and tellurium.
  • the slimes are added to the bath when it is molten or mixed with the salts before they are heated.
  • the bath is preferably agitated to obtain good distribution of slimes and gas.
  • the bath may be mechanically agitated, e.g. by an impeller.
  • the slimes are believed to be in a physical state of suspension in the molten salt bath. Relatively large amounts of slimes may be added to the bath, e.g. 500 grams of slime per 1700 grams of molten salt in the bath.
  • low concentrations of slimes in the bath may be used, it is not an economical utilization of equipment. As the slime concentration in the bath is raised to very high concentrations, the viscosity of the resultant bath is increased.
  • the maximum practicable concentration of slimes in a given bath is that at which the viscosity is increased to the point where effective agitation is difiicult and the resultant distribution of chlorine gas in the melt becomes uneven.
  • Suitable baths include the alkali metal halides and the alkaline earth metal halides with the chlorides being preferred. These are sodium chloride, potassium chloride, lithium chloride, rubidium chloride, cesium chloride, magnesium chloride, calcium chloride, strontium chloride, and barium chloride. Generally those electrolytes having lower melting points are preferred. The low melting mixtures of potassium chloride and sodium chloride are preferred because of their excellent bat-h properties and low cost.
  • the preferred baths are those in which chlorine is at least somewhat soluble.
  • the chlorination process may be carried out at all tem- "ice peratures at which the electrolyte is molten. It is generally preferred that the temperature should not be higher than about 900 C. to prevent vapor losses when low melting salts, e.g., the eutectic mixture of sodium and potassium chloride with a melting point of about 650- 675 C., are used. These vapor losses are undesirable in two respects: The obvious loss of bath salts which must be replaced, and the contamination of the volatile chloride products from which they must be separated. Although it is preferred that the chlorination reaction be carried out between about 750 and 900 C., the reaction may be carried out at temperatures as low as about 350 C.
  • low melting salts e.g., the eutectic mixture of sodium and potassium chloride with a melting point of about 650- 675 C.
  • Baths having relatively low melting points may be obtained by incorporating one or more additional components such as aluminum chloride and the like into the system to effect depression of the melting point. Depression of the melting point of the bath is likewise effected by the accumulation in the bath of soluble chloride salts e.g. of lead, silver etc. during the chlorina tion reaction.
  • the process may be carried out in a continuous manner, the contemplated commercial process based upon the quantity of slimes available for treatment indicates that a batch process should be most economical.
  • chlorine gas is passed through the electrolyte. It is preferably inserted at or near the lower portions of the chamber holding the bath.
  • the total chlorine required varies with the amount of metal value in the slimes susceptible to chlorination. Generally, the use of between about 0.3 pound of chlorine to about 0.7 pound of chlorine per pound of slimes is satisfactory. It is preferred to utilize sufficient chlorine so that the higher chlorides of the metals are formed and go off in the form of the volatile reaction products.
  • a reducing agent during the chlorination process. This may be accomplished by the addition of finely subdivided carbon, e.g. coke breeze, with the slimes in the charge to the reaction chamber. It is more conveniently accomplished by passing carbon monoxide through the reaction chamber simultaneously with the introductionof chlorine gas to the reaction chamber.
  • finely subdivided carbon e.g. coke breeze
  • the reaction chamber is formed from refractory materials, e.g. quartz, and the acid or basic refractories.
  • the cell is closed with exit ports above the molten bath through which the volatile reaction products are withdrawn.
  • Slimes often also contain antimony, arsenic and tin. When slimes containing such metals are treated by the instant process, these metals are largely eliminated from the bath through formation of their volatile chlorides.
  • the volatile chloride products produced during the chlorination are vented from the closed space above the molten bath to and through an aqueous scrubber.
  • a portion of the selenium chloride and the tellurium chloride dissolves in the aqueous solution with the remainder precipitating in the scrubber.
  • Most of the antimony chloride and arsenic chloride go into solution in the scrubber.
  • Successful recovery has been obtained utilizing water, alkaline solutions (e.g. 30% NaOH) and also acid solutions (e.g. 6 N HCl and 20% H 80 in the scrubber.
  • the preferred recovery system consists of passing the volatile products through two water scrubbers in series followed by final cleaning in a sodium hydroxide solution.
  • the volatile chlorides may be separated and recovered after removal from the scrubbing system by separatory techniques, e.g. precipitating the selenium and tellurium separately from a hydrochloric acid solution with additions of S0 washed and the washed solution is combined with the hydrochloric acid solution.
  • the residual slimes from the chlorination'reaction may be separated from the salt bath by dissolving the salts away in aqueous solution.
  • the residue may then be dechlorinated and treated to recover the remaining metal values which include the precious metals.
  • the process described herein is relatively simple and economical.
  • the process also yields a slime residue containing the precious metals which is susceptible to treatment by a novel and economical process.
  • ess comprising the steps of providing a molten salt bath consisting essentially of at least one salt selected fromthe group consisting of alkali metal halides, alkaline earth metal halides, and mixtures thereof and containing said electrolytic copper refinery slimes, passing gaseous chlorine through the molten bath while maintaining said bath at a temperature of from 350 to 900 C. whereby the selenium, tellurium, antimony, arsenic and tin values are converted to volatile chlorides and collectively separating said volatile chorides from the nonvolatile substances.
  • said process comprising the steps of providing a molten salt bath consisting essentially of at least one salt selected from the .group consisting of alkali metal halides, alkaline earth metal halides and mixtures thereof and containing said electrolytic copper refinery slimes, passing gaseous chlorine and carbon monoxide gas concomitantly through the molten bath while maintaining said 'bath at a temperature of from 350 to 900 C. and collectively separating the resulting volatile chlorides from the non-volatile substances.
  • a molten salt bath consisting essentially of at least one salt selected from the .group consisting of alkali metal halides, alkaline earth metal halides and mixtures thereof and containing said electrolytic copper refinery slimes, passing gaseous chlorine and carbon monoxide gas concomitantly through the molten bath while maintaining said 'bath at a temperature of from 350 to 900 C. and collectively separating the resulting volatile chlorides from the non-volatile substances.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Metallurgy (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Geology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Description

United States, Patent CHLORINATIGN 0F ELECTROLYTIC COPPER REFINERY SLIMES IN A MOLTEN SALT BATH Svante Mellgren, Metuchen, William R. Opie, Keyport,
and Lamar D. Catlin, Edison, N.J., assignors to American Metal Climax, Inc., New York, N.Y., a corporation of New York No Drawing. Filed May 5, 1964, Ser. No. 365,164 9 Claims. (Cl. 23-98) The present invention is directed to a process for treating electrolytic copper refinery slimes.
Almost all selenium and tellurium are obtained as a by-product of precious metals recovery from electrolytic copper refinery slimes, often also called anode mud, electrolytic residues, and sludges, which are all meant to be included in the term slimes as used herein. Slimes usually contain gold, silver, platinum group metals, copper, lead, tin, antimony, selenium, tellurium, arsenic, etc., and minor amounts of all other metals dependent upon the source.
It is an object of the present invention to provide an economical process for treating slimes. It is also an object of the present invention to provide a process for recovering selenium and tellurium from slimes. Other objects and advantages of this invention will become apparent from the specification.
The present invention contemplates the chlorination of slimes in a molten salt environment at elevated temperatures to convert selenium and tellurium found in the slimes to the respective chlorides and recovering said chlorides as volatile products.
Slimes, as collected periodically from the copper refinery tanks, are usually screened to remove large particles of metallic copper. They are then usually decopperized as, for example, by subjecting the material to 'an acid leach preliminary to further treatment. In accordance with the present invention, the decopperized slimes are added to a molten salt bath and treated with gaseous chlorine, to form the chlorides of selenium and tellurium.
The slimes are added to the bath when it is molten or mixed with the salts before they are heated. The bath is preferably agitated to obtain good distribution of slimes and gas. The bath may be mechanically agitated, e.g. by an impeller. The slimes are believed to be in a physical state of suspension in the molten salt bath. Relatively large amounts of slimes may be added to the bath, e.g. 500 grams of slime per 1700 grams of molten salt in the bath. Although low concentrations of slimes in the bath may be used, it is not an economical utilization of equipment. As the slime concentration in the bath is raised to very high concentrations, the viscosity of the resultant bath is increased. The maximum practicable concentration of slimes in a given bath is that at which the viscosity is increased to the point where effective agitation is difiicult and the resultant distribution of chlorine gas in the melt becomes uneven. Suitable baths include the alkali metal halides and the alkaline earth metal halides with the chlorides being preferred. These are sodium chloride, potassium chloride, lithium chloride, rubidium chloride, cesium chloride, magnesium chloride, calcium chloride, strontium chloride, and barium chloride. Generally those electrolytes having lower melting points are preferred. The low melting mixtures of potassium chloride and sodium chloride are preferred because of their excellent bat-h properties and low cost. The preferred baths are those in which chlorine is at least somewhat soluble.
The chlorination process may be carried out at all tem- "ice peratures at which the electrolyte is molten. It is generally preferred that the temperature should not be higher than about 900 C. to prevent vapor losses when low melting salts, e.g., the eutectic mixture of sodium and potassium chloride with a melting point of about 650- 675 C., are used. These vapor losses are undesirable in two respects: The obvious loss of bath salts which must be replaced, and the contamination of the volatile chloride products from which they must be separated. Although it is preferred that the chlorination reaction be carried out between about 750 and 900 C., the reaction may be carried out at temperatures as low as about 350 C. Baths having relatively low melting points may be obtained by incorporating one or more additional components such as aluminum chloride and the like into the system to effect depression of the melting point. Depression of the melting point of the bath is likewise effected by the accumulation in the bath of soluble chloride salts e.g. of lead, silver etc. during the chlorina tion reaction.
Although the process may be carried out in a continuous manner, the contemplated commercial process based upon the quantity of slimes available for treatment indicates that a batch process should be most economical. After the addition of the slimes to the molten salt electrolyte, chlorine gas is passed through the electrolyte. It is preferably inserted at or near the lower portions of the chamber holding the bath. The total chlorine required varies with the amount of metal value in the slimes susceptible to chlorination. Generally, the use of between about 0.3 pound of chlorine to about 0.7 pound of chlorine per pound of slimes is satisfactory. It is preferred to utilize sufficient chlorine so that the higher chlorides of the metals are formed and go off in the form of the volatile reaction products.
In the treatment of slimes from certain sources it may be useful to employ a reducing agent during the chlorination process. This may be accomplished by the addition of finely subdivided carbon, e.g. coke breeze, with the slimes in the charge to the reaction chamber. It is more conveniently accomplished by passing carbon monoxide through the reaction chamber simultaneously with the introductionof chlorine gas to the reaction chamber.
The reaction chamber is formed from refractory materials, e.g. quartz, and the acid or basic refractories. The cell is closed with exit ports above the molten bath through which the volatile reaction products are withdrawn.
Slimes often also contain antimony, arsenic and tin. When slimes containing such metals are treated by the instant process, these metals are largely eliminated from the bath through formation of their volatile chlorides.
The invention is illustrated in the examples but is not to 'be construed as limited to the details described therein. The parts and percentages are by weight except where specifically indicated otherwise.
1700 gms. of a mixture of potassium chloride and sodium chloride (the eutectic mixture having a 1:1 molar ratio) was melted in a quartz cylinder 7% inches high and 5 inches in diameter. The heat was applied externally. The temperature of the bath was brought to 750 C. and maintained there. 500 gms. of slimes containing selenium, tellurium, antimony, arsenic, tin, lead and precious metals were added to the bath. The bath Was agitated by rotation of a quartz impeller at the end of a quartz rod which was suspended above the bath. After the addition of the slimes, the bath was still very fluid. Chlorine gas was passed through the bath by means of an input tube which extended through the top surface of the bath almost to the bottom of the crucible. The chlorine gas was added over a period of 2% hours. The
' A similar test was run following the procedure described in the preceding paragraph with the exception that carbon monoxide was added with the chlorine; the proportion of chlorine to carbon monoxide being 5:1 by volume. Similar results were obtained.
Similar results are obtained using other baths and different concentrations of slimes in the bath. Longer reaction time and somewhat higher temperautres, e.g. 900? 0, result in the obtention of better yields of the desired chlorides.
The volatile chloride products produced during the chlorination are vented from the closed space above the molten bath to and through an aqueous scrubber. A portion of the selenium chloride and the tellurium chloride dissolves in the aqueous solution with the remainder precipitating in the scrubber. Most of the antimony chloride and arsenic chloride go into solution in the scrubber. Successful recovery has been obtained utilizing water, alkaline solutions (e.g. 30% NaOH) andalso acid solutions (e.g. 6 N HCl and 20% H 80 in the scrubber. The preferred recovery system consists of passing the volatile products through two water scrubbers in series followed by final cleaning in a sodium hydroxide solution. The volatile chlorides may be separated and recovered after removal from the scrubbing system by separatory techniques, e.g. precipitating the selenium and tellurium separately from a hydrochloric acid solution with additions of S0 washed and the washed solution is combined with the hydrochloric acid solution.
The residual slimes from the chlorination'reaction may be separated from the salt bath by dissolving the salts away in aqueous solution. The residue may then be dechlorinated and treated to recover the remaining metal values which include the precious metals.
The process described herein is relatively simple and economical. The process also yields a slime residue containing the precious metals which is susceptible to treatment by a novel and economical process.
Obviously, many modifications and variations of the invention are possible in the light of the above teachings.
It is therefore to be understood that, within the scope of the appended claims, the invention may be practiced otherwise than as specifically described.
What is claimed is:
1. A process for simultaneously separating selenium and tellurium together with any antimony, arsenic and tin values present in electrolytic copper refinery slimes from other metal values contained in said slimes the chlorides of which are relatively non-volatile at temperatures of up to 900 C. compared to the chorides of selenium, tellurium, antimony, arsenic and tin, said proc- The precipitated material is.
ess comprising the steps of providing a molten salt bath consisting essentially of at least one salt selected fromthe group consisting of alkali metal halides, alkaline earth metal halides, and mixtures thereof and containing said electrolytic copper refinery slimes, passing gaseous chlorine through the molten bath while maintaining said bath at a temperature of from 350 to 900 C. whereby the selenium, tellurium, antimony, arsenic and tin values are converted to volatile chlorides and collectively separating said volatile chorides from the nonvolatile substances.
2. The process of claim 1 wherein aluminum chloride is additionally included in the salt bath to lower the melting point thereof.
3. The process of claim 1 wherein the alkali metal halides and alkaline earth halides are chlorides.
4. The process of claim 1 wherein the bath is agitated during the passage of chlorine therethrough.
5. The process of claim 4 wherein the total amount of chlorine passed through the bath is between 0.3 and 0.7 pound per pound of electrolytic copper refinery slimes in the bath.
6. The process of claim 1 wherein the salt bath consists essentially of the eutectic mixture of potassium chloride and sodium chloride.
7. The process of claim 1 wherein a reducing agent is additionally included in the molten salt bath when passing chlorine therethrough.
8. The process of claim 1 wherein the electrolytic copper refinery slimes are decopperized prior to use in the molten salt bath.
9. A process for simultaneously separating selenium and tellurium together with any antimony, arsenic and tin values present in electrolytic copper refinery slimes from other metal values contained in said slimes the chlorides of which are relatively non-volatile at temperatures of up to 900 C. compared to the chlorides of selenium, tellurium, antimony, arsenic and tin, said process comprising the steps of providing a molten salt bath consisting essentially of at least one salt selected from the .group consisting of alkali metal halides, alkaline earth metal halides and mixtures thereof and containing said electrolytic copper refinery slimes, passing gaseous chlorine and carbon monoxide gas concomitantly through the molten bath while maintaining said 'bath at a temperature of from 350 to 900 C. and collectively separating the resulting volatile chlorides from the non-volatile substances.
References Cited by the Examiner UNITED STATES PATENTS 845,868 3/1907 Fronek 23--1 890,432 6/1908 Masson 2398 X 1,931,944 10/1933 Wood et al 23--98 OTHER REFERENCES I Ser..No. 292,742, Beck et al. (A.P.C.), published July 1943.
MILTQN WEISSMAN, Primary Examiner.
EDWARD STERN, Examiner.

Claims (1)

1. A PROCESS FOR SIMULTANEOUSLY SEPARATING SELENIUM AND TELLURIUM TOGETHER WITH ANY ANTIMONY, ARSENIC AND TIN VALUES PRESENT IN ELECTROLYTIC COPPER REFINERYY SLIMES FROM OTHER METAL VALUES CONTAINED IN SAID SLIMES THE CHLORIDES OF WHICH ARE RELATIVELY NON-VOLATILE AT TEMPERATURES OF UP TO 900*C. COMPARED TO THE CHLORIDES OF SELENIU, TELLURIUM, ANTIMONY, ARSENIC AND TIN, SAID PROCESS COMPRISING THE STEPS OF PROVIDING A MOLTEN SALT BATH CONSISTING ESSENTIALLY OF AT LEAST ONE SALT SELECTED FROM THE GROUP CONSISTING OF ALKALI METAL HALIDES, ALKALINE EARTHP METAL HALIDES AND MIXTURES THEREOF AND CONTAINING SAID ELECTROLYTIC COPPER REFINERY SLIMES, PASSING GASEOUS CHLORINE THROUGH THE MOLTEN BATH WHILE MAINTAINING SAID BATH AT A TEMPERATURE OF FROM 350 TO 900*C. WHEREBY THE SELENIU, TELLURIUM, ANTIMONY, ARSENIC AND TIN VALUES ARE CONVERTED TO VOLATILE CHLORIDES AND COLLECTIVELY SEPARATING SAID VOLATILE CHLORIDES FROM THE NONVOLATILE SUBSTANCES.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3938989A (en) * 1973-07-05 1976-02-17 The International Nickel Company, Inc. Arsenic removal from nickel matte
EP0271845A1 (en) * 1986-12-12 1988-06-22 Mitsubishi Kinzoku Kabushiki Kaisha Process for recovering gallium trichloride from gallium-containing waste
US5362470A (en) * 1991-05-30 1994-11-08 Konica Corporation Ultrafine gold and/or silver chalcogenide and production thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US845868A (en) * 1906-04-06 1907-03-05 Gen Lab Company Process of treating sulfid ores.
US890432A (en) * 1907-08-02 1908-06-09 John Roy Masson Wet process of recovering antimony in a pure state from ores, concentrates, tailings, and slimes containing it.
US1931944A (en) * 1932-06-15 1933-10-24 Wood Louis Albert Extraction of tin from ores

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US845868A (en) * 1906-04-06 1907-03-05 Gen Lab Company Process of treating sulfid ores.
US890432A (en) * 1907-08-02 1908-06-09 John Roy Masson Wet process of recovering antimony in a pure state from ores, concentrates, tailings, and slimes containing it.
US1931944A (en) * 1932-06-15 1933-10-24 Wood Louis Albert Extraction of tin from ores

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3938989A (en) * 1973-07-05 1976-02-17 The International Nickel Company, Inc. Arsenic removal from nickel matte
EP0271845A1 (en) * 1986-12-12 1988-06-22 Mitsubishi Kinzoku Kabushiki Kaisha Process for recovering gallium trichloride from gallium-containing waste
US5362470A (en) * 1991-05-30 1994-11-08 Konica Corporation Ultrafine gold and/or silver chalcogenide and production thereof

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