CA1319826C - Treatment of sulphuric acid solutions containing tellurium, copper sulphate and minor impurity elements - Google Patents
Treatment of sulphuric acid solutions containing tellurium, copper sulphate and minor impurity elementsInfo
- Publication number
- CA1319826C CA1319826C CA000520041A CA520041A CA1319826C CA 1319826 C CA1319826 C CA 1319826C CA 000520041 A CA000520041 A CA 000520041A CA 520041 A CA520041 A CA 520041A CA 1319826 C CA1319826 C CA 1319826C
- Authority
- CA
- Canada
- Prior art keywords
- solution
- copper
- copper sulphate
- tellurium
- sulphuric acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- 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
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0084—Treating solutions
- C22B15/0089—Treating solutions by chemical methods
- C22B15/0091—Treating solutions by chemical methods by cementation
-
- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
-
- 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
- C22B61/00—Obtaining metals not elsewhere provided for in this subclass
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Geochemistry & Mineralogy (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
Abstract of the Disclosure:
A process for the treatment of a sulphuric acid solution containing tellurium, copper sulphate, and minor impurity elements is disclosed. The process comprises the steps of recirculating the sulphuric acid solution between a first tank containing such solution and a second reactor tank containing a bed of copper particles for a time interval sufficient to cement substantially all the tellurium present in the leach liquor as copper telluride, adding oxygen to the first and/or second tank to form a copper sulphate solution during recirculation of the sulphuric acid solution between the first and second tanks, and separating the cemented copper telluride from the copper sulphate solution.
A process for the treatment of a sulphuric acid solution containing tellurium, copper sulphate, and minor impurity elements is disclosed. The process comprises the steps of recirculating the sulphuric acid solution between a first tank containing such solution and a second reactor tank containing a bed of copper particles for a time interval sufficient to cement substantially all the tellurium present in the leach liquor as copper telluride, adding oxygen to the first and/or second tank to form a copper sulphate solution during recirculation of the sulphuric acid solution between the first and second tanks, and separating the cemented copper telluride from the copper sulphate solution.
Description
TREATMENT OF SULPHURIC ACID SOLUTIONS CONTAINING TELLURIUM, COPPER SULPHATE AND MINOR IMPURITY ELEMENTS
This invention relates to tne treatment of sulphuric acid solutions containing tellurium, copper sulphate and minor impurity elements, and more particularly to the treatment of leach liquor originating from the treatment of slimes produced during electrolytic refining of copper.
Canadian Patent No. 1091035 discloses a process for treating slimes from the electrolytic refining of copper wherein the slimes are leached with sulphuric acid under an oxygen partial pressure of up to 50 p8i and at elevated temperature until copper and tellurium in the slimes are substantially dissolved. A liguid-solid separation is then performed to separate the solid leached slimes from the leach liquor and the leach liquor is further treated in a cementation reactor with metallic copper to cement tellurium as copper telluride. The remaining solution is sent to a copper sulphate plant for the production of copper sulphate. In the copper sulphate plant, the leach liquor remaining after removal of tellurium is passed through a bed of copper particles to form a copper sulphate solution which is later crystallized to form CuS04 5H20.
The above process requires two separate beds of copper particles, one for the cementation of tellurium and one for the production of a copper sulphate solution prior to crystalization of copper sulphate.
Applicant has surprisingly found that cementation of the tellurium as copper telluride and production of the copper sulphate solution can be carried out in the same reaction vessel thereby eliminating a lot of eguipment and simplifying the process.
The process, in accordance with the present invention, comprises the steps of recirculating the sulphuric acid solution containing tellurium, copper sulphate and minor impurity elements between a first tank containing the solution and a second reactor tank containing a bed of copper particles for a time interval 6ufficient to cement eubstantially all (i.e. over 95% of) the tellurium present in the sulphuric acid solution as copper telluride, adding oxygen to the first and/or the second tank to form a copper sulphate solution during recirculation of the sulphuric acid solution between the first and second tanks, and separating the cemented copper telluride from the copper sulphate solution.
The process is normally carried out at a temperature higher than 70C, preferably near the boiling point of the sulphuric acid solution and the sulphuric acid content of the solution is preferably between about 100 and 150 g/l at the beginning of the operation. These are known requirements for tellurium cementation.
When the tellurium concentration in the sulphuric 131982~
This invention relates to tne treatment of sulphuric acid solutions containing tellurium, copper sulphate and minor impurity elements, and more particularly to the treatment of leach liquor originating from the treatment of slimes produced during electrolytic refining of copper.
Canadian Patent No. 1091035 discloses a process for treating slimes from the electrolytic refining of copper wherein the slimes are leached with sulphuric acid under an oxygen partial pressure of up to 50 p8i and at elevated temperature until copper and tellurium in the slimes are substantially dissolved. A liguid-solid separation is then performed to separate the solid leached slimes from the leach liquor and the leach liquor is further treated in a cementation reactor with metallic copper to cement tellurium as copper telluride. The remaining solution is sent to a copper sulphate plant for the production of copper sulphate. In the copper sulphate plant, the leach liquor remaining after removal of tellurium is passed through a bed of copper particles to form a copper sulphate solution which is later crystallized to form CuS04 5H20.
The above process requires two separate beds of copper particles, one for the cementation of tellurium and one for the production of a copper sulphate solution prior to crystalization of copper sulphate.
Applicant has surprisingly found that cementation of the tellurium as copper telluride and production of the copper sulphate solution can be carried out in the same reaction vessel thereby eliminating a lot of eguipment and simplifying the process.
The process, in accordance with the present invention, comprises the steps of recirculating the sulphuric acid solution containing tellurium, copper sulphate and minor impurity elements between a first tank containing the solution and a second reactor tank containing a bed of copper particles for a time interval 6ufficient to cement eubstantially all (i.e. over 95% of) the tellurium present in the sulphuric acid solution as copper telluride, adding oxygen to the first and/or the second tank to form a copper sulphate solution during recirculation of the sulphuric acid solution between the first and second tanks, and separating the cemented copper telluride from the copper sulphate solution.
The process is normally carried out at a temperature higher than 70C, preferably near the boiling point of the sulphuric acid solution and the sulphuric acid content of the solution is preferably between about 100 and 150 g/l at the beginning of the operation. These are known requirements for tellurium cementation.
When the tellurium concentration in the sulphuric 131982~
acid solution is hlgh, it i8 preferable to recirculate the solution until the tellurium content falls below about 2.0 g/l before adding oxygen to form the copper sulphate solution.
The invention will now be disclosed, by way of example, with reference to the accompanying drawings and examples. In the drawings, Figure 1 is a flow diagram of the treatment process in accordance with the present invention; and Figure 2 is a diagram illustrating the concentration of tellurium in solution versus reaction time.
Referring to Figure 1, there is shown a flow diagram of the process in accordance with the present lS invention. The sulphuric acid solution containing tellurium, copper sulphate and minor impurity elements, hereinafter called leach liguor, which is stored in a container 10 is introduced into a first tank 12. The liquor in the tank is agitated by a stirrer 14 and recirculated several times by a pump 16 between the first tank 12 and a second reactor tank 18 filled with copper particles for a period of time sufficient to cement substantially all the tellurium present in solution as copper telluride. The preferred reactor tank is made as described in Canadian application no. 439,206 filed October 18, 1985. Applicant has surprisingly found that the copper telluride cement did not firmly adhere to the 13~9~26 copper particles but was immediately released upon formation and remained in suspension in the solution. The size of the tanks and the flow rate of the leach liguor is preferably such that the retention time of the liquor in the first tank is about two minutes and in the 6econd reactor tank about 0.5 minute. Air is introduced in the first tank or the second tank or both to oxidize the remaining leach liquor to form a copper sulphate solution.
The so-produced copper sulphate solution containing the copper telluride cement is then passed through a filter press 20 to separate the cemented copper telluride from the copper sulphate solution.
Various tests were made to determine:
1) The compatibility of the simultaneous treatment of the leach liquor for the removal of tellurium and for the production of a copper sulphate solution in the same bed of copper particles.
2) The degree of precipitation of copper telluride.
3) The efficiency of production of copper sulphate solution.
It was surprisingly found that the precipitation of copper telluride did not affect the circulation of the leach liquor or the formation of the copper sulphate solution. Generally, the flow of solution remained constant during recirculation and gradually decreased at 13198~6 the end as the specific gravity of the copper sulphate solution approached 1.4, as it normally happens when treating a leach liquor from which tellurium has been previously removed. The pressure at the base of the tank 18 remained normal. No pumping problems were encountered during transfer of the solution between the first and the second tanks. There was no blocking of the reaction vessel during the continued production of copper telluride and of copper sulphate solutlon which i8 believed to be due to the fact that the copper telluride cement did not adhere to the copper particles but was immediate~y released upon cementation and remained in suspension in the copper sulphate solution while said solution was circulated in the two tanks.
The results of the tests carried out to determine the degree of precipitation of copper telluride are shown in the following Table I and Figure 2.
U ~ . _ N
æ o % ~ ~
O O ~ O O O
. z ~ O O O O O
~u _ c, -- O _ ~N N
I,U ~ N N ~ N N
~-- y ~;;; ~ O ~ I~ ~ o U ~ ' ~ t~ O.
~ ~ -- N O O~ In O O~
$~ æ æ æ æ æ
Z "~
~n~ ______ ~ <I ~ ~ ~ N 58 ,~
~oU~ _____--U ~y ~ o o U~ o o o ~ O t-- ~ N O~ N
l_ .
V O _ N ~ ~ U~
~3~9826 Table I and Figure 2 lllustrate that more than 96.5% of the tellurium was precipitated in the first two tests. The tellurium concentration at the beginning of the first two tests was 0.44 and 1.44 g/l respectively and after 4 hours, was reduced to 0.01 and 0.05 g/l, respectively, as shown in Figure 2. However, in the third test, wherein the tellurium concentration was higher at the beginning of the test ~2.4 g/l), the tellurium concentration was only reduced to 1.5 g/l within the total reaction time.
The results of the third test indicated that for a relatively high initial tellurium concentration (e.g. ~ than 2 g/l), precipitation of copper telluride was incomplete within the time period normally required for the formation of the copper sulphate solution.
In tests 4 and 6, oxygen addition was delayed by 2 and 4 hours, respectively. The initial tellurium concentration was 2.56 and 1.70 g/l, respectively, and after 2 and 3 hours, respectively, was reduced to 0.05 g/l.
For comparison purposes, it may be seen that in test 5 wherein oxygen was added from the beginning, it took five hours to reduce a tellurium concentration of 1.79 g/l whereas the same reduction in test 6 was achieved after only three hours. From the above results, it appears that, for high tellurium concentrations, it is preferable to delay the addition of oxygen required for the formation of the copper sulphate solution until the tellurium 1319~2g concentration in solution i8 lower than 2 g/l in order to be able to reduce the tellurium concentration in the solution to less than 0.05 g/l within the time period normally required for the formation of the copper sulphate solution.
As shown in Table I, the temperature of the leaeh liquor during the reaction should be highsr than 70-C, preferably close to the boiling point of the solution.
Steam addition into tank 12 i~ thus required to heat the solution. The free acid eoneentration should also be higher than about 100 g/l but lower than 150 g/l at the beginning of the reaction. Sulphuric acid addition into the tank 12 may be required to ad~ust the H2S04 concentration.
When comparing ths effieiency of production of the eopper sulphate solution, using the process in aceordance with the invention wherein tellurium is eoneurrently removed with the produetion of the eopper sulphate solution, with that obtained when using a leaeh liquor from which tellurium had been previously removed, it was found that the percentages of copper dissolution and oxygen utilization were about the same. Efficieneies higher than 90% for Cu and about 60% for 2 respeetively, were obtained. The two concurrent reactions taking plaee in accordance with this invention are:
Te(OH)6 + 5Cu- + 3H2S04 ~ Cu2Te + 3CuS04 + 6H20 (1) 131982~
_9_ Cu + ~2 + H2S4 ~ CuS04 + H20 (2) Although reaction (1) produces some copper sulphate, the ma;or portion of the copper sulphate solution is produced by reaction (2). The reaction times during simultaneous precipitation of copper telluride and production of copper sulphate solution were between 7 and 12 hours which is about the same as during th- production of copper sulphate solution from a leach llquor from which tellurium had been previously removed.
The invention will now be disclosed, by way of example, with reference to the accompanying drawings and examples. In the drawings, Figure 1 is a flow diagram of the treatment process in accordance with the present invention; and Figure 2 is a diagram illustrating the concentration of tellurium in solution versus reaction time.
Referring to Figure 1, there is shown a flow diagram of the process in accordance with the present lS invention. The sulphuric acid solution containing tellurium, copper sulphate and minor impurity elements, hereinafter called leach liguor, which is stored in a container 10 is introduced into a first tank 12. The liquor in the tank is agitated by a stirrer 14 and recirculated several times by a pump 16 between the first tank 12 and a second reactor tank 18 filled with copper particles for a period of time sufficient to cement substantially all the tellurium present in solution as copper telluride. The preferred reactor tank is made as described in Canadian application no. 439,206 filed October 18, 1985. Applicant has surprisingly found that the copper telluride cement did not firmly adhere to the 13~9~26 copper particles but was immediately released upon formation and remained in suspension in the solution. The size of the tanks and the flow rate of the leach liguor is preferably such that the retention time of the liquor in the first tank is about two minutes and in the 6econd reactor tank about 0.5 minute. Air is introduced in the first tank or the second tank or both to oxidize the remaining leach liquor to form a copper sulphate solution.
The so-produced copper sulphate solution containing the copper telluride cement is then passed through a filter press 20 to separate the cemented copper telluride from the copper sulphate solution.
Various tests were made to determine:
1) The compatibility of the simultaneous treatment of the leach liquor for the removal of tellurium and for the production of a copper sulphate solution in the same bed of copper particles.
2) The degree of precipitation of copper telluride.
3) The efficiency of production of copper sulphate solution.
It was surprisingly found that the precipitation of copper telluride did not affect the circulation of the leach liquor or the formation of the copper sulphate solution. Generally, the flow of solution remained constant during recirculation and gradually decreased at 13198~6 the end as the specific gravity of the copper sulphate solution approached 1.4, as it normally happens when treating a leach liquor from which tellurium has been previously removed. The pressure at the base of the tank 18 remained normal. No pumping problems were encountered during transfer of the solution between the first and the second tanks. There was no blocking of the reaction vessel during the continued production of copper telluride and of copper sulphate solutlon which i8 believed to be due to the fact that the copper telluride cement did not adhere to the copper particles but was immediate~y released upon cementation and remained in suspension in the copper sulphate solution while said solution was circulated in the two tanks.
The results of the tests carried out to determine the degree of precipitation of copper telluride are shown in the following Table I and Figure 2.
U ~ . _ N
æ o % ~ ~
O O ~ O O O
. z ~ O O O O O
~u _ c, -- O _ ~N N
I,U ~ N N ~ N N
~-- y ~;;; ~ O ~ I~ ~ o U ~ ' ~ t~ O.
~ ~ -- N O O~ In O O~
$~ æ æ æ æ æ
Z "~
~n~ ______ ~ <I ~ ~ ~ N 58 ,~
~oU~ _____--U ~y ~ o o U~ o o o ~ O t-- ~ N O~ N
l_ .
V O _ N ~ ~ U~
~3~9826 Table I and Figure 2 lllustrate that more than 96.5% of the tellurium was precipitated in the first two tests. The tellurium concentration at the beginning of the first two tests was 0.44 and 1.44 g/l respectively and after 4 hours, was reduced to 0.01 and 0.05 g/l, respectively, as shown in Figure 2. However, in the third test, wherein the tellurium concentration was higher at the beginning of the test ~2.4 g/l), the tellurium concentration was only reduced to 1.5 g/l within the total reaction time.
The results of the third test indicated that for a relatively high initial tellurium concentration (e.g. ~ than 2 g/l), precipitation of copper telluride was incomplete within the time period normally required for the formation of the copper sulphate solution.
In tests 4 and 6, oxygen addition was delayed by 2 and 4 hours, respectively. The initial tellurium concentration was 2.56 and 1.70 g/l, respectively, and after 2 and 3 hours, respectively, was reduced to 0.05 g/l.
For comparison purposes, it may be seen that in test 5 wherein oxygen was added from the beginning, it took five hours to reduce a tellurium concentration of 1.79 g/l whereas the same reduction in test 6 was achieved after only three hours. From the above results, it appears that, for high tellurium concentrations, it is preferable to delay the addition of oxygen required for the formation of the copper sulphate solution until the tellurium 1319~2g concentration in solution i8 lower than 2 g/l in order to be able to reduce the tellurium concentration in the solution to less than 0.05 g/l within the time period normally required for the formation of the copper sulphate solution.
As shown in Table I, the temperature of the leaeh liquor during the reaction should be highsr than 70-C, preferably close to the boiling point of the solution.
Steam addition into tank 12 i~ thus required to heat the solution. The free acid eoneentration should also be higher than about 100 g/l but lower than 150 g/l at the beginning of the reaction. Sulphuric acid addition into the tank 12 may be required to ad~ust the H2S04 concentration.
When comparing ths effieiency of production of the eopper sulphate solution, using the process in aceordance with the invention wherein tellurium is eoneurrently removed with the produetion of the eopper sulphate solution, with that obtained when using a leaeh liquor from which tellurium had been previously removed, it was found that the percentages of copper dissolution and oxygen utilization were about the same. Efficieneies higher than 90% for Cu and about 60% for 2 respeetively, were obtained. The two concurrent reactions taking plaee in accordance with this invention are:
Te(OH)6 + 5Cu- + 3H2S04 ~ Cu2Te + 3CuS04 + 6H20 (1) 131982~
_9_ Cu + ~2 + H2S4 ~ CuS04 + H20 (2) Although reaction (1) produces some copper sulphate, the ma;or portion of the copper sulphate solution is produced by reaction (2). The reaction times during simultaneous precipitation of copper telluride and production of copper sulphate solution were between 7 and 12 hours which is about the same as during th- production of copper sulphate solution from a leach llquor from which tellurium had been previously removed.
Claims (5)
1. Process for the treatment of a sulphuric acid solution containing tellurium, copper sulphate, and minor impurity elements comprising the steps of:
a) recirculating the solution between a first tank containing said solution and a second reactor tank containing a bed of copper particles for a time interval sufficient to cement substantially all the tellurium present in the leach liquor as copper telluride:
b) adding oxygen to said first and/or second tank to form a copper sulphate solution during recirculation of said sulphuric acid solution between said first and second tanks; and c) separating the cemented copper telluride from the copper sulphate solution.
a) recirculating the solution between a first tank containing said solution and a second reactor tank containing a bed of copper particles for a time interval sufficient to cement substantially all the tellurium present in the leach liquor as copper telluride:
b) adding oxygen to said first and/or second tank to form a copper sulphate solution during recirculation of said sulphuric acid solution between said first and second tanks; and c) separating the cemented copper telluride from the copper sulphate solution.
2. Process as defined in claim 1, wherein the solution is maintained at a temperature higher than 70-C.
3. Process as defined in claim 2, wherein the temperature is maintained near the boiling point of the solution.
4. Process as defined in claim 1, wherein the acidity of the solution is between 100 and 150 g/l at the beginning of the operation.
5. Process as defined in claim 1, wherein the solution is recirculated for a predetermined time period before oxygen addition is initiated to reduce the concentration of tellurium in the solution to less than 2.0 g/l before starting the formation of the copper sulphate solution in the reactor tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA000520041A CA1319826C (en) | 1986-10-07 | 1986-10-07 | Treatment of sulphuric acid solutions containing tellurium, copper sulphate and minor impurity elements |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA000520041A CA1319826C (en) | 1986-10-07 | 1986-10-07 | Treatment of sulphuric acid solutions containing tellurium, copper sulphate and minor impurity elements |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1319826C true CA1319826C (en) | 1993-07-06 |
Family
ID=4134111
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA000520041A Expired - Fee Related CA1319826C (en) | 1986-10-07 | 1986-10-07 | Treatment of sulphuric acid solutions containing tellurium, copper sulphate and minor impurity elements |
Country Status (1)
| Country | Link |
|---|---|
| CA (1) | CA1319826C (en) |
-
1986
- 1986-10-07 CA CA000520041A patent/CA1319826C/en not_active Expired - Fee Related
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