CN111286607A - Production method for extracting cobalt from copper extraction tail liquid - Google Patents
Production method for extracting cobalt from copper extraction tail liquid Download PDFInfo
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- CN111286607A CN111286607A CN202010179117.6A CN202010179117A CN111286607A CN 111286607 A CN111286607 A CN 111286607A CN 202010179117 A CN202010179117 A CN 202010179117A CN 111286607 A CN111286607 A CN 111286607A
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- 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
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
- C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
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- 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
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
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- 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
- C22B3/02—Apparatus therefor
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Abstract
The invention discloses a production method for extracting cobalt from copper extraction tail liquid, which adopts a continuous fluid separation system filled with chelating resin to realize the extraction of cobalt through continuous fluid separation. By adopting the technical scheme, the invention has the beneficial effects that: the method replaces the steps of adding a precipitator, an extracting agent and the like to precipitate cobalt in the traditional production method, reduces the production cost, simplifies the production method, shortens the production period, increases the total yield, and improves the efficiency and the effect of purifying cobalt in the cobalt ore production.
Description
Technical Field
The invention relates to the technical field of product fluid separation, in particular to a production method for extracting cobalt from copper extraction tail liquid.
Background
The symbol Co of the cobalt element and the silver-white ferromagnetic metal are silver white and light pink on the surface, are positioned in 4 th period and VIII group in the periodic table, have the atomic number of 27 and the atomic weight of 58.9332, are closely arranged hexagonal crystals, and have the common valence of +2 and + 3. Cobalt is a shiny, steel grey metal, relatively hard and brittle, ferromagnetic, and disappears magnetically when heated to 1150 ℃. The valency of cobalt is +2 and + 3. It is stable in humid air and does not react with water at normal temperature. When heated to 300 ℃ or higher in air, CoO is generated by oxidation, and when the furnace is in white heat, Co3O4 is generated by combustion. The fine metal cobalt powder prepared by the hydrogen reduction method can spontaneously generate cobalt oxide in the air.
Cobalt is an important raw material for producing heat-resistant alloy, hard alloy, anticorrosive alloy, magnetic alloy and various cobalt salts. The types of cobalt ores are mainly: copper-cobalt ores, nickel-copper-cobalt sulfide ores, laterite-nickel-cobalt ores and other types; the purification process of cobalt mainly comprises a cobalt precipitation process, the cobalt precipitation process is complex, the purity of a cobalt hydroxide product is low, the activity of magnesium oxide influences the cobalt precipitation rate, the energy consumption for treating magnesium salts and drying the cobalt hydroxide is high, the separation and purification process of crude cobalt hydroxide is complex, a large amount of wastewater is generated by the cobalt precipitation process, the environmental protection pressure is high, and the resource utilization rate is low.
Disclosure of Invention
Aiming at the problems, the invention aims to provide a production method for extracting cobalt from copper extraction tail liquid, which reduces the environmental protection pressure, improves the resource utilization rate, has high automation degree and stable product purity and yield.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a production method for extracting cobalt from copper extraction tail liquid adopts a continuous fluid separation system filled with chelating resin, and realizes the extraction of cobalt through continuous fluid separation.
Furthermore, the continuous fluid separation system is divided into a first separation area and a second separation area, the separation units of the first separation area are respectively filled with inlet chelate resins, and the separation units of the second separation area are respectively filled with domestic chelate resins. And (3) carrying out heavy metal exchange adsorption removal on the copper extraction tail liquid through a first separation zone, and finishing exchange enrichment of cobalt elements through a second separation zone to obtain a high-purity cobalt product.
Further, the continuous fluid separation system is divided into:
a product adsorption zone: including 5 the separator element of first separation zone and 5 the separator element of second separation zone, adopt forward series connection feeding mode, pending feed liquid passes through five separator element of first separation zone in proper order earlier, and effluent liquid returns the head tank after passing through five separator element of second separation zone in proper order again.
A water material ejection area: the device comprises 1 separation unit of a first separation area and 1 separation unit of a second separation area, and the discharged liquid returns to a raw material tank by adopting a mode of feeding pure water in the forward direction.
A gas pressing area: the device comprises 1 separation unit of a first separation area and 1 separation unit of a second separation area, and pure water in the separation units is removed in a forward air inlet mode.
A dilute acid resolving area: including 2 the separator unit of first separator region and 2 the separator unit of second separator region, adopt forward series connection feeding mode, utilize the dilute acid in the intermediate tank as the feed liquid, the play feed liquid that 2 the separator unit of first separator region produced returns the head tank, the play feed liquid that 2 the separator unit of second separator region produced gets into the product jar.
Acid resolution zone: the device comprises 1 separation unit of a first separation area and 1 separation unit of a second separation area, wherein a forward feeding mode is adopted, feeding liquid is 10% sulfuric acid, and discharging liquid enters an intermediate tank.
A water washing area: the device comprises 3 separation units of a first separation area and 3 separation units of a second separation area, wherein a forward series feeding mode is adopted, feeding liquid is pure water, and discharging liquid enters an intermediate tank.
Further, in order to ensure the process operation flexibility, the continuous fluid separation system further comprises a spare area, wherein the spare area comprises one or more separation units of the first separation area and one or more separation units of the second separation area.
Furthermore, the product adsorption area, the water top material area, the air pressure material area, the dilute acid analysis area, the water washing area and the spare part area are sequentially arranged along the circumferential direction.
Wherein the feed rate to the product adsorption zone is from 12 to 18 mL/min.
Wherein the feeding speeds of the water top material area and the water washing area are both 28-35 mL/min.
Wherein the feeding speed of the dilute acid analysis zone and the acid analysis zone is 40-50 mL/min.
Preferably, the imported chelating resin is Dusheng CH-90, and the domestic chelating resin is D463.
Further, in the continuous fluid separation system, the filling amount of each separation unit is 300-500 ml.
The invention has the following beneficial effects:
(1) the process is simplified, the cost is reduced, the production period is shortened, the yield is improved, and the yield can be improved by 10 percent through verification.
(2) The continuous fluid separation technology has the following advantages:
1) due to continuous operation, the product components and concentration are kept stable, and the matching of a downstream working section is facilitated.
2) Because of continuous production, the transfer tank and the matching are very small, the equipment is compact, the transfer tank is easy to be installed at any position and is easy to be matched with the old production process and equipment, and the occupied area is only about 10 percent of the same scale.
3) Compared with the traditional cobalt precipitation process, the method saves a large amount of occupied land and a large amount of extracting agents and chemicals.
4) At the same time, substances having different properties can be removed or separated, so that a complicated process can be simplified.
5) The rotating speed can be automatically adjusted along with the change of the mass and the flow of the inflow fluid according to the requirements of the production process; thus ensuring an economically optimum operation.
6) The flow direction of the fluid can be connected in a counter-flow or co-flow manner according to the convenience of the production process.
7) Due to the adoption of a plurality of separation units, the production method flow can be flexibly changed.
Drawings
FIG. 1 is a schematic view of a continuous fluid separation system of the present invention.
Detailed Description
The invention is further described with reference to the following drawings and detailed description.
The invention aims to provide an improved cobalt extraction production method based on an advanced separation method of a continuous fluid separation device aiming at the defects of complicated steps, low yield, high cost, large wastewater quantity and the like of the conventional production method for extracting cobalt from copper-cobalt ores, so as to achieve the purposes of reducing the production cost, simplifying the production method, shortening the production period and improving the total yield.
The technical scheme of the invention is as follows: the advanced separation method of the continuous fluid separation device is adopted, and the functions of adding an extracting agent and the like in the traditional method are replaced. The design improvement production method comprises the following processes: cobalt-containing raw material solution, a raw material tank, a continuous fluid separation device, a product and a downstream working section. The method is characterized in that crude cobalt hydroxide passes through a separation unit in a continuous fluid separation device filled with chelating resin. In a unit in the continuous fluid separation device, other impurity elements such as copper, nickel, manganese and the like are exchanged and adsorbed in odd-numbered resin columns, the effluent is feed liquid with the purity of the cobalt element reaching more than 99%, the feed liquid containing the cobalt passes through the even-numbered resin columns to complete the exchange and enrichment of the cobalt element, the exchanged resin enters a regeneration zone along with the rotation of the system and is regenerated and activated by sulfuric acid in the regeneration zone, and thus the transformed resin enters the exchange zone again to continuously produce high-purity cobalt products.
The continuous fluid separation device technology used in the method realizes the steps of exchange, water washing, regeneration and the like according to the time lapse in the traditional production in a continuous production method, continuously feeds materials and continuously discharges products, and completely renovates the traditional fixed bed technology. In the invention, a plurality of intermediate links in the traditional production method are also saved. Within the continuous separation process: washing water, chemical reagents and the like are recycled in the system, and a large intermediate tank of the traditional fixed bed method, namely batch application is not needed. Simultaneously, due to the continuous operation of the continuous fluid separation device and the sequential switching of the fluid distribution valves, each separation unit can pump liquids of different media such as: raw materials, water, different chemical reagents, etc.
As shown in figure 1, the continuous fluid separation device independently developed by the company is adopted, imported chelate resin is adopted for odd-numbered resin columns, the model of the imported chelate resin is Dusheng CH-90, the imported chelate resin has a strong adsorption effect on heavy metals such as copper, nickel and manganese in feed liquid, domestic chelate resin is adopted for even-numbered resin columns, the model of the domestic chelate resin is D463, the adsorption capacity of the domestic chelate resin on cobalt is stronger than that of other metal elements, the adsorption capacity is used for enrichment adsorption of the cobalt element, the design treatment capacity is 0.9L/H, and the filling amount of each resin is 400ml according to the characteristics of the resin. The following segmentation zones are divided:
(1) and in the product adsorption zones (17-29 and 18-24), after the raw material liquid enters a 17-29 unit, impurity elements in the raw material liquid are adsorbed, the outlet liquid (rich in cobalt elements) of the 29 unit enters a 18-24 unit again for adsorption and enrichment of the cobalt elements, and the feeding speed of the feed liquid is 15ml/min in a forward feeding mode.
(2) And a water washing area (unit 15/16) adopts a single-string positive feeding mode, the feed liquid at the outlet of the water washing area returns to the raw material tank, and the water washing flow rate is 30 ml/min.
(3) Pneumatic water zone (13/14 cell): air is adopted to remove pure water in the resin column in a pressing mode, and the purpose is to improve the product concentration of a subsequent resolving area.
(4) Resolving regions (7-9, 8-12): adopting 10% sulfuric acid to carry out resolution, mixing with the former stage water washing acid, and then entering a subsequent dilute acid resolution area, wherein the resolution speed is 45 ml/min.
(5) The water wash zone (1-3 units) washes the acid remaining in the resin tank and returns directly to the regeneration zone intermediate tank at a feed rate of 30 ml/min.
In the production method, the continuous fluid separation device technology replaces the functions of the traditional cobalt precipitation process and other steps, and compared with the prior art, the product yield and purity are as follows:
the acid consumption is saved by 20%;
the product yield is improved by 10 percent;
the purity of the product is improved by 20 percent.
While the invention has been particularly shown and described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A production method for extracting cobalt from copper extraction tail liquid is characterized in that: cobalt extraction was achieved by continuous fluid separation using a continuous fluid separation system filled with chelating resin.
2. The production method for extracting cobalt from the copper extraction tail liquid as claimed in claim 1, characterized in that: the continuous fluid separation system is divided into a first separation area and a second separation area, the separation units of the first separation area are respectively filled with imported chelate resin, the separation units of the second separation area are respectively filled with domestic chelate resin, copper extraction tail liquid is firstly subjected to heavy metal exchange adsorption removal through the first separation area, and then the exchange enrichment of cobalt element is completed through the second separation area to obtain a high-purity cobalt product.
3. The production method for extracting cobalt from the copper extraction tail liquid as claimed in claim 2, characterized in that: the continuous fluid separation system comprises:
a product adsorption zone: the device comprises 5 separation units of a first separation area and 5 separation units of a second separation area, and adopts a forward series feeding mode, feed liquid to be treated sequentially passes through five separation units of the first separation area, and effluent liquid sequentially passes through five separation units of the second separation area and then returns to a raw material tank;
a water material ejection area: the device comprises 1 separation unit of a first separation area and 1 separation unit of a second separation area, and the discharged liquid returns to a raw material tank in a mode of feeding pure water in the forward direction;
a gas pressing area: the device comprises 1 separation unit of a first separation area and 1 separation unit of a second separation area, and pure water in the separation units is removed in a forward air inlet mode;
a dilute acid resolving area: the device comprises 2 separation units of a first separation area and 2 separation units of a second separation area, wherein a forward series feeding mode is adopted, dilute acid in an intermediate tank is used as feeding liquid, discharging liquid generated by the 2 separation units of the first separation area returns to a raw material tank, and discharging liquid generated by the 2 separation units of the second separation area enters a product tank;
acid resolution zone: the device comprises 1 separation unit of a first separation area and 1 separation unit of a second separation area, wherein a forward feeding mode is adopted, feeding liquid is sulfuric acid with the concentration of 10%, and discharging liquid enters an intermediate tank;
a water washing area: the device comprises 3 separation units of a first separation area and 3 separation units of a second separation area, wherein a forward series feeding mode is adopted, feeding liquid is pure water, and discharging liquid enters an intermediate tank.
4. A production method for extracting cobalt from copper extraction tail liquid according to claim 3, which is characterized by comprising the following steps: the continuous fluid separation system also includes a spare area including one or more separation units of the first separation zone and one or more separation units of the second separation zone.
5. The production method for extracting cobalt from the copper extraction tail liquid as claimed in claim 4, characterized in that: the product adsorption area, the water ejection area, the air pressure material area, the dilute acid analysis area, the water washing area and the spare part area are sequentially arranged along the circumferential direction.
6. A production method for extracting cobalt from copper extraction tail liquid according to claim 3, which is characterized by comprising the following steps: the feed rate to the product adsorption zone is 12-18 mL/min.
7. A production method for extracting cobalt from copper extraction tail liquid according to claim 3, which is characterized by comprising the following steps: the feeding speeds of the water top material area and the water washing area are both 28-35 mL/min.
8. A production method for extracting cobalt from copper extraction tail liquid according to claim 3, which is characterized by comprising the following steps: the feeding speed of the dilute acid analysis zone and the acid analysis zone is 40-50 mL/min.
9. The production method for extracting cobalt from the copper extraction tail liquid as claimed in claim 2, characterized in that: the type of the imported chelate resin is Dusheng CH-90, and the type of the domestic chelate resin is D463.
10. A process for producing cobalt from copper extraction tailings as claimed in any one of claims 3 to 9, wherein: in the continuous fluid separation system, the filling amount of each separation unit is 300-500 ml.
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| CN202010179117.6A CN111286607A (en) | 2020-03-13 | 2020-03-13 | Production method for extracting cobalt from copper extraction tail liquid |
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| CN202010179117.6A CN111286607A (en) | 2020-03-13 | 2020-03-13 | Production method for extracting cobalt from copper extraction tail liquid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115354152A (en) * | 2022-08-25 | 2022-11-18 | 上海锦源晟新能源材料有限公司 | Continuous operation system and method for separating enriched cobalt from high-impurity cobalt-containing solution |
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| CN102978395A (en) * | 2012-12-03 | 2013-03-20 | 吉林大学 | Method for separating and enriching Cu and Co from sulfate diluted solution containing Co |
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2020
- 2020-03-13 CN CN202010179117.6A patent/CN111286607A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102978395A (en) * | 2012-12-03 | 2013-03-20 | 吉林大学 | Method for separating and enriching Cu and Co from sulfate diluted solution containing Co |
| CN107804875A (en) * | 2017-11-14 | 2018-03-16 | 厦门世达膜科技有限公司 | The method that the high miscellaneous tungsten resource of high molybdenum is carried out to tungsten separation progress APT productions |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115354152A (en) * | 2022-08-25 | 2022-11-18 | 上海锦源晟新能源材料有限公司 | Continuous operation system and method for separating enriched cobalt from high-impurity cobalt-containing solution |
| CN115354152B (en) * | 2022-08-25 | 2023-12-29 | 上海锦源晟新能源材料有限公司 | Continuous operation system and method for separating and enriching cobalt from high-impurity cobalt-containing solution |
| WO2024040900A1 (en) * | 2022-08-25 | 2024-02-29 | 上海锦源晟新能源材料有限公司 | Continuously operating system for separating and enriching cobalt from high-impurity content cobalt solution and method therefor |
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