CN103789541A - Calcium removing equipment and process in cobalt wet metallurgy process - Google Patents
Calcium removing equipment and process in cobalt wet metallurgy process Download PDFInfo
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- CN103789541A CN103789541A CN201410034446.6A CN201410034446A CN103789541A CN 103789541 A CN103789541 A CN 103789541A CN 201410034446 A CN201410034446 A CN 201410034446A CN 103789541 A CN103789541 A CN 103789541A
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Abstract
The invention relates to calcium removing equipment and process in a cobalt wet metallurgy process. The calcium removing equipment comprises an extracting tank and an alkali adjusting agitating tank which are communicated by a pipeline, wherein the extracting tank comprises a plurality of grades of extracting grooves which are connected in series. The calcium removing equipment is characterized in that each extracting groove comprises a mixing chamber and a clarifying chamber; a cobalt washing acid feeding opening, a washing liquid feeding opening and a liquid alkali feeding opening are formed in the top face of the alkali adjusting agitating tank; a filter pressing outlet is formed in the bottom of the alkali adjusting agitating tank; the filter pressing outlet is connected with a filter press.
Description
Technical field
The present invention relates to cobalt hydrometallurgy field, be specifically related to deliming equipment and process in a kind of cobalt hydrometallurgy process.
Background technology
In cobalt hydrometallurgical processes, the removal of impurity is essential operation, and in common impurity, calcium impurities is because it is more special, and the difficulty of removal is larger.Being to have two kinds substantially take the technique of heterogenite, rough cobaltous carbonate, the deliming in the full wet processing of cobalt raw material of rough cobaltous hydroxide, the one, fluorochemical deliming method and cobalt raw material through reduction leach, after iron removal step, copper extraction extraction copper, under PH4.5 to 5.0, the reaction conditions of temperature at 75-80 ℃, add Sodium Fluoride or Neutral ammonium fluoride that calcium is precipitated with the form of Calcium Fluoride (Fluorspan), the method is owing to being to react under higher PH condition, easily valuable metal cobalt and copper are precipitated, reduce the rate of recovery of cobalt, copper, required temperature is higher in addition, and the steam of consumption is more; The 2nd, P204 extraction process deliming method: solution is after copper extraction process extraction copper, the PH3.5 to 4.0, temperature that adjusts solution at 35 to 45 ℃, the saponification degree of P204 65-75%, use P204 extraction agent to carry out removing calcium with solvent extraction, the required temperature of the method is not high, solution after deironing just can meet the demands, do not need extra heating, save steam, deliming substep tandem in extraction box completes in addition, before and after deliming, PH variation range is in 1 PH, PH is lower, thus can not produce the phenomenon of cobalt, copper precipitation, little on the rate of recovery impact of cobalt, copper.Owing to there being above-mentioned advantage, so part producing unit adopts second method deliming in cobalt hydrometallurgy operation.But cobalt nickel hydrometallurgical processes, what adopt is sulfuric acid system, in extraction box in deliming process, because the solubleness of calcium sulfate is lower, easily in extraction box pipeline and above stirring rake, form calcium sulphate crystal, pipeline, damage stirring rake and the motor reducer etc. of obstruction.In order to remove the calcium sulphate crystal of formation, what need intermittent carries out artificial scarfing cinder to extraction box, so causes producing the running balance of liquid before interrupting, destroy extraction agent and extracting, and waste of manpower, material resources.
Summary of the invention
Utilize calcium in P204 extraction agent deliming process in extraction box precipitation and the higher problem of P204 saponification degree, to the invention provides deliming equipment and process in a kind of cobalt hydrometallurgy process for solving in cobalt hydrometallurgy, fully, effect of extracting is good in this equipment extraction.
For reaching above object, the technical scheme that the present invention takes is:
Deliming equipment in a kind of cobalt hydrometallurgy process, comprises abstraction pool and tune alkali agitated pool through pipeline UNICOM, and described abstraction pool comprises the extraction tank of plural serial stage, and described extraction tank comprises mixing section and clarifying chamber.
Further, between described mixing section and clarifying chamber, be provided with dividing plate, the bottom of described mixing section is provided with organic import and water import, is provided with stirring rake in mixing section, and the bottom of described clarifying chamber is provided with water outlet, and the top of clarifying chamber is provided with organic outlet.
Further, described mixing section and clarifying chamber are arranged in parallel perpendicular to extraction tank series connection direction, and the mixing section of adjacent two-stage extraction tank and clarifying chamber are oppositely arranged in a crossed manner.
Further, it is characterized in that, organic outlet of the clarifying chamber of described higher level's extraction tank is connected through pipeline with organic import of subordinate's extraction tank mixing section, and the water outlet of the clarifying chamber of described higher level's extraction tank is connected through pipeline with the water import of subordinate's extraction tank mixing section.
Further, described in adjust and reduce steel basin end face be provided with and wash cobalt acid opening for feed, washings opening for feed and liquid caustic soda opening for feed, adjust the bottom of alkali agitated pool to be provided with press filtration outlet, described press filtration outlet connects pressure filter.
Further, the height of described dividing plate is lower than extraction tank height.
Further, in described tune alkali agitated pool, be provided with whipping appts.
Again further, in cobalt hydrometallurgy process, the technique of deliming equipment deliming comprises the steps:
(1) choose the abstraction pool that 30 grades of extraction tanks are connected, the water outlet of higher level's extraction tank connects the water import of subordinate's extraction tank, organic outlet of subordinate's extraction tank connects organic import of grade extraction tank, organic outlet of higher level's extraction tank connects organic import of subordinate's extraction tank, and the water outlet of subordinate's extraction tank connects the water import of grade extraction tank; Extraction liquid flows from left to right through organic import of first step extraction tank, the front liquid pH value of extraction is adjusted to the water import right-to-left through the 8th grade of extraction tank after 2.5 and flows, extraction liquid and the front liquid counter-current extraction of extraction, in extraction tanks at different levels, extraction liquid first fully mixes at mixing section with liquid before extraction, extraction extraction liquid is by Ca, the Cu extraction in liquid before extraction, overflow to clarifying chamber clarifies again, before extraction after clarification, liquid flows out through the outlet water outlet from first step extraction tank, and extraction liquid is continued to flow to the right by organic outlet of the 8th grade of extraction tank;
(2) washing composition flows from the water import right-to-left of the 16 grade of extraction tank, extraction liquid and washing composition countercurrent washing, in extraction tanks at different levels, extraction liquid and washing composition are first after the abundant mixing, washing of mixing section, overflow to clarifying chamber clarifies again, in extraction liquid, Ca, Cu continue to flow to the right from the 16 grade of organic outlet of extraction tank after being washed agent washing, and the organic outlet from last step extraction tank after multi-stage solvent extraction groove is processed is flowed out; The washing composition that contains Ca, Cu enters and adjusts in alkali agitated pool through the water outlet of the 9th grade of extraction tank.
(3) adjust the liquid after cobalt acid opening for feed input extraction copper of washing of alkali agitated pool, liquid caustic soda opening for feed input sodium hydroxide solution, tune alkali agitated pool pH value is adjusted to 2.5, in washing composition Ca, Cu ion respectively with sodium hydroxide and extraction copper after sulfuric acid reaction in liquid, generate copper hydroxide, calcium hydroxide precipitation and calcium sulphate crystal;
(4) adjust the throw out in alkali agitated pool to send into press filtration separation in pressure filter through press filtration outlet.
Further, the extraction liquid in described step 1 is that concentration is the P204 solution of 25%-30%.
Again further, the hydrochloric acid soln that described washing composition is 1.1-1.3mol/l.
Take after above technical scheme, beneficial effect of the present invention is:
1. the abstraction pool of deliming equipment is provided with the extraction tank of plural serial stage, reverse convection extraction between liquid before extraction agent and extraction, in extraction tank, be provided with mixing section and clarifying chamber, before extraction, liquid and extraction agent first enter clarifying chamber's clarification after the abundant hybrid extraction of mixing section, flow to again next stage extraction tank and repeat hybrid extraction, clarification, extract more fully, effect of extracting is better.
2. in mixing section, be provided with stirring rake, be convenient to extract fully mixing of front liquid and extraction agent, the superior and the subordinate's cell body is produced to suction function simultaneously, make the smooth inflow of the solution in the superior and the subordinate's cell body.
3. change the outlet of liquid after washing and flow to, no longer directly enter extraction tank, adjust alkali groove but enter, make to wash in rear liquid most of calcium and precipitate adjusting in alkali groove, greatly reduced the calcium entering in extracting system, except low running cost.
4. utilize the deliming technique of this deliming equipment accurately to control the pH value of the front liquid of extraction, reduce the saponification degree of P204 extraction agent, and regeneration calcium sulphate crystal not in extraction process, control lower saponification degree, in extraction process, extraction process solution PH changes very little, be conducive to the extraction of calcium, make the removal degree of calcium very high.
Accompanying drawing explanation
Fig. 1 is the structural representation of extraction tank;
Fig. 2 is the structural representation of adjusting alkali agitated pool;
Fig. 3 is extraction tank serial connection schematic diagram.
In Fig. 1: extraction tank 1, mixing section 11, clarifying chamber 12, stirring rake 13, organic import 14, water import 15, dividing plate 16, organic outlet 17, water outlet 18.
In Fig. 2: adjust alkali agitated pool 2, wash cobalt acid opening for feed 21, washings opening for feed 22, liquid caustic soda opening for feed 23, whipping appts 24, press filtration outlet 25.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is further described:
As shown in the figure, in a kind of cobalt hydrometallurgy process, deliming equipment comprises abstraction pool and adjusts alkali agitated pool 2.Described abstraction pool comprises 30 grades of extraction tanks 1 of series connection successively, and described extraction tank 1 comprises mixing section 11, clarifying chamber 12, stirring rake 13, organic import 14, water import 15, dividing plate 16, organic outlet 17 and water outlet 18.Mixing section 11 in described extraction tank 1 and clarifying chamber 12 are arranged in parallel perpendicular to extraction tank series connection direction, between mixing section 11 and clarifying chamber 12, be provided with dividing plate 16, the height of described dividing plate 16 is lower than the height of extraction tank 1, solution overflow in mixing section 11 is crossed dividing plate 16 and is entered clarifying chamber 12, the bottom of described mixing section 11 is provided with organic import 14 and water import 15, in mixing section, be provided with stirring rake 13, the bottom of described clarifying chamber is provided with water outlet 18, and the top of clarifying chamber is provided with organic outlet 17; Mixing section 11 and the clarifying chamber 12 of adjacent two-stage extraction tank 1 are oppositely arranged in a crossed manner, between organic import 14 that described extraction tanks at different levels are 1 and organic outlet 17, be connected through pipeline,
Organic outlet 17 of the clarifying chamber 12 of described higher level's extraction is connected through pipeline with organic import 14 of subordinate's extraction mixing section 11, and the water outlet 18 of the clarifying chamber 12 of described higher level's extraction tank 1 is connected through pipeline with the water import 15 of subordinate's extraction tank 1 mixing section 11.
Described tune alkali agitated pool 2 comprises washes cobalt acid opening for feed 21, washings opening for feed 22, liquid caustic soda opening for feed 23, whipping appts 24 and press filtration outlet 25.Describedly comprise that washing cobalt acid opening for feed 21, washings opening for feed 22 and liquid caustic soda opening for feed 23 is arranged at the top of adjusting alkali agitated pool 2, in described tune alkali agitated pool 2, be provided with whipping appts 24, adjust alkali agitated pool 2 bottoms to be provided with press filtration outlet 25, described press filtration outlet 25 is connected with pressure filter.
The wherein water outlet 18 of a joint extraction tank of described abstraction pool is connected with the washings opening for feed 22 of adjusting alkali agitated pool 2 through pipeline.
Use the technique of deliming equipment deliming to be:
(1) choose the abstraction pool by 30 grades of extraction tank series connection, P204 solution using concentration as 25%-30% is as extraction liquid, described extraction liquid flows from left to right through organic import of first step extraction tank, the front liquid pH value of extraction is adjusted to the water import right-to-left through the 8th grade of extraction tank after 2.5 and flows, extraction liquid and the front liquid counter-current extraction of extraction, extraction liquid is by Ca, the Cu extraction in liquid before extraction, and the front liquid of extraction of removing after Ca, Cu flows out from the outlet water outlet of first step extraction tank;
(2) extraction liquid that contains Ca, Cu continues to flow to the right from the 8th grade of extraction tank flows out, using the hydrochloric acid soln of 1.1-1.3mol/l as washing composition, washing composition flows from the water import right-to-left of the 16 grade of extraction tank, extraction liquid and washing composition countercurrent washing, Ca, the Cu in extraction liquid enters and adjusts in alkali agitated pool through the water outlet of the 9th grade of extraction tank with washing composition after being washed agent washing; The extraction liquid of removing Ca, Cu continues to flow to the right from the 16 grade of extraction tank flows out, and the organic outlet from last step extraction tank after multi-stage solvent extraction groove is processed is flowed out;
(3) adjust the liquid after cobalt acid opening for feed input extraction copper of washing of alkali agitated pool, liquid caustic soda opening for feed input sodium hydroxide solution, tune alkali agitated pool pH value is adjusted to 2.5, in washing composition Ca, Cu ion respectively with sodium hydroxide and extraction copper after sulfuric acid reaction in liquid, generate copper hydroxide, calcium hydroxide precipitation and calcium sulphate crystal;
(4) adjusting copper hydroxide, calcium hydroxide precipitation and calcium sulphate crystal in alkali agitated pool or throw out to send into press filtration in pressure filter through press filtration outlet separates.
Claims (10)
1. a deliming equipment in cobalt hydrometallurgy process, comprises abstraction pool and tune alkali agitated pool through pipeline UNICOM, and described abstraction pool comprises the extraction tank of plural serial stage, it is characterized in that, described extraction tank comprises mixing section and clarifying chamber.
2. deliming equipment in a kind of cobalt hydrometallurgy process according to claim 1, it is characterized in that, between described mixing section and clarifying chamber, be provided with dividing plate, the bottom of described mixing section is provided with organic import and water import, in mixing section, be provided with stirring rake, the bottom of described clarifying chamber is provided with water outlet, and the top of clarifying chamber is provided with organic outlet.
3. deliming equipment in a kind of cobalt hydrometallurgy process according to claim 2, is characterized in that, described mixing section and clarifying chamber are arranged in parallel perpendicular to extraction tank series connection direction, and the mixing section of adjacent two-stage extraction tank and clarifying chamber are oppositely arranged in a crossed manner.
4. according to deliming equipment in a kind of cobalt hydrometallurgy process described in claim 1 or 2 or 3, it is characterized in that, organic outlet of the clarifying chamber of described higher level's extraction tank is connected through pipeline with organic import of subordinate's extraction tank mixing section, and the water outlet of the clarifying chamber of described higher level's extraction tank is connected through pipeline with the water import of subordinate's extraction tank mixing section.
5. deliming equipment in a kind of cobalt hydrometallurgy process according to claim 1, it is characterized in that, described end face of adjusting and reducing steel basin is provided with washes cobalt acid opening for feed, washings opening for feed and liquid caustic soda opening for feed, adjusts the bottom of alkali agitated pool to be provided with press filtration outlet, and described press filtration outlet connects pressure filter.
6. deliming equipment in a kind of cobalt hydrometallurgy process according to claim 2, is characterized in that, the height of described dividing plate is lower than extraction tank height.
7. deliming equipment in a kind of cobalt hydrometallurgy process according to claim 5, is characterized in that, in described tune alkali agitated pool, is provided with whipping appts.
8. a technique for deliming equipment deliming in cobalt hydrometallurgy process according to claim 1, comprises the steps:
(1) choose the abstraction pool that 30 grades of extraction tanks are connected, the water outlet of higher level's extraction tank connects the water import of subordinate's extraction tank, organic outlet of subordinate's extraction tank connects organic import of grade extraction tank, organic outlet of higher level's extraction tank connects organic import of subordinate's extraction tank, and the water outlet of subordinate's extraction tank connects the water import of grade extraction tank; Extraction liquid flows from left to right through organic import of first step extraction tank, the front liquid pH value of extraction is adjusted to the water import right-to-left through the 8th grade of extraction tank after 2.5 and flows, extraction liquid and the front liquid counter-current extraction of extraction, in extraction tanks at different levels, extraction liquid first fully mixes at mixing section with liquid before extraction, extraction extraction liquid is by Ca, the Cu extraction in liquid before extraction, overflow to clarifying chamber clarifies again, before extraction after clarification, liquid flows out through the outlet water outlet from first step extraction tank, and extraction liquid is continued to flow to the right by organic outlet of the 8th grade of extraction tank;
(2) washing composition flows from the water import right-to-left of the 16 grade of extraction tank, extraction liquid and washing composition countercurrent washing, in extraction tanks at different levels, extraction liquid and washing composition are first after the abundant mixing, washing of mixing section, overflow to clarifying chamber clarifies again, in extraction liquid, Ca, Cu continue to flow to the right from the 16 grade of organic outlet of extraction tank after being washed agent washing, and the organic outlet from last step extraction tank after multi-stage solvent extraction groove is processed is flowed out; The washing composition that contains Ca, Cu enters and adjusts in alkali agitated pool through the water outlet of the 9th grade of extraction tank;
(3) adjust the liquid after cobalt acid opening for feed input extraction copper of washing of alkali agitated pool, liquid caustic soda opening for feed input sodium hydroxide solution, tune alkali agitated pool pH value is adjusted to 2.5, in washing composition Ca, Cu ion respectively with sodium hydroxide and extraction copper after sulfuric acid reaction in liquid, generate copper hydroxide, calcium hydroxide precipitation and calcium sulphate crystal;
(4) adjust the throw out in alkali agitated pool to send into press filtration separation in pressure filter through press filtration outlet.
9. deliming technique in a kind of cobalt hydrometallurgy process according to claim 7, is characterized in that, the extraction liquid in described step 1 is that concentration is the P204 solution of 25%-30%.
10. deliming technique in a kind of cobalt hydrometallurgy process according to claim 7, is characterized in that the hydrochloric acid soln that described washing composition is 1.1-1.3mol/l.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112760482A (en) * | 2019-11-05 | 2021-05-07 | 格林美股份有限公司 | Method for reducing calcium sulfate deposition in P204 extraction impurity removal process |
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Application publication date: 20140514 |