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A high-purity, cobalt solution technology, applied in photographic process, instrument, photographic auxiliary process, etc., can solve the problems of affecting product purity, diaphragm maintenance, high renewal cost, and increased cost.
Inactive Publication Date: 2016-01-27
GENERAL RESEARCH INSTITUTE FOR NONFERROUS METALS BEIJNG
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Among them, the electrolytic refining or electrolytic deposition of high-purity cobalt solution is an indispensable key process. At present, this process usually uses a diaphragm electrolytic cell with a diaphragm bag or a diaphragm plate. The diaphragm of this electrolytic cell is easily damaged, and the damage of the diaphragm will cause anode, Mutual contamination of the anode solution, thereby polluting the purity of the product; in addition, the maintenance and renewal of the
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Embodiment 1
[0032] 5 liters of P507 organic extractant was added to 20 liters of sulfonated kerosene, and under stirring, 20% of P507 extractant was evenly mixed, and then 900 ml of 12N sodium hydroxide was added for saponification reaction.
[0033] Add 8 liters of cobalt chloride feed liquid, wherein the cobalt concentration is 40%, and the P507 extractant after the saponification is stirred, extracted and separated, the stirring speed is 60 rev / min, the two-phase mixing time is 15 minutes, the cobalt is extracted into the organic phase, and the P507 extractant It becomes the loaded organic phase. At this time, the color of the cobalt solution changes from rose red to blue, and the color of the organic phase changes from pale yellow to colorless.
[0034] with [H + ] is a 2.0 mol / L hydrochloric acid solution as a washing solution to wash the cobalt-loaded P507 organic phase until the pH of the aqueous phase of the washing solution is 3.5.
[0035] reuse [H + ] is 1.0 mol / L hydrochloric ...
Embodiment 2
[0047] Configure 30 liters of 30% P507 extractant, and the test operation method is the same as that of Example 1. Add 15 liters of cobalt chloride feed solution, the concentration of cobalt solution is 60%, add to the P507 extractant after saponification, stir and extract and separate, stirring speed is 60 rev / min, two-phase mixing time is 15 minutes, cobalt enters the organic phase, P507 The extractant becomes the loaded organic phase. At this time, the color of the cobalt solution changes from rose red to blue, and the color of the organic phase changes from light yellow to very light pink.
[0048] with [H + ] is a 2.0 mol / L hydrochloric acid solution as a washing solution to wash the cobalt-loaded P507 organic phase until the pH of the aqueous phase of the washing solution is 3.5.
[0049] reuse [H + ] is 1.0 mol / L hydrochloric acid solution as the back-extracting liquid to back-extract the cobalt in the loaded organic phase into the aqueous phase, until the pH of the a...
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Abstract
The present invention relates to a high-purity cobalt preparation method, which comprises: cobalt solution extraction separation and purification, wherein a P507 organic extractant is prepared from P507 by using a saponification way, a cobalt chloride solution is added, extraction separation is performed by using a stirring extraction method, acid liquid washing and acid liquid back extraction are performed, the solution obtained after the back extraction is subjected to deep purification treatment by using a macroporous adsorption resin, and the obtained solution is concentrated to obtain the high-purity cobalt solution; electrodepositing, wherein the high-purity cobalt solution enters a self-heating electrolysis bath through a flow baffle from the bottom portion of the electrolysis bath from bottom to top so as to carry out single circulation electrodepositing, the concentration, the amount and the pH value of the solution in the electrolysis bath maintain the consistent state, and electrodepositing is performed to obtain high-purity electrodepositing cobalt; and vacuum melting, wherein the high-purity electrodepositing cobalt is subjected to vacuum melting so as to prepare the high-purity cobalt. According to the present invention, the product purity is more than 5N, the impurity enrichment problem caused by the electrolyte concentration difference is successfully solved, the cost is reduced, and the cross-contamination of the electrolyte is prevented.
Description
technical field [0001] The invention relates to a method for preparing high-purity cobalt, in particular to a method for preparing high-purity cobalt by using cobalt chloride salt system extraction and separation, deep purification of macroporous adsorption resin, electrolytic deposition, and vacuum smelting. Background technique [0002] High-purity cobalt is one of the important high-purity metal materials. Cobalt with a purity of 3N to 4N (99.9% to 99.99%) has been widely used in the manufacture of magnetic materials and super alloys. Cobalt of 5N (99.999%) and higher purity Sputtering targets for advanced electronic components. [0003] At present, the metals that are difficult to separate in high-purity cobalt are transition metal impurities such as Ni, Fe, Zn, Mn, Cu, etc. For several difficult-to-remove metals, the effective measures are to first adopt some solution purification methods such as ion exchange or extraction, etc. , first reduce most metal impurities to ...
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IPC IPC(8): C25C1/08C25C7/00C22B23/06
Inventor 蔡振平陈松郎书玲吴延科薛红霞
Owner GENERAL RESEARCH INSTITUTE FOR NONFERROUS METALS BEIJNG
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