CN101148698A - Extraction method for removing calcium and magnesium from copper-cobalt ore leachate - Google Patents
Extraction method for removing calcium and magnesium from copper-cobalt ore leachate Download PDFInfo
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- CN101148698A CN101148698A CNA2007100715004A CN200710071500A CN101148698A CN 101148698 A CN101148698 A CN 101148698A CN A2007100715004 A CNA2007100715004 A CN A2007100715004A CN 200710071500 A CN200710071500 A CN 200710071500A CN 101148698 A CN101148698 A CN 101148698A
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Abstract
The process of extracting Co and eliminating Ca from copper-cobalt ore includes obtaining mixture leachate with soluble sulfate of Co, Ni, Ca and Mg; and extracting the mixture leachate with organic solvent, which comprises organic matter bis(2-ethyl hexyl) phosphoric acid or 2- ethyl hexyl phosphonate ester in 15-25 vol% and kerosene in 75-85 vol%. The organic solvent extracting procedure includ es two steps, the first step of transferring Ca into the organic phase while leaving Co, Ni and Mg in the water phase, and the second step of transferring Co to the organic phase while leaving Ni and Mg in the water phase. The process can obtain cobalt sulfate solution with Co content up to 90-100 g/l, Ca ion content lowered to 0.01 g/l, Ni ion content lowered to 0.005 g/l, and Mg ion content lowered to 0.1 g/l and suitable for producing T-cobalt oxide and cobalt salt.
Description
Technical field
The present invention relates to a kind of extracting method of cobalt, particularly a kind of method from copper-cobalt mine leachate removing calcium with solvent extraction magnesium.
Background technology
The general operation that adopts traditional chemical precipitation purification and solvent extraction to combine of the sour molten leach liquor of copper cobalt ore is carried out purification and impurity removal, its flow process is: the solution that contains cobalt and impurity Ni, Fe, Ca, Mg, Cu, Mn, Zn etc. is earlier in oxidation and deironing, reagent precipitation calcium-magnesium removing is then through solvent extraction deep impurity-removing and separation of Cobalt and Nickel.
Reagent precipitation calcium-magnesium removing, method in common is to add Sodium Fluoride or ammonium fluoride at present, makes calcium magnesium and fluorine form the fluorochemical precipitation of indissoluble, removes by filter.The shortcoming of this method is: (1) Sodium Fluoride solubleness is little, and long reaction time needs heating, and energy consumption of reaction is big, and the fluorochemical sedimentation and filtration poor performance that generates; (2) Sodium Fluoride or ammonium fluoride cost an arm and a leg, and it is higher to purify the calcium-magnesium removing cost; (3) because the solubility product of cobaltous fluoride in water is smaller, in Sodium Fluoride or ammonium fluoride precipitator method calcium-magnesium removing, also there is a certain amount of cobalt to generate the cobaltous fluoride precipitation and enters in the slag, cause the yield of cobalt to reduce; (4) fluorine-containing in the waste water, cause the wastewater treatment difficulty.
Summary of the invention
The objective of the invention is provides a kind of method technology simple, reliable in order to solve above-mentioned the deficiencies in the prior art, the purification expense is low, and cobalt yield height is energy-conservation, need not increase facility investment, removal effect is good and can not cause the method from copper-cobalt mine leachate removing calcium with solvent extraction magnesium of environmental pollution.
In order to achieve the above object, a kind of method provided by the invention from copper-cobalt mine leachate removing calcium with solvent extraction magnesium, it comprises the solubility rose vitriol that obtains from the copper cobalt ore, nickel, calcium, magnesium mixing leach liquor, it is characterized in that the solubility rose vitriol, nickel, calcium, magnesium mixing leach liquor organic solvent extraction, described organic extraction solvent is to contain the organism of volume ratio 15% to 25% and contain 75% to 85% kerosene, described organism is di-(2-ethylhexyl)phosphoric acid or di-2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester, described is that leach liquor is carried out two step removing calcium with solvent extraction magnesium with organic solvent extraction: the first step is with the solubility rose vitriol after the deironing, nickel, calcium, the magnesium leach liquor is regulated the pH value 2.0 to 5.0, extract with the extraction solvent that contains di-(2-ethylhexyl)phosphoric acid earlier, make calcium change organic phase over to and cobalt, nickel, magnesium remaines in aqueous phase; Dilute sulphuric acid with 0.5N to 2.0N concentration washs load organic phases again, make cobalt, nickel, magnesium further enter water, load organic phases is again through the hydrochloric acid back extraction of 1N to 4N concentration, calcium back extraction in the organic phase is come out, after the anti-iron of the hydrochloric acid of 5N to 7N concentration remaining iron back extraction in the organic phase is come out; Second step was with the extraction solvent that contains di-2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester the di-(2-ethylhexyl)phosphoric acid raffinate to be extracted again, make cobalt change organic phase over to, and nickel, magnesium change aqueous phase over to, dilute sulphuric acid with 0.5N to 2.0N concentration washs load organic phases again, and then with the dilute sulphuric acid of 2.0N to 4.0N concentration the cobalt back extraction in the organic phase is come out, after the hydrochloric acid of 5N to 7N concentration the iron back extraction in the organic phase is come out.
Describedly carry out in the two step removing calcium with solvent extraction magnesium processes: when the di-(2-ethylhexyl)phosphoric acid extraction calcium of the first step at leach liquor, adopt 8 grades to 15 grades extractions, dilute sulphuric acid with 0.5N to 2.0N concentration carries out 6 grades to 10 grades washings to load organic phases again, the hydrochloric acid of 1N to 4N concentration carries out 3 grades to 6 grades back extraction calcium, and the hydrochloric acid of 5N to 7N concentration carries out 3 grades to 5 grades back extraction iron; When the di-2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester extracting and separating cobalt in second step and nickel, magnesium, adopt 7 grades to 12 grades extractions, dilute sulphuric acid with 0.5N to 2.0N concentration carries out 5 grades to 8 grades washings to load organic phases again, with the dilute sulphuric acid of 2.0N to 4.0N concentration the cobalt in the organic phase is carried out 3 grades to 7 grades back extractions again and come out, the hydrochloric acid of last 5N to 7N concentration carries out 3 grades to 5 grades back extractions with the iron in the organic phase and comes out.The expression of above-mentioned " level " is number of times.As " 7 grades of extractions " is 7 extractions, and " 5 grades of washings " is 5 washings, and " 4 grades of anti-iron " is 4 times the iron back extraction to be operated.
During extraction, organic extraction solvent and the throughput ratio that is extracted between the phase are: the throughput ratio of di-(2-ethylhexyl)phosphoric acid extraction calcium is O/A=1: 2-3, and the throughput ratio of di-2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester separation of cobalt and nickel, magnesium is O/A=1: 1-2.At this, described O/A is: organic extraction solvent/be extracted phase.
Organism in the described organic extraction solvent, earlier carry out saponification with sodium hydroxide, control saponification degree by add-on to sodium hydroxide, wherein: the saponification degree of di-(2-ethylhexyl)phosphoric acid is controlled at 65%-68%, and the saponification degree of di-2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester is controlled at 62%-65%.
Because di-(2-ethylhexyl)phosphoric acid represents with normally used commodity chemical name P204, di-2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester represents with normally used commodity chemical name P507, and below both represent with P204 and P507 respectively.
In the present invention, because the calcium, the magnesium that exist in the extraction of sulfate medium are tedious, surpass 0.05g/L if enter the long-time calcic of feed liquid of P507 extracting and separating cobalt, nickel system, then after extraction for some time, might produce calcium sulfate precipitation in extraction section, so can by control P204 abstraction impurity removal compare (compare by flow and recently embody), saponification degree and pH, just can make P204 reach the purpose of preferential collection calcium.For the calcium sulfate precipitation of avoiding stripping section to generate indissoluble influences normally carrying out of extraction, so select for use hydrochloric acid to do reverse-extraction agent.
The invention has the beneficial effects as follows: (1) is combined as a whole P204 abstraction impurity removal and P507 separation of cobalt, nickel and deliming, magnesium dexterously; (2) the present invention separates calcium, nickel, magnesium from cobalt sulfate solution, make the cobalt contents in the cobalt sulfate solution reach 90g/L-100g/L, calcium ion is reduced to 0.01g/L, o.005g/L nickel ion is reduced to, magnesium ion is reduced to the following level of 0.1g/L, produces T-cobalt oxide and the specification of quality of producing cobalt salt thereby cobalt sulfate solution is met; (3) cost of the present invention is low, the efficient height; (4) technology of the present invention is simple, reliable, strong operability, safety; (5) to purify expense low in the present invention, and cobalt yield height is energy-conservation, need not increase facility investment, and removal effect is good and can not cause environmental pollution; (6) the present invention has the versatility on deliming, the magnesium method, promptly can be used for the cobalt sulfate solution calcium-magnesium removing of other any methods productions etc.
Description of drawings
Fig. 1 is an embodiment of the invention P204 extraction tandem table as a result;
Fig. 2 is an embodiment of the invention P507 extraction tandem table as a result.
Embodiment
The invention will be further described in conjunction with the accompanying drawings below by embodiment.
Embodiment
Embodiment:
A kind of method that present embodiment provides from copper-cobalt mine leachate removing calcium with solvent extraction magnesium, be that the sulphuric leachate of the copper cobalt ore after the deironing is regulated its pH value 3.5 to 4.0 with sodium hydroxide, organic phase is by constituting as the P204 of extraction agent with as the kerosene of thinner, wherein the volume ratio of P204 is 15%, kerosene is 85%, saponification degree is 68%, stream is than O/A=1: 2-3, after 9 grades of contact extractions, make calcium change organic phase over to and cobalt, nickel, magnesium is stored among the water, dilute sulphuric acid with 1.2N concentration carries out 7 grades of washings to load organic phases again, make cobalt, nickel, magnesium enters water, and load organic phases comes out the calcium back extraction in the organic phase through 5 grades of back extractions of hydrochloric acid of 3N concentration, after 4 grades of anti-iron of the hydrochloric acid of 6N concentration remaining iron back extraction in the organic phase is come out.The result as shown in Figure 1.
The P204 raffinate is made the P507 feed liquid carry out 7 grades of extractions, make cobalt change organic phase over to, and nickel, magnesium change aqueous phase over to, dilute sulphuric acid with 1.2N concentration carries out 5 grades of washings to load organic phases again, isolate nickel in the organic phase, magnesium, and then with the dilute sulphuric acid of 3N concentration the cobalt back extraction in the organic phase is come out, after 4 grades of anti-iron of the hydrochloric acid of 6N concentration the iron back extraction in the organic phase is come out.Described organic phase is by constituting as the P507 of extraction agent with as the kerosene of thinner, and the volume ratio of P507 is 25%, kerosene is 75%, and saponification degree is 65%, and stream is than O/A=1: 1.The result as shown in Figure 2.
A kind of method provided by the invention from copper-cobalt mine leachate removing calcium with solvent extraction magnesium, in comprehensive extracting and washing back extraction process, the total recovery of cobalt is greater than 99.5%, and the clearance of calcium is 98.2%, and the clearance of magnesium, nickel all can reach more than 97%.
Claims (5)
1. method from copper-cobalt mine leachate removing calcium with solvent extraction magnesium, it comprises the solubility rose vitriol that obtains from the copper cobalt ore, nickel, calcium, magnesium mixing leach liquor, it is characterized in that the solubility rose vitriol, nickel, calcium, magnesium mixing leach liquor organic solvent extraction, described organic extraction solvent is to contain the organism of volume ratio 15% to 25% and contain 75% to 85% kerosene, described organism is di-(2-ethylhexyl)phosphoric acid or di-2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester, described is that leach liquor is carried out two step removing calcium with solvent extraction magnesium with organic solvent extraction: the first step is with the solubility rose vitriol after the deironing, nickel, calcium, the magnesium leach liquor is regulated the pH value 2.0 to 5.0, extract with the extraction solvent that contains di-(2-ethylhexyl)phosphoric acid earlier, make calcium change organic phase over to and cobalt, nickel, magnesium remaines in aqueous phase; Dilute sulphuric acid with 0.5N to 2.0N concentration washs load organic phases again, make cobalt, nickel, magnesium further enter water, load organic phases is again through the hydrochloric acid back extraction of 1N to 4N concentration, calcium back extraction in the organic phase is come out, after the anti-iron of the hydrochloric acid of 5N to 7N concentration remaining iron back extraction in the organic phase is come out; Second step was with the extraction solvent that contains di-2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester the di-(2-ethylhexyl)phosphoric acid raffinate to be extracted again, make cobalt change organic phase over to, and nickel, magnesium change aqueous phase over to, dilute sulphuric acid with 0.5N to 2.0N concentration washs load organic phases again, and then with the dilute sulphuric acid of 2.0N to 4.0N concentration the cobalt back extraction in the organic phase is come out, after the hydrochloric acid of 5N to 7N concentration the iron back extraction in the organic phase is come out.
2. a kind of method according to claim 1 from copper-cobalt mine leachate removing calcium with solvent extraction magnesium, it is characterized in that carrying out in the two step removing calcium with solvent extraction magnesium processes: when the di-(2-ethylhexyl)phosphoric acid of the first step extracts calcium at leach liquor, adopt 8 grades to 15 grades extractions, dilute sulphuric acid with 0.5N to 2.0N concentration carries out 6 grades to 10 grades washings to load organic phases again, the hydrochloric acid of 1N to 4N concentration carries out 3 grades to 6 grades back extraction calcium, and the hydrochloric acid of 5N to 7N concentration carries out 3 grades to 5 grades back extraction iron; When the di-2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester extracting and separating cobalt in second step and nickel, magnesium, adopt 7 grades to 12 grades extractions, dilute sulphuric acid with 0.5N to 2.0N concentration carries out 5 grades to 8 grades washings to load organic phases again, with the dilute sulphuric acid of 2.0N to 4.0N concentration the cobalt in the organic phase is carried out 3 grades to 7 grades back extractions again and come out, the hydrochloric acid of last 5N to 7N concentration carries out 3 grades to 5 grades back extractions with the iron in the organic phase and comes out.
3. a kind of method according to claim 1 and 2 from copper-cobalt mine leachate removing calcium with solvent extraction magnesium, when it is characterized in that extracting, organic extraction solvent and the throughput ratio that is extracted between the phase are: the throughput ratio of di-(2-ethylhexyl)phosphoric acid extraction calcium is O/A=1: 2-3, and the throughput ratio of di-2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester separation of cobalt and nickel, magnesium is O/A=1: 1-2.
4. a kind of method according to claim 1 and 2 from copper-cobalt mine leachate removing calcium with solvent extraction magnesium, it is characterized in that the organism in the described organic extraction solvent, earlier carry out saponification with sodium hydroxide, control saponification degree by add-on to sodium hydroxide, wherein: the saponification degree of di-(2-ethylhexyl)phosphoric acid is controlled at 65%-68%, and the saponification degree of di-2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester is controlled at 62%-65%.
5. a kind of method according to claim 3 from copper-cobalt mine leachate removing calcium with solvent extraction magnesium, it is characterized in that the organism in the described organic extraction solvent, earlier carry out saponification with sodium hydroxide, control saponification degree by add-on to sodium hydroxide, wherein: the saponification degree of di-(2-ethylhexyl)phosphoric acid is controlled at 65%-68%, and the saponification degree of di-2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester is controlled at 62%-65%.
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| KR101021180B1 (en) | 2010-07-27 | 2011-03-15 | 코스모화학 주식회사 | Method for producing high purity cobalt surfate |
| CN101643859B (en) * | 2008-08-07 | 2011-04-20 | 北京有色金属研究总院 | Process method for separating and purifying cobalt solution by extraction chromatography |
| CN102061390A (en) * | 2010-12-03 | 2011-05-18 | 安化金源新材料有限责任公司 | Method for directly producing high-purity electronic level cobaltous sulfate by using cobalt-containing waste |
| CN102181666A (en) * | 2011-05-06 | 2011-09-14 | 广西银亿科技矿冶有限公司 | Method for treating red soil nickel ore leaching liquid |
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