CN202658207U - Device for deeply removing copper from nickel-containing solution by nickel thiocarbonate - Google Patents

Device for deeply removing copper from nickel-containing solution by nickel thiocarbonate Download PDF

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CN202658207U
CN202658207U CN2012203271919U CN201220327191U CN202658207U CN 202658207 U CN202658207 U CN 202658207U CN 2012203271919 U CN2012203271919 U CN 2012203271919U CN 201220327191 U CN201220327191 U CN 201220327191U CN 202658207 U CN202658207 U CN 202658207U
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nickel
copper
solution containing
thiocarbonic acid
solution
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陈星宇
何利华
赵中伟
陈爱良
陈自江
刘旭恒
赵重
刘冬莉
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Central South University
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Central South University
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Abstract

The utility model discloses a device for deeply removing copper from a nickel-containing solution by nickel thiocarbonate. The device comprises a nickel thiocarbonate slurry tank, a nickel thiocarbonate slurry feeding pump, a nickel-containing solution feeding pump, a pipeline reactor and a pipeline mixing device, wherein the nickel thiocarbonate slurry feeding pump is arranged in front of the nickel-containing solution feeding pump; firstly nickel thiocarbonate is injected into a nickel-containing solution main pipeline through a pump, and then the nickel thiocarbonate is mixed with a nickel-containing solution through the nickel-containing solution feeding pump to be injected into the pipeline reactor; and a net-shaped grid is arranged on a connecting place of the pipeline reactor and is used for enhancing the mixing of a copper removing agent and the nickel-containing solution. The device can realize the purpose of deeply removing the copper in the nickel-containing solution under the condition of continuous operation, can simultaneously obtain copper-removed slag with a high copper-nickel ratio, is simple in control, and is easily realized in industrialized automation.

Description

The device of a kind of thiocarbonic acid SOH nickel deep copper removal from solution containing nickel
Technical field
The utility model relates to copper nickel hydrometallurgy field, particularly the device of a kind of thiocarbonic acid SOH nickel deep copper removal from solution containing nickel.
Background technology
The content of impurity Cu is the element of being strict with in the electric nickel, and its content requirement is lower than 0.01% in electric nickel standard (GB/T6516-1997Ni9996).Therefore requiring before electro deposited nickel the impurity copper in the solution containing nickel to be carried out the degree of depth removes.But because copper nickel chemical property is quite similar, for a long time, the degree of depth is removed the difficult problem that copper in the solution containing nickel becomes the domestic and international metallurgical boundary of puzzlement under technical scale.Under the technical scale from solution containing nickel the key of efficient copper removal be the copper degree of depth can be removed, simultaneously except copper nickel in the copper ashes than high.For this difficult problem, China classifies this research as key research projects twice in " eight or five " and the ninth five-year plan, domestic scholars is attempted the whole bag of tricks, remove process for copper such as active nickel sulfide, nickel thiosulfate, active sulphur powder etc., but problem fails still to be well solved.
Correlation technique and thinking in using for reference " active nickel sulfide " and " degree of depth is except molybdenum in the tungstate solution ", metallurgical institute of Central South University develops a kind of new decoppering agent---thiocarbonic acid SOH nickel.This new decoppering agent has very high reactive behavior, can the degree of depth rapidly and efficiently remove copper in the solution containing nickel.Therefore, thiocarbonic acid SOH nickel can be used as a kind of efficient Decoppering agent fully for solution containing nickel copper removal industrial production.
Utilize traditional slot type stirred reactor, as long as an amount of thiocarbonic acid SOH nickel and the copper in the solution containing nickel homogeneous mixture solotion can be down to below the 3mg/L, except copper nickel ratio in the copper ashes is higher than 15, reach the requirement of the qualified electric nickel of industrial production fully.Smaller when industry generation scale, when the amount of solution of required processing was little, this reaction unit can also be dealt with.But when being on a grand scale, such as Jinchuan Non-ferrous Metals Company, need solution containing nickel to be processed to reach 300m 3/ h, this intermittent type slot type stirred reactor just can't have been processed.Therefore, in large-scale industrial production, need to adopt the continuously device of copper removal.
For a long time, Jinchuan Non-ferrous Metals Company always is that the boiling copper removal groove of employing energy serialization production is as the copper removal device.Boiling copper removal groove is to add the anode sludge for nickel ore concentrate specially to develop except process for copper.This device is well considered the physicochemical property such as density, granularity and reactive behavior of nickel ore concentrate, when the top of decoppering agent from boiling copper removal groove adds, because density is larger, in the decline process, constantly mix with solution and contact, since the reaction continue carry out, except copper ashes density diminishes, just can discharge from the overflow port at copper removal groove top with solution, thereby finish whole copper removal process.But because itself there is defective in this technique, cause behind its copper removal the copper ashes amount of output large, nickeliferous height in the copper ashes, nickel-copper ratio reaches 2:1, can't directly return the copper production system.
Can thiocarbonic acid SOH nickel adapt to the boiling copper removal except process for copper, reach the copper removal effect of using in the intermittent type groove-type stirrer? we find, because thiocarbonic acid SOH nickel is owing to being newborn synthetic, although its reactive behavior is very high, but with respect to nickel ore concentrate, its granularity is thin, density is lower.If adopt boiling copper removal groove as the copper removal device, add thiocarbonic acid SOH nickel from the reactive tank top, under the same industrial scale condition of assurance, namely do not reduce in the treatment capacity situation, because solution flow is very large, thiocarbonic acid SOH nickel will be taken out of reactive tank fast by solution.Therefore will cause thiocarbonic acid SOH nickel can't with solution contact reacts in reactive tank, thereby cause the copper removal deleterious.
Based on above analysis, for thiocarbonic acid SOH nickel copper removal process characteristic, extremely be necessary to adopt a kind of copper-stripping reaction device of energy non-stop run newly.
Summary of the invention
Essence of the present utility model is, proposes a kind of device of deep copper removal from solution containing nickel that is adapted to thiocarbonic acid SOH nickel physicochemical property.This device can realize under the condition of non-stop run that the copper degree of depth in the solution containing nickel removes, obtain simultaneously to have high-copper nickel ratio except copper ashes, control simply, be easy to realize industrial automation.
The technical solution of the utility model is, the device of a kind of thiocarbonic acid SOH nickel deep copper removal from solution containing nickel, comprise thiocarbonic acid SOH nickel slurry tank, thiocarbonic acid SOH nickel slurry feed pump, solution containing nickel feed pipe, solution containing nickel fresh feed pump and pipeline reactor, described thiocarbonic acid SOH nickel slurry tank by thiocarbonic acid SOH nickel slurry feed pump be connected to the solution containing nickel feed pipe with mix sulphur for nickelous carbonate slurry and solution containing nickel, mixed thiocarbonic acid SOH nickel slurry and solution containing nickel export pipeline reactor to through the solution containing nickel fresh feed pump.
The device of described a kind of thiocarbonic acid SOH nickel deep copper removal from solution containing nickel is provided with pipeline mixing device in the described pipeline reactor, and described pipeline mixing device is cellular grid, in order to strengthen thiocarbonic acid SOH nickel slurry and solution containing nickel hybrid reaction.
Use said apparatus to carry out the method for thiocarbonic acid SOH nickel copper removal from solution containing nickel, may further comprise the steps successively:
(1) the pH value with solution containing nickel transfers to 3.0 ~ 7.0, then the mol ratio by nickel in thio-carbonate and the solution containing nickel is 0.3～1.0 adding thio-carbonate solution, and stirring reaction 5～30 minutes, obtain thiocarbonic acid SOH nickel slurry without filtration, place thiocarbonic acid SOH nickel slurry tank;
(2) also can carry out first filtering separation and obtain solid sulfur for nickelous carbonate obtaining thiocarbonic acid SOH nickel slurry in the step (1), then with solid sulfur for nickelous carbonate and solution containing nickel or water mixing pulp, obtain thiocarbonic acid SOH nickel slurry, place thiocarbonic acid SOH nickel slurry tank;
Described thio-carbonate solution is Na 2CS 3, Na 2CS 4, Na 2CS 5, Na 2C 2S 5, K 2CS 3, K 2CS 4, K 2CS 5, K 2C 2S 5In one or more mixture;
Described solution containing nickel is nickle electrolysis anode solution, NiSO 4, NiCl 2, Ni (NO 3) 2The mixture of one or more in the solution.
(3) then the pH value of solution containing nickel is adjusted to 2.0～6.5, and is heated to 60 ℃ ~ 90 ℃;
(4) be 1.1～1.5 to be injected in solution containing nickel feed pipe thiocarbonic acid SOH nickel slurry by the mol ratio of the copper in thio-carbonate and the solution containing nickel with mashing pump first;
(5) with mashing pump solution containing nickel and thiocarbonic acid SOH nickel slurry are mixed together to be injected into again and react copper removal in the pipeline reactor, reaction time is 15～60min.
Technique effect of the present utility model is,
(1) because whole reaction process is to carry out in pipeline, have under the certain flow rate condition at fluid, and the liquid that the interval exists in pipeline stream mixing device, can guarantee the abundant hybrid reaction of decoppering agent and solution, therefore can eliminate fully because of the low detrimentally affect that causes of thiocarbonic acid SOH nickel density;
(2) since in present method the decoppering agent that uses be easy to pulp as thiocarbonic acid SOH nickel, can add as required getting final product with pump by the control flow, then together be injected in the pipeline by the mechanically mixing pump with nickle electrolysis anode solution and get final product.This operating method can make the copper removal operating process become very simple, can realize the automatization of decoppering agent adding procedure fully, reduces greatly labour intensity.
(3) whole process is to react in closed reactor, can reduce greatly calorific loss.
The utility model is described in further detail below in conjunction with accompanying drawing.
Description of drawings
Fig. 1 is structural representation of the present utility model;
Wherein, 1 is thiocarbonic acid SOH nickel slurry tank, and 2 is thiocarbonic acid SOH nickel slurry feed pump, and 3 is the solution containing nickel feed pipe, and 4 is the solution containing nickel fresh feed pump, and 5 is pipeline reactor, and 6 is pipeline mixing device.
Embodiment
Referring to Fig. 1, the utility model comprises thiocarbonic acid SOH nickel slurry tank 1, thiocarbonic acid SOH nickel slurry feed pump 2, solution containing nickel feed pipe 3, solution containing nickel fresh feed pump 4 and pipeline reactor 5, thiocarbonic acid SOH nickel slurry tank 1 by thiocarbonic acid SOH nickel slurry feed pump 2 be connected to solution containing nickel feed pipe 3 with mix sulphur for nickelous carbonate slurry and solution containing nickel, mixed thiocarbonic acid SOH nickel slurry and solution containing nickel export pipeline reactor 5 to through solution containing nickel fresh feed pump 4.Be provided with pipeline mixing device 6 in the pipeline reactor 5, pipeline mixing device 6 is cellular grid, in order to strengthen thiocarbonic acid SOH nickel slurry and solution containing nickel hybrid reaction.
Embodiment 1
The pH value that with nickel concentration is first the nickle electrolysis anode solution of 70g/l transfers to 4.0, then is 0.3 ratio and Na in the mol ratio of nickel in thio-carbonate and the electrolytic solution 2CS 3 Solution hybrid reaction 10 minutes obtains thio-carbonate concentration and is the thiocarbonic acid SOH nickel slurry of 0.5mol/l as decoppering agent; Then the nickle electrolysis anode solution pH that with copper concentration is 0.5g/l transfers to 4.5, and temperature is heated to 60 ℃; Then be that 1.3 ratio is mixed in the mol ratio of the copper in thio-carbonate in the decoppering agent and the nickle electrolysis anode solution, the input speed of control thiocarbonic acid SOH nickel slurry feed pump is 1.56m 3/ h is injected in the solution containing nickel feed pipe, mixes rear with 76.56m with nickle electrolysis anode solution 3The input speed of/h is injected into diameter 40cm by the solution containing nickel fresh feed pump, and length is in the pipeline reactor of 305m, and feed liquid residence time in pipeline reactor is 30 minutes.After reaction is finished in the electrolytic solution copper concentration reduce to 0.002g/L, except copper nickel ratio in the copper ashes is 25.
Embodiment 2
The pH value that with nickel concentration is first the nickel sulfate solution of 70g/l transfers to 5.0, then is 0.4 ratio and Na in the mol ratio of nickel in thio-carbonate and the electrolytic solution 2CS 3Solution hybrid reaction 20 minutes obtains thio-carbonate concentration and is the thiocarbonic acid SOH nickel slurry of 1.2mol/l as decoppering agent; Then the nickle electrolysis anode solution pH that with copper concentration is 0.6g/l transfers to 5.0, and temperature is heated to 65 ℃; Then be that 1.4 ratio is mixed in the mol ratio of the copper in thio-carbonate in the decoppering agent and the nickle electrolysis anode solution, the input speed of control thiocarbonic acid SOH nickel slurry feed pump is 0.82m 3/ h is injected in the solution containing nickel feed pipe, mixes rear with 75.82m with nickle electrolysis anode solution 3The input speed of/h is injected into diameter 30cm by the solution containing nickel fresh feed pump, and length is in the pipeline reactor of 268m, and feed liquid residence time in pipeline reactor is 15 minutes.After reaction is finished in the electrolytic solution copper concentration reduce to 0.0018g/L, except copper nickel ratio in the copper ashes is 22.
Embodiment 3
The pH value that with nickel concentration is first the nickle electrolysis anode solution of 70g/l transfers to 5.0, then is 0.4 ratio and Na in the mol ratio of nickel in thio-carbonate and the electrolytic solution 2C 2S 5Solution hybrid reaction 15 minutes obtains thio-carbonate concentration and is the thiocarbonic acid SOH nickel slurry of 0.8mol/l as decoppering agent; Then the nickle electrolysis anode solution pH that with copper concentration is 0.5g/l transfers to 4.8, and temperature is heated to 60 ℃; Then be that 1.2 ratio is mixed in the mol ratio of the copper in thio-carbonate in the decoppering agent and the nickle electrolysis anode solution, the input speed of control thiocarbonic acid SOH nickel slurry feed pump is 0.82m 3/ h is injected in the solution containing nickel feed pipe, mixes rear with 75.82m with nickle electrolysis anode solution 3The input speed of/h is injected into diameter 35cm by the solution containing nickel fresh feed pump, and length is in the pipeline reactor of 329m, and feed liquid residence time in pipeline reactor is 25 minutes.After reaction is finished in the electrolytic solution copper concentration reduce to 0.0022g/L, except copper nickel ratio in the copper ashes is 27.
Embodiment 4
The pH value that with nickel concentration is first the nickle electrolysis anode solution of 70g/l transfers to 5.2, then is 0.6 ratio and Na in the mol ratio of nickel in thio-carbonate and the electrolytic solution 2CS 5Solution hybrid reaction 12 minutes refilters and obtains thiocarbonic acid SOH nickel solid, and then solid and nickel sulfate solution being mixed with and obtaining thio-carbonate concentration is that the thiocarbonic acid SOH nickel slurry of 1.5mol/l is as decoppering agent; Then the nickle electrolysis anode solution pH that with copper concentration is 0.45g/l transfers to 4.2, and temperature is heated to 63 ℃; Then be that 1.5 ratio is mixed in the mol ratio of the copper in thio-carbonate in the decoppering agent and the nickle electrolysis anode solution, the input speed of control thiocarbonic acid SOH nickel slurry feed pump is 0.18m 3/ h is injected in the solution containing nickel feed pipe, mixes rear with 75.18m with nickle electrolysis anode solution 3The input speed of/h is injected into diameter 50cm by the solution containing nickel fresh feed pump, and length is in the pipeline reactor of 383m, and feed liquid residence time in pipeline reactor is 60 minutes.After reaction is finished in the electrolytic solution copper concentration reduce to 0.0016g/L, except copper nickel ratio in the copper ashes is 17.
Embodiment 5
The pH value that with nickel concentration is first the nickel chloride solution of 70g/l transfers to 4.5, then is 0.8 ratio and K in the mol ratio of nickel in thio-carbonate and the electrolytic solution 2CS 3Solution hybrid reaction 15 minutes refilters and obtains thiocarbonic acid SOH nickel solid, then solid and aqueous solution is prepared thio-carbonate concentration and be the thiocarbonic acid SOH nickel slurry of 1.8mol/l as decoppering agent; Then the nickle electrolysis anode solution pH that with copper concentration is 0.7g/l transfers to 4.0, and temperature is heated to 66 ℃; Then be that 1.2 ratio is mixed in the mol ratio of the copper in thio-carbonate in the decoppering agent and the nickle electrolysis anode solution, the input speed of control thiocarbonic acid SOH nickel slurry feed pump is 0.55m 3/ h is injected in the solution containing nickel feed pipe, mixes rear with 75.55m with nickle electrolysis anode solution 3The input speed of/h is injected into diameter 45cm by the solution containing nickel fresh feed pump, and length is in the pipeline reactor of 158m, and feed liquid residence time in pipeline reactor is 20 minutes.After reaction is finished in the electrolytic solution copper concentration reduce to 0.0022g/L, except copper nickel ratio in the copper ashes is 30.
Embodiment 6
The pH value that with nickel concentration is first the nickel nitrate solution of 70g/l transfers to 5.0, then is 1.0 ratio and K in the mol ratio of nickel in thio-carbonate and the electrolytic solution 2C 2S 5Solution hybrid reaction 15 minutes prepares concentration and is thio-carbonate and be the thiocarbonic acid SOH nickel slurry of 1.0mol/l as decoppering agent; Then the nickle electrolysis anode solution pH that with copper concentration is 0.55g/l transfers to 4.2, and temperature is heated to 70 ℃; Then be that 1.22 ratio is mixed in the mol ratio of the copper in thio-carbonate in the decoppering agent and the nickle electrolysis anode solution, the input speed of control thiocarbonic acid SOH nickel slurry feed pump is 0.79m 3/ h is injected in the solution containing nickel feed pipe, mixes rear with 75.79m with nickle electrolysis anode solution 3The input speed of/h is injected into diameter 35cm by the solution containing nickel fresh feed pump, and length is in the pipeline reactor of 197m, and feed liquid residence time in pipeline reactor is 15 minutes.After reaction is finished in the electrolytic solution copper concentration reduce to 0.0025g/L, except copper nickel ratio in the copper ashes is 26.
Embodiment 7
The pH value that with nickel concentration is first the nickle electrolysis anode solution of 70g/l transfers to 4.9, then is 0.7 ratio and Na in the mol ratio of nickel in thio-carbonate and the electrolytic solution 2CS 4Solution hybrid reaction 30 minutes prepares concentration and is thio-carbonate and be the thiocarbonic acid SOH nickel slurry of 1.3mol/l as decoppering agent; Then the nickle electrolysis anode solution pH that with copper concentration is 0.52g/l transfers to 4.0, and temperature is heated to 90 ℃; Then be that 1.3 ratio is mixed in the mol ratio of the copper in thio-carbonate in the decoppering agent and the nickle electrolysis anode solution, the input speed of control thiocarbonic acid SOH nickel slurry feed pump is 0.61m 3/ h is injected in the solution containing nickel feed pipe, mixes rear with 75.61m with nickle electrolysis anode solution 3The input speed of/h is injected into diameter 25cm by the solution containing nickel fresh feed pump, and length is in the pipeline reactor of 514m, and feed liquid residence time in pipeline reactor is 20 minutes.After reaction is finished in the electrolytic solution copper concentration reduce to 0.0025g/L, except copper nickel ratio in the copper ashes is 26.
Embodiment 8
The pH value that with nickel concentration is first the nickle electrolysis anode solution of 70g/l transfers to 5.0, then is 0.5 ratio and Na in the mol ratio of nickel in thio-carbonate and the electrolytic solution 2CS 3Solution hybrid reaction 20 minutes refilters and obtains thiocarbonic acid SOH nickel solid, and then solid and nickel sulfate solution being mixed with and obtaining thio-carbonate concentration is that the thiocarbonic acid SOH nickel slurry of 1.6mol/l is as decoppering agent; Then the nickle electrolysis anode solution pH that with copper concentration is 0.65g/l transfers to 4.5, and temperature is heated to 65 ℃; Then be that 1.4 ratio is mixed in the mol ratio of the copper in thio-carbonate in the decoppering agent and the nickle electrolysis anode solution, the input speed of control thiocarbonic acid SOH nickel slurry feed pump is 0.67m 3/ h is injected in the solution containing nickel feed pipe, mixes rear with 75.67m with nickle electrolysis anode solution 3The input speed of/h is injected into diameter 32cm by the solution containing nickel fresh feed pump, and length is in the pipeline reactor of 235m, and feed liquid residence time in pipeline reactor is 15 minutes.After reaction is finished in the electrolytic solution copper concentration reduce to 0.0021g/L, except copper nickel ratio in the copper ashes is 28.

Claims (2)

1. the device of thiocarbonic acid SOH nickel deep copper removal from solution containing nickel, it is characterized in that, comprise thiocarbonic acid SOH nickel slurry tank, thiocarbonic acid SOH nickel slurry feed pump, solution containing nickel feed pipe, solution containing nickel fresh feed pump and pipeline reactor, described thiocarbonic acid SOH nickel slurry tank by thiocarbonic acid SOH nickel slurry feed pump be connected to the solution containing nickel feed pipe with mix sulphur for nickelous carbonate slurry and solution containing nickel, mixed thiocarbonic acid SOH nickel slurry and solution containing nickel export pipeline reactor to through the solution containing nickel fresh feed pump.
2. the device of a kind of thiocarbonic acid SOH nickel according to claim 1 deep copper removal from solution containing nickel, it is characterized in that, be provided with pipeline mixing device in the described pipeline reactor, described pipeline mixing device is cellular grid, in order to strengthen thiocarbonic acid SOH nickel slurry and solution containing nickel hybrid reaction.
CN2012203271919U 2012-07-06 2012-07-06 Device for deeply removing copper from nickel-containing solution by nickel thiocarbonate Expired - Fee Related CN202658207U (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102719671A (en) * 2012-07-06 2012-10-10 中南大学 Method and device for deeply removing copper of nickel thiocarbonate from nickel-containing solution
CN105821206A (en) * 2016-05-10 2016-08-03 中国恩菲工程技术有限公司 Solution purifying system and method
CN105838883A (en) * 2016-05-10 2016-08-10 中国恩菲工程技术有限公司 System and method for treating lead-bearing solution
CN105950867A (en) * 2016-05-10 2016-09-21 中国恩菲工程技术有限公司 System and method for treating copper-bearing solution
CN105950887A (en) * 2016-05-10 2016-09-21 中国恩菲工程技术有限公司 System and method for treating cadmium-bearing solution

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102719671A (en) * 2012-07-06 2012-10-10 中南大学 Method and device for deeply removing copper of nickel thiocarbonate from nickel-containing solution
CN102719671B (en) * 2012-07-06 2015-02-04 中南大学 Method and device for deeply removing copper of nickel thiocarbonate from nickel-containing solution
CN105821206A (en) * 2016-05-10 2016-08-03 中国恩菲工程技术有限公司 Solution purifying system and method
CN105838883A (en) * 2016-05-10 2016-08-10 中国恩菲工程技术有限公司 System and method for treating lead-bearing solution
CN105950867A (en) * 2016-05-10 2016-09-21 中国恩菲工程技术有限公司 System and method for treating copper-bearing solution
CN105950887A (en) * 2016-05-10 2016-09-21 中国恩菲工程技术有限公司 System and method for treating cadmium-bearing solution
WO2017193726A1 (en) * 2016-05-10 2017-11-16 中国恩菲工程技术有限公司 Solution purification system and method

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