CN201704381U - Extraction box - Google Patents
Extraction box Download PDFInfo
- Publication number
- CN201704381U CN201704381U CN2010202033153U CN201020203315U CN201704381U CN 201704381 U CN201704381 U CN 201704381U CN 2010202033153 U CN2010202033153 U CN 2010202033153U CN 201020203315 U CN201020203315 U CN 201020203315U CN 201704381 U CN201704381 U CN 201704381U
- Authority
- CN
- China
- Prior art keywords
- solvent
- solution
- chamber
- clarifying chamber
- mixing section
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
The utility model provides an extraction box for extracting and removing organic matters in cobalt solution, which has the advantages of simple operation and low consumption. The extraction box comprises a motor, a mixer, a filtering plate and a box body. The box body comprises a mixing chamber and a clarifying chamber communicated with each other on the upper part. A solution inlet is arranged at the lower part of the mixing chamber. A solvent inlet is arranged at the bottom of the mixing chamber. The mixer is arranged in the mixing chamber and is electrically connected with the motor. The filtering plate is vertically fixed at the bottom of the clarifying chamber. The clarifying chamber is divided into left and right parts; wherein, the right clarifying chamber is close to the mixing chamber; a solvent outlet is arranged at the bottom of the right clarifying chamber; a solution outlet is arranged on the upper part of the side face of the left clarifying chamber; the solution outlet is not higher than the top of the filtering plate. With compact structure and convenient operation, the extraction box can realize continuous and automatic production, thereby saving time and force. When solution flowing out of the solution outlet contains too many organic matters, the solution inlet, the solution outlet and the solvent inlet are closed. After standing, all bottom valves at the bottom of the extraction box and the solvent inlet are opened so that the solvent in light yellow at the lower part is discharged and then regenerated through fractional distillation.
Description
Technical field
The utility model relates to a kind of extraction box.
Background technology
Anode material of lithium battery before calcining, if carry organic class impurity secretly in its preceding operation cobalt chloride or the rose vitriol, shortcoming such as will cause the crystalline structure of the finished product poor, density is little, battery capacity is low.
Cobalt is as the raw material of a kind of anode material of lithium battery processing, is a kind of main existence form of cobalt ore when being applied to industry, so, how obtaining high purity, the cobalt salt that has good processing characteristics becomes investigators' a important subject.The waste material that the process of producing of cobalt salt normally will contain cobalt ore product or recovery through fragmentation, acidleach, removal of impurities, extraction, back extraction, remove operation such as oil refining and be prepared into purified cobalt chloride or rose vitriol etc., be the basis of production lithium battery material.
A large amount of patents has just been reported different extraction agent performances with document and how have been utilized extraction to carry out effective isolating method under the situation of multiple metal ion coexistence in the solution after acidleach, this technology has been used in the cognitive already also grasp of cobalt goods processing industry both at home and abroad at present, generally take earlier to go out impurity such as copper in the acidleach mixed solution, manganese, iron, aluminium, zinc with a certain trade mark extraction agent extracting and separating, and then with other model extraction agent slective extraction cobalts, realization effectively separates with nickel.We know, nearly all extraction agent, dilution are exactly a kind of organic substance with solvent oil itself, occur miscible inevitably with water in extraction process and carry phenomenon secretly, and organic for trace in the cobalt salt solution of how eliminating after the back extraction, relevant report is but paid close attention to very fewly.Factory continues to use with gac more and comes organism (promptly removing organism) in the adsorption removal cobalt liquor in production application.This organism method cost height that removes, efficient is low, the regeneration difficulty, and cobalt salt is adsorbed simultaneously and is difficult to reclaim, cause the cobalt rate of recovery low, the depleted gac pollutes to environment, and organic content is more than 20ppm in the cobalt liquor after the oil removing, can't satisfy the requirement of lithium battery material industry production, press for a kind of effective measure and solved this difficult problem.
The utility model content
The utility model provides a kind of extraction box, is used for extracting the organism that removes cobalt liquor, simple to operate, consume low.
Described extraction box, comprise motor, agitator, screen plate and casing, casing is made up of mixing section and the clarifying chamber that top is communicated with, the mixing section bottom is provided with solution inlet port, the bottom is provided with solvent inlet, and agitator is located in the mixing section, and is electrically connected with motor, the screen plate vertical fixing is in the bottom, clarifying chamber, the clarifying chamber is divided into left and right two portions, and wherein right clarifying chamber is near mixing section, and bottom, right clarifying chamber is provided with solvent outlet, top, side, clarifying chamber, a left side is provided with taphole, and described taphole is not higher than the screen plate top.The height of screen plate can be by the speed decision of extraction solution.
As preferred version, described mixing section comprises main mixing chamber and at least one time mixing section, main mixing chamber is positioned at outermost one side of clarifying chamber (promptly away from), be between main mixing chamber and time mixing section and be set up in parallel, be equipped with the agitator that is electrically connected with motor in each master or the inferior mixing section, solvent inlet and solution inlet port are located at the bottom and the bottom of main mixing chamber respectively, and the bottom of each time mixing section is equipped with bottom valve.Obviously, a plurality of agitators can be connected with same motor, also can be connected respectively with multiple electric motors.
Above-mentioned extraction box is used for extraction when removing the cobalt liquor organism, the solvent that will be used to extract and go out by acidleach, the cobalt chloride mother liquor that extraction and back extraction step obtain adds in the mixing section through solvent inlet and solution inlet port respectively, after mixing, naturally overflow to clarifying chamber's right part from the top connection of mixing section and clarifying chamber, here the solvent of being carried secretly since density much larger than cobalt liquor, can fall to the bottom, clarifying chamber rapidly, cobalt liquor then floats, through entering clarifying chamber's left part natural subsidence after the filter plate filtering separation, after taphole flows out, the little liquid integument screen plate 5 of the trace solvent that may contain in the cobalt liquor isolates and falls to the bottom, clarifying chamber, thereby obtains the cobalt liquor of organic content below 10ppm.Adopt that mixing section arranged side by side can make mixing more even more than two, further improve extraction efficiency.Suitable stirring velocity is 150～180 rev/mins, is preferably 180 rev/mins.The settled solvent in right clarifying chamber can be discharged from bottom valve, continues on for above-mentioned extraction step.Described solvent comprises extraction agent, and described extraction agent is 1-bromo-3-chloropropane, carbon trichloride, tetracol phenixin or 1-bromo-2-monochloroethane.As improvement, also contain solid cobaltic naphthenate in the described solvent, the quality of solid cobaltic naphthenate is 0.01%～0.1% of an extraction agent quality, is preferably 0.01%～0.015%.The applicant finds after deliberation: can make organic content in the cobalt salt solution from being reduced to more than the 35ppm below the 10ppm though use 1-bromo-3-chloropropane, carbon trichloride, tetracol phenixin or 1-bromo-2-monochloroethane to make solvent merely, but the cobalt liquor that the discovery of process mensuration removes behind the organism all is entrained with micro-above-mentioned extraction agent ninety-nine times out of a hundred, and organic content is also not really stable; The solid cobaltic naphthenate that in these extraction agents, adds 0.005%, 0.01%, 0.02%, 0.05%, 0.1% mass ratio as stablizer after, remove organism under the same conditions, add the stablizer of less than 0.01%, organic content fluctuates between 2.8-6.5ppm usually, the extraction agent that remains in the cobalt liquor is difficult to eliminate fully, increase gradually along with the stablizer addition, situation progressively takes a turn for the better, when addition reaches 0.01%, cobalt liquid oil content after the processing can reach 1.5-4.5ppm, the residual extraction agent content is very little in the solution, can't detect.This moment, cobalt liquor can satisfy the production needs of anode material of lithium battery fully.But solid cobaltic naphthenate price height is excessive for saving the therefore unsuitable addition of cost.
Above-mentioned extraction box compact construction, easy and simple to handle is used for the utility model and can realizes serialization, automatic production, and is time saving and energy saving.Once prepare solvent, can use repeatedly, move continuously more than 1 year and to keep removing organic effect.When too high, can directly closing solution inlet port, outlet and solvent inlet from the effusive solution organic content of taphole, again all bottom valves and the solvent inlet of extraction box bottom are opened after leaving standstill, make lower floor be lurid solvent and discharge, regenerate through fractionation.
The solvent that the utility model is used for extracting consumes low removing the organism process, preparation once can be used for removing the organism of cobalt liquor more than 1 year continuously, organic content is reduced to below the 10ppm, change simultaneously and still can be recycled very environmental protection after the solvent that comes out is handled through simple vacuum fractionation.
Described cobalt liquor by known acidleach go out, extraction and back extraction step obtain, be raw material preferably wherein with heterogenite or cobalt-containing alloy waste material, leach with sulfuric acid, extraction step after acidleach goes out is a prior art, preferred version is as follows: the aqueous solution that adopts P204 extraction acidleach to go out, the gained raffinate contacts with P507, separates to obtain organic phase.
With cobalt ore or to contain the cobalt reclaimed materials as follows through the concrete steps that acidleach goes out to obtain cobalt liquor (as cobalt chloride, rose vitriol, Xiao Suangu):
1. ball milling: heterogenite is milled to 80～120 orders through ball mill, preferably to 120 orders.
2. leach: according to liquid-solid ratio 3.0-3.6,80～90 ℃ of temperature of reaction were reacted 2.5～6.0 hours under the condition that reduction is leached, and preferred 4.0 hours, it is qualified after the pressure filter solid-liquid separation is collected filtrate that slag contains cobalt.
3. deironing: according to Fe in the filtrate
2+Content add the sodium chlorate of 0.25～0.40 times of amount (preferred 0.3 times of amount), in 80～95 ℃ of temperature (preferred 85 ℃), 20～45 minutes reaction times (preferred 30 minutes), deironing under endpoint pH 3.5～3.8 conditions is collected filtrate for later use after the pressure filter solid-liquid separation.
4. deliming, magnesium: the solution after the deironing filtration is pumped into reactive tank, the Sodium Fluoride deliming, the magnesium that add calcium, 3.5～6.0 times of amounts of magnesium ion concentration summation (preferred 4 times of amounts), keep 65～85 ℃ of temperature (preferred 80 ℃), filtrate is collected in about 1.5～3.0 hours (preferred 2.5 hours) of reaction under pH value 4.0～5.5 (preferred 5.0) condition after the pressure filter solid-liquid separation.
5.P204 abstraction impurity removal: will remove solution behind calcium, the magnesium through the P204 extraction liquid, further remove element cobalt solution by purifying such as copper, manganese, zinc, iron, the P204 extraction liquid is made up of P204 and solvent oil, wherein the concentration of volume percent of P204 is 18%～28%, be preferably 25%, solvent oil is selected the 260# solvent oil usually for use.
6.P507 collection cobalt: the P204 raffinate is passed through the P507 extraction liquid, extract the cobalt ion in the solution, the P507 extraction liquid is made up of P507 and solvent oil, and wherein the concentration of volume percent of P507 is 18%～28%, be preferably 25%, solvent oil is selected the 260# solvent oil usually for use.
7. back extraction: at the extraction box internal reaction, the solution that back extraction goes out is the cobalt chloride solution that contains the oily organism and be not less than 30ppm, and (this moment, if the solution of output was cobalt sulfate solution with the sulfuric acid back extraction of preparation with the P507 organic phase of the hydrochloric acid for preparing and load cobalt; Xiao Suangu promptly comes back extraction with the nitric acid of preparation).
Above-mentioned cobalt liquor can be obtained cobalt salt through following steps, and cobalt salt can be used for the production of lithium cell:
1. remove organism: solvent is added in the extraction box, and cobalt chloride mother liquor and solvent mixing, extraction in casing back extraction goes out after 2 minutes natural subsidence, can obtain the refining cobalt chloride solution of organic content less than 10ppm in the exit of water.
2. crystallization: heating under vacuum makes crystal through cooling, crystallization, filtration, drying after concentrating the purified cobalt chloride solution.
The utility model, compact construction, easy and simple to handle, can realize serialization, automatic production, time saving and energy saving, can guarantee extraction solvent and need can maximum area contact between the material of purification, accelerated rate of extraction, fast and effeciently remove the organic impurities in the liquid such as cobalt chloride, organic content such as the cobalt salt solution oil content after the oil removing are below 10ppm, no solid waste, cost is low, efficient is high, and the anode material of lithium battery that removes cobalt salt behind the organism and be raw material processing has satisfied the requirement of the low organic content of battery material.
Description of drawings
Fig. 1 is the structural representation of the used extraction box of the utility model.
Embodiment
The used extraction box structure of following examples is as shown in Figure 1: comprise motor 1, agitator 3, screen plate 5 and casing, casing is made up of mixing section 4 and the clarifying chamber 6 that top is communicated with, bottom, mixing section 4 side is provided with solution inlet port 2, agitator 3 is located in the mixing section 4, and is electrically connected with motor 1, and (material is polypropylene hollow fiber, aperture 30-50 micron to screen plate 5 for the fibre deposition plate; Hangzhou Kaihong Membrane Technology Co., Ltd.; The trade mark: PP, X50/80 MODIFIED PP), vertical fixing is 6 bottoms in the clarifying chamber, clarifying chamber 6 is divided into left and right two portions, right clarifying chamber is near mixing section 4, the bottom is provided with bottom valve 10, top, side, clarifying chamber, a left side is provided with taphole 7, and taphole 7 is not higher than the top of screen plate 5, and the height of screen plate 5 can be by the speed decision of extraction solution.Mixing section 4 comprises the primary and secondary mixing section that is set up in parallel, and main mixing chamber is positioned at the outside, promptly away from a side of clarifying chamber, is equipped with the agitator 3 that is electrically connected with motor 1 in the primary and secondary mixing section.The bottom of main mixing chamber is provided with solvent inlet 8, inferior mixing section bottom is provided with bottom valve 9.Extraction box is of a size of: 5.6m*2.6m*1.2m; Mixing section is of a size of: 1.4m*1.2m*1.2m; The clarifying chamber is of a size of: 3.9m*1.2m*1.2m; Screen plate: 1.2m*1.0m*0.0085m.
The used preparation process by the cobalt chloride solution (hereinafter to be referred as the cobalt chloride mother liquor) that acidleach goes out, extraction and back extraction step obtain of following examples is as follows:
1. ball milling: with heterogenite (African the Congo gold; The cobalt oxide raw ore; Contain cobalt 5.0%-12%) be milled to 120 order granularities through ball mill.
2. leach: according to the vitriol oil of liquid-solid ratio 3.3 addings 98%, 80～90 ℃ of temperature of reaction, reaction is 4.0 hours under the condition that reduction is leached, and treats that the content of cobalt in the cobalt slag is lower than at 2% o'clock, collects filtrate through the pressure filter solid-liquid separation.
3. deironing: record Fe in the filtrate
2+Content be 200ppm, in filtrate, add the sodium chlorate of 60ppm, in 85 ℃ of temperature, 30 minutes reaction times, deironing under endpoint pH 3.5～3.8 conditions is collected filtrate for later use after the pressure filter solid-liquid separation.The content of measuring after deironing is filtered that contains calcium ions and magnesium ions in the cobalt filtrate is respectively 100ppm and 150ppm.
4. deliming, magnesium: the solution after the deironing filtration is pumped into reactive tank, add the deliming of 1000ppm Sodium Fluoride, magnesium, keep 80 ℃ of temperature, reaction is 2.5 hours under pH value 5.0 conditions, collects filtrate after the pressure filter solid-liquid separation.
5.P204 abstraction impurity removal: will remove solution behind calcium, the magnesium through the P204 extraction agent, further remove element cobalt solution by purifying such as copper, manganese, zinc, iron, the P204 extraction agent is made up of P204 and solvent oil, wherein the concentration of volume percent of P204 is 25% (volume ratio that is P204 and solvent oil is 4: 12), and solvent oil is the 260# solvent oil.
6.P507 collection cobalt: with the P204 raffinate with 5dm
3The flow velocity of/s extracts the cobalt ion in the solution by the P507 extraction agent, and the P507 extraction agent is made up of P507 and solvent oil, and wherein the concentration of volume percent of P507 is 25% (volume ratio that is P507 and solvent oil is 4: 12), and solvent oil is the 260# solvent oil.
7. back extraction: with concentration is that the hydrochloric acid of 3M is according to 10dm
3The P507 organic phase of the flow velocity of/s and load cobalt is at the extraction box internal reaction, and the solution that back extraction goes out is the cobalt chloride mother liquor that contains oily organism 39ppm.
The technological operation rules of purification cobalt chloride solution are as follows:
Under 180 rev/mins of stirring velocitys, with solvent and cobalt chloride mother liquor (pH value 1.5-2.5, temperature is not more than 35 ℃), pump in the mixing section 4 (mixing section) and the stirring solvent mixing through solvent inlet 8 and solution inlet port 2 respectively, after carrying out secondary extraction, overflow and enter clarifying chamber's 6 right part sedimentations through the primary and secondary mixing section, through filter plate 5 filtering separation, enter clarifying chamber's 6 left parts again, flow out from taphole 7 after the sedimentation.The inflow velocity of cobalt chloride mother liquor is 1.8-2.0m
3/ h, the inflow velocity of control solvent, the volume ratio that makes mixing section internal solvent and cobalt chloride mother liquor is 1: 3.0-1: 3.5.Take-off rate and inflow velocity are basic identical.
Embodiment 1
Solvent is by 0.17 kilogram of solid cobaltic naphthenate and 1.0m
31-bromo-3-chloropropane mix and to obtain (mass percent concentration of solid cobaltic naphthenate is 0.01%), solvent and mother liquor volume ratio are 1: 3.3.
Under 180 rev/mins of stirring velocitys, with solvent and cobalt chloride mother liquor (pH value 1.5-2.5, temperature is not more than 35 ℃), in solution inlet port 2 pumps into mixing section 4 with the stirring solvent mixing, after carrying out secondary extraction, overflow and enter clarifying chamber's 6 right part sedimentations through the primary and secondary mixing section, through filter plate 5 filtering separation, enter clarifying chamber's 6 left parts again, flow out from taphole 7 after the sedimentation.The inflow velocity of cobalt chloride mother liquor is 1.8m
3/ h, take-off rate and inflow velocity are basic identical.The organic content of gained cobalt chloride solution is 2.3ppm.
Above-mentioned solvent need not regeneration after clarifying chamber's bottom valve is got rid of, can continue on for above-mentioned extraction process, handles the cobalt chloride mother liquor.The cobalt chloride mother liquor total amount of handling reaches 1100m
3After, the organic content of gained cobalt chloride solution is 3.4 ppm.
When the organic content of effusive cobalt chloride solution reaches 6.5ppm, with 0.98m
3Containing the smeary solvent discharges from extraction box and regenerates.During regeneration, rectifying under 76 ℃ of temperature, pressure-0.083MPa condition is collected after condensation, obtains 1-bromo-3-chloropropane 0.94m
3
Embodiment 2
Solvent is by 0.24 kilogram of solid cobaltic naphthenate and 1.0m
31-bromo-3-chloropropane mix and to obtain (mass percent concentration of solid cobaltic naphthenate is 0.015%), solvent: the mother liquor volume ratio is 1: 3.0.
Under 180 rev/mins of stirring velocitys, with solvent and cobalt chloride mother liquor (pH value 1.5-2.5, temperature is not more than 35 ℃), in solution inlet port 2 pumps into mixing section 4 with the stirring solvent mixing, after carrying out secondary extraction, overflow and enter clarifying chamber's 6 right part sedimentations through the primary and secondary mixing section, through filter plate 5 filtering separation, enter clarifying chamber's 6 left parts again, flow out from taphole 7 after the sedimentation.The inflow velocity of cobalt chloride mother liquor is 1.9m
3/ h, take-off rate and inflow velocity are basic identical.The organic content of gained cobalt chloride solution is 1.9ppm.
Above-mentioned solvent need not regeneration after clarifying chamber's bottom valve is got rid of, can continue on for above-mentioned extraction process, handles the cobalt chloride mother liquor.The cobalt chloride mother liquor total amount of handling reaches 1100m
3After, the organic content of gained cobalt chloride solution is 2.9ppm.
Embodiment 3
Solvent is by 0.225 kilogram of solid cobaltic naphthenate and 1.0m
31-bromo-3-chloropropane mix and to obtain (mass percent concentration of solid cobaltic naphthenate is 0.014%), solvent: the mother liquor volume ratio is 1: 3.5.
Under 180 rev/mins of stirring velocitys, with solvent and cobalt chloride mother liquor (pH value 1.5-2.5, temperature is not more than 35 ℃), in solution inlet port 2 pumps into mixing section 4 with the stirring solvent mixing, after carrying out secondary extraction, overflow and enter clarifying chamber's 6 right part sedimentations through the primary and secondary mixing section, through filter plate 5 filtering separation, enter clarifying chamber's 6 left parts again, flow out from taphole 7 after the sedimentation.The inflow velocity of cobalt chloride mother liquor is 1.8m
3/ h, take-off rate and inflow velocity are basic identical.The organic content of gained cobalt chloride solution is 3.1ppm.
Above-mentioned solvent need not regeneration after clarifying chamber's bottom valve is got rid of, can continue on for above-mentioned extraction process, handles the cobalt chloride mother liquor.The cobalt chloride mother liquor total amount of handling reaches 1100m
3After, the organic content of gained cobalt chloride solution is 3.7ppm.
Embodiment 4
Solvent is by 0.22 kilogram of solid cobaltic naphthenate and 1.0m
31-bromo-3-chloropropane mix and to obtain (mass percent concentration of solid cobaltic naphthenate is 0.014%), solvent: the mother liquor volume ratio is 1: 3.5.
Under 180 rev/mins of stirring velocitys, with solvent and cobalt chloride mother liquor (pH value 1.5-2.5, temperature is not more than 35 ℃), in solution inlet port 2 pumps into mixing section 4 with the stirring solvent mixing, after carrying out secondary extraction, overflow and enter clarifying chamber's 6 right part sedimentations through the primary and secondary mixing section, through filter plate 5 filtering separation, enter clarifying chamber's 6 left parts again, flow out from taphole 7 after the sedimentation.The inflow velocity of cobalt chloride mother liquor is 2.0m
3/ h, take-off rate and inflow velocity are basic identical.The organic content of gained cobalt chloride solution is 4.2ppm.
Above-mentioned solvent need not regeneration after clarifying chamber's bottom valve is got rid of, can continue on for above-mentioned extraction process, handles the cobalt chloride mother liquor.The cobalt chloride mother liquor total amount of handling reaches 1100m
3After, the organic content of gained cobalt chloride solution is 4.9ppm.
Embodiment 5
Solvent is by 0.225 kilogram of solid cobaltic naphthenate and 1.0m
31-bromo-3-chloropropane mix and to obtain (mass percent concentration of solid cobaltic naphthenate is 0.014%), solvent: the mother liquor volume ratio is 1: 3.0.
Under 180 rev/mins of stirring velocitys, with solvent and cobalt chloride mother liquor (pH value 1.5-2.5, temperature is not more than 35 ℃), in solution inlet port 2 pumps into mixing section 4 with the stirring solvent mixing, after carrying out secondary extraction, overflow and enter clarifying chamber's 6 right part sedimentations through the primary and secondary mixing section, through filter plate 5 filtering separation, enter clarifying chamber's 6 left parts again, flow out from taphole 7 after the sedimentation.The inflow velocity of cobalt chloride mother liquor is 1.8m
3/ h, take-off rate and inflow velocity are basic identical.The organic content of gained cobalt chloride solution is 2.7ppm.
Above-mentioned solvent need not regeneration after clarifying chamber's bottom valve is got rid of, can continue on for above-mentioned extraction process, handles the cobalt chloride mother liquor.The cobalt chloride mother liquor total amount of handling reaches 1100m
3After, the organic content of gained cobalt chloride solution is 3.5ppm.
Embodiment 6
Solvent is by 0.22 kilogram of solid cobaltic naphthenate and 1.0m
3Carbon trichloride mix and to obtain (mass percent concentration of solid cobaltic naphthenate be 0.014% convert be 0.015%), solvent: the mother liquor volume ratio is 1: 3.5.
Under 180 rev/mins of stirring velocitys, with solvent and cobalt chloride mother liquor (pH value 2-3, temperature is not more than 30 ℃), in solution inlet port 2 pumps into mixing section 4 with the stirring solvent mixing, after carrying out secondary extraction, overflow and enter clarifying chamber's 6 right part sedimentations through the primary and secondary mixing section, through filter plate 5 filtering separation, enter clarifying chamber's 6 left parts again, flow out from taphole 7 after the sedimentation.The inflow velocity of cobalt chloride mother liquor is 1.8m
3/ h, take-off rate and inflow velocity are basic identical.The organic content of gained cobalt chloride solution is 8ppm.
Above-mentioned solvent need not regeneration after clarifying chamber's bottom valve is got rid of, can continue on for above-mentioned extraction process, handles the cobalt chloride mother liquor.The cobalt chloride mother liquor total amount of handling reaches 110m
3After, the organic content of gained cobalt chloride solution is 8.4ppm.
Embodiment 7
Solvent is by 0.24 kilogram of solid cobaltic naphthenate and 1.0m
3Tetracol phenixin mix and to obtain (mass percent concentration of solid cobaltic naphthenate is 0.015%), solvent: the mother liquor volume ratio is 1: 3.0.
Under 180 rev/mins of stirring velocitys, with solvent and cobalt chloride mother liquor (pH value 2-3, temperature is not more than 30 ℃), in solution inlet port 2 pumps into mixing section 4 with the stirring solvent mixing, after carrying out secondary extraction, overflow and enter clarifying chamber's 6 right part sedimentations through the primary and secondary mixing section, through filter plate 5 filtering separation, enter clarifying chamber's 6 left parts again, flow out from taphole 7 after the sedimentation.The inflow velocity of cobalt chloride mother liquor is 1.8m
3/ h, take-off rate and inflow velocity are basic identical.The organic content of gained cobalt chloride solution is 5ppm.
Above-mentioned solvent need not regeneration after clarifying chamber's bottom valve is got rid of, can continue on for above-mentioned extraction process, handles the cobalt chloride mother liquor.The cobalt chloride mother liquor total amount of handling reaches 110m
3After, the organic content of gained cobalt chloride solution is 5.3ppm.
Embodiment 8
Solvent is by 0.17 kilogram of solid cobaltic naphthenate and 1.0m
31-bromo-2-monochloroethane mix and to obtain (mass percent concentration of solid cobaltic naphthenate is 0.01%), solvent: the mother liquor volume ratio is 1: 3.5.
Under 180 rev/mins of stirring velocitys, with solvent and cobalt chloride mother liquor (pH value 1.5-3.0, temperature is not more than 40 ℃), in solution inlet port 2 pumps into mixing section 4 with the stirring solvent mixing, after carrying out secondary extraction, overflow and enter clarifying chamber's 6 right part sedimentations through the primary and secondary mixing section, through filter plate 5 filtering separation, enter clarifying chamber's 6 left parts again, flow out from taphole 7 after the sedimentation.The inflow velocity of cobalt chloride mother liquor is 2.0m
3/ h, take-off rate and inflow velocity are basic identical.The organic content of gained cobalt chloride solution is 5.5ppm.
Above-mentioned solvent need not regeneration after clarifying chamber's bottom valve is got rid of, can continue on for above-mentioned extraction process, handles the cobalt chloride mother liquor.The cobalt chloride mother liquor total amount of handling reaches 110m
3After, the organic content of gained cobalt chloride solution is 5.9ppm.
Claims (3)
1. extraction box, it is characterized in that, comprise motor, agitator, screen plate and casing, casing is made up of mixing section and the clarifying chamber that top is communicated with, and the mixing section bottom is provided with solution inlet port, and the bottom is provided with solvent inlet, agitator is located in the mixing section, and be electrically connected with motor, the screen plate vertical fixing is divided into left and right two portions in the bottom, clarifying chamber with the clarifying chamber, wherein right clarifying chamber is near mixing section, bottom, right clarifying chamber is provided with solvent outlet, and top, side, left clarifying chamber is provided with taphole, and described taphole is not higher than the screen plate top.
2. extraction box as claimed in claim 1, it is characterized in that, described mixing section comprises main mixing chamber and at least one time mixing section, main mixing chamber is positioned at outermost, be between main mixing chamber and time mixing section and be set up in parallel, be equipped with the agitator that is electrically connected with motor in each master or the inferior mixing section, solvent inlet and solution inlet port are located at the bottom and the bottom of main mixing chamber respectively, and the bottom of each time mixing section is equipped with bottom valve.
3. extraction box as claimed in claim 2 is characterized in that, described mixing section comprises main mixing chamber and one mixing section.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010202033153U CN201704381U (en) | 2010-05-26 | 2010-05-26 | Extraction box |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010202033153U CN201704381U (en) | 2010-05-26 | 2010-05-26 | Extraction box |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN201704381U true CN201704381U (en) | 2011-01-12 |
Family
ID=43441535
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010202033153U Expired - Lifetime CN201704381U (en) | 2010-05-26 | 2010-05-26 | Extraction box |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN201704381U (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106867568A (en) * | 2015-12-10 | 2017-06-20 | 中国石油天然气股份有限公司 | Double-tank pre-extraction device and double-tank pre-extraction method |
| CN107252572A (en) * | 2017-07-24 | 2017-10-17 | 河北金力新能源科技股份有限公司 | A kind of efficient low-consume water seal lithium ion cell film extraction process |
| CN109985415A (en) * | 2019-04-19 | 2019-07-09 | 杭州天易成环保设备股份有限公司 | The energy-efficient automatic control extracting system of one kind and its extracting process |
| WO2022228233A1 (en) * | 2021-04-25 | 2022-11-03 | 湖南金源新材料股份有限公司 | Method for extracting and preparing battery-grade lithium carbonate from p507 raffinate, and extraction device |
-
2010
- 2010-05-26 CN CN2010202033153U patent/CN201704381U/en not_active Expired - Lifetime
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106867568A (en) * | 2015-12-10 | 2017-06-20 | 中国石油天然气股份有限公司 | Double-tank pre-extraction device and double-tank pre-extraction method |
| CN106867568B (en) * | 2015-12-10 | 2018-07-13 | 中国石油天然气股份有限公司 | Double-tank pre-extraction device and double-tank pre-extraction method |
| CN107252572A (en) * | 2017-07-24 | 2017-10-17 | 河北金力新能源科技股份有限公司 | A kind of efficient low-consume water seal lithium ion cell film extraction process |
| CN109985415A (en) * | 2019-04-19 | 2019-07-09 | 杭州天易成环保设备股份有限公司 | The energy-efficient automatic control extracting system of one kind and its extracting process |
| CN109985415B (en) * | 2019-04-19 | 2023-12-08 | 杭州天易成新能源科技股份有限公司 | Efficient energy-saving automatic control extraction system and extraction method thereof |
| WO2022228233A1 (en) * | 2021-04-25 | 2022-11-03 | 湖南金源新材料股份有限公司 | Method for extracting and preparing battery-grade lithium carbonate from p507 raffinate, and extraction device |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101831547B (en) | Method for purifying cobalt solution | |
| JP7482558B2 (en) | Process, Apparatus, and System for Recovering Materials from Batteries | |
| CN101383440B (en) | Method for recycling and preparing superfine nickel powder from nickel-hydrogen cell | |
| CN102061390B (en) | Method for directly producing high-purity electronic level cobaltous sulfate by using cobalt-containing waste | |
| CN102531002B (en) | Method for purifying lithium carbonate | |
| CN101476041B (en) | Method for separating and recycling copper, nickel and regenerative plastic from waste electroplating plastic | |
| KR101648693B1 (en) | Valuable metals recovery system from the waste slurry of lithium secondary battery | |
| CN107381604A (en) | A kind of method that lithium carbonate is reclaimed from ferric phosphate lithium cell | |
| CN102557153B (en) | Method for removing calcium-magnesium impurities from nickel sulfate solution | |
| CN107416908B (en) | A kind of method that low cost prepares high-purity sulphuric acid manganese solution | |
| CN201704381U (en) | Extraction box | |
| CN104659438A (en) | Method for preparing ternary positive electrode material precursor by virtue of waste batteries | |
| CN101974687A (en) | Extraction process for preparing electronic-grade cobalt sulfate from cobalt-containing waste material | |
| CN113321194A (en) | Method for recovering phosphorus iron slag after lithium extraction from waste lithium iron phosphate powder | |
| CN107083484A (en) | A kind of method that metal is reclaimed from waste lithium cell | |
| CN109761250A (en) | A method of lithium ion sieve is prepared using waste and old lithium ion battery | |
| CN102088124A (en) | High-purity polymetallic-element solid mixed salt and preparation method and application thereof | |
| CN105293584A (en) | Method for purifying manganese sulfate solution | |
| CN113122725A (en) | Method for improving metal recovery rate and purity of waste lithium battery | |
| CN102010999B (en) | Method for separating impurities from cobalt and/or nickel solution by non-saponifiable extraction | |
| CN101760652B (en) | Technological method for treating refractory complex molybdenum ore by combined dressing and smelting process | |
| CN102643986A (en) | Method for producing electrolytic manganese by taking pyrolusite as raw material through wet method reduction leaching | |
| CN102965520B (en) | Method for separating and enriching copper in leachate of acid leaching sulfide mine tailing | |
| CN102994778A (en) | Method for separating and enriching cobalt from leach liquor used for pickling and vulcanizing tailing | |
| CN211004551U (en) | Device for recovering iodine from iodine-containing ion waste liquid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address |
Address after: 225400 No. 8 Binjiang North Road, Taixing Economic Development Zone, Jiangsu Patentee after: Grammy (Jiangsu) cobalt industry Limited by Share Ltd Address before: 225400 Taixing Economic Development Zone, Jiangsu, Binjiang, North Road, No. 8, No. Patentee before: Jiangsu Cobalt Nickel Metal Co., Ltd. |
|
| CP03 | Change of name, title or address | ||
| CX01 | Expiry of patent term |
Granted publication date: 20110112 |
|
| CX01 | Expiry of patent term |