CN116143185A - Method for preparing high-purity cobalt sulfate from electrolytic manganese sulfide slag - Google Patents
Method for preparing high-purity cobalt sulfate from electrolytic manganese sulfide slag Download PDFInfo
- Publication number
- CN116143185A CN116143185A CN202211579679.5A CN202211579679A CN116143185A CN 116143185 A CN116143185 A CN 116143185A CN 202211579679 A CN202211579679 A CN 202211579679A CN 116143185 A CN116143185 A CN 116143185A
- Authority
- CN
- China
- Prior art keywords
- current
- pulse width
- determining
- current output
- manganese
- 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.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 48
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 title claims abstract description 35
- 229940044175 cobalt sulfate Drugs 0.000 title claims abstract description 34
- 229910000361 cobalt sulfate Inorganic materials 0.000 title claims abstract description 34
- 239000002893 slag Substances 0.000 title claims abstract description 30
- CADICXFYUNYKGD-UHFFFAOYSA-N sulfanylidenemanganese Chemical compound [Mn]=S CADICXFYUNYKGD-UHFFFAOYSA-N 0.000 title claims abstract description 27
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims abstract description 78
- 230000000903 blocking effect Effects 0.000 claims abstract description 50
- 229940099596 manganese sulfate Drugs 0.000 claims abstract description 28
- 239000011702 manganese sulphate Substances 0.000 claims abstract description 28
- 235000007079 manganese sulphate Nutrition 0.000 claims abstract description 28
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims abstract description 28
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 claims abstract description 16
- 238000007873 sieving Methods 0.000 claims abstract description 7
- 238000012544 monitoring process Methods 0.000 claims description 33
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 24
- 238000011217 control strategy Methods 0.000 claims description 21
- 238000001914 filtration Methods 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000012535 impurity Substances 0.000 claims description 18
- 239000012074 organic phase Substances 0.000 claims description 15
- 229910017052 cobalt Inorganic materials 0.000 claims description 14
- 239000010941 cobalt Substances 0.000 claims description 14
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 14
- 239000000706 filtrate Substances 0.000 claims description 12
- 238000002386 leaching Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000003350 kerosene Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 239000002244 precipitate Substances 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000000605 extraction Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000012806 monitoring device Methods 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- 239000013049 sediment Substances 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 4
- YPIFGDQKSSMYHQ-UHFFFAOYSA-N 7,7-dimethyloctanoic acid Chemical compound CC(C)(C)CCCCCC(O)=O YPIFGDQKSSMYHQ-UHFFFAOYSA-N 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 3
- 239000005843 Thiram Substances 0.000 claims description 3
- LRDDEBYPNRKRRK-UHFFFAOYSA-N [Mg].[Co].[Ni] Chemical compound [Mg].[Co].[Ni] LRDDEBYPNRKRRK-UHFFFAOYSA-N 0.000 claims description 3
- GZMKWMMWAHQTHD-UHFFFAOYSA-L [Mn++].OS([O-])(=O)=O.OS([O-])(=O)=O Chemical compound [Mn++].OS([O-])(=O)=O.OS([O-])(=O)=O GZMKWMMWAHQTHD-UHFFFAOYSA-L 0.000 claims description 3
- MYYPUXZNVLDNLK-UHFFFAOYSA-N [Ni].[Co].S(O)(O)(=O)=O Chemical compound [Ni].[Co].S(O)(O)(=O)=O MYYPUXZNVLDNLK-UHFFFAOYSA-N 0.000 claims description 3
- 239000008346 aqueous phase Substances 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 3
- CJDPJFRMHVXWPT-UHFFFAOYSA-N barium sulfide Chemical class [S-2].[Ba+2] CJDPJFRMHVXWPT-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000005868 electrolysis reaction Methods 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- ATTFYOXEMHAYAX-UHFFFAOYSA-N magnesium nickel Chemical compound [Mg].[Ni] ATTFYOXEMHAYAX-UHFFFAOYSA-N 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 239000011572 manganese Substances 0.000 claims description 3
- 239000011268 mixed slurry Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 3
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 239000012286 potassium permanganate Substances 0.000 claims description 3
- 238000007670 refining Methods 0.000 claims description 3
- 238000007127 saponification reaction Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- YOCZZJWFWDUAAR-UHFFFAOYSA-N sulfanyl-sulfanylidene-bis(2,4,4-trimethylpentyl)-$l^{5}-phosphane Chemical compound CC(C)(C)CC(C)CP(S)(=S)CC(C)CC(C)(C)C YOCZZJWFWDUAAR-UHFFFAOYSA-N 0.000 claims description 3
- 230000002195 synergetic effect Effects 0.000 claims description 3
- 229960002447 thiram Drugs 0.000 claims description 3
- KUAZQDVKQLNFPE-UHFFFAOYSA-N thiram Chemical compound CN(C)C(=S)SSC(=S)N(C)C KUAZQDVKQLNFPE-UHFFFAOYSA-N 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 14
- 230000008569 process Effects 0.000 abstract description 8
- 239000000126 substance Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- 230000006870 function Effects 0.000 description 8
- 230000008901 benefit Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 2
- 238000003491 array Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 230000019635 sulfation Effects 0.000 description 2
- 238000005670 sulfation reaction Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003674 animal food additive Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/10—Sulfates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/02—Oxides; Hydroxides
-
- 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
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention belongs to the technical field of chemical materials, and discloses a method for preparing high-purity cobalt sulfate from electrolytic manganese sulfide slag, which adopts manganese sulfate solution prepared from rhodochrosite and manganese sulfate solution prepared from industrial manganese sulfate by dissolving; preparing manganese dioxide by manganese sulfate; and crushing and sieving manganese dioxide and electrolytic manganese sulfide slag. The invention can prepare high-quality manganese dioxide by a manganese dioxide preparation method; thereby greatly improving the quality of preparing cobalt sulfate; meanwhile, the current output current and the current output pulse width of the motor of the centrifugal device can be obtained in the running process of the centrifugal device through the centrifugal control method of the centrifugal device, so that the blocking condition of the current top cover of the centrifugal device is judged by combining the obtained current output current and the obtained current output pulse width, the safety is greatly improved, and the normal preparation is ensured.
Description
Technical Field
The invention belongs to the technical field of chemical materials, and particularly relates to a method for preparing high-purity cobalt sulfate from electrolytic manganese sulfide slag.
Background
Cobalt sulfate is an inorganic compound, has a chemical formula of CoSO4 and is rose-red crystalline powder, and is mainly used as a ceramic glaze and paint drier, is also used for electroplating, alkaline batteries and producing cobalt-containing pigment and other cobalt products, and can also be used as a catalyst, an analysis reagent, a feed additive, a tire adhesive, a lithopone additive and the like; however, the existing method for preparing high-purity cobalt sulfate from electrolytic manganese sulfide slag adopts poor quality of manganese dioxide raw materials, and affects the quality of preparing cobalt sulfate; meanwhile, the centrifugal device adopted in the preparation process is easy to generate safety accidents, and normal preparation is influenced.
Through the above analysis, the problems and defects existing in the prior art are as follows:
(1) The existing method for preparing high-purity cobalt sulfate from electrolytic manganese sulfide slag adopts poor quality of manganese dioxide raw materials, and influences the quality of preparing cobalt sulfate.
(2) The centrifugal device adopted in the preparation process is easy to generate safety accidents, and the normal operation of the preparation is influenced.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides a method for preparing high-purity cobalt sulfate from electrolytic manganese sulfide slag.
The invention is realized in such a way that a method for preparing high-purity cobalt sulfate from electrolytic manganese sulfide slag comprises the following steps:
step one, configuring parameters of monitoring equipment, and monitoring the working state of a crushing device through the monitoring equipment; crushing rhodochrosite by a crushing device and sieving; mixing rhodochrosite powder with water of the same mass at room temperature; fully mixing the mixed slurry with sodium hydroxide or ammonium metavanadate, stirring at the temperature of 66 ℃, and continuously introducing air; filtering and separating to obtain precipitate and filtrate; finally, drying the obtained precipitate at 55 ℃ to obtain sulfur-removed rhodochrosite; the manganese sulfate solution prepared from rhodochrosite is adopted, and industrial manganese sulfate is dissolved to prepare the manganese sulfate solution; preparing manganese dioxide by manganese sulfate; crushing and sieving manganese dioxide and electrolytic manganese sulfide slag;
the monitoring device monitors the method:
monitoring voltage data of the crushing device through a voltmeter in the monitoring equipment;
monitoring current data of the crushing device through an ammeter in the monitoring equipment;
monitoring resistance data of the crushing device through a resistance meter in the monitoring equipment;
monitoring the comminution device fault data by a diagnostic circuit in the monitoring device;
step two, adding dilute sulfuric acid, saponified P204 and sulfonated kerosene into the sieved manganese dioxide and electrolytic manganese sulfide slag to obtain a manganese-loaded organic phase and a cobalt-nickel-magnesium-rich solution;
step three, taking cobalt-rich nickel-magnesium solution, and adding saponified neodecanoic acid, sulfonated kerosene, dilute sulfuric acid and saponified P507-Cyanex301 to obtain cobalt-rich organic phase and nickel sulfate solution; separating out a cobalt-rich organic phase, adding sulfuric acid for back extraction to obtain a high-purity cobalt-rich sulfate solution and a P507-Cyanex301 organic phase;
and step four, separating high-purity cobalt sulfate-enriched solution, evaporating, concentrating, crystallizing and centrifuging by a centrifugal device to obtain high-purity cobalt sulfate.
Further, the mass ratio of the manganese dioxide to the electrolytic sulfation slag is 3:1, the mass concentration of the dilute sulfuric acid is 100g/L, the liquid-solid ratio of the reaction is 8:1, the leaching temperature is 95 ℃, the oxygen pressure is 1MPa, the leaching time is 190min, and the end point pH of leaching is 5;
the pH value of the separated cobalt-nickel sulfuric acid solution is adjusted to 5; the fourth organic extractant is prepared by mixing a P507-Cyanex301 synergistic extraction system with sulfonated kerosene according to the volume fraction of 10% -40%, wherein the mass ratio of the P507 to the Cyanex301 is 3:1, and then the mixture is saponified by sodium hydroxide, the saponification rate is 53%, and the O/A=3:1 of an organic phase to an aqueous phase is achieved.
Further, the method for preparing manganese dioxide comprises the following steps:
(1) The manganese sulfate solution prepared from rhodochrosite is adopted, and industrial manganese sulfate is dissolved to prepare the manganese sulfate solution; then refining and removing impurities; inputting the manganese sulfate leaching solution into a container, adding modified barium sulfide, and starting a stirring rod arranged on an outer shaft to stir so as to precipitate the solution; lifting the outer shaft upwards to expose a section of the hollow inner shaft arranged in the outer shaft close to the bottom end of the container, and filtering out sediment from the solution in the container through the exposed section of the inner shaft;
(2) The filtered filtrate flows out from the inner cavity of the inner shaft, and the flowing filtrate enters a purifying tank arranged at the lower side of the container; adding sodium thiram into the purifying pond to react with the filtrate to generate precipitate; after the reaction is finished, filtering out sediment by a filtering device at the bottom of the purifying tank to obtain purified liquid; performing two-stage impurity removal on the purifying liquid;
(3) Standing the solution subjected to the second-stage impurity removal and filtration, and carrying out superfine filtration to the solution in a heating container for heating; and then the solution in the heating container is conveyed to a diaphragm electrolytic tank, the sulfuric acid-manganese sulfate system is adopted for electrolysis, manganese dioxide is separated out on the anode, and the separated manganese dioxide is peeled off, crushed, rinsed, milled and blended to obtain a manganese dioxide product.
Further, the stirring time was 45min.
Further, the filter device comprises a sealing cover plate which is arranged at the bottom of the purifying tank and is movably connected with the purifying tank, and a filter plate is arranged on the cover plate.
Further, the second-stage impurity removal is to add potassium permanganate for first-stage impurity removal, and then add activated carbon for second-stage impurity removal.
Further, the centrifugal control method of the centrifugal device comprises the following steps:
1) Configuring parameters of a centrifugal device, and obtaining the current output current and the current output pulse width of a motor of the centrifugal device through monitoring equipment;
2) Determining a target control strategy of the centrifugal device motor according to the current output current and the current output pulse width; and controlling the centrifugal device motor to execute the target control strategy.
Further, the determining a target control strategy of the centrifugal device motor according to the current output current and the current output pulse width includes:
determining the blocking probability of blocking the top cover of the centrifugal device according to the current output current and the current output pulse width;
and determining a target control strategy of the motor of the centrifugal device according to the blocking probability.
Further, the determining, according to the current output current and the current output pulse width, a blocking probability that a top cover of the centrifugal device is blocked includes:
determining a current influence factor for judging the blocking condition of the top cover according to the current output current;
determining a pulse width influence factor for judging the blocking condition of the top cover according to the current output pulse width;
calculating blocking probability of the top cover being blocked according to the current influence factor and the pulse width influence factor;
the calculating the blocking probability of the top cover being blocked according to the current influence factor and the pulse width influence factor comprises the following steps:
A＝K*i+(1-K)*t
wherein A is the blocking probability, K is the reference factor, i is the current influencing factor, and t is the pulse width influencing factor.
Further, the determining a current influence factor for determining the blocking condition of the top cover according to the current output current includes:
inputting the current output current to a preset membership function;
and determining the membership degree output by the preset membership function as a current influence factor for judging the blocking condition of the top cover.
The determining a pulse width influence factor for determining the blocking condition of the top cover according to the current output pulse width comprises the following steps:
inputting the current output pulse width to a preset membership function;
determining the membership degree output by the preset membership function as a pulse width influence factor for judging the blocking condition of the top cover;
the determining a target control strategy of the centrifugal device motor according to the blocking probability comprises the following steps:
determining a probability interval in which the blocking probability is located;
according to a preset corresponding relation, determining a control strategy corresponding to the probability interval as a target control strategy of the centrifugal device motor;
the device for obtaining the output pulse width comprises a magnetic piece for generating a pulse signal and a Hall element for determining the pulse signal width, and the device for obtaining the current output pulse width comprises:
acquiring a current pulse signal acquired by the device;
and determining the width of the current pulse signal as the current output pulse width.
In combination with the above technical solution and the technical problems to be solved, please analyze the following aspects to provide the following advantages and positive effects:
first, aiming at the technical problems in the prior art and the difficulty in solving the problems, the technical problems solved by the technical proposal of the invention are analyzed in detail and deeply by tightly combining the technical proposal to be protected, the results and data in the research and development process, and the like, and some technical effects brought after the problems are solved have creative technical effects. The specific description is as follows:
the invention can prepare high-quality manganese dioxide by a manganese dioxide preparation method; thereby greatly improving the quality of preparing cobalt sulfate; meanwhile, the current output current and the current output pulse width of the motor of the centrifugal device can be obtained in the running process of the centrifugal device through the centrifugal control method of the centrifugal device, so that the blocking condition of the current top cover of the centrifugal device is judged by combining the obtained current output current and the obtained current output pulse width, the safety is greatly improved, and the normal preparation is ensured.
Secondly, the technical scheme is regarded as a whole or from the perspective of products, and the technical scheme to be protected has the following technical effects and advantages:
the invention can prepare high-quality manganese dioxide by a manganese dioxide preparation method; thereby greatly improving the quality of preparing cobalt sulfate; meanwhile, the current output current and the current output pulse width of the motor of the centrifugal device can be obtained in the running process of the centrifugal device through the centrifugal control method of the centrifugal device, so that the blocking condition of the current top cover of the centrifugal device is judged by combining the obtained current output current and the obtained current output pulse width, the safety is greatly improved, and the normal preparation is ensured.
Drawings
FIG. 1 is a flow chart of a method for preparing high-purity cobalt sulfate from electrolytic manganese sulfide slag according to an embodiment of the invention.
Fig. 2 is a flow chart of a method for preparing manganese dioxide according to an embodiment of the present invention.
Fig. 3 is a flowchart of a centrifugal control method of a centrifugal device according to an embodiment of the invention.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
1. The embodiments are explained. In order to fully understand how the invention may be embodied by those skilled in the art, this section is an illustrative embodiment in which the claims are presented for purposes of illustration.
As shown in fig. 1, the invention provides a method for preparing high-purity cobalt sulfate from electrolytic manganese sulfide slag, which comprises the following steps:
s101, configuring parameters of monitoring equipment, and monitoring the working state of the crushing device through the monitoring equipment; crushing rhodochrosite by a crushing device and sieving; mixing rhodochrosite powder with water of the same mass at room temperature; fully mixing the mixed slurry with sodium hydroxide or ammonium metavanadate, stirring at the temperature of 66 ℃, and continuously introducing air; filtering and separating to obtain precipitate and filtrate; finally, drying the obtained precipitate at 55 ℃ to obtain sulfur-removed rhodochrosite; the manganese sulfate solution prepared from rhodochrosite is adopted, and industrial manganese sulfate is dissolved to prepare the manganese sulfate solution; preparing manganese dioxide by manganese sulfate; crushing and sieving manganese dioxide and electrolytic manganese sulfide slag;
the monitoring device monitors the method:
monitoring voltage data of the crushing device through a voltmeter in the monitoring equipment;
monitoring current data of the crushing device through an ammeter in the monitoring equipment;
monitoring resistance data of the crushing device through a resistance meter in the monitoring equipment;
monitoring the comminution device fault data by a diagnostic circuit in the monitoring device;
s102, adding dilute sulfuric acid, saponified P204 and sulfonated kerosene into sieved manganese dioxide and electrolytic manganese sulfide slag to obtain a manganese-loaded organic phase and a cobalt-nickel-magnesium-rich solution;
s103, taking cobalt-rich nickel-magnesium solution, and adding saponified neodecanoic acid, sulfonated kerosene, dilute sulfuric acid and saponified P507-Cyanex301 to obtain cobalt-rich organic phase and nickel sulfate solution; separating out a cobalt-rich organic phase, adding sulfuric acid for back extraction to obtain a high-purity cobalt-rich sulfate solution and a P507-Cyanex301 organic phase;
s104, separating out a high-purity cobalt sulfate-rich solution, evaporating, concentrating, crystallizing and centrifuging by a centrifugal device to obtain the high-purity cobalt sulfate.
The mass ratio of manganese dioxide to electrolytic sulfation slag is 3:1, the mass concentration of dilute sulfuric acid is 100g/L, the liquid-solid ratio of reaction is 8:1, the leaching temperature is 95 ℃, the oxygen pressure is 1MPa, the leaching time is 190min, and the end point pH of leaching is 5;
the pH value of the separated cobalt-nickel sulfuric acid solution is adjusted to 5; the fourth organic extractant is prepared by mixing a P507-Cyanex301 synergistic extraction system with sulfonated kerosene according to the volume fraction of 10% -40%, wherein the mass ratio of the P507 to the Cyanex301 is 3:1, and then the mixture is saponified by sodium hydroxide, the saponification rate is 53%, and the O/A=3:1 of an organic phase to an aqueous phase is achieved.
As shown in fig. 2, the method for preparing manganese dioxide provided by the invention is as follows:
s201, adopting a manganese sulfate solution prepared from rhodochrosite, and dissolving industrial manganese sulfate to prepare the manganese sulfate solution; then refining and removing impurities; inputting the manganese sulfate leaching solution into a container, adding modified barium sulfide, and starting a stirring rod arranged on an outer shaft to stir so as to precipitate the solution; lifting the outer shaft upwards to expose a section of the hollow inner shaft arranged in the outer shaft close to the bottom end of the container, and filtering out sediment from the solution in the container through the exposed section of the inner shaft;
s202, filtering the filtrate to flow out from the inner cavity of the inner shaft, and enabling the flowing filtrate to enter a purifying tank arranged at the lower side of the container; adding sodium thiram into the purifying pond to react with the filtrate to generate precipitate; after the reaction is finished, filtering out sediment by a filtering device at the bottom of the purifying tank to obtain purified liquid; performing two-stage impurity removal on the purifying liquid;
s203, standing the solution after the two-stage impurity removal and filtration, and carrying out superfine filtration to the solution in a heating container for heating; and then the solution in the heating container is conveyed to a diaphragm electrolytic tank, the sulfuric acid-manganese sulfate system is adopted for electrolysis, manganese dioxide is separated out on the anode, and the separated manganese dioxide is peeled off, crushed, rinsed, milled and blended to obtain a manganese dioxide product.
The stirring time provided by the invention is 45min.
The filtering device provided by the invention comprises a sealing cover plate which is arranged at the bottom of the purifying tank and is movably connected, and a filter plate is arranged on the cover plate.
The second-stage impurity removal provided by the invention is to add potassium permanganate for first-stage impurity removal, and then add activated carbon for second-stage impurity removal.
As shown in fig. 3, the centrifugal control method of the centrifugal device provided by the invention is as follows:
s301, configuring parameters of a centrifugal device, and obtaining the current output current and the current output pulse width of a motor of the centrifugal device through monitoring equipment;
s302, determining a target control strategy of the motor of the centrifugal device according to the current output current and the current output pulse width; and controlling the centrifugal device motor to execute the target control strategy.
The invention provides a method for determining a target control strategy of a motor of a centrifugal device according to the current output current and the current output pulse width, comprising the following steps:
determining the blocking probability of blocking the top cover of the centrifugal device according to the current output current and the current output pulse width;
and determining a target control strategy of the motor of the centrifugal device according to the blocking probability.
The invention provides a method for determining the blocking probability of the top cover of the centrifugal device according to the current output current and the current output pulse width, comprising the following steps:
determining a current influence factor for judging the blocking condition of the top cover according to the current output current;
determining a pulse width influence factor for judging the blocking condition of the top cover according to the current output pulse width;
calculating blocking probability of the top cover being blocked according to the current influence factor and the pulse width influence factor;
the calculating the blocking probability of the top cover being blocked according to the current influence factor and the pulse width influence factor comprises the following steps:
A＝K*i+(1-K)*t
wherein A is the blocking probability, K is the reference factor, i is the current influencing factor, and t is the pulse width influencing factor.
The invention provides a method for determining a current influence factor for judging the blocking condition of a top cover according to the current output current, which comprises the following steps:
inputting the current output current to a preset membership function;
determining the membership degree output by the preset membership function as a current influence factor for judging the blocking condition of the top cover;
the determining a pulse width influence factor for determining the blocking condition of the top cover according to the current output pulse width comprises the following steps:
inputting the current output pulse width to a preset membership function;
determining the membership degree output by the preset membership function as a pulse width influence factor for judging the blocking condition of the top cover;
the determining a target control strategy of the centrifugal device motor according to the blocking probability comprises the following steps:
determining a probability interval in which the blocking probability is located;
according to a preset corresponding relation, determining a control strategy corresponding to the probability interval as a target control strategy of the centrifugal device motor;
the device for obtaining the output pulse width comprises a magnetic piece for generating a pulse signal and a Hall element for determining the pulse signal width, and the device for obtaining the current output pulse width comprises:
acquiring a current pulse signal acquired by the device;
and determining the width of the current pulse signal as the current output pulse width.
2. Application example. In order to prove the inventive and technical value of the technical solution of the present invention, this section is an application example on specific products or related technologies of the claim technical solution.
The invention can prepare high-quality manganese dioxide by a manganese dioxide preparation method; thereby greatly improving the quality of preparing cobalt sulfate; meanwhile, the current output current and the current output pulse width of the motor of the centrifugal device can be obtained in the running process of the centrifugal device through the centrifugal control method of the centrifugal device, so that the blocking condition of the current top cover of the centrifugal device is judged by combining the obtained current output current and the obtained current output pulse width, the safety is greatly improved, and the normal preparation is ensured.
It should be noted that the embodiments of the present invention can be realized in hardware, software, or a combination of software and hardware. The hardware portion may be implemented using dedicated logic; the software portions may be stored in a memory and executed by a suitable instruction execution system, such as a microprocessor or special purpose design hardware. Those of ordinary skill in the art will appreciate that the apparatus and methods described above may be implemented using computer executable instructions and/or embodied in processor control code, such as provided on a carrier medium such as a magnetic disk, CD or DVD-ROM, a programmable memory such as read only memory (firmware), or a data carrier such as an optical or electronic signal carrier. The device of the present invention and its modules may be implemented by hardware circuitry, such as very large scale integrated circuits or gate arrays, semiconductors such as logic chips, transistors, etc., or programmable hardware devices such as field programmable gate arrays, programmable logic devices, etc., as well as software executed by various types of processors, or by a combination of the above hardware circuitry and software, such as firmware.
3. Evidence of the effect of the examples. The embodiment of the invention has a great advantage in the research and development or use process, and has the following description in combination with data, charts and the like of the test process.
The invention can prepare high-quality manganese dioxide by a manganese dioxide preparation method; thereby greatly improving the quality of preparing cobalt sulfate; meanwhile, the current output current and the current output pulse width of the motor of the centrifugal device can be obtained in the running process of the centrifugal device through the centrifugal control method of the centrifugal device, so that the blocking condition of the current top cover of the centrifugal device is judged by combining the obtained current output current and the obtained current output pulse width, the safety is greatly improved, and the normal preparation is ensured.
The foregoing is merely illustrative of specific embodiments of the present invention, and the scope of the invention is not limited thereto, but any modifications, equivalents, improvements and alternatives falling within the spirit and principles of the present invention will be apparent to those skilled in the art within the scope of the present invention.
Claims (10)
1. A method for preparing high-purity cobalt sulfate from electrolytic manganese sulfide slag, which is characterized by comprising the following steps:
step one, configuring parameters of monitoring equipment, and monitoring the working state of a crushing device through the monitoring equipment; crushing rhodochrosite by a crushing device and sieving; mixing rhodochrosite powder with water of the same mass at room temperature; fully mixing the mixed slurry with sodium hydroxide or ammonium metavanadate, stirring at the temperature of 66 ℃, and continuously introducing air; filtering and separating to obtain precipitate and filtrate; finally, drying the obtained precipitate at 55 ℃ to obtain sulfur-removed rhodochrosite; the manganese sulfate solution prepared from rhodochrosite is adopted, and industrial manganese sulfate is dissolved to prepare the manganese sulfate solution; preparing manganese dioxide by manganese sulfate; crushing and sieving manganese dioxide and electrolytic manganese sulfide slag;
the monitoring device monitors the method:
monitoring voltage data of the crushing device through a voltmeter in the monitoring equipment;
monitoring current data of the crushing device through an ammeter in the monitoring equipment;
monitoring resistance data of the crushing device through a resistance meter in the monitoring equipment;
monitoring the comminution device fault data by a diagnostic circuit in the monitoring device;
step two, adding dilute sulfuric acid, saponified P204 and sulfonated kerosene into the sieved manganese dioxide and electrolytic manganese sulfide slag to obtain a manganese-loaded organic phase and a cobalt-nickel-magnesium-rich solution;
step three, taking cobalt-rich nickel-magnesium solution, and adding saponified neodecanoic acid, sulfonated kerosene, dilute sulfuric acid and saponified P507-Cyanex301 to obtain cobalt-rich organic phase and nickel sulfate solution; separating out a cobalt-rich organic phase, adding sulfuric acid for back extraction to obtain a high-purity cobalt-rich sulfate solution and a P507-Cyanex301 organic phase;
and step four, separating high-purity cobalt sulfate-enriched solution, evaporating, concentrating, crystallizing and centrifuging by a centrifugal device to obtain high-purity cobalt sulfate.
2. The method for preparing high-purity cobalt sulfate from electrolytic manganese sulfide slag according to claim 1, wherein the mass ratio of manganese dioxide to electrolytic sulfide slag is 3:1, the mass concentration of dilute sulfuric acid is 100g/L, the liquid-solid ratio of reaction is 8:1, the leaching temperature is 95 ℃, the oxygen pressure is 1MPa, the leaching time is 190min, and the end-point pH of leaching is 5;
the pH value of the separated cobalt-nickel sulfuric acid solution is adjusted to 5; the fourth organic extractant is prepared by mixing a P507-Cyanex301 synergistic extraction system with sulfonated kerosene according to the volume fraction of 10% -40%, wherein the mass ratio of the P507 to the Cyanex301 is 3:1, and then the mixture is saponified by sodium hydroxide, the saponification rate is 53%, and the O/A=3:1 of an organic phase to an aqueous phase is achieved.
3. The method for preparing high-purity cobalt sulfate from electrolytic manganese sulfide slag according to claim 1, wherein the method for preparing manganese dioxide comprises the following steps:
(1) The manganese sulfate solution prepared from rhodochrosite is adopted, and industrial manganese sulfate is dissolved to prepare the manganese sulfate solution; then refining and removing impurities; inputting the manganese sulfate leaching solution into a container, adding modified barium sulfide, and starting a stirring rod arranged on an outer shaft to stir so as to precipitate the solution; lifting the outer shaft upwards to expose a section of the hollow inner shaft arranged in the outer shaft close to the bottom end of the container, and filtering out sediment from the solution in the container through the exposed section of the inner shaft;
(2) The filtered filtrate flows out from the inner cavity of the inner shaft, and the flowing filtrate enters a purifying tank arranged at the lower side of the container; adding sodium thiram into the purifying pond to react with the filtrate to generate precipitate; after the reaction is finished, filtering out sediment by a filtering device at the bottom of the purifying tank to obtain purified liquid; performing two-stage impurity removal on the purifying liquid;
(3) Standing the solution subjected to the second-stage impurity removal and filtration, and carrying out superfine filtration to the solution in a heating container for heating; and then the solution in the heating container is conveyed to a diaphragm electrolytic tank, the sulfuric acid-manganese sulfate system is adopted for electrolysis, manganese dioxide is separated out on the anode, and the separated manganese dioxide is peeled off, crushed, rinsed, milled and blended to obtain a manganese dioxide product.
4. The method for preparing high-purity cobalt sulfate from electrolytic manganese sulfide slag according to claim 3, wherein the stirring time is 45min.
5. The method for preparing high-purity cobalt sulfate from electrolytic manganese sulfide slag according to claim 3, wherein the filtering device comprises a sealing cover plate which is arranged at the bottom of the purifying tank and is movably connected with the purifying tank, and a filter plate is arranged on the cover plate.
6. The method for preparing high-purity cobalt sulfate from electrolytic manganese sulfide slag according to claim 3, wherein the secondary impurity removal is performed by adding potassium permanganate for primary impurity removal and then adding activated carbon for secondary impurity removal.
7. The method for preparing high-purity cobalt sulfate from electrolytic manganese sulfide slag according to claim 1, wherein the centrifugal control method of the centrifugal device is as follows:
1) Configuring parameters of a centrifugal device, and obtaining the current output current and the current output pulse width of a motor of the centrifugal device through monitoring equipment;
2) Determining a target control strategy of the centrifugal device motor according to the current output current and the current output pulse width; and controlling the centrifugal device motor to execute the target control strategy.
8. The method of producing high purity cobalt sulfate from electrolytic manganese sulfide slag according to claim 7, wherein said determining a target control strategy for said centrifuge motor based on said present output current and said present output pulse width comprises:
determining the blocking probability of blocking the top cover of the centrifugal device according to the current output current and the current output pulse width;
and determining a target control strategy of the motor of the centrifugal device according to the blocking probability.
9. The method for preparing high purity cobalt sulfate from electrolytic manganese sulfide slag according to claim 7, wherein said determining a blocking probability of a top cover of said centrifuge device being blocked based on said current output current and said current output pulse width comprises:
determining a current influence factor for judging the blocking condition of the top cover according to the current output current;
determining a pulse width influence factor for judging the blocking condition of the top cover according to the current output pulse width;
calculating blocking probability of the top cover being blocked according to the current influence factor and the pulse width influence factor;
the calculating the blocking probability of the top cover being blocked according to the current influence factor and the pulse width influence factor comprises the following steps:
A＝K*i+(1-K)*t
wherein A is the blocking probability, K is the reference factor, i is the current influencing factor, and t is the pulse width influencing factor.
10. The method for preparing high purity cobalt sulfate from electrolytic manganese sulfide slag according to claim 9, wherein said determining a current influencing factor for determining a top cover blocking condition based on said current output current comprises:
inputting the current output current to a preset membership function;
determining the membership degree output by the preset membership function as a current influence factor for judging the blocking condition of the top cover;
the determining a pulse width influence factor for determining the blocking condition of the top cover according to the current output pulse width comprises the following steps:
inputting the current output pulse width to a preset membership function;
determining the membership degree output by the preset membership function as a pulse width influence factor for judging the blocking condition of the top cover;
the determining a target control strategy of the centrifugal device motor according to the blocking probability comprises the following steps:
determining a probability interval in which the blocking probability is located;
according to a preset corresponding relation, determining a control strategy corresponding to the probability interval as a target control strategy of the centrifugal device motor;
the device for obtaining the output pulse width comprises a magnetic piece for generating a pulse signal and a Hall element for determining the pulse signal width, and the device for obtaining the current output pulse width comprises:
acquiring a current pulse signal acquired by the device;
and determining the width of the current pulse signal as the current output pulse width.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211579679.5A CN116143185A (en) | 2022-12-08 | 2022-12-08 | Method for preparing high-purity cobalt sulfate from electrolytic manganese sulfide slag |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211579679.5A CN116143185A (en) | 2022-12-08 | 2022-12-08 | Method for preparing high-purity cobalt sulfate from electrolytic manganese sulfide slag |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116143185A true CN116143185A (en) | 2023-05-23 |
Family
ID=86339822
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211579679.5A Pending CN116143185A (en) | 2022-12-08 | 2022-12-08 | Method for preparing high-purity cobalt sulfate from electrolytic manganese sulfide slag |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116143185A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1112248A (en) * | 1994-05-16 | 1995-11-22 | 南京理工大学 | Intelligent monitor for extrusion crusher |
| CN103131847A (en) * | 2013-03-16 | 2013-06-05 | 重庆大学 | Method for desulphurizing high-sulphur rhodochrosite |
| CN107419115A (en) * | 2017-09-30 | 2017-12-01 | 柳州凯通新材料科技有限公司 | A kind of processing method of electrolytic manganese dioxide |
| CN112662877A (en) * | 2020-12-02 | 2021-04-16 | 广西科技师范学院 | Method for preparing high-purity nickel sulfate from electrolytic manganese sulfide slag |
| CN114377862A (en) * | 2021-11-30 | 2022-04-22 | 青岛海尔生物医疗科技有限公司 | Method and device for controlling a centrifuge, centrifuge and storage medium |
-
2022
- 2022-12-08 CN CN202211579679.5A patent/CN116143185A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1112248A (en) * | 1994-05-16 | 1995-11-22 | 南京理工大学 | Intelligent monitor for extrusion crusher |
| CN103131847A (en) * | 2013-03-16 | 2013-06-05 | 重庆大学 | Method for desulphurizing high-sulphur rhodochrosite |
| CN107419115A (en) * | 2017-09-30 | 2017-12-01 | 柳州凯通新材料科技有限公司 | A kind of processing method of electrolytic manganese dioxide |
| CN112662877A (en) * | 2020-12-02 | 2021-04-16 | 广西科技师范学院 | Method for preparing high-purity nickel sulfate from electrolytic manganese sulfide slag |
| CN114377862A (en) * | 2021-11-30 | 2022-04-22 | 青岛海尔生物医疗科技有限公司 | Method and device for controlling a centrifuge, centrifuge and storage medium |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP3904546A1 (en) | Process for recovering components from alkaline batteries | |
| CN104039991B (en) | Lead is reclaimed from mixed oxidization section bar material | |
| CN104911359A (en) | Process method for extracting cobalt and nickel from manganese waste slag | |
| CN105087935B (en) | The method of copper, indium and gallium is separately recovered in a kind of gallium waste target from copper and indium | |
| Huang et al. | A novel approach to recover lead oxide from spent lead acid batteries by desulfurization and crystallization in sodium hydroxide solution after sulfation | |
| CN103342395B (en) | A kind of preparation method of low-sulfur ternary precursor | |
| CN107623124B (en) | Preparation method of spherical nickel-cobalt-manganese precursor material | |
| EP4067366A1 (en) | Method for purifying progesterone | |
| CN106119560A (en) | Zinc-cobalt separation method | |
| CN116143185A (en) | Method for preparing high-purity cobalt sulfate from electrolytic manganese sulfide slag | |
| CN105753038B (en) | A kind of production technology of feed grade monohydrate zinc sulphate | |
| CN109943733A (en) | A kind of crude cobalt/nickel salt raw material efficiently separates cobalt/nickel magnesium manganese method | |
| CN105839134A (en) | Method for preparing beta-menadione by indirect electrooxidation method | |
| CN113755702A (en) | Rhodium-iridium separation refining process | |
| CN115448335B (en) | Recycling method of waste lithium iron manganese phosphate battery | |
| CN112961987A (en) | Harmless and recycling treatment method for arsenic alkali slag | |
| US11566333B2 (en) | Method for cleanly extracting metallic silver | |
| CN110453096A (en) | A kind of method that the Whote-wet method smelting molybdenum concentrate of environment-friendly type prepares high-purity ammonium heptamolybdate | |
| CN107675201A (en) | The preparation method of electrolytic manganese dioxide | |
| CN102876897A (en) | Recovery and purification method of manganese dioxide in electrolytic manganese anode mud | |
| CN115472943A (en) | Recovery method and application of waste Prussian sodium battery positive electrode material | |
| CN101691240B (en) | Method for preparing electronic grade high-purity copper chloride dihydrate | |
| CN113429281A (en) | High-purity vanadyl oxalate crystal and preparation method thereof | |
| CN103204544B (en) | Sulfur dioxide liquid and low-grade manganese dioxide is utilized to prepare the method for manganous sulfate | |
| TWI626985B (en) | Systems for separating metal ion by electrodialysis synergized complexation and method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20230523 |