CN117083398A - Laterite nickel ore hydrometallurgy pre-neutralization system and pre-neutralization method - Google Patents
Laterite nickel ore hydrometallurgy pre-neutralization system and pre-neutralization method Download PDFInfo
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- CN117083398A CN117083398A CN202380010000.7A CN202380010000A CN117083398A CN 117083398 A CN117083398 A CN 117083398A CN 202380010000 A CN202380010000 A CN 202380010000A CN 117083398 A CN117083398 A CN 117083398A
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- 238000006386 neutralization reaction Methods 0.000 title claims abstract description 163
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 65
- 238000000034 method Methods 0.000 title claims abstract description 36
- 229910001710 laterite Inorganic materials 0.000 title claims description 9
- 239000011504 laterite Substances 0.000 title claims description 9
- 238000009854 hydrometallurgy Methods 0.000 title abstract description 17
- 239000002893 slag Substances 0.000 claims abstract description 163
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 152
- 239000002002 slurry Substances 0.000 claims abstract description 112
- 229910052742 iron Inorganic materials 0.000 claims abstract description 99
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 claims abstract description 86
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 71
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 54
- 238000000151 deposition Methods 0.000 claims abstract description 25
- 238000002386 leaching Methods 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims description 196
- KCZFLPPCFOHPNI-UHFFFAOYSA-N alumane;iron Chemical compound [AlH3].[Fe] KCZFLPPCFOHPNI-UHFFFAOYSA-N 0.000 claims description 70
- -1 iron ion Chemical class 0.000 claims description 47
- 239000003795 chemical substances by application Substances 0.000 claims description 44
- 239000002562 thickening agent Substances 0.000 claims description 36
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 29
- 235000011152 sodium sulphate Nutrition 0.000 claims description 29
- 238000001556 precipitation Methods 0.000 claims description 25
- 229910052782 aluminium Inorganic materials 0.000 claims description 18
- 239000007791 liquid phase Substances 0.000 claims description 7
- 238000012544 monitoring process Methods 0.000 claims description 7
- 238000004062 sedimentation Methods 0.000 claims description 6
- 239000007790 solid phase Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 abstract description 11
- 230000008901 benefit Effects 0.000 abstract description 8
- 230000008021 deposition Effects 0.000 description 11
- 238000001514 detection method Methods 0.000 description 11
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 7
- 235000011941 Tilia x europaea Nutrition 0.000 description 7
- 239000004571 lime Substances 0.000 description 7
- 239000008267 milk Substances 0.000 description 7
- 210000004080 milk Anatomy 0.000 description 7
- 235000013336 milk Nutrition 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 239000010941 cobalt Substances 0.000 description 5
- 229910017052 cobalt Inorganic materials 0.000 description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 5
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 4
- 229910001453 nickel ion Inorganic materials 0.000 description 4
- 238000003723 Smelting Methods 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000013049 sediment Substances 0.000 description 3
- 235000019738 Limestone Nutrition 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000006028 limestone Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- JWZZKOKVBUJMES-UHFFFAOYSA-N (+-)-Isoprenaline Chemical compound CC(C)NCC(O)C1=CC=C(O)C(O)=C1 JWZZKOKVBUJMES-UHFFFAOYSA-N 0.000 description 1
- XTOOSYPCCZOKMC-UHFFFAOYSA-L [OH-].[OH-].[Co].[Ni++] Chemical compound [OH-].[OH-].[Co].[Ni++] XTOOSYPCCZOKMC-UHFFFAOYSA-L 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000011481 absorbance measurement Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- UUCGKVQSSPTLOY-UHFFFAOYSA-J cobalt(2+);nickel(2+);tetrahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[Co+2].[Ni+2] UUCGKVQSSPTLOY-UHFFFAOYSA-J 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229960004042 diazoxide Drugs 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
Classifications
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- 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
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to the technical field of hydrometallurgy, in particular to a laterite-nickel ore hydrometallurgy pre-neutralization system and a pre-neutralization method; the preneutralization system comprises an iron depositing unit, a first neutralization unit, a second neutralization unit and a control unit, wherein the iron depositing unit receives high-pressure leaching slurry, the first neutralization unit is connected with the iron depositing unit and can receive the slurry after the fed anhydrous sodium sulfate, and the second neutralization unit is connected with the first neutralization unit and can receive the slurry after the fed anhydrous sodium sulfate and nickel cobalt slag and is used for neutralizing acid in the slurry through the feeding neutralizer, and meanwhile, the control unit accurately controls the anhydrous sodium sulfate, the nickel cobalt slag and the neutralizer, so that the quantity of the added anhydrous sodium sulfate, the added anhydrous sodium sulfate and nickel cobalt slag and the neutralizer can be in a proper range, and the economic benefit of laterite-nickel ore hydrometallurgy is improved.
Description
Technical Field
The invention relates to the technical field of hydrometallurgy, in particular to a laterite-nickel ore hydrometallurgy pre-neutralization system and a pre-neutralization method.
Background
The laterite-nickel ore is subjected to high-pressure acid leaching treatment, valuable metals such as Ni (nickel) and Co (cobalt) in the raw ore are selectively leached, and impurities such as Fe (iron) and Al (aluminum) stay in a slag phase. The wet high-pressure acid leaching process of the laterite nickel ore comprises mineral separation, high-pressure leaching, pre-neutralization, CCD countercurrent washing, iron and aluminum deposition of 1 section, iron and aluminum deposition of 2 sections, nickel and cobalt deposition of 1 section, and nickel and cobalt deposition of 2 sections. After the preneutralization, the slurry enters a CCD countercurrent washing process, slag in the preneutralization reaction tank is sequentially countercurrent washed through 6 thickeners connected in series, and finally, the slag is discharged to the tail slag filter pressing outside by the bottom flow of the five thickeners of the CCD countercurrent washing process, and finally enters a tailing pond.
In the production of nickel cobalt hydroxide by wet smelting of laterite-nickel ore disclosed in the patent document with publication number CN108913883A, the laterite-nickel ore is leached under pressure or normal pressure to obtain leached ore pulp; then carrying out pre-neutralization treatment on the leached ore pulp, and controlling the pH value of the end point to be 1.1-1.8; removing iron and aluminum from the ore pulp after the pre-neutralization treatment, controlling the pH value of the end point to be 3.5-4.2, and introducing compressed air in the process; carrying out CCD washing on ore pulp after iron and aluminum removal; deep impurity removal is carried out on overflow washed by CCD, the pH value of the end point is controlled to be 4.8-5.2, and compressed air is introduced in the process; and finally, precipitating overflow subjected to deep impurity removal by adopting lime milk to obtain a gypsum-cobalt nickel hydroxide mixture, and separating the gypsum-cobalt nickel hydroxide mixture to obtain a cobalt nickel hydroxide product.
Although the existing laterite-nickel ore wet smelting can realize the control of the pH value of slurry after high-pressure leaching through the pre-neutralization treatment, the production of nickel and cobalt is conveniently realized, as the neutralizing agents such as secondary iron-aluminum slag, secondary nickel-cobalt slag, lime milk and the like are uniformly filled into a neutralization pond filled with the high-pressure leaching slurry for neutralization in the pre-neutralization treatment process, the amounts of the secondary iron-aluminum slag, the secondary nickel-cobalt slag and the lime milk are difficult to effectively regulate and control, and the filled secondary iron-aluminum slag, secondary nickel-cobalt slag and lime milk are easy to produce excessive or insufficient, so that the economic benefit of laterite-nickel ore wet smelting is reduced.
Disclosure of Invention
The invention aims to overcome the technical defects, and provides a laterite-nickel ore hydrometallurgical pre-neutralization method, which solves the technical problem that the production benefit of laterite-nickel ore hydrometallurgy is reduced because the two-stage iron-aluminum slag, the two-stage nickel-cobalt slag and lime milk are difficult to control to be added in the pre-neutralization treatment of the laterite-nickel ore hydrometallurgy in the prior art.
In order to achieve the above purpose, the technical scheme of the invention provides a hydrometallurgical preneutralization system of laterite-nickel ores, which comprises the following steps:
an iron depositing unit;
the first neutralization unit is connected with the iron depositing unit;
the second neutralization unit is connected with the first neutralization unit;
the control unit is connected with the first neutralization unit and the second neutralization unit and is used for detecting the pH values in the first neutralization unit and the second neutralization unit and respectively controlling the adding amount of the ferro-aluminum slag and the nickel-cobalt slag in the first neutralization unit and the adding amount of the neutralizing agent in the second neutralization unit according to the detected pH values.
Optionally, the first neutralization unit includes feed equipment, first retort and second retort, first retort with the discharge end of heavy indisputable unit is connected, feed equipment with first retort is connected for to first retort feeding iron aluminum slag and nickel cobalt sediment, the feed end of second retort with first retort is connected, the discharge end with the second neutralization unit is connected.
Optionally, the control unit includes first control module and pH monitor, the pH monitor with the second retort is connected, is used for monitoring the pH value of thick liquids in the second retort, first control module with the pH monitor with feed equipment is connected, is used for through the pH value that the pH monitor detected, control feed equipment supplies the quantity of iron aluminium sediment and nickel cobalt sediment of first retort.
Optionally, the second neutralization unit includes a feed pump and a third reaction tank, a fourth reaction tank and a fifth reaction tank which are sequentially connected, wherein the third reaction tank is connected with the discharge end of the first neutralization unit, and the feed pump is connected with the third reaction tank and the fourth reaction tank and is used for introducing a neutralizing agent into the third reaction tank and the fourth reaction tank.
Optionally, the control unit further includes a second control module and a pH detector, the pH detector is connected with the fifth reaction tank and is used for monitoring the pH value of the slurry in the fifth reaction tank, the second control module is connected with the pH detector and the feed pump and is used for controlling the amount of the neutralizing agent fed into the third reaction tank and the fourth reaction tank by the feed pump according to the pH value detected by the pH detector.
Optionally, the iron depositing unit comprises a sixth reaction tank and a feeding device, wherein the feeding device is connected with the sixth reaction tank and is used for adding anhydrous sodium sulphate into the sixth reaction tank.
Optionally, the control unit is further configured to detect the iron ion content in the sixth reaction tank and control whether the feeding device is fed with anhydrous sodium sulphate according to the iron ion content.
Optionally, the hydrometallurgical pre-neutralization system for laterite nickel ore further comprises a plurality of thickeners, each thickener is arranged in sequence, the thickener at the head end is connected with the second neutralization unit, and the thickener at the tail end is used for reducing the iron ion content in the liquid phase and the nickel content in the solid phase of the underflow discharged from the thickener at the tail end by controlling the water inflow.
Compared with the prior art, the laterite-nickel ore hydrometallurgical preneutralization system provided by the invention has the beneficial effects that: the method comprises the steps of setting an iron depositing unit, a first neutralizing unit, a second neutralizing unit and a control unit, wherein the iron depositing unit receives high-pressure leaching slurry, supplying anhydrous sodium sulphate to the iron depositing unit to reduce the iron ion content in the received slurry, and the first neutralizing unit is connected with the iron depositing unit and can receive the slurry after the supplied anhydrous sodium sulphate and can react the iron aluminum slag and the nickel cobalt slag with acid in the slurry and neutralize the acid in the slurry and simultaneously dissolve iron and nickel in the iron aluminum slag and the nickel cobalt slag; the second neutralization unit is connected with the first neutralization unit, the first neutralization unit can receive the slurry fed with the iron aluminum slag and the nickel cobalt slag and is used for neutralizing the acid in the slurry by feeding a neutralizing agent, and the control unit can realize the accurate control of the feeding amount of the iron aluminum slag and the nickel cobalt slag of the first neutralization unit and the neutralizing agent of the second neutralization unit by detecting the pH values in the first neutralization unit and the second neutralization unit and finally realize the accurate control of the pH value in the slurry;
because the iron depositing unit, the first neutralizing unit and the second neutralizing unit are independently arranged, the amount of the added sodium sulfate, the iron aluminum slag, the nickel cobalt slag and the neutralizing agent is in a proper range through the accurate control of the control unit according to the reaction conditions of the slurry inside the iron depositing unit, the first neutralizing unit and the second neutralizing unit and the added sodium sulfate, the iron aluminum slag, the nickel cobalt slag and the neutralizing agent, so that the amount of the added sodium sulfate, the iron aluminum slag, the nickel cobalt slag and the neutralizing agent can be accurately controlled, and the economic benefit of laterite-nickel ore hydrometallurgy is improved.
In order to achieve the above purpose, the technical scheme of the invention also provides a laterite-nickel ore hydrometallurgical pre-neutralization method, which is executed by the laterite-nickel ore hydrometallurgical pre-neutralization system according to the claims, and comprises the following steps:
s100: introducing the high-pressure leaching slurry into an iron precipitation unit;
s200: adding anhydrous sodium sulphate into the iron precipitation unit to reduce the content of iron ions in the slurry;
s300: inputting the slurry processed by the sedimentation unit into a first neutralization unit, adding iron aluminum slag and nickel cobalt slag into the first neutralization unit, detecting the pH value in the first neutralization unit, and controlling the addition amount of the iron aluminum slag and the nickel cobalt slag according to the pH value;
s400: and inputting the slurry processed by the first neutralization unit into a second neutralization unit, adding a neutralizing agent into the second neutralization unit, detecting the pH value in the second neutralization unit, and controlling the adding amount of the neutralizing agent according to the pH value.
Optionally, the step S200 further includes: detecting the content of iron ions in the iron precipitation unit and controlling whether anhydrous sodium sulphate is fed according to the content of the iron ions; wherein when the iron ion content is more than 1g/L, the feeding of the anhydrous sodium sulphate is controlled, and when the iron ion content is less than 1g/L, the feeding of the anhydrous sodium sulphate is controlled to be stopped.
Optionally, the step S300 includes:
inputting the slurry treated by the sedimentation unit into a first reaction tank of a first neutralization unit, and adding iron aluminum slag and nickel cobalt slag into the first reaction tank;
and inputting the slurry after the neutralization reaction in the first reaction tank into a second reaction tank of the first neutralization unit, detecting the pH value in the second reaction tank, and controlling the adding amount of the iron aluminum slag and the nickel cobalt slag in the first reaction tank according to the pH value.
Optionally, the detecting the pH value in the second reaction tank and controlling the adding amount of the iron aluminum slag and the nickel cobalt slag in the first reaction tank according to the pH value includes:
if the pH value in the second reaction tank is detected to be higher than a first threshold range, controlling to increase the addition amount of the iron aluminum slag and the nickel cobalt slag in the first reaction tank;
and if the pH value in the second reaction tank is detected to be lower than the first threshold range, controlling to reduce the addition amount of the iron aluminum slag and the nickel cobalt slag in the first reaction tank.
Optionally, the first threshold range is 0.9-1.1.
Optionally, the step S400 includes:
inputting the slurry processed by the first neutralization unit into a third reaction tank of a second neutralization unit, and adding a neutralizer into the third reaction tank;
inputting the slurry after the neutralization reaction in the third reaction tank into a fourth reaction tank of the second neutralization unit, and adding a neutralizing agent into the fourth reaction tank;
and inputting the slurry after the neutralization reaction in the fourth reaction tank into a fifth reaction tank of the second neutralization unit, detecting the pH value in the fifth reaction tank, and controlling the addition amount of the neutralizing agent in the third reaction tank and the fourth reaction tank according to the pH value.
Optionally, the detecting the pH value in the fifth reaction tank and controlling the addition amount of the neutralizing agent in the third reaction tank and the fourth reaction tank according to the pH value includes:
if the pH value in the fifth reaction tank is detected to be higher than the second threshold range, controlling to increase the addition amount of the neutralizer in the third reaction tank and the fourth reaction tank;
and if the pH value in the fifth reaction tank is detected to be lower than the second threshold range, controlling to reduce the addition amount of the neutralizer in the third reaction tank and the fourth reaction tank.
Optionally, the second threshold range is 1.5-2.
Compared with the prior art, the laterite-nickel ore hydrometallurgical preneutralization method provided by the invention has the beneficial effects that: through the above treatment mode of pre-neutralization, the iron removal process of the slurry, the dissolution and neutralization process of the iron aluminum slag and the nickel cobalt slag and the neutralization process of the neutralizer can be independently carried out, so that the amount of the added sodium sulphate, iron aluminum slag, nickel cobalt slag and the neutralizer is in a proper range according to the reaction conditions of the slurry in the iron precipitation unit, the first neutralization unit and the second neutralization unit, and the added sodium sulphate, iron aluminum slag, nickel cobalt slag and the neutralizer, and by combining the pH values in the first neutralization unit and the second neutralization unit, the sodium sulphate, iron aluminum slag, nickel cobalt slag and the neutralizer are accurately controlled, the amount of the added sodium sulphate, iron aluminum slag, nickel cobalt slag and the neutralizer in the slurry is accurately controlled, and the economic benefits of laterite nickel ore hydrometallurgy are improved.
Drawings
Fig. 1 is a schematic structural diagram of a hydrometallurgical preneutralization system of laterite-nickel ore provided by the embodiment of the invention.
Fig. 2 is a flow chart of a hydrometallurgical preneutralization method of laterite-nickel ore provided by an embodiment of the invention.
Wherein, each reference sign in the figure:
10-iron precipitation unit 11-sixth reaction tank 20-first neutralization unit
21-first reaction tank 22-second reaction tank 30-second neutralization unit
31-third reaction tank 32-fourth reaction tank 33-fifth reaction tank
40-head thickener 50-tail thickener.
Detailed Description
The present invention will be described in further detail with reference to the drawings and 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.
The embodiment of the invention provides a laterite-nickel ore hydrometallurgy pre-neutralization system, which is used in a laterite-nickel ore hydrometallurgy pre-neutralization treatment process and comprises an iron precipitation unit 10, a first neutralization unit 20, a second neutralization unit 20 and a control unit (not identified in the figure), wherein the first neutralization unit 20 is connected with the iron precipitation unit 10; the second neutralization unit 30 is connected to the first neutralization unit 20; the control unit is connected with the first neutralization unit 20 and the second neutralization unit 30, and is used for detecting the pH values in the first neutralization unit and the second neutralization unit, and respectively controlling the adding amount of the iron aluminum slag and the nickel cobalt slag in the first neutralization unit and the adding amount of the neutralizing agent in the second neutralization unit according to the detected pH values.
Specifically, by providing the iron precipitation unit 10, the first neutralization unit 20 and the second neutralization unit 30, the iron precipitation unit 10 receives the high-pressure leaching slurry, the anhydrous sodium sulfate is supplied to the iron precipitation unit 10, the iron ion content in the received slurry is reduced, the first neutralization unit 20 is connected with the iron precipitation unit 10, the slurry after the supplied anhydrous sodium sulfate can be received, and the iron aluminum slag and the nickel cobalt slag can be reacted with acid in the slurry by supplying the iron aluminum slag and the nickel cobalt slag, so that the acid in the slurry is neutralized, and meanwhile, the iron and the nickel in the iron aluminum slag and the nickel cobalt slag are dissolved; the second neutralization unit 30 is connected with the first neutralization unit 20, the first neutralization unit 20 can receive the slurry fed with the ferro-aluminum slag and the nickel-cobalt slag, and is used for neutralizing the acid in the slurry by feeding a neutralizing agent, and the control unit can realize the accurate control of the ferro-aluminum slag and the nickel-cobalt slag of the first neutralization unit 20 and the feeding amount of the neutralizing agent of the second neutralization unit 30 by detecting the pH values in the first neutralization unit 20 and the second neutralization unit 30, and finally realize the accurate control of the pH value in the slurry;
through the independent setting of the iron precipitation unit 10, the first neutralization unit 20 and the second neutralization unit 30, according to the reaction conditions of the slurry in the iron precipitation unit 10, the first neutralization unit 20 and the second neutralization unit 30 and the added anhydrous sodium sulfate, the iron aluminum slag, the nickel cobalt slag and the neutralizer, simultaneously, the control unit is used for precisely controlling the anhydrous sodium sulfate, the iron aluminum slag, the nickel cobalt slag and the neutralizer, so that the added anhydrous sodium sulfate, the added iron aluminum slag, the added nickel cobalt slag and the neutralizer are in a proper range, the amount of the iron ions and the nickel ions in the slurry can be precisely controlled, and the economic benefit of laterite-nickel ore hydrometallurgy is improved.
In the embodiment, the laterite-nickel ore hydrometallurgy mainly comprises mineral separation, high-pressure leaching, pre-neutralization, CCD countercurrent washing, 1-stage iron-aluminum deposition, 2-stage iron-aluminum deposition, 1-stage nickel-cobalt deposition, 2-stage nickel-cobalt deposition, and the pre-neutralization method is mainly used for the pre-neutralization after the high-pressure leaching of the laterite-nickel ore hydrometallurgy and in the CCD countercurrent washing process flow, wherein iron-aluminum slag and nickel-cobalt slag are 2-stage iron-aluminum deposition and 2-stage nickel-cobalt deposition, 2-stage iron-aluminum slag and 2-stage nickel-cobalt deposition are generated after the ore is subjected to high-pressure leaching to form slurry, the slurry is formed at the temperature of about 95 ℃, iron ions and residual acid are contained in the slurry, the iron ion content of the slurry is about 5g/L, and the residual acid content is 45-50g/L.
It will be appreciated that the iron precipitation unit 10, the first neutralization unit 20 and the second neutralization unit 30 may be formed by combining one or more sections of tanks.
In this embodiment, in the iron precipitation unit 10, the control unit controls the amount of anhydrous sodium sulfate added to the slurry so that the iron ion content of the slurry after the reaction is less than 1g/L. Specifically, by controlling the iron ions in the reacted slurry to be less than 1g/L, the iron ions in the slurry can be effectively removed, the adding amount of the anhydrous sodium sulphate can be effectively controlled, and the excessive anhydrous sodium sulphate can be avoided.
In this embodiment, as shown in fig. 1, the first neutralization unit 20 includes a feeding device (not identified in the drawing), a first reaction tank 21 and a second reaction tank 22, the first reaction tank 21 is connected to the discharge end of the iron precipitation unit 10, the feeding device is connected to the first reaction tank 21 for feeding iron aluminum slag and nickel cobalt slag to the first reaction tank 21, the feed end of the second reaction tank 22 is connected to the first reaction tank 21, and the discharge end of the second reaction tank is connected to the second neutralization unit 30.
Specifically, the feeding device may provide the first reaction tank 21 with the iron aluminum slag and the nickel cobalt slag, the first reaction tank 21 may react the iron aluminum slag and the nickel cobalt slag with the slurry, dissolve metal oxides such as iron aluminum slag and nickel cobalt slag, and the like, to form a corresponding ionic structure, and the second reaction tank 22 may receive the reacted slurry, and through sufficient reaction and standing of the first reaction tank 21, the purer slurry after the reaction may be obtained.
In this example, the pH value of the slurry was further controlled to be between 0.9 and 1.1 by controlling the amounts of the iron-aluminum slag and the nickel-cobalt slag introduced. Specifically, by controlling the pH of the slurry to be between 0.9 and 1.1, the maximum efficiency of dissolution of the slurry to the ferro-aluminum slag and the nickel-cobalt slag can be achieved, that is, if the pH of the slurry is higher than 1.1, it is indicated that the feeding amount of the ferro-aluminum slag and the nickel-cobalt slag is excessive, so that the excessive ferro-aluminum slag and nickel-cobalt slag cannot be effectively dissolved under the acidic condition, and if the pH is lower than 0.9, it is indicated that the feeding amount of the ferro-aluminum slag and the nickel-cobalt slag is insufficient, the acidity of the slurry can be further dissolved to the more excessive ferro-aluminum slag and nickel-cobalt slag, so that the acidity of the slurry cannot be fully utilized, and the acidity of the slurry is difficult to be fully neutralized.
In this embodiment, the control unit includes a first control module and a pH monitor, where the pH monitor is connected to the second reaction tank 22 and is used to monitor the pH value of the slurry in the second reaction tank 22, and the first control module is connected to the pH monitor and the feeding device and is used to control the amounts of the iron-aluminum slag and the nickel-cobalt slag fed into the first reaction tank 21 by the feeding device through the pH value detected by the pH monitor.
Specifically, the pH value of the slurry in the second reaction tank 22 is monitored by the pH monitor, so that the pH value of the slurry reacted with the iron aluminum slag and the nickel cobalt slag can be effectively obtained, and the pH value of the slurry in the second reaction tank 22 and the added quantity of the iron aluminum slag and the nickel cobalt slag can be automatically controlled by the first control module through the detection of the pH value of the slurry in the second reaction tank 22 and the control of the feeding equipment, so that the labor is reduced, and the pH value of the slurry reacted with the iron aluminum slag and the nickel cobalt slag and the quantity of the added iron aluminum slag and the added nickel cobalt slag can be effectively and accurately controlled.
In this embodiment, as shown in fig. 1, the second neutralization unit 30 includes a feed pump (not shown) and third, fourth and fifth reaction tanks 31, 32 and 33 sequentially connected, the third reaction tank 31 is connected to the discharge end of the first neutralization unit 20, and the feed pump is connected to the third and fourth reaction tanks 31 and 32 for introducing a neutralizing agent into the third and fourth reaction tanks 31 and 32.
Specifically, the feeding pump may provide the neutralizing agent for the third reaction tank 31 and the fourth reaction tank 32, the third reaction tank 31 and the fourth reaction tank 32 may react the neutralizing agent with the slurry, neutralize the slurry after reacting the neutralizing agent with the slurry, increase the pH of the slurry, and the second reaction tank 22 may receive the reacted slurry, and may further obtain purer slurry after reaction by fully reacting and standing the first reaction tank 21.
In this example, the pH of the slurry after the addition of the neutralizing agent was further between 1.5 and 2.0.
In this embodiment, the hydrometallurgical pre-neutralization system for laterite nickel ore further includes a second control module (not shown), the control unit further includes a second control module and a pH detector, the pH detector is connected to the fifth reaction tank 33 and is used for monitoring the pH value of the slurry in the fifth reaction tank 33, and the second control module is connected to the pH detector and the feed pump and is used for controlling the amount of the neutralizing agent fed into the third reaction tank 31 and the fourth reaction tank 32 by the feed pump according to the pH value detected by the pH detector.
Specifically, the pH detector can effectively obtain the pH of the slurry after the reaction with the neutralizing agent by monitoring the pH of the slurry in the fifth reaction tank 33, and the pH detector can realize automatic control of the addition amount of the neutralizing agent by detecting the pH of the slurry in the fifth reaction tank 33 and controlling the feeding device by the second control module, thereby reducing manpower and simultaneously effectively and accurately controlling the pH of the slurry after the reaction with the neutralizing agent and the amount of the neutralizing agent added.
In this embodiment, as shown in fig. 1, the iron precipitation unit 10 includes a sixth reaction tank 11, and the sixth reaction tank 11 receives high-pressure leach slurry and reacts anhydrous sodium sulphate with the high-pressure leach slurry.
In this embodiment, the control unit is further configured to detect the iron ion content in the sixth reaction tank 11, and control whether the feeding device is fed with anhydrous sodium sulfate according to the iron ion content. Specifically, the control unit can realize accurate control of the addition amount of the anhydrous sodium sulphate through detection of the content of the iron ions.
In this embodiment, through the setting of controller, feed equipment, detection module, pH monitor, feed equipment, pH detector and charge pump, can realize the automated control to whole preneutralization technology, and then effectively alleviate the manpower that preneutralization process consumed.
In this embodiment, as shown in fig. 1, the hydrometallurgical pre-neutralization system for laterite nickel ore further includes a plurality of thickeners, each thickener is sequentially arranged, the thickener at the head end is connected to the second neutralization unit 30, and the thickener at the tail end 50 is used for reducing the iron ion content in the liquid phase and the nickel content in the solid phase of the underflow discharged from the thickener at the tail end 50 by controlling the water inflow. Specifically, by controlling the water inflow of the tail thickener 50, the liquid phase ratio of the underflow discharged from the tail thickener 50 can be made to be 50-60%, and by detecting iron ions in the liquid phase of the underflow and nickel in the solid phase, the content of iron ions and nickel ions in the slurry in the tail thickener 50 can be relatively accurately reflected, so that the overflow amount of iron, nickel and cobalt from one thickener can be effectively reacted.
In this embodiment, further, as shown in fig. 1, the number of the thickeners is 6, the head thickener 40 is connected with the fifth reaction tank 33, the bottom stream discharged from each thickener is sent to the next thickener until entering the tail thickener 50, and is discharged from the tail thickener 50; clear water is fed into the tail thickener 50, overflows from the tail thickener 50 in sequence until entering the head thickener 40, and finally enters the iron sedimentation workshop from the head thickener 40.
The embodiment of the invention also provides a laterite-nickel ore hydrometallurgical pre-neutralization method, which is executed by the laterite-nickel ore hydrometallurgical pre-neutralization system, as shown in fig. 2, and comprises the following steps:
s100: passing the high pressure leach slurry into the iron precipitation unit 10;
s200: adding anhydrous sodium sulphate into the iron precipitation unit 10 to reduce the iron ion content in the slurry;
s300: inputting the slurry processed by the sedimentation unit 10 into a first neutralization unit 20, adding ferro-aluminum slag and nickel-cobalt slag into the first neutralization unit 20, detecting the pH value in the first neutralization unit 20, and controlling the addition amount of the ferro-aluminum slag and the nickel-cobalt slag according to the pH value;
s400: the slurry processed by the first neutralization unit 20 is input into the second neutralization unit 30, a neutralizing agent is added into the second neutralization unit 30, the pH value in the second neutralization unit 30 is detected, and the addition amount of the neutralizing agent is controlled according to the pH value.
Specifically, through the above treatment mode of pre-neutralization, the iron removal process of the slurry, the dissolution and neutralization process of the iron aluminum slag and the nickel cobalt slag, and the neutralization process of the neutralizer can be independently performed, so that according to the reaction conditions of the slurry in the iron precipitation unit 10, the first neutralization unit 20 and the second neutralization unit 30 and the added sodium sulfate, the iron aluminum slag, the nickel cobalt slag and the neutralizer, and by combining the pH values in the first neutralization unit 20 and the second neutralization unit 30, the sodium sulfate, the iron aluminum slag, the nickel cobalt slag and the neutralizer are precisely controlled, the amounts of the added sodium sulfate, the iron aluminum slag, the nickel cobalt slag and the neutralizer are in a proper range, and the amounts of iron ions and nickel ions in the slurry can be precisely controlled, so that the economic benefits of laterite-nickel ore hydrometallurgy are improved.
In this embodiment, in step S300, the pH value of the slurry after adding the iron aluminum slag and the nickel cobalt slag is monitored online by the pH monitor, and the first control module controls the feeding device to reduce or increase the amount of the iron aluminum slag and the nickel cobalt slag by the pH value monitored by the pH monitor, so as to control the pH value monitored by the pH monitor to be within a first threshold range, where the first threshold range is between 0.9 and 1.1. Specifically, the pH value of the slurry after the iron aluminum slag and the nickel cobalt slag are added is monitored by a pH monitor, and the amount of the iron aluminum slag and the nickel cobalt slag introduced into the feeding equipment is controlled by a first control module, so that the automatic control of the high-efficiency feeding process of the iron aluminum slag and the nickel cobalt slag can be realized, and the strength of the pre-neutralization process is further effectively reduced.
In this embodiment, further, the slurry is introduced into the first reaction tank 21 after the reaction in the sixth reaction tank 11, the first reaction tank 21 is used for reacting the iron aluminum slag and the nickel cobalt slag in the slurry, the second reaction tank 22 receives the slurry reacted with the iron aluminum slag and the nickel cobalt slag in the first reaction tank 21, and the pH monitor and the second reaction tank 22 monitor the pH value of the slurry reacted with the iron aluminum slag and the nickel cobalt slag in real time;
if the pH value in the second reaction tank is detected to be higher than a first threshold range, controlling to increase the addition amount of the iron aluminum slag and the nickel cobalt slag in the first reaction tank;
and if the pH value in the second reaction tank is detected to be lower than the first threshold range, controlling to reduce the addition amount of the iron aluminum slag and the nickel cobalt slag in the first reaction tank.
That is, when the pH value monitored by the pH monitor is less than 0.9, the first control module controls the feeding device to increase the amount of the iron aluminum slag and the nickel cobalt slag charged into the second reaction tank 22, and when the pH value monitored by the pH monitor is greater than 1.1, the first control module controls the feeding device to decrease the amount of the iron aluminum slag and the nickel cobalt slag charged into the second reaction tank 22.
In this embodiment, in step S500, the pH detector detects the pH value of the slurry after the neutralizing agent is added, and the second control module controls the feed pump to decrease or increase the amount of the neutralizing agent by the pH value detected by the pH detector, so as to control the pH value detected by the pH detector to be within a second threshold range, where the second threshold range is between 1.5 and 2.0. Specifically, the pH value of the slurry after the neutralizing agent is added is monitored by the pH detector, and the amount of the neutralizing agent fed into the feed pump is controlled by the second control module, so that the automatic control of the slurry neutralization process can be realized, and the strength of the pre-neutralization process is effectively reduced.
In this embodiment, further, the slurry sequentially enters the third reaction tank 31, the fourth reaction tank 32 and the fifth reaction tank after being monitored by the second reaction tank 22, the neutralizing agent is added into the third reaction tank 31 and the fourth reaction tank 32, and the pH value of the slurry of the fourth reaction tank 32 and the fifth reaction tank is detected by the pH detector;
if the pH value in the fifth reaction tank is detected to be higher than the second threshold range by the pH detector, controlling and increasing the addition amount of the neutralizer in the third reaction tank and the fourth reaction tank;
and if the pH value in the fifth reaction tank is lower than the second threshold range, controlling to reduce the addition amount of the neutralizing agent in the third reaction tank and the fourth reaction tank.
That is, the second control module controls the feed pump to increase the amount of neutralizing agent charged into the third reaction tank 31 and the fourth reaction tank 32 when the pH value monitored by the pH detector is less than 1.5, and controls the feed pump to decrease the amount of neutralizing agent charged into the third reaction tank 31 and the fourth reaction tank 32 when the pH value monitored by the pH detector is greater than 2.0.
In this embodiment, in step S200, the detection module detects the content of iron ions in the slurry after adding anhydrous sodium sulfate, and controls whether to supply anhydrous sodium sulfate according to the content of iron ions; when the detection module detects that the iron ion content is greater than 1g/L, the control unit controls the feeding equipment to feed anhydrous sodium sulfate into the slurry, and when the detection module detects that the iron ion content is less than 1g/L, the control unit controls the feeding equipment to stop feeding anhydrous sodium sulfate into the slurry. Specifically, through the monitoring of detection module to iron ion content to and the control of the control unit to the amount of feed equipment lets in anhydrous sodium sulfate, can realize the automatic control to the iron ion treatment process in the thick liquids, and then effectively alleviate the intensity of preneutralization technology.
In this embodiment, further, the detection module and the feeding device are connected to the sixth reaction tank 11, when the iron ion content detected by the detection module is less than 1g/L, the control unit controls the feeding device to reduce the amount of anhydrous sodium sulfate to be added to the sixth reaction tank 11, and when the iron ion content detected by the detection module is greater than 1g/L, the control unit controls the feeding device to increase the amount of anhydrous sodium sulfate to be added to the sixth reaction tank 11.
In this embodiment, the detection module may be a 3S-CL-Fe iron ion online analyzer, and the content of iron ions in the sixth reaction tank 11 is detected by online sampling analysis of the online analyzer, or the 1, 10-phosphorus diazoxide and the sampled iron ions in the solution undergo a display reaction by a color reaction to become an orange solution; or quantitatively analyzing absorbance to determine the iron ion content; or by a combination of on-line analyzers, chromogenic reactions and absorbance measurements.
In this embodiment, in step S400, the content of iron ions in the liquid phase of the underflow discharged from the tail thickener 50 is less than 0.08g/L, and the mass fraction of nickel in the solid phase is less than 0.06%. Specifically, by controlling the content of liquid phase iron ions in the underflow of the thickener effluent to less than 0.08g/L and the mass fraction of nickel in the solid phase to less than 0.06%, the content of iron and nickel in the underflow of the effluent can be controlled to a lower level, thereby controlling the content of iron ions and nickel ions in the slurry exiting the head thickener 40 to a higher level.
In this embodiment, in step S500, the neutralizing agent is one or more of limestone, lime milk and sodium hydroxide. Specifically, by providing a combination of one or more of limestone, lime milk and sodium hydroxide, efficient neutralization of the slurry can be achieved.
The above-described embodiments of the present invention do not limit the scope of the present invention. Any other corresponding changes and modifications made in accordance with the technical idea of the present invention shall be included in the scope of the claims of the present invention.
Claims (16)
1. A laterite-nickel ore hydrometallurgical preneutralization system, comprising:
an iron depositing unit;
the first neutralization unit is connected with the iron depositing unit;
the second neutralization unit is connected with the first neutralization unit;
the control unit is connected with the first neutralization unit and the second neutralization unit and is used for detecting the pH values in the first neutralization unit and the second neutralization unit and respectively controlling the adding amount of the ferro-aluminum slag and the nickel-cobalt slag in the first neutralization unit and the adding amount of the neutralizing agent in the second neutralization unit according to the detected pH values.
2. The laterite-nickel ore hydrometallurgical pre-neutralization system according to claim 1, wherein the first neutralization unit comprises a feeding device, a first reaction tank and a second reaction tank, the first reaction tank is connected with the discharge end of the iron precipitation unit, the feeding device is connected with the first reaction tank and is used for feeding ferro-aluminum slag and nickel-cobalt slag into the first reaction tank, the feeding end of the second reaction tank is connected with the first reaction tank, and the discharge end of the second reaction tank is connected with the second neutralization unit.
3. The laterite-nickel ore hydrometallurgical preneutralization system according to claim 2, wherein the control unit comprises a first control module and a pH monitor, the pH monitor being connected to the second reaction tank for monitoring the pH value of the slurry in the second reaction tank, the first control module being connected to the pH monitor and the feed device for controlling the amounts of iron aluminum slag and nickel cobalt slag fed to the first reaction tank by the feed device, through the pH value detected by the pH monitor.
4. The laterite-nickel ore hydrometallurgical pre-neutralization system of claim 1, wherein the second neutralization unit comprises a feed pump and a third reaction tank, a fourth reaction tank and a fifth reaction tank which are sequentially connected, wherein the third reaction tank is connected with a discharge end of the first neutralization unit, and the feed pump is connected with the third reaction tank and the fourth reaction tank and is used for introducing neutralizing agent into the third reaction tank and the fourth reaction tank.
5. The laterite-nickel ore hydrometallurgical preneutralization system according to claim 4, wherein the control unit further comprises a second control module and a pH detector, the pH detector being connected to the fifth reaction tank for monitoring the pH of the slurry in the fifth reaction tank, the second control module being connected to the pH detector and the feed pump for controlling the amount of neutralizer fed to the third and fourth reaction tanks by the pH detected by the pH detector.
6. The laterite-nickel ore hydrometallurgical preneutralization system according to claims 1 to 5, wherein the iron precipitation unit comprises a sixth reaction tank and a charging device connected to the sixth reaction tank and adapted to add anhydrous sodium sulphate to the sixth reaction tank.
7. The laterite-nickel ore hydrometallurgical preneutralization system according to claim 6, wherein the control unit is further adapted to detect the iron ion content in the sixth reaction tank and to control whether the charging device is supplied with anhydrous sodium sulphate based on the iron ion content.
8. The hydrometallurgical pre-neutralization system for laterite nickel ores according to any of claims 1 to 5, further comprising a plurality of thickeners, each thickener being arranged in sequence, the thickener at the head end being connected to the second neutralization unit, the thickener at the tail end being adapted to reduce the iron ion content in the liquid phase and the nickel content in the solid phase of the underflow of the discharge of the thickener at the tail end by controlling the water inflow.
9. A laterite-nickel ore hydrometallurgical preneutralization method, characterized by being performed by a laterite-nickel ore hydrometallurgical preneutralization system according to any of claims 1 to 8, comprising the steps of:
s100: introducing the high-pressure leaching slurry into an iron precipitation unit;
s200: adding anhydrous sodium sulphate into the iron precipitation unit to reduce the content of iron ions in the slurry;
s300: inputting the slurry processed by the sedimentation unit into a first neutralization unit, adding iron aluminum slag and nickel cobalt slag into the first neutralization unit, detecting the pH value in the first neutralization unit, and controlling the addition amount of the iron aluminum slag and the nickel cobalt slag according to the pH value;
s400: and inputting the slurry processed by the first neutralization unit into a second neutralization unit, adding a neutralizing agent into the second neutralization unit, detecting the pH value in the second neutralization unit, and controlling the adding amount of the neutralizing agent according to the pH value.
10. The laterite-nickel ore hydrometallurgical preneutralization method according to claim 9, wherein step S200 further comprises: detecting the content of iron ions in the iron precipitation unit and controlling whether anhydrous sodium sulphate is fed according to the content of the iron ions; wherein when the iron ion content is more than 1g/L, the feeding of the anhydrous sodium sulphate is controlled, and when the iron ion content is less than 1g/L, the feeding of the anhydrous sodium sulphate is controlled to be stopped.
11. The laterite-nickel ore hydrometallurgical preneutralization method according to claim 9, wherein step S300 comprises:
inputting the slurry treated by the sedimentation unit into a first reaction tank of a first neutralization unit, and adding iron aluminum slag and nickel cobalt slag into the first reaction tank;
and inputting the slurry after the neutralization reaction in the first reaction tank into a second reaction tank of the first neutralization unit, detecting the pH value in the second reaction tank, and controlling the adding amount of the iron aluminum slag and the nickel cobalt slag in the first reaction tank according to the pH value.
12. The hydrometallurgical preneutralization method of laterite-nickel ore according to claim 11, wherein the detecting pH value in the second reaction tank and controlling the addition amount of iron aluminum slag and nickel cobalt slag in the first reaction tank according to the pH value comprises:
if the pH value in the second reaction tank is detected to be higher than a first threshold range, controlling to increase the addition amount of the iron aluminum slag and the nickel cobalt slag in the first reaction tank;
and if the pH value in the second reaction tank is detected to be lower than the first threshold range, controlling to reduce the addition amount of the iron aluminum slag and the nickel cobalt slag in the first reaction tank.
13. The laterite-nickel ore hydrometallurgical preneutralization method according to claim 12, wherein the first threshold value is in the range of 0.9 to 1.1.
14. The laterite-nickel ore hydrometallurgical preneutralization method according to claim 9, wherein step S400 comprises:
inputting the slurry processed by the first neutralization unit into a third reaction tank of a second neutralization unit, and adding a neutralizer into the third reaction tank;
inputting the slurry after the neutralization reaction in the third reaction tank into a fourth reaction tank of the second neutralization unit, and adding a neutralizing agent into the fourth reaction tank;
and inputting the slurry after the neutralization reaction in the fourth reaction tank into a fifth reaction tank of the second neutralization unit, detecting the pH value in the fifth reaction tank, and controlling the addition amount of the neutralizing agent in the third reaction tank and the fourth reaction tank according to the pH value.
15. The method of hydrometallurgical preneutralization of laterite nickel ore according to claim 14, wherein the detecting pH in the fifth reaction tank and controlling the addition amount of the neutralizer in the third and fourth reaction tanks according to the pH comprises:
if the pH value in the fifth reaction tank is detected to be higher than the second threshold range, controlling to increase the addition amount of the neutralizer in the third reaction tank and the fourth reaction tank;
and if the pH value in the fifth reaction tank is detected to be lower than the second threshold range, controlling to reduce the addition amount of the neutralizer in the third reaction tank and the fourth reaction tank.
16. The laterite-nickel ore hydrometallurgical preneutralization method according to claim 15, wherein the second threshold value is in the range of 1.5 to 2.
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