CN114921647B - Oxygen pressure leaching method of high nickel matte under sulfuric acid - Google Patents
Oxygen pressure leaching method of high nickel matte under sulfuric acid Download PDFInfo
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- 238000002386 leaching Methods 0.000 title claims abstract description 149
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 142
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 122
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 122
- 239000001301 oxygen Substances 0.000 title claims abstract description 122
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 65
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000010949 copper Substances 0.000 claims abstract description 57
- 239000002893 slag Substances 0.000 claims abstract description 49
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 44
- 229910052802 copper Inorganic materials 0.000 claims abstract description 44
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 35
- 239000002253 acid Substances 0.000 claims abstract description 29
- 239000007788 liquid Substances 0.000 claims abstract description 29
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 21
- 239000010941 cobalt Substances 0.000 claims abstract description 21
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000000926 separation method Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000004070 electrodeposition Methods 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 12
- 239000002699 waste material Substances 0.000 claims description 11
- 230000035484 reaction time Effects 0.000 claims description 9
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 8
- 229910052717 sulfur Inorganic materials 0.000 claims description 8
- 239000011593 sulfur Substances 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 3
- 230000003472 neutralizing effect Effects 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 239000007790 solid phase Substances 0.000 claims description 2
- 239000000243 solution Substances 0.000 description 28
- 238000006243 chemical reaction Methods 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 6
- 238000003723 Smelting Methods 0.000 description 5
- 229920006395 saturated elastomer Polymers 0.000 description 5
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 description 4
- 241000080590 Niso Species 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 description 2
- 239000003929 acidic solution Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002659 electrodeposit Substances 0.000 description 1
- 238000005363 electrowinning Methods 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000010583 slow cooling Methods 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0065—Leaching or slurrying
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Geochemistry & Mineralogy (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses an oxygen pressure leaching method of high nickel matte under sulfuric acid, which comprises the steps of adding water into the high nickel matte to grind the high nickel matte to prepare ore pulp; mixing the ore pulp with an acid solution, and introducing oxygen to perform primary oxygen pressure leaching to obtain primary oxygen pressure leaching liquid and primary oxygen pressure leaching slag; adding an acid solution into the primary oxygen pressure leaching slag to neutralize until the pH value is 1-2, and carrying out solid-liquid separation to obtain a neutralization slag and a neutralization liquid; adding partial neutralization solution into the neutralization slag for size mixing, adding an acid solution and introducing oxygen to perform secondary oxygen pressure leaching to obtain secondary oxygen pressure leaching solution and secondary oxygen pressure leaching slag. The leaching of nickel and cobalt is realized through one-stage oxygen pressure leaching, copper is inhibited in leaching slag, and the separation of nickel and cobalt from copper is realized; and then through neutralization and two-stage oxygen pressure leaching, copper leaching and acid balance are realized, and the leaching process is greatly shortened.
Description
Technical Field
The invention relates to an oxygen pressure leaching method of high nickel matte under sulfuric acid, and belongs to the technical field of hydrometallurgy.
Background
At present, most of nickel sulfide concentrate is treated by adopting a fire method, namely flash smelting or molten pool smelting is performed to remove gangue, slag formation is performed to produce low nickel matte, and blowing iron removal is performed to produce high nickel matte, wherein the total content of nickel and copper is generally 70-80%. For high nickel matte with low copper content (Cu 10%), the anode plate is generally cast for direct electrolysis to produce electric nickel, and for high nickel matte with high copper content (Cu 20% or more), the secondary copper concentrate can be separated by slow cooling flotation, and the obtained secondary nickel concentrate is cast into a nickel sulfide anode for electrolysis to produce electric nickel. Another wet treatment method for high nickel matte is sulfuric acid selective leaching, namely, normal pressure leaching and air pressurizing leaching are combined, so that most of nickel and cobalt are leached, most of copper is inhibited in leaching slag, and the aim of separating and recycling valuable metals such as nickel, copper, cobalt and the like is fulfilled. However, the sulfuric acid selective leaching of the high nickel matte adopts two-stage normal pressure leaching and one-stage air pressurizing leaching, so that most of nickel and cobalt can be leached, the leaching process is long, and the copper precipitation process has strict control requirements on raw material sulfur. The generated leaching slag is generally treated by adopting a fire-wet method to leach copper, namely two-stage roasting and two-stage leaching, and the problems of long flow, more equipment and large metal loss exist.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide an oxygen pressure leaching method of high nickel matte under sulfuric acid, wherein the leaching of nickel cobalt is realized through one-stage oxygen pressure leaching, copper is inhibited in leaching slag, the separation of nickel cobalt and copper is realized, and then the leaching and acid balance of copper are realized through neutralization and two-stage oxygen pressure leaching, so that the leaching flow is greatly shortened.
The technical scheme adopted by the application is as follows:
an oxygen pressure leaching method of high nickel matte under sulfuric acid comprises the following steps:
s1, adding water into high nickel matte, and grinding to obtain ore pulp;
s2, mixing the ore pulp with an acid solution for one-stage oxygen pressure leaching, controlling the liquid-solid ratio to be 5-6:1, and the concentration of starting acid to be 40-50g/L, and carrying out solid-liquid separation when the pH value of the solution is 3-4 to obtain one-stage oxygen pressure leaching liquid and one-stage oxygen pressure leaching slag;
wherein, during the first stage of oxygen pressure leaching, oxygen is introduced, the leaching temperature is controlled to be 180-190 ℃, the pressure is controlled to be 1.4-1.5Mpa, and the reaction time is controlled to be 2-3h;
s3, adding an acid solution into the first-stage oxygen pressure leaching slag for neutralization, controlling the liquid-solid ratio to be 2.5-3.5:1, controlling the temperature to be 60-70 ℃ and the reaction time to be 1.0-1.5h, neutralizing until the pH value is 1-2, and carrying out solid-liquid separation to obtain neutralized slag and neutralized liquid;
s4, adding part of neutralization solution into the neutralization slag for size mixing, adding an acid solution for secondary oxygen pressure leaching, controlling the liquid-solid ratio to be 2.5-3.5:1, the initial acid concentration to be 90-100g/L, the secondary oxygen pressure leaching final acid concentration to be 40-50g/L, and carrying out solid-liquid separation to obtain secondary oxygen pressure leaching liquid and secondary oxygen pressure leaching slag;
wherein, during the second stage oxygen pressure leaching, oxygen is introduced, the leaching temperature is controlled to be 170-180 ℃, the pressure is 1.4-1.5Mpa, and the reaction time is 2-3h.
In the above steps, the pressures are all total pressures, which are equal to the partial pressure of oxygen plus the saturated vapor pressure at the temperature; the primary oxygen pressure leaching slag is copper slag, and the secondary oxygen pressure leaching slag is sulfur slag.
Further, in S4, the volume of the neutralization solution added into the neutralization residue accounts for 40-50% of the total volume of the neutralization solution.
Further, the second-stage oxygen pressure leaching solution produced in the step S4 is returned to the step S3 as an acid solution.
Further, purifying and removing impurities from the first-stage oxygen pressure leaching solution to obtain a purified solution, delivering the purified solution to electro-deposition, producing electro-deposited nickel, and returning the obtained nickel waste electro-deposition solution as an acid solution to the step S2.
Further, the neutralization solution produced in the step S3 is sent to electro-deposition to produce electro-deposited copper, and the obtained copper waste electro-deposition solution is returned to the step S4 as an acidic solution.
Further, in the solid phase matters of the ore pulp, the material with the particle size smaller than 30 μm accounts for more than or equal to 90wt%.
Chinese patent application publication No. CN101705367B discloses a copper and nickel smelting process by oxygen-enriched side-blown bath smelting method, wherein the furnace burden is added into an oxygen-enriched side-blown furnace, and oxygen-enriched air is blown in to perform oxygen-enriched bath smelting to obtain low nickel matte, and then the low nickel matte is depleted by an electric furnace and is blown to obtain high nickel matte. Specifically, the content ranges of the main components of the obtained high nickel matte are as follows: the content of nickel is 36-46wt%, copper is 32-36wt%, cobalt is 0.1-1wt%, sulfur is 16-20wt%, and the sum of the contents of the components is 100wt%.
Further, the concentration of oxygen is not less than 99vol%.
The main reaction principle of the invention is as follows:
in the primary oxygen pressure leach, nickel and cobalt enter the primary oxygen pressure leach liquor, and copper enters the primary oxygen pressure leach slag:
Cu 2 S+H 2 SO 4 +0.5O 2 ＝CuSO 4 +CuS+H 2 O (1)
Cu+H 2 SO 4 +0.5O 2 ＝CuSO 4 +H 2 O (2)
Ni 3 S 2 +H 2 SO 4 +0.5O 2 ＝NiSO 4 +2NiS+H 2 O (3)
NiS+CuSO 4 ＝NiSO 4 +CuS (4)
Ni+H 2 SO 4 +0.5O 2 ＝NiSO 4 +H 2 O (5)
among the above reactions, reaction (4) is the main reaction, and the reaction rate depends on the primary oxygen pressure leaching temperature. Reactions (3), (4) and (5) lead to the leaching of the nickel for the most part. H 2 SO 4 CuSO 4 The amount of Cu required for the reaction decreases rapidly 2+ Supplementing by two reactions (1) and (2), and transferring copper into slag by CuS. As the one-stage oxygen pressure leaching proceeds, the starting acid is reduced from 40-50g/L to around ph=4, at which time the copper in solution is about 1g/L, or even lower. Therefore, proper starting and terminating acids, as well as pressure, are chosen, which would otherwise lead to an increase in copper leaching or a decrease in nickel and cobalt leaching.
In the two-stage oxygen pressure leach, copper enters the two-stage oxygen pressure leach solution:
CuS+2O 2 ＝CuSO 4 (6)
Cu 2 S+2.5O 2 +H 2 SO 4 ＝2CuSO 4 +H 2 O (7)
the beneficial effects of the invention are as follows:
(1) The first-stage oxygen pressure leaching is adopted to replace the second-stage normal pressure leaching and the first-stage air pressure leaching, the second-stage oxygen pressure leaching neutralization slag is adopted to replace the second-stage roasting and the second-stage leaching, the flow is short, the equipment is few, and the efficiency is high.
(2) The leaching rate of nickel and cobalt is more than 90% by adopting one-stage oxygen pressure leaching, most copper is inhibited in one-stage oxygen pressure leaching slag, effective separation and enrichment of copper, nickel and cobalt are achieved, the pH value of one-stage oxygen pressure leaching liquid is reduced to 3-4 from 40-50g/L, and the subsequent purification and impurity removal and electrowinning production of electrolytic nickel can be directly carried out without a neutralization process.
(3) The secondary oxygen pressure leaching neutralization slag is adopted, the copper leaching rate can be more than 95%, the nickel cobalt is leached along with the secondary oxygen pressure leaching neutralization slag, the total nickel cobalt leaching rate can be more than 97%, the secondary oxygen pressure leaching initial acid is reduced to 40-50g/L from 90-100g/L, the primary oxygen pressure leaching slag is directly used for neutralization until the pH value is 1-2, the primary oxygen pressure leaching slag is used as a neutralizer to produce neutralization slag, the neutralization slag returns to the secondary oxygen pressure leaching, and no metal loss is taken away by the neutralization slag.
(4) Because the acid concentration of the copper waste electrodeposit liquid is high, the returned neutralization liquid is adopted to carry out slurry mixing on copper slag, the secondary oxygen pressure leaching is carried out after the starting acid is reduced to 90-100g/L, and the redundant sulfur is discharged from the sulfur slag, so that the acid balance of the system is ensured.
Drawings
FIG. 1 is a flow chart of an oxygen pressure leaching method of high nickel matte in sulfuric acid according to the present invention.
Detailed Description
The present invention will be described in detail with reference to examples. It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other. The following percentages refer to mass percentages unless otherwise indicated.
Example 1:
200g of high nickel matte (containing 40% of Ni, 34% of Cu, 0.44% of Co and 16% of S) is taken, water is added for grinding until the grain size of 90% is smaller than 30 mu m, and nickel waste electro-deposition liquid (containing 60g/L of Ni) is added into the ore pulp after fine grinding, and the liquid-solid ratio is controlled to be 5.0:1, and the starting acid is 40g/L. Adding the prepared ore pulp into a first-stage autoclave for one-stage oxygen pressure leaching, simultaneously introducing oxygen with the concentration of 99vol%, controlling the temperature to 180 ℃, controlling the pressure to 1.4Mpa, and reacting for 2 hours to obtain 1000mL (containing 133g/L Ni, 1g/L Cu, 0.80g/L Co and pH=4) of an oxygen pressure leaching solution. The pressure is the total pressure and is equal to the partial pressure of oxygen plus the saturated vapor pressure at the temperature. Wherein, the leaching rate of nickel is 91 percent and the leaching rate of cobalt is 91 percent. And adding the produced primary oxygen pressure leaching slag, namely copper slag, into the secondary oxygen pressure leaching liquid to neutralize, controlling the liquid-solid ratio to be 3.5:1, controlling the temperature to be 60 ℃, reacting for 1.0h, and producing 560mL of neutralizing liquid to be sent to the subsequent working procedure. Adding 230mL of returned neutralization solution into the produced neutralization slag, mixing pulp, adding the mixture into a two-stage autoclave, adding copper waste electro-deposition solution (containing Cu 40 g/L), controlling the liquid-solid ratio to be 3.5:1, starting acid to be 90g/L, introducing oxygen with the concentration of 99vol% to perform two-stage oxygen pressure leaching, controlling the temperature to be 170 ℃, the pressure to be 1.4Mpa, reacting for 2 hours, producing 560mL of two-stage oxygen pressure leaching solution (containing Cu 184g/L, ni 9.6g/L, co 0.10g/L and sulfuric acid 41 g/L), and producing 64g of two-stage oxygen pressure leaching slag (containing Ni 2.5%, cu 5.2%, co 0.04% and S43.8%). Wherein the two-stage oxygen pressure leaching slag is sulfur slag which can be sold. Copper leaching rate is 95%, nickel leaching rate is 98% and cobalt leaching rate is 97%.
Example 2:
200g of high nickel matte (containing 40% of Ni, 34% of Cu, 0.44% of Co and 16% of S) is taken, water is added for grinding until the grain size of 90% is smaller than 30 mu m, nickel waste electro-deposition solution (containing 60g/L of Ni) is added into the ore pulp after fine grinding, the liquid-solid ratio is controlled to be 5.5:1, and the starting acid is 45g/L. The prepared ore pulp is added into a first-stage autoclave for one-stage oxygen pressure leaching, meanwhile, oxygen with the concentration of 99vol percent is introduced, the temperature is controlled at 185 ℃, the pressure is controlled at 1.45Mpa, the reaction time is 2.5h, and 1100mL (containing Ni 122g/L, cu 1g/L, co 0.74g/L and pH=3) of one-stage oxygen pressure leaching liquid is produced. The pressure is the total pressure and is equal to the partial pressure of oxygen plus the saturated vapor pressure at the temperature. Wherein, the leaching rate of nickel is 92.5 percent and the leaching rate of cobalt is 92 percent. Adding the produced primary oxygen pressure leaching slag, namely copper slag, into a secondary oxygen pressure leaching solution for neutralization, controlling the liquid-solid ratio to be 2.5:1, the temperature to be 65 ℃, the reaction time to be 1.2h, producing 400mL of neutralization liquid to be sent to a subsequent process, adding 180mL of returned neutralization liquid to the produced neutralization slag, mixing slurry, adding copper waste electro-deposition liquid (containing Cu 40 g/L), controlling the liquid-solid ratio to be 2.5:1, starting acid to be 95g/L, introducing oxygen with the concentration of 99vol% to perform secondary oxygen pressure leaching, controlling the temperature to be 175 ℃, the pressure to be 1.45Mpa, the reaction time to be 2.5h, producing 400mL of secondary oxygen pressure leaching solution (containing Cu 253g/L, ni 11.4g/L, cu 0.13g/L and sulfuric acid to be 42 g/L), and producing 60g of secondary oxygen pressure leaching slag (containing Ni 2.4%, cu 5.1%, co 0.03% and S42.9%). Wherein the two-stage oxygen pressure leaching slag is sulfur slag which can be sold. Copper leaching rate is 95.4%, nickel leaching rate is 98.2%, and cobalt leaching rate is 97.9%.
Comparative example 1:
the first stage oxygen pressure leaching of example 1 was repeated, with the only difference that: the initial acid of the first stage oxygen pressure leaching is controlled to be 60g/L. After the reaction, a section of oxygen pressure leaching solution 1000mL (containing Ni 135g/L, cu 15g/L and Co 0) is produced.83g/L，H 2 SO 4 12 g/L), nickel leaching rate 94%, cobalt leaching rate 94%, copper leaching rate 22%.
The above comparative example 1 shows that the initial acid of the first stage oxygen pressure leaching is high, and the final acid of the first stage oxygen pressure leaching is also high, so that the leaching rate of copper in the high nickel matte is high, and the selective leaching of nickel and cobalt is not realized.
Comparative example 2:
the first stage oxygen pressure leaching of example 1 was repeated, with the only difference that: the pressure of the oxygen pressure leaching in the first stage is controlled to be 1.3Mpa. The pressure is the total pressure and is equal to the partial pressure of oxygen plus the saturated vapor pressure at the temperature. After the reaction, a section of oxygen pressure leaching solution 1000mL (containing 130g/L Ni, 1g/L Cu, 0.78g/L Co and H) 2 SO 4 7 g/L), 88% of nickel leaching rate, 89% of cobalt leaching rate and 2% of copper leaching rate.
Comparative example 2 above shows that as the partial pressure of oxygen introduced in the first stage of oxygen pressure leaching is reduced, the leaching rate of nickel and cobalt is reduced.
Comparative example 3
The first stage oxygen pressure leaching of example 1 was repeated, with the only difference that: the pressure of the oxygen pressure leaching in the first stage is controlled to be 1.6Mpa. The pressure is the total pressure and is equal to the partial pressure of oxygen plus the saturated vapor pressure at the temperature. After the reaction, a section of oxygen pressure leaching solution 1000mL (containing Ni 135g/L, cu 8g/L, co 0.84g/L and pH 3.5) is produced, the nickel leaching rate is 94%, the cobalt leaching rate is 95%, and the copper leaching rate is 12%.
Comparative example 3 above shows that when the partial pressure of oxygen introduced in the first stage of oxygen pressure leaching is increased, copper leaching is increased, and selective leaching of nickel and cobalt cannot be achieved.
The foregoing examples are set forth in order to provide a more thorough description of the present invention, and are not intended to limit the scope of the invention, since modifications of the invention in various equivalent forms will occur to those skilled in the art upon reading the present invention, and are within the scope of the invention as defined in the appended claims.
Claims (5)
1. The oxygen pressure leaching method of the high nickel matte under sulfuric acid is characterized by comprising the following steps of:
s1, adding water into high nickel matte, and grinding to obtain ore pulp;
s2, mixing the ore pulp and the nickel waste electro-deposition liquid for one-stage oxygen pressure leaching, controlling the liquid-solid ratio to be 5-6:1, and the concentration of the starting acid to be 40-50g/L, and carrying out solid-liquid separation when the pH value of the solution is 3-4 to obtain one-stage oxygen pressure leaching liquid and one-stage oxygen pressure leaching slag;
purifying and removing impurities from the primary oxygen pressure leaching solution to obtain purified solution, carrying out electro-deposition to produce electro-deposited nickel, and returning the obtained nickel waste electro-deposition solution to be mixed with ore pulp for primary oxygen pressure leaching;
wherein, during the first stage of oxygen pressure leaching, oxygen is introduced, the leaching temperature is controlled to be 180-190 ℃, the pressure is controlled to be 1.4-1.5Mpa, and the reaction time is controlled to be 2-3h;
s3, adding a second-stage oxygen pressure leaching solution into the first-stage oxygen pressure leaching slag for neutralization, controlling the liquid-solid ratio to be 2.5-3.5:1, controlling the temperature to be 60-70 ℃ and the reaction time to be 1.0-1.5h, neutralizing until the pH value is 1-2, and carrying out solid-liquid separation to obtain neutralized slag and neutralized liquid;
partial neutralization solution is sent to electro-deposition to produce electro-deposition copper, and copper waste electro-deposition solution is obtained;
s4, adding part of neutralization liquid into the neutralization slag for size mixing, simultaneously adding copper waste electrodeposited liquid for secondary oxygen pressure leaching, controlling the liquid-solid ratio to be 2.5-3.5:1, the concentration of initial acid to be 90-100g/L, the concentration of final acid for secondary oxygen pressure leaching to be 40-50g/L, and carrying out solid-liquid separation to obtain secondary oxygen pressure leaching liquid and secondary oxygen pressure leaching slag, wherein the secondary oxygen pressure leaching liquid returns to S3;
wherein, during the second stage oxygen pressure leaching, oxygen is introduced, the leaching temperature is controlled to be 170-180 ℃, the pressure is 1.4-1.5Mpa, and the reaction time is 2-3h.
2. The oxygen pressure leaching method of high nickel matte under sulfuric acid according to claim 1, wherein in S4, the volume of the neutralization solution added to the neutralization residue is 40-50% of the total neutralization solution volume.
3. The method for oxygen pressure leaching of high nickel matte in sulfuric acid according to claim 1, wherein the solid phase of the ore pulp has a material ratio of more than or equal to 90wt% and a particle size of less than 30 μm.
4. The oxygen pressure leaching method of high nickel matte according to claim 1, wherein the content ranges of the main components of the high nickel matte are as follows: the content of nickel is 36-46wt%, copper is 32-36wt%, cobalt is 0.1-1wt%, sulfur is 16-20wt%, and the sum of the contents of the components is 100wt%.
5. The oxygen pressure leaching method of high nickel matte according to any of claims 1-4, wherein the concentration of oxygen is not less than 99vol%.
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN112342377A (en) * | 2020-11-13 | 2021-02-09 | 中国恩菲工程技术有限公司 | Treatment process of nickel concentrate |
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| CN113215398A (en) * | 2021-05-06 | 2021-08-06 | 长沙有色冶金设计研究院有限公司 | Oxygen pressure leaching method of nickel sulfide concentrate |
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2022
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| US4093526A (en) * | 1977-09-08 | 1978-06-06 | Amax Inc. | Hydrometallurgical leaching and refining of nickel-copper concentrates, and electrowinning of copper |
| US4323541A (en) * | 1979-06-29 | 1982-04-06 | Outokumpu Oy | Selective two stage leaching of nickel from nickel-copper matte |
| GB2108480A (en) * | 1981-10-30 | 1983-05-18 | Sherritt Gordon Mines Ltd | Acid leach process for treating magnetic and non-magnetic nickel-copper mattes |
| CN1352308A (en) * | 2001-11-09 | 2002-06-05 | 北京矿冶研究总院 | Method for extracting nickel from nickel sulfide material with low copper content |
| CN1544664A (en) * | 2003-11-13 | 2004-11-10 | 吉林吉恩镍业股份有限公司 | Technology for preparing cell-level high purified nickel sulfate by the selective leach of water quenching high grade nickel and sulfuric acid |
| CN101886167A (en) * | 2010-07-01 | 2010-11-17 | 北京矿冶研究总院 | Method for producing cathode nickel by selective leaching-electrodeposition of high nickel matte |
| CN112095016A (en) * | 2020-08-27 | 2020-12-18 | 矿冶科技集团有限公司 | Method for reducing nickel content of high nickel matte leaching residues through hot pressing treatment |
| CN112342377A (en) * | 2020-11-13 | 2021-02-09 | 中国恩菲工程技术有限公司 | Treatment process of nickel concentrate |
| CN113215399A (en) * | 2021-05-06 | 2021-08-06 | 长沙有色冶金设计研究院有限公司 | Oxygen pressure leaching method of nickel sulfide concentrate |
| CN113215398A (en) * | 2021-05-06 | 2021-08-06 | 长沙有色冶金设计研究院有限公司 | Oxygen pressure leaching method of nickel sulfide concentrate |
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