CN114921647A - Oxygen pressure leaching method of nickel matte under sulfuric acid - Google Patents
Oxygen pressure leaching method of nickel matte under sulfuric acid Download PDFInfo
- Publication number
- CN114921647A CN114921647A CN202210616437.2A CN202210616437A CN114921647A CN 114921647 A CN114921647 A CN 114921647A CN 202210616437 A CN202210616437 A CN 202210616437A CN 114921647 A CN114921647 A CN 114921647A
- Authority
- CN
- China
- Prior art keywords
- oxygen pressure
- leaching
- pressure leaching
- solution
- nickel
- 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.)
- Granted
Links
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 160
- 238000002386 leaching Methods 0.000 title claims abstract description 142
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 123
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 123
- 239000001301 oxygen Substances 0.000 title claims abstract description 123
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 73
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000010949 copper Substances 0.000 claims abstract description 63
- 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
- 239000000243 solution Substances 0.000 claims abstract description 44
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 30
- 239000002253 acid Substances 0.000 claims abstract description 29
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 24
- 239000010941 cobalt Substances 0.000 claims abstract description 24
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 20
- 238000000926 separation method Methods 0.000 claims abstract description 9
- 239000003929 acidic solution Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000007787 solid Substances 0.000 claims description 13
- 239000002699 waste material Substances 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
- 230000035484 reaction time Effects 0.000 claims description 7
- 238000004070 electrodeposition Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 230000003472 neutralizing effect Effects 0.000 claims description 2
- 238000005363 electrowinning Methods 0.000 claims 4
- 238000006243 chemical reaction Methods 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 6
- 238000003723 Smelting Methods 0.000 description 5
- 239000003792 electrolyte Substances 0.000 description 5
- 229920006395 saturated elastomer Polymers 0.000 description 5
- 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
- 238000007664 blowing Methods 0.000 description 2
- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000001698 pyrogenic effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000010583 slow cooling Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
Images
Classifications
-
- 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
Landscapes
- 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 and grinding the high nickel matte to prepare ore pulp; mixing the ore pulp with an acid solution and introducing oxygen to carry out primary oxygen pressure leaching to obtain primary oxygen pressure leaching liquid and primary oxygen pressure leaching slag; adding an acid solution into the first-stage oxygen pressure leaching slag for neutralization until the pH value is 1-2, and carrying out solid-liquid separation to produce neutralized slag and neutralized liquid; and adding part of the neutralization solution into the neutralization slag for size mixing, simultaneously adding an acidic solution and introducing oxygen for secondary oxygen pressure leaching to obtain secondary oxygen pressure leaching solution and secondary oxygen pressure leaching slag. Leaching nickel and cobalt is realized through one-stage oxygen pressure leaching, and copper is inhibited in leaching slag to realize the separation of nickel and cobalt from copper; then, the leaching and acid balance of copper are realized through neutralization and two-stage oxygen pressure leaching, 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, belonging to the technical field of hydrometallurgy.
Background
At present, most of nickel sulfide concentrates are treated by a pyrogenic process, namely flash smelting or molten pool smelting is adopted to remove gangue and slag to produce low nickel matte, and then blowing is carried out to remove iron to produce high nickel matte, wherein the total content of nickel and copper is generally 70-80%. The high nickel matte with low copper content (Cu 10%) is generally cast into an anode plate to directly produce the electrolytic nickel, and the high nickel matte with high copper content (more than Cu 20%) can be separated into secondary copper concentrate by slow cooling flotation, so that the secondary nickel concentrate is cast into a nickel sulfide anode to produce the electrolytic nickel. The other wet method for treating nickel matte is selective leaching with sulfuric acid, i.e. atmospheric pressure leaching and air pressure leaching are combined to leach most of nickel and cobalt, while most of copper is inhibited in leached slag, so as to achieve the purpose of separating and recovering valuable metals such as nickel, copper, cobalt and the like. However, the sulfuric acid selective leaching of nickel matte adopts two-stage atmospheric pressure leaching and one-stage air pressure leaching to leach most of nickel and cobalt, the leaching process is long, and the control requirement of the copper precipitation process on the raw material sulfur is strict. The produced leaching slag is generally treated by 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 a method for leaching nickel matte under the condition of sulfuric acid under oxygen pressure, wherein the nickel and cobalt are leached through primary oxygen pressure leaching, copper is inhibited in leaching slag, the nickel and cobalt are separated from the copper, and then the copper is leached and acid balance is realized through neutralization and secondary oxygen pressure leaching, so that the leaching process is greatly shortened.
The technical scheme adopted by the application is as follows:
a method for oxygen pressure leaching of nickel matte under sulfuric acid comprises the following steps:
s1, adding water into the high nickel matte to grind the high nickel matte to prepare ore pulp;
s2, mixing the ore pulp with an acidic solution for primary oxygen pressure leaching, controlling the liquid-solid ratio to be 5-6:1, controlling the initial acid concentration to be 40-50g/L, and when the pH value of the solution is 3-4, carrying out solid-liquid separation to obtain primary oxygen pressure leaching liquid and primary oxygen pressure leaching slag;
wherein, during the first stage of oxygen pressure leaching, oxygen is required to be introduced, the leaching temperature is controlled to be 180-190 ℃, the pressure is 1.4-1.5Mpa, and the reaction time is 2-3 h;
s3, adding an acid solution into the primary oxygen pressure leaching slag for neutralization, controlling the liquid-solid ratio to be 2.5-3.5:1, the temperature to be 60-70 ℃, the reaction time to be 1.0-1.5h, neutralizing until the pH value is 1-2, carrying out solid-liquid separation, and producing neutralized slag and neutralized liquid;
s4, adding part of the neutralization solution into the neutralization slag for size mixing, simultaneously 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 final acid concentration of the secondary oxygen pressure leaching to be 40-50g/L, and carrying out solid-liquid separation to obtain secondary oxygen pressure leaching solution and secondary oxygen pressure leaching slag;
wherein, during the two-stage oxygen pressure leaching, oxygen is required to be introduced, the leaching temperature is controlled to be 170-180 ℃, the pressure is 1.4-1.5Mpa, and the reaction time is 2-3 h.
In the above steps, the pressures are total pressures equal to the oxygen partial pressure plus the saturated vapor pressure at the temperature; the first-stage oxygen pressure leaching slag is copper slag, and the second-stage oxygen pressure leaching slag is sulfur slag.
Further, in S4, the volume of the neutralization solution added to the neutralized slag is 40-50% of the total volume of the neutralization solution.
Further, the secondary oxygen pressure leach liquor produced in S4 was returned to S3 as an acidic solution.
Further, purifying the primary oxygen pressure leaching solution to remove impurities to obtain a purified solution, conveying the purified solution to electrodeposition to produce electrodeposited nickel, and returning the obtained nickel waste electrolyte to S2 as an acid solution.
Further, the neutralization solution produced in the step S3 is sent to electrodeposition to produce electrodeposited copper, and the obtained copper waste electrodeposition liquid is returned to the step S4 as an acid solution.
Furthermore, in the solid phase matter of the ore pulp, the material with the particle size of less than 30 mu m accounts for more than or equal to 90 wt%.
Chinese patent application publication No. CN101705367B discloses a process for smelting copper and nickel by an oxygen-enriched side-blown molten pool smelting method, charging materials are added into an oxygen-enriched side-blown furnace, oxygen-enriched air is blown into the oxygen-enriched side-blown furnace to carry out oxygen-enriched molten pool smelting to obtain low nickel matte, and then the low nickel matte is obtained by depletion and blowing in an electric furnace. Specifically, the content ranges of the main components of the obtained high nickel matte are as follows: the nickel content is 36-46 wt%, the copper content is 32-36 wt%, the cobalt content is 0.1-1 wt%, the sulfur content is 16-20 wt%, and the sum of the contents of all the components is 100 wt%.
Further, the concentration of oxygen is not less than 99 vol%.
The main reaction principle of the invention is as follows:
in primary oxygen pressure leaching, nickel and cobalt enter the primary oxygen pressure leach liquor, while copper enters the primary oxygen pressure leach residue:
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)
in the above reaction, the reaction (4) is the main reaction, and the reaction rate depends on the primary oxygen pressure leaching temperature. The reactions (3), (4), (5) cause the nickel to be largely leached. H 2 SO 4 And CuSO 4 The amount of Cu required for the reaction is rapidly reduced 2+ By the supplement of the two reactions (1) and (2), copper is transferred into slag as CuS. As the one-stage oxygen pressure leach proceeds, the starting acid is lowered from 40-50g/L to a pH of about 4, at which point the copper in the solution is about 1g/L, or even lower. Therefore, the proper starting and final acids, and pressures, are selected to result in an increased copper or decreased nickel and cobalt leaching rate.
In the second stage oxygen pressure leaching, copper enters a second stage oxygen pressure leaching 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:
(1) one-stage oxygen pressure leaching is adopted to replace two-stage atmospheric pressure leaching and one-stage air pressure leaching, and two-stage oxygen pressure leaching neutralization slag is adopted to replace two-stage roasting and two-stage leaching, so that the process is short, the equipment is less, and the efficiency is high.
(2) The nickel matte is leached by adopting one-stage oxygen pressure, the leaching rate of nickel and cobalt is more than 90 percent, most of copper is inhibited in one-stage oxygen pressure leaching slag, the effective separation and enrichment of copper and nickel are achieved, the initial acid of one-stage oxygen pressure leaching liquid is reduced from 40-50g/L to the pH value of 3-4, and the nickel matte can be directly subjected to subsequent purification and impurity removal and electrodeposition to produce the nickel matte without a neutralization process.
(3) The second-stage oxygen pressure leaching neutralization slag is adopted, the copper leaching rate can be higher than 95%, nickel and cobalt can be leached along with the copper leaching rate, the total leaching rate of nickel and cobalt can be higher than 97%, the initial acid of the second-stage oxygen pressure leaching solution is reduced to 40-50g/L from 90-100g/L, the first-stage oxygen pressure leaching slag is directly used for neutralization until the pH value is 1-2, the first-stage oxygen pressure leaching slag is used as a neutralizer to produce neutralization slag, the neutralization slag returns to the second-stage oxygen pressure leaching, and no metal loss brought away by the neutralization slag exists.
(4) Because the copper waste electrolyte has high acid concentration, the returned neutralization solution is adopted to size the copper slag, the secondary oxygen pressure leaching is carried out after the initial 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 a process for the oxygen pressure leaching of nickel matte under 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 the embodiments and features of the embodiments may be combined with each other without conflict. Unless otherwise specified, the following percentages are all by mass.
Example 1:
200g of 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 particle size of 90% is less than 30 mu m, nickel waste electrolyte (containing 60g/L of Ni) is added into the ore pulp after fine grinding, the liquid-solid ratio is controlled to be 5.0:1, and the starting acid is 40 g/L. Adding the prepared ore pulp into a first-stage autoclave for first-stage oxygen pressure leaching, introducing oxygen with the concentration of 99 vol%, controlling the temperature at 180 ℃, the pressure at 1.4Mpa, and reacting for 2h to obtain 1000mL of first-stage oxygen pressure leaching solution (containing 133g/L of Ni, 1g/L of Cu and 0.80g/L of Co, and the pH value is 4). The pressure is the total pressure, equal to the partial pressure of oxygen plus the saturated vapor pressure at that temperature. Wherein, the leaching rate of nickel is 91 percent, and the leaching rate of cobalt is 91 percent. And adding the produced first-stage oxygen pressure leaching slag, namely copper slag, into a second-stage oxygen pressure leaching solution for neutralization, controlling the liquid-solid ratio to be 3.5:1, the temperature to be 60 ℃, reacting for 1.0h, and producing 560mL of a neutralization solution to be sent to the subsequent working procedures. 230mL of returned neutralization solution is added into the produced neutralization slag, the neutralization solution is added into a second-stage autoclave, copper waste electro-hydraulic fluid (containing 40g/L of Cu) is added at the same time, the liquid-solid ratio is controlled to be 3.5:1, the initial acid is 90g/L, oxygen with the concentration of 99 vol% is introduced at the same time for second-stage oxygen pressure leaching, the temperature is controlled to be 170 ℃, the pressure is 1.4Mpa, the reaction time is 2h, 560mL of second-stage oxygen pressure leaching solution (containing 184g/L of Cu, 9.6g/L of Ni, 0.10g/L of Co and 41g/L of sulfuric acid) is produced, and 64g of second-stage oxygen pressure leaching slag (containing 2.5% of Ni, 5.2% of Cu, 0.04% of Co and 43.8%) is produced. Wherein the second-stage oxygen pressure leaching slag is the sulfur slag which can be sold. The leaching rate of copper is 95%, the total leaching rate of nickel is 98%, and the total leaching rate of cobalt is 97%.
Example 2:
200g of 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 particle size of 90% is less than 30 mu m, nickel waste electrolyte (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 initial acid is controlled to be 45 g/L. Adding the prepared ore pulp into a first-stage high-pressure kettle for first-stage oxygen pressure leaching, introducing oxygen with the concentration of 99 vol%, controlling the temperature at 185 ℃, the pressure at 1.45Mpa, and reacting for 2.5 hours to obtain 1100mL (containing 122g/L of Ni, 1g/L of Cu, 0.74g/L of Co, and the pH value of 3) of first-stage oxygen pressure leaching solution. The pressure is the total pressure, equal to the partial pressure of oxygen plus the saturated vapor pressure at that temperature. Wherein, the leaching rate of nickel is 92.5 percent, and the leaching rate of cobalt is 92 percent. Adding the produced first-stage oxygen pressure leaching slag, namely copper slag, into second-stage oxygen pressure leaching liquid for neutralization, controlling the liquid-solid ratio to be 2.5:1, the temperature to be 65 ℃, reacting for 1.2h, producing 400mL of neutralized liquid, sending the neutralized liquid to the subsequent process, adding 180mL of returned neutralized liquid into the produced neutralized slag, mixing, adding copper waste electrolyte (containing 40g/L of Cu), controlling the liquid-solid ratio to be 2.5:1, starting acid to be 95g/L, introducing oxygen with the concentration of 99 vol% to carry out second-stage oxygen pressure leaching, controlling the temperature to be 175 ℃, the pressure to be 1.45Mpa, reacting for 2.5h, producing 400mL of second-stage oxygen pressure leaching liquid (containing 253g/L of Cu, 11.4g/L of Ni, 0.13g/L of Cu and 42g/L of sulfuric acid), and producing 60g of second-stage oxygen pressure leaching slag (containing 2.4% of Ni, 5.1% of Cu, 0.03% of Co and 42.9%). Wherein the second-stage oxygen pressure leaching slag is the sulfur slag which can be sold. The copper leaching rate is 95.4 percent, the total nickel leaching rate is 98.2 percent, and the total cobalt leaching rate is 97.9 percent.
Comparative example 1:
the first stage oxygen pressure leach of example 1 was repeated except that: the initial acid of the first stage oxygen pressure leaching is controlled to be 60 g/L. After the reaction, 1000mL of primary oxygen pressure leaching solution (containing 135g/L of Ni, 15g/L of Cu, 0.83g/L of Co and H) is produced 2 SO 4 12g/L), the leaching rate of nickel is 94%, the leaching rate of cobalt is 94% and the leaching rate of copper is 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 nickel matte is high, and the selective leaching of nickel and cobalt is not realized.
Comparative example 2:
the first stage oxygen pressure leach of example 1 was repeated except that: the pressure of the first stage oxygen pressure leaching is controlled to be 1.3 Mpa. The pressure is the total pressure, equal to the partial pressure of oxygen plus the saturated vapor pressure at that temperature. After the reaction, 1000mL of primary oxygen pressure leaching solution (containing Ni 130g/L, Cu 1g/L, Co 0.78g/L and H) is produced 2 SO 4 7g/L), the leaching rate of nickel is 88 percent, the leaching rate of cobalt is 89 percent, and the leaching rate of copper is 2 percent.
The above comparative example 2 shows that when the partial pressure of oxygen introduced in the first stage oxygen pressure leaching is reduced, the leaching rates of nickel and cobalt are reduced.
Comparative example 3
The first stage oxygen pressure leach of example 1 was repeated except that: the pressure of the first stage oxygen pressure leaching is controlled to be 1.6 Mpa. The pressure is the total pressure, equal to the partial pressure of oxygen plus the saturated vapor pressure at that temperature. After the reaction, 1000mL of primary oxygen pressure leaching solution (containing 135g/L of Ni, 8g/L of Cu and 0.84g/L of Co and having a pH value of 3.5) is produced, wherein the leaching rate of nickel is 94%, the leaching rate of cobalt is 95% and the leaching rate of copper is 12%.
The above comparative example 3 shows that when the partial pressure of oxygen introduced in the first stage of oxygen pressure leaching is increased, the leaching of copper is increased, and the selective leaching of nickel and cobalt cannot be realized.
The foregoing examples are set forth to illustrate the present invention more clearly and are not to be construed as limiting the scope of the invention, which is defined in the appended claims to which the invention pertains, as modified in all equivalent forms, by those skilled in the art after reading the present invention.
Claims (8)
1. The method for leaching the nickel matte under the oxygen pressure of sulfuric acid is characterized by comprising the following steps of:
s1, adding water into the high nickel matte for grinding to prepare ore pulp;
s2, mixing the ore pulp with an acidic solution for primary oxygen pressure leaching, controlling the liquid-solid ratio to be 5-6:1, controlling the initial acid concentration to be 40-50g/L, and when the pH value of the solution is 3-4, carrying out solid-liquid separation to obtain primary oxygen pressure leaching liquid and primary oxygen pressure leaching slag;
wherein, in the period of one-stage oxygen pressure leaching, oxygen is required to be introduced, the leaching temperature is controlled to be 180 ℃ and 190 ℃, the pressure is 1.4-1.5Mpa, and the reaction time is 2-3 h;
s3, adding an acidic solution into the first-stage oxygen pressure leaching slag for neutralization, controlling the liquid-solid ratio to be 2.5-3.5:1, the temperature to be 60-70 ℃, the reaction time to be 1.0-1.5h, neutralizing until the pH value is 1-2, carrying out solid-liquid separation, and producing neutralized slag and neutralized liquid;
s4, adding part of the neutralization solution into the neutralization slag for size mixing, simultaneously 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 final acid concentration of the secondary oxygen pressure leaching to be 40-50g/L, and carrying out solid-liquid separation to obtain secondary oxygen pressure leaching solution and secondary oxygen pressure leaching slag;
wherein, during the two-stage oxygen pressure leaching, oxygen is required to be introduced, the leaching temperature is controlled at 170-180 ℃, the pressure is 1.4-1.5Mpa, and the reaction time is 2-3 h.
2. The method for oxygen pressure leaching of nickel matte according to claim 1, wherein in S4, the volume of the neutralization solution added to the neutralized slag is 40-50% of the total neutralization solution volume.
3. The nickel freeite oxygen pressure leaching process under sulfuric acid according to claim 1, wherein the secondary oxygen pressure leaching solution produced in S4 is returned to S3 as an acidic solution.
4. The method for leaching nickel matte under sulfuric acid by using oxygen pressure as claimed in claim 1, wherein the primary oxygen pressure leaching solution is purified to remove impurities, so as to obtain a purified solution, the purified solution is sent to electrowinning to produce electrowinning nickel, and the obtained nickel waste electrowinning solution is returned to S2 as an acidic solution.
5. The process of oxygen pressure leaching of nickel matte under sulfuric acid as claimed in claim 1, wherein the neutralized solution produced in S3 is sent to electrodeposition to produce electrodeposited copper, and the obtained copper waste electrowinning solution is returned to S4 as an acidic solution.
6. The method for leaching high nickel matte through oxygen pressure under sulfuric acid according to claim 1, wherein the solid matter in the ore pulp contains materials with the particle size of less than 30 μm by weight of more than or equal to 90 wt%.
7. The method for oxygen pressure leaching of nickel matte under sulfuric acid according to claim 1, wherein the content range of each main component of the obtained nickel matte is as follows: the nickel content is 36-46 wt%, the copper content is 32-36 wt%, the cobalt content is 0.1-1 wt%, the sulfur content is 16-20 wt%, and the sum of the contents of all the components is 100 wt%.
8. A nickel homomatte oxygen pressure leaching process according to any one of claims 1-7, wherein the concentration of oxygen is not less than 99 vol%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210616437.2A CN114921647B (en) | 2022-06-01 | 2022-06-01 | Oxygen pressure leaching method of high nickel matte under sulfuric acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210616437.2A CN114921647B (en) | 2022-06-01 | 2022-06-01 | Oxygen pressure leaching method of high nickel matte under sulfuric acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114921647A true CN114921647A (en) | 2022-08-19 |
| CN114921647B CN114921647B (en) | 2024-01-30 |
Family
ID=82812546
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210616437.2A Active CN114921647B (en) | 2022-06-01 | 2022-06-01 | Oxygen pressure leaching method of high nickel matte under sulfuric acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114921647B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115948662A (en) * | 2022-12-31 | 2023-04-11 | 广西中伟新能源科技有限公司 | Method for leaching sulfide minerals |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 | A kind of high matte nickel selective leaching-electrowinning method for producing cathode nickel |
| 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 |
-
2022
- 2022-06-01 CN CN202210616437.2A patent/CN114921647B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 | A kind of high matte nickel selective leaching-electrowinning method for producing cathode nickel |
| 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 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115948662A (en) * | 2022-12-31 | 2023-04-11 | 广西中伟新能源科技有限公司 | Method for leaching sulfide minerals |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114921647B (en) | 2024-01-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| RU2741429C1 (en) | Method and system for complete reprocessing of copper-nickel sulphide ore | |
| CN110241310B (en) | Method for enriching noble metals by selective oxygen pressure leaching of high-iron high-copper nickel-containing material | |
| EP0930373B1 (en) | Recovery of nickel and/or cobalt from a hydroxide concentrate with an ammonium leach solution | |
| AU740712B2 (en) | Chloride assisted hydrometallurgical extraction of nickel and cobalt from sulphide or laterite ores | |
| US7666371B2 (en) | Method for recovering metal values from metal-containing materials using high temperature pressure leaching | |
| RU2149195C1 (en) | Method of hydrometallurgical recovery of nickel from nickel matte of two types | |
| US7811357B2 (en) | Method for recovering rare metals in zinc leaching process | |
| US4008076A (en) | Method for processing manganese nodules and recovering the values contained therein | |
| CN107630146B (en) | Nickel recovery process | |
| KR20090042996A (en) | Manufacture of metal nickel with low iron content | |
| CN112342377B (en) | Treatment process of nickel concentrate | |
| CA2251433C (en) | Process for upgrading copper sulphide residues containing nickel and iron | |
| WO2013030450A1 (en) | Method for recovering metals from material containing them | |
| US11584974B2 (en) | System and method including multi-circuit solution extraction for recovery of metal values from metal-bearing materials | |
| CN113215399B (en) | Oxygen pressure leaching method of nickel sulfide concentrate | |
| WO2020062145A1 (en) | Oxygen pressure leaching method for copper sulfide concentrate and copper smelting method | |
| JP2024528355A (en) | Copper leaching method using pressure leaching | |
| KR102178219B1 (en) | Economical Smelting Method for Nickel from Nickel Sulfide ore, combined Hydrometallurgical and Pyrometallurgical Process | |
| CN114921647B (en) | Oxygen pressure leaching method of high nickel matte under sulfuric acid | |
| CN114502752B (en) | Method for processing copper sulfide and nickel sulfide materials | |
| CN110777257B (en) | Method for selectively leaching iron from low grade nickel matte | |
| US20240240279A1 (en) | Method for producing aqueous solution containing nickel, cobalt and manganese | |
| WO2020166735A1 (en) | Economical method, using combination of wet and dry processes, for smelting nickel from nickel sulfide ores | |
| CN116162802A (en) | Method for extracting nickel and cobalt by using laterite-nickel ore type high nickel matte | |
| CN116377218A (en) | Method and system for comprehensively utilizing high-magnesium nickel sulfide ore by low-temperature oxygen enrichment method |
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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |