CN103773951A - Method for recovering nickel and cobalt through leaching laterite-nickel ore by using sulfuric and hydrochloric acid containing mixed waste acid - Google Patents
Method for recovering nickel and cobalt through leaching laterite-nickel ore by using sulfuric and hydrochloric acid containing mixed waste acid Download PDFInfo
- Publication number
- CN103773951A CN103773951A CN201410027777.7A CN201410027777A CN103773951A CN 103773951 A CN103773951 A CN 103773951A CN 201410027777 A CN201410027777 A CN 201410027777A CN 103773951 A CN103773951 A CN 103773951A
- Authority
- CN
- China
- Prior art keywords
- nickel
- cobalt
- hydrochloric acid
- acid
- deironing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 165
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims abstract description 91
- 239000002253 acid Substances 0.000 title claims abstract description 80
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 74
- 239000010941 cobalt Substances 0.000 title claims abstract description 29
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 29
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 19
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title abstract description 24
- 238000002386 leaching Methods 0.000 title abstract description 13
- 239000010812 mixed waste Substances 0.000 title abstract 8
- 238000011084 recovery Methods 0.000 claims abstract description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 37
- 238000002156 mixing Methods 0.000 claims description 37
- 239000000203 mixture Substances 0.000 claims description 35
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 32
- 239000011593 sulfur Substances 0.000 claims description 32
- 229910052717 sulfur Inorganic materials 0.000 claims description 32
- 239000002689 soil Substances 0.000 claims description 31
- 239000007788 liquid Substances 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 239000011777 magnesium Substances 0.000 claims description 23
- 238000001914 filtration Methods 0.000 claims description 17
- 238000013019 agitation Methods 0.000 claims description 12
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 claims description 11
- 239000000706 filtrate Substances 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 11
- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- ASKVAEGIVYSGNY-UHFFFAOYSA-L cobalt(ii) hydroxide Chemical compound [OH-].[OH-].[Co+2] ASKVAEGIVYSGNY-UHFFFAOYSA-L 0.000 claims description 9
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 9
- 239000000347 magnesium hydroxide Substances 0.000 claims description 9
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 9
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 claims description 9
- 239000012065 filter cake Substances 0.000 claims description 8
- 229910052742 iron Inorganic materials 0.000 claims description 8
- 238000013467 fragmentation Methods 0.000 claims description 5
- 238000006062 fragmentation reaction Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 230000007062 hydrolysis Effects 0.000 claims description 5
- 238000006460 hydrolysis reaction Methods 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 230000003472 neutralizing effect Effects 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 239000000047 product Substances 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 38
- 239000002699 waste material Substances 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000010409 ironing Methods 0.000 abstract 1
- 230000001376 precipitating effect Effects 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 229910000831 Steel Inorganic materials 0.000 description 10
- 239000010959 steel Substances 0.000 description 10
- 238000003756 stirring Methods 0.000 description 9
- 239000000243 solution Substances 0.000 description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- 239000004571 lime Substances 0.000 description 4
- 239000012530 fluid Substances 0.000 description 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 235000012204 lemonade/lime carbonate Nutrition 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000002910 solid waste Substances 0.000 description 2
- 239000012267 brine Substances 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 150000001868 cobalt Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for recovering nickel and cobalt through leaching laterite-nickel ore by using sulfuric and hydrochloric acid containing mixed waste acid. The method comprises the processes of carrying out stirred leaching on sulfuric and hydrochloric acid containing mixed waste acid, de-ironing a leachate and precipitating nickel and cobalt. According to the method, sulfuric and hydrochloric acid containing mixed waste acid generated during chemical industry production can be treated, meanwhile, the comprehensive utilization of sulfuric and hydrochloric acid containing mixed waste acid is realized, the waste is changed into the valuable, the laterite-nickel ore is leached, nickel and cobalt are recovered simultaneously, the recovery ratio of nickel and cobalt is high, the production scale can be large and small, and the range of used sulfuric and hydrochloric acid containing mixed waste acid is large; the method disclosed by the invention has the characteristics of simple process path, small investment, low energy consumption, low operating cost, no environmental pollution, comprehensive utilization in sulfuric and hydrochloric acid containing mixed waste acid, simplicity and convenience in operation, low production cost and the like, so that an extremely effective, economical and applicable way for the treatment and comprehensive utilization of sulfuric and hydrochloric acid containing mixed waste acid and the recovery of nickel and cobalt through laterite-nickel ore leaching is provided.
Description
Technical field
The mixing spent acid that the present invention relates to sulfur acid, hydrochloric acid leaches the method for red soil nickel ore recovery nickel cobalt, and especially, containing the mixing spent acid comprehensive utilization of low-concentration hcl, sulfuric acid, leaching red soil nickel ore reclaims the method for nickel cobalt, belongs to resource recycling field.
Background technology
The sulfur acid that chemical industry produces, the mixing spent acid of hydrochloric acid, contain organic impurity, contains again sulfuric acid, hydrochloric acid simultaneously, and reclaim equiment requires high, and running cost is high, directly recycling difficulty.The mixing spent acid of lime treatment sulfur acid, hydrochloric acid, need to consume large quantities of lime, and produces a large amount of solid wastes and waste water, and cost is high, there is no persistence.
The wet processing of red soil nickel ore, adopts technical hydrochloric acid, sulfuric acid leaching, and speed is fast, and leaching yield is high, but technical hydrochloric acid, sulfuric acid price are higher, there is no economy.
The traditional method of processing the mixing spent acid of sulfur acid, hydrochloric acid is to adopt lime or calcium carbonate neutralization, and average spent acid per ton consumes lime or calcium carbonate 200kg, 0.8 ton of output brine waste, output Industrial Solid Waste weight in wet base 400kg, moisture 50%.Therefore, how fully, fully utilize limited chemical industry sulfur acid, the mixing spent acid of hydrochloric acid, low-cost processes red soil nickel ore, has become the main goal in research of scientific and technical personnel.
Summary of the invention
For overcoming the processing of mixing spent acid, the utilization difficulty of chemical industry sulfur acid, hydrochloric acid, existing red soil nickel ore wet processing high in cost of production deficiency, the invention provides a kind of investment little, technique is simple, energy consumption is low, production cost is low, and the chemical industry sulfur acid that nickel and cobalt recovery rate is high, the mixing spent acid of hydrochloric acid are in conjunction with the method that leaches red soil nickel ore recovery nickel cobalt.
The present invention is achieved through the following technical solutions: the mixing spent acid of a kind of sulfur acid, hydrochloric acid leaches the method for red soil nickel ore recovery nickel cobalt, the mixing spent acid agitation leach of sulfur acid, hydrochloric acid, and deironing, heavy nickel, cobalt, specifically realize by following steps:
1, the mixing spent acid agitation leach of sulfur acid, hydrochloric acid:
Red soil nickel ore fragmentation, ore grinding to 0.15mm, with sulfur acid, hydrochloric acid mix spent acid by liquid-solid ratio 3～5:1, temperature 60～80, ℃ agitation leach 3～6h, has leached rear filtration, washing, merging filtrate and wash water, obtain filter cake leached mud, leach liquor;
2, leach liquor deironing:
Leach liquor hydro-oxidation magnesium hydrolysis deironing, controls deironing temperature of reaction 60～80, ℃ deironing terminal PH2.5～4, and deironing reaction 3h, deironing completes carries out solid-liquid separation, obtains liquid after crude iron ore deposit, deironing.
3, heavy nickel, cobalt:
Liquid hydro-oxidation sodium solution after deironing, 20～40 ℃ of heavy nickel, cobalt, heavy nickel, cobalt terminal PH8.5～9, heavy nickel, cobalt reaction 1h, heavy nickel, cobalt complete and carry out solid-liquid separation, obtain liquid after nickel hydroxide and cobaltous hydroxide product, heavy nickel.
Above-mentioned operation is all to carry out in unlimited steel basin.
H in described sulfur acid, the mixing spent acid of hydrochloric acid
2sO
4massfraction is that the massfraction of 10～50%, HCl is 10～30%.
The neutralizing agent adopting in described leach liquor deironing is magnesium hydroxide powder, or water and magnesium hydroxide are made into the slurry containing magnesium hydroxide 10～30wt%.
The massfraction of the sodium hydroxide solution adopting in described heavy nickel, cobalt is 5～20%.
The present invention compared with prior art has following advantages and effect: (1) can process the sulfur acid producing in chemical process, the mixing spent acid of hydrochloric acid, realize sulfur acid simultaneously, the mixing spent acid comprehensive utilization of hydrochloric acid, turn waste into wealth, leach red soil nickel ore, reclaim nickel cobalt simultaneously, nickel and cobalt recovery rate is high, its industrial scale is changeable, the sulfur acid using, the mixing spent acid scope of hydrochloric acid is wide, it is simple that the present invention's processing method has processing route, invest little, energy consumption is low, working cost is low, free from environmental pollution, sulfur acid, the mixing spent acid comprehensive utilization of hydrochloric acid, easy and simple to handle, the features such as production cost is low.Thereby, be the processing of the mixing spent acid of sulfur acid, hydrochloric acid, comprehensive utilization is leached red soil nickel ore and is reclaimed nickel cobalt very effective and affordable approach is provided.
Embodiment
Below in conjunction with specific embodiment, the present invention is described further.
Embodiment 1
1, the mixing spent acid agitation leach of sulfur acid, hydrochloric acid
Red soil nickel ore fragmentation, ore grinding, to 0.15mm, uses filtration area 8m
2plate-and-frame filter press press filtration becomes filter cake, prepares 400kg(moisture 50%, containing dry ore deposit 200kg).Its chemical composition is as following table.
Red soil nickel ore chemical composition
| Ni% | Fe% | Mg% | Co% |
| 1.4 | 13.8 | 12.2 | 0.10 |
The mixing spent acid 400kg of sulfur acid, hydrochloric acid, H
2sO
4content is that the massfraction of 50%, HCl is 10%, joins 2m
3in steel basin, in the situation that stirring, add ready 400kg red soil nickel ore (liquid-solid ratio 3:1), be heated to temperature 80, ℃ agitation leach 6h, has leached rear employing filtration area 8m
2plate-and-frame filter press filters, and directly, in add water 110kg washing of pressure filter, merging filtrate and wash water, obtain filter cake leached mud, leach liquor, and its chemical composition is as following table.
Red soil nickel ore mixing waste acid leaching fluid chemical composition
| Volume L | Ni?g/L | Fe?g/L | Mg?g/L | Co?g/L |
| 602 | 4.3 | 31.6 | 36.2 | 0.3 |
The red soil nickel ore mixing waste acid leaching chemical composition of slagging tap
| Weight in wet base kg | Dry weight kg | Moisture % | Ni% | Fe% | Mg% | Co% |
| 220 | 110 | 50 | 0.2 | 7.8 | 2.40 | 0.02 |
2, leach liquor deironing
At 2m
3in steel basin, add water 60kg, be heated to 80 ℃, add leach liquor with the speed of 300L/h, add leach liquor to add moisture 75% magnesium hydroxide slurry 190kg simultaneously, control reaction system PH2.5, hydrolysis deironing, deironing completes and adopts filtration area 4m
2plate-and-frame filter press filters, and directly in add water 48kg washing of pressure filter, merging filtrate and wash water, obtain liquid after crude iron ore deposit, deironing.Its chemical composition is as following table.
Liquid chemical composition after deironing
| Volume L | Ni?g/L | Fe?g/L | Mg?g/L | Co?g/L |
| 750 | 3.45 | ≤0.01 | 53.7 | 0.24 |
Crude iron ore deposit chemical composition
| Weight in wet base kg | Dry weight kg | Moisture % | Ni% | Fe% | Mg% | Co% |
| 96 | 48 | 50 | 0.01 | 39.6 | 1.2 | 0.001 |
3, heavy nickel, cobalt
After deironing, liquid is added to 2m
3in steel basin, be heated to 40 ℃, stirring state adds and slowly adds 20wt% sodium hydroxide solution 26kg, stirs 1h, heavy nickel, cobalt terminal PH8.5.Employing filtration area 4m after heavy nickel, cobalt complete
2plate-and-frame filter press filters, and directly in add water 15kg washing of pressure filter, merging filtrate and wash water, obtain liquid after nickel hydroxide and cobaltous hydroxide, heavy nickel.Its chemical composition is as following table.
Liquid chemical composition after heavy nickel
| Volume L | Ni?g/L | Fe?g/L | Mg?g/L | Co?g/L |
| 760 | 0.005 | ≤0.01 | 45.2 | ≤0.001 |
Nickel hydroxide and cobaltous hydroxide chemical composition
| Weight in wet base kg | Dry weight kg | Moisture % | Ni% | Fe% | Mg% | Co% |
| 21.6 | 6.5 | 70 | 39.8 | ≤0.01 | 2.2 | 2.7 |
Embodiment 2
1, the mixing spent acid agitation leach of sulfur acid, hydrochloric acid
Red soil nickel ore fragmentation, ore grinding, to 0.15mm, uses filtration area 100m
2plate-and-frame filter press press filtration becomes filter cake, prepares 4t(moisture 50%, containing dry ore deposit 2t).Its chemical composition is as following table.
Red soil nickel ore chemical composition
| Ni% | Fe% | Mg% | Co% |
| 1.2 | 8.0 | 14.4 | 0.05 |
The mixing spent acid 6t of sulfur acid, hydrochloric acid, H
2sO
4content is that the massfraction of 10%, HCl is 30%, joins 12m
3in steel basin (liquid-solid ratio 5:1), in the situation that stirring, add ready 4t red soil nickel ore, be heated to temperature 60, ℃ agitation leach 3h, has leached rear employing filtration area 100m
2plate-and-frame filter press filters, and directly, in add water 1.1t washing of pressure filter, merging filtrate and wash water, obtain filter cake leached mud, leach liquor, and its chemical composition is as following table.
Red soil nickel ore mixing waste acid leaching fluid chemical composition
| Volume m 3 | Ni?g/L | Fe?g/L | Mg?g/L | Co?g/L |
| 5.9 | 3.73 | 19.3 | 41 | 0.15 |
The red soil nickel ore mixing waste acid leaching chemical composition of slagging tap
| Weight in wet base t | Dry weight t | Moisture % | Ni% | Fe% | Mg% | Co% |
| 2.2 | 1.1 | 50 | 0.18 | 4.2 | 2.40 | 0.01 |
2, leach liquor deironing
At 12m
3in steel basin, add water 0.1m
3, be heated to 60 ℃, with 3m
3the speed of/h adds leach liquor, adds leach liquor to add moisture 75% magnesium hydroxide slurry 2.5t simultaneously, controls reaction system PH4, hydrolysis deironing, and deironing completes and adopts filtration area 100m
2plate-and-frame filter press filters, and directly in add water 48kg washing of pressure filter, merging filtrate and wash water, obtain liquid after crude iron ore deposit, deironing.Its chemical composition is as following table.
Liquid chemical composition after deironing
| Volume m 3 | Ni?g/L | Fe?g/L | Mg?g/L | Co?g/L |
| 7.4 | 2.98 | ≤0.01 | 54.2 | 0.12 |
Crude iron ore deposit chemical composition
| Weight in wet base t | Dry weight t | Moisture % | Ni% | Fe% | Mg% | Co% |
| 0.56 | 0.28 | 50 | 0.01 | 40.6 | 1.2 | 0.0005 |
3, heavy nickel, cobalt
After deironing, liquid is added to 12m
3in steel basin, be heated to 20 ℃, stirring state adds and slowly adds 5% sodium hydroxide solution 880kg, stirs 1h, heavy nickel, cobalt terminal PH9.Employing filtration area 40m after heavy nickel, cobalt complete
2plate-and-frame filter press filters, and directly in add water 125kg washing of pressure filter, merging filtrate and wash water, obtain liquid after nickel hydroxide and cobaltous hydroxide, heavy nickel.Its chemical composition is as following table.
Liquid chemical composition after heavy nickel
| Volume m 3 | Ni?g/L | Fe?g/L | Mg?g/L | Co?g/L |
| 7.7 | 0.005 | ≤0.01 | 45.3 | ≤0.001 |
Nickel hydroxide and cobaltous hydroxide chemical composition
| Weight in wet base kg | Dry weight kg | Moisture % | Ni% | Fe% | Mg% | Co% |
| 180 | 55 | 69.4 | 40 | ≤0.01 | 2.2 | 1.6 |
Embodiment 3
1, the mixing spent acid agitation leach of sulfur acid, hydrochloric acid
Red soil nickel ore fragmentation, ore grinding, to 0.15mm, uses filtration area 100m
2plate-and-frame filter press press filtration becomes filter cake, prepares 4t(moisture 50%, containing dry ore deposit 2t).Its chemical composition is as following table.
Red soil nickel ore chemical composition
| Ni% | Fe% | Mg% | Co% |
| 1.3 | 10.0 | 11.2 | 0.05 |
The mixing spent acid 6t of sulfur acid, hydrochloric acid, H
2sO
4content is that the massfraction of 30%, HCl is 20%, joins 12m
3in steel basin (liquid-solid ratio 4:1), in the situation that stirring, add ready 4t red soil nickel ore, be heated to temperature 70 C, agitation leach 4.5h, has leached rear employing filtration area 100m
2plate-and-frame filter press filters, and directly, in add water 1.1t washing of pressure filter, merging filtrate and wash water, obtain filter cake leached mud, leach liquor, and its chemical composition is as following table.
Red soil nickel ore mixing waste acid leaching fluid chemical composition
| Volume m 3 | Ni?g/L | Fe?g/L | Mg?g/L | Co?g/L |
| 6.0 | 4.04 | 26 | 33.3 | 0.15 |
The red soil nickel ore mixing waste acid leaching chemical composition of slagging tap
| Weight in wet base t | Dry weight t | Moisture % | Ni% | Fe% | Mg% | Co% |
| 2.2 | 1.1 | 50 | 0.16 | 4.0 | 2.20 | 0.01 |
2, leach liquor deironing
At 12m
3in steel basin, add water 0.1m
3, be heated to 70 ℃, with 2m
3the speed of/h adds leach liquor, adds leach liquor to add moisture 75% magnesium hydroxide slurry 2.5t simultaneously, controls reaction system PH 3.2, hydrolysis deironing, and deironing completes and adopts filtration area 100m
2plate-and-frame filter press filters, and directly in add water 390kg washing of pressure filter, merging filtrate and wash water, obtain liquid after crude iron ore deposit, deironing.Its chemical composition is as following table.
Liquid chemical composition after deironing
| Volume m 3 | Ni?g/L | Fe?g/L | Mg?g/L | Co?g/L |
| 7.5 | 3.22 | ≤0.01 | 57.5 | 0.12 |
Crude iron ore deposit chemical composition
| Weight in wet base t | Dry weight t | Moisture % | Ni?% | Fe?% | Mg?% | Co?% |
| 0.78 | 0.39 | 50 | 0.01 | 40.1 | 1.2 | 0.0005 |
3, heavy nickel, cobalt
After deironing, liquid is added to 12m
3in steel basin, be heated to 20 ℃, stirring state adds and slowly adds 5% sodium hydroxide solution 880kg, stirs 1h, heavy nickel, cobalt terminal PH 8.7.Employing filtration area 40m after heavy nickel, cobalt complete
2plate-and-frame filter press filters, and directly in add water 150kg washing of pressure filter, merging filtrate and wash water, obtain liquid after nickel hydroxide and cobaltous hydroxide, heavy nickel.Its chemical composition is as following table.
Liquid chemical composition after heavy nickel
| Volume m 3 | Ni?g/L | Fe?g/L | Mg?g/L | Co?g/L |
| 7.7 | 0.005 | ≤0.01 | 56 | ≤0.001 |
Nickel hydroxide and cobaltous hydroxide chemical composition
| Weight in wet base kg | Dry weight kg | Moisture % | Ni?% | Fe?% | Mg?% | Co?% |
| 210 | 60 | 69.4 | 40.3 | ≤0.01 | 2.2 | 1.6 |
Nickel hydroxide and cobaltous hydroxide can be used as the raw material of producing electrolytic nickel, nickel salt, cobalt salt.
Following table has provided the mixing spent acid that is suitable for sulfur acid of the present invention, hydrochloric acid in conjunction with the Main Economic technical indicator that leaches red soil nickel ore and reclaim nickel cobalt:
Claims (3)
1. the mixing spent acid of sulfur acid, hydrochloric acid leaches a method for red soil nickel ore recovery nickel cobalt, it is characterized in that comprising the mixing spent acid agitation leach of sulfur acid, hydrochloric acid, deironing, and heavy nickel, specifically realize by following steps:
The mixing spent acid agitation leach of step 1, sulfur acid, hydrochloric acid:
Red soil nickel ore fragmentation, ore grinding to 0.15mm, with sulfur acid, hydrochloric acid mix spent acid by liquid-solid ratio 3～5:1,60～80 ℃ of temperature, agitation leach 3～6h, has leached rear filtration, washing, merging filtrate and wash water, obtain filter cake leached mud, leach liquor;
Step 2, leach liquor deironing:
Leach liquor hydro-oxidation magnesium hydrolysis deironing, controls 60～80 ℃ of deironing temperature of reaction, deironing terminal PH2.5～4, and deironing reaction 3h, deironing completes carries out solid-liquid separation, obtains liquid after crude iron ore deposit, deironing.
Step 3, heavy nickel, cobalt:
Liquid hydro-oxidation sodium solution after deironing, 20～40 ℃ of heavy nickel, cobalt, heavy nickel, cobalt terminal PH8.5～9, heavy nickel, cobalt reaction 1h, heavy nickel, cobalt complete and carry out solid-liquid separation, obtain liquid after nickel hydroxide and cobaltous hydroxide product, heavy nickel.
2. the mixing spent acid of sulfur acid according to claim 1, hydrochloric acid leaches red soil nickel ore and reclaims the method for nickel cobalt, it is characterized in that H in the mixing spent acid of the sulfur acid described in step 1, hydrochloric acid
2sO
4massfraction is that the massfraction of 10～50%, HCl is 10～30%.
3. the mixing spent acid of sulfur acid according to claim 1, hydrochloric acid leaches the method for red soil nickel ore recovery nickel cobalt, it is characterized in that the neutralizing agent adopting in the leach liquor deironing described in step 2 is magnesium hydroxide powder, or water and magnesium hydroxide are made into the slurry containing magnesium hydroxide 10～30wt%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410027777.7A CN103773951A (en) | 2014-01-21 | 2014-01-21 | Method for recovering nickel and cobalt through leaching laterite-nickel ore by using sulfuric and hydrochloric acid containing mixed waste acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410027777.7A CN103773951A (en) | 2014-01-21 | 2014-01-21 | Method for recovering nickel and cobalt through leaching laterite-nickel ore by using sulfuric and hydrochloric acid containing mixed waste acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103773951A true CN103773951A (en) | 2014-05-07 |
Family
ID=50566704
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410027777.7A Pending CN103773951A (en) | 2014-01-21 | 2014-01-21 | Method for recovering nickel and cobalt through leaching laterite-nickel ore by using sulfuric and hydrochloric acid containing mixed waste acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103773951A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104531997A (en) * | 2014-12-25 | 2015-04-22 | 广东省工业技术研究院(广州有色金属研究院) | Method for removing iron from magnesium-containing sulfuric acid leaching liquid |
| CN108998682A (en) * | 2018-07-11 | 2018-12-14 | 中铁资源集团有限公司 | A method of the Call Provision from cobalt sulfate solution |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101255494A (en) * | 2008-04-11 | 2008-09-03 | 中南大学 | Method for leaching nickel and cobalt from low-grade lateritic nickel ore |
| CN101270417A (en) * | 2008-04-30 | 2008-09-24 | 江西稀有稀土金属钨业集团有限公司 | Method for extracting nickel and/or cobalt |
| CN101289704A (en) * | 2008-06-18 | 2008-10-22 | 北京矿冶研究总院 | A kind of processing method of high magnesium laterite nickel ore |
| WO2009039579A1 (en) * | 2007-09-26 | 2009-04-02 | Bhp Billiton Ssm Development Pty Ltd | Acid recovery from metal sulfates |
| CN102329955A (en) * | 2011-08-25 | 2012-01-25 | 云南锡业集团（控股）有限责任公司 | Comprehensive method for processing laterite nickel ore to produce electrolytic nickel through full wet method |
| CN102876892A (en) * | 2012-10-30 | 2013-01-16 | 杭州蓝普水处理设备有限公司 | Method for leaching nickel and cobalt form low-iron and high-magnesium and high-iron and low-magnesium laterite-nickel ore by using waste dilute sulphuric acid |
| CN102994754A (en) * | 2011-09-14 | 2013-03-27 | 郴州市金贵银业股份有限公司 | Technology for comprehensively recovering complex material containing lead, bismuth, cobalt and nickel through wet method |
-
2014
- 2014-01-21 CN CN201410027777.7A patent/CN103773951A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009039579A1 (en) * | 2007-09-26 | 2009-04-02 | Bhp Billiton Ssm Development Pty Ltd | Acid recovery from metal sulfates |
| CN101255494A (en) * | 2008-04-11 | 2008-09-03 | 中南大学 | Method for leaching nickel and cobalt from low-grade lateritic nickel ore |
| CN101270417A (en) * | 2008-04-30 | 2008-09-24 | 江西稀有稀土金属钨业集团有限公司 | Method for extracting nickel and/or cobalt |
| CN101289704A (en) * | 2008-06-18 | 2008-10-22 | 北京矿冶研究总院 | A kind of processing method of high magnesium laterite nickel ore |
| CN102329955A (en) * | 2011-08-25 | 2012-01-25 | 云南锡业集团（控股）有限责任公司 | Comprehensive method for processing laterite nickel ore to produce electrolytic nickel through full wet method |
| CN102994754A (en) * | 2011-09-14 | 2013-03-27 | 郴州市金贵银业股份有限公司 | Technology for comprehensively recovering complex material containing lead, bismuth, cobalt and nickel through wet method |
| CN102876892A (en) * | 2012-10-30 | 2013-01-16 | 杭州蓝普水处理设备有限公司 | Method for leaching nickel and cobalt form low-iron and high-magnesium and high-iron and low-magnesium laterite-nickel ore by using waste dilute sulphuric acid |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104531997A (en) * | 2014-12-25 | 2015-04-22 | 广东省工业技术研究院(广州有色金属研究院) | Method for removing iron from magnesium-containing sulfuric acid leaching liquid |
| CN108998682A (en) * | 2018-07-11 | 2018-12-14 | 中铁资源集团有限公司 | A method of the Call Provision from cobalt sulfate solution |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102011010A (en) | Method for totally extracting vanadium, gallium and scandium by using titanium dioxide hydrolysis waste acid to leach steel slag containing vanadium | |
| CN102206755A (en) | Method for separating and recovering valuable elements from neodymium-iron-boron wastes | |
| CN103193213B (en) | Method for comprehensively utilizing low-grade phosphate ores | |
| CN101372402A (en) | Method for preparing magnesian by calcining ammonium salt and magnesium-containing ore | |
| CN103740931B (en) | Containing the method for ferronickel mixing solutions goethite precipitation iron | |
| CN111498820A (en) | Process for simultaneously preparing high-quality calcium sulfate whiskers from phosphorus concentrate enriched by medium-low-grade phosphate ore or phosphorus tailings | |
| CN103834805A (en) | Method of leaching divalent cobalt from cobalt copper bidery metal | |
| CN111500864A (en) | Method for recycling electroplating sludge based on chromium recovery | |
| CN101760646A (en) | Leaching method of magnesium-containing ore | |
| CN102583458A (en) | Method for extracting basic magnesium carbonate, iron hydroxide and calcium sulfate from serpentine under normal temperature and pressure | |
| CN102485922B (en) | Method for extracting nickel, cobalt, magnesium and iron from laterite-nickel ore under conditions of normal temperature and normal pressure and using waste residues | |
| CN101760637B (en) | Leaching technology of magnesium-containing ore | |
| CN102816927A (en) | Method for efficiently removing ferrum in red soil nickel mineral leaching liquid | |
| CN102994746A (en) | Method for producing nickel sulfide ore concentrate by use of industrial waste acid | |
| CN107287428B (en) | A method of Copper in Electroplating Sludge, nickel, zinc is separately recovered | |
| CN109022806A (en) | A method of utilizing the vanadium liquid removal of impurities clay standby vanadic anhydride of vanadium | |
| CN106629757B (en) | Recycling silicon prepares the method that calcium silicates removes nitrogen phosphorus in water removal in a kind of red mud | |
| CN101328540A (en) | Method for reclaiming sodium molybdate solution from molybdenum-containing leached residue | |
| CN103773951A (en) | Method for recovering nickel and cobalt through leaching laterite-nickel ore by using sulfuric and hydrochloric acid containing mixed waste acid | |
| CN106755997A (en) | A kind of method of nickel-containing ore comprehensive utilization | |
| CN103757259B (en) | A kind of chemical waste sulfuric acid, waste hydrochloric acid combine the method for each element of process red soil nickel ore synthetical recovery | |
| CN104711428B (en) | Method for preparing and recovering metal in pickling sludge | |
| CN101760638A (en) | Method for recovering magnesium from magnesium sulfate solution | |
| CN101723431B (en) | Method for recovering magnesium from magnesium sulfate solution | |
| CN111363927A (en) | A method for recycling electroplating sludge based on nickel recovery |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20140507 |