CN103374656A - Technique for recycling nickel, ferrum and cobalt from nickel oxide ore - Google Patents
Technique for recycling nickel, ferrum and cobalt from nickel oxide ore Download PDFInfo
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- CN103374656A CN103374656A CN2012101268672A CN201210126867A CN103374656A CN 103374656 A CN103374656 A CN 103374656A CN 2012101268672 A CN2012101268672 A CN 2012101268672A CN 201210126867 A CN201210126867 A CN 201210126867A CN 103374656 A CN103374656 A CN 103374656A
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Abstract
The invention relates to a technique for recycling nickel, ferrum and cobalt from nickel oxide ore. The technique comprises the following steps of: A. crushing and ball-milling the nickel oxide ore; B. chloridizing and roasting the nickel oxide ore; C. preparing hydrochloric acid leachate of chloridized and roasted nickel oxide ore; and D. producing a mixture product containing nickel, ferrum and cobalt compounds. The mixture product containing nickel, ferrumand cobalt compound is low in sulfur content, high in nickel grade, and can be used for producing stainless steel. Compared with the traditional wet-process technique of the nickel oxide ore, the method for recycling nickel, ferrum and cobalt from the nickel oxide ore is high in comprehensive resource utilization efficiency, low in energy consumption, environment-friendly and easy to implement.
Description
Technical field
The present invention relates to hydrometallurgy, in particular to the technique that from nickel oxide ore, reclaims the nickel ferro-cobalt.
Background technology
Normally a kind of mineral association that contains Determination of multiple metal elements of nickel oxide ore.Contain iron, nickel, cobalt, manganese, aluminium and magnesium etc.In order to recycle these valuable metal elements, people have adopted the methods such as pyrometallurgy and hydrometallurgy.
Traditional nickel oxide ore pyrometallurgy treatment technology has rotary kiln drying prereduction-electric furnace reduction melting to produce ferronickel; Sintering-blast furnace sulfiding smelting is produced low nickel matte; And the nickel pig iron is produced in sintering-blast furnace retailoring.Rotary kiln drying prereduction-electric furnace reduction melting is the classical technique of processing nickel oxide ore, technological process is as follows: moisture about 30% nickel oxide ore through rotary kiln after 800～900 ℃ of lower drying and dehydratings and prereduction are processed, send into again ore-smelting furnace, under about 1550～1600 ℃ high temperature the retailoring output nickeliferous＞10% ferronickel, be enriched to more than 25% through the further refining of converter again and sell, for producing stainless steel.The method has that Technological adaptability is strong, flow process is brief, the nickel recovery high.The blast furnace sulfiding smelting be with nickel oxide ore after allocating an amount of CaO and SiO2 into, under about 1100 ℃, sinter piece (or push agglomerating, naturally dry) into, allocate again 10～20% pyrite and about 20～30% coke into, melting under the about 1350 ℃ temperature in blast furnace, the low nickel matte product of output nickeliferous 8～15%.Sintering-blast furnace retailoring is the nickel oxide ore treatment process of developing on the basis of using for reference blast furnace iron-making process, produces nickeliferous 2～5% the nickel pig iron.
Because every kind of valuable metal constituent content is relatively less in nickel oxide ore, so the energy consumption that adopts pyrometallurgy to smelt is higher, this is the main drawback of nickel oxide ore pyrometallurgical smelting.So people adopt the method for hydrometallurgy, optionally extract valuable metal wherein.In recent years, nickel oxide ore sulfuric acid wet process extractive technique obtains to develop rapidly.
Nickel oxide ore sulfuric acid wet process extractive technique commonly used has: sulfuric acid pressure leaching, sulfuric acid normal pressure leach, sulfuric acid dump leaching and reducing roasting--and ammonia soaks etc.
The sulfuric acid pressure leaching is processed nickel oxide ore, is that (4～5MPa) times leachings, nickel, cobalt leaching yield can reach about 95% at high temperature (230～260 ℃) and high pressure.Reduction roasting-ammonia leaching technique has reagent N H3 and can be recycled, and energy input is little, can comprehensive recovery nickel, the advantages such as cobalt, iron, and nickel, the cobalt leaching yield is on the low side is its main drawback.
The sulfuric acid normal pressure leaches nickel oxide ore, is that the mineral composition according to handled nickel oxide ore prepares leach liquor under normal pressure, usually contains the iron of 10～30g/L, the nickel of 3～5g/L, the cobalt of 0.1～0.3g/L, the magnesium of 30～40g/L in the resulting leach liquor.Usually adopt calcium oxide or calcium hydroxide to neutralize in advance the iron in the deposition removal leach liquor and aluminium; And then neutralization precipitation nickel and cobalt or with carbonate deposition nickel and cobalt or with sulfide precipitation nickel and cobalt.The emphasis of above-mentioned technique is nickel and the cobalt of recycling in the solution, and all processes valuable element iron, magnesium etc. discarded as impurity element.In addition, in the first step of this technique, namely remove in iron and the aluminium process neutralizing in advance with calcium oxide or calcium hydroxide since with the adsorption coprecipitation of iron and aluminium, and local basicity is too high, often causes valuable nickel and cobalt to lose in a large number.
201110008541.5) and a kind of method (patent No.: 201110008553.8) from nickel oxide ore recovery nickel ferro-cobalt manganese magnesium reclaim the technique (patent No.: of nickel ferro-cobalt magnesium at a kind of nickel oxide ore of first to file, although realized in the nickel oxide ore sulphuric leachate, the recycling of nickel ferro-cobalt manganese and magnesium multiple element, that a kind of comprehensive utilization of resources rate is high, energy consumption is low, technique environmentally friendly and easy to implement.But the mix product sulfur-bearing of the nickel ferro-cobalt of producing in this way is very high.Be difficult to remove when producing stainless steel, have a strong impact on the quality of stainless steel product, remove sulphur, need expend a large amount of energy, manufacturer is difficult to accept.In addition, with the direct acidleach nickel oxide ore of hydrochloric acid, the nickel leaching yield is not high, and the rate of recovery is low, especially bad filtration.Be difficult to large-scale production.
Summary of the invention
Purpose of the present invention is exactly in order to overcome problems of the prior art, and a kind of method that reclaims the nickel ferro-cobalt from nickel oxide ore is provided.The present invention recycles nickel, cobalt and three kinds of elements of iron as valuable element, particularly can improve the rate of recovery of nickel, cobalt and iron.
Goal of the invention of the present invention realizes by the following technical solutions:
A kind of technique that reclaims the nickel ferro-cobalt from nickel oxide ore may further comprise the steps:
A, preparation raw material nickel oxide ore
Nickel oxide ore is transported to the raw ore stockyard, nickel oxide ore is broken, ball milling;
B, nickelous oxide mine chloridization roasting
In the nickel oxide ore after the A step preparation, admix chlorizating agent and stir.The nickel oxide ore that to admix again chlorizating agent carries out chloridizing roasting, cools off after the roasting;
C, preparation are through the nickel oxide ore hydrochloric acid leachate of chloridizing roasting
Described nickel oxide ore through chloridizing roasting is put into leaching vat, add hydrochloric acid and leach processing; Leach the complete rear pressure filter press filtration of using, make solid-liquid separation;
D, production contain the mix product of nickel hydroxide, cobaltous hydroxide, ironic hydroxide
Add neutralizing agent calcium oxide or calcium hydroxide in the leach liquor that obtains in the C step, stir and carry out neutralizing treatment, make nickel, cobalt, iron cpd co-precipitation, use the plate-and-frame filter press press filtration, output contains the mixture of nickel hydroxide, cobaltous hydroxide, ironic hydroxide.
The present invention has compared with prior art obtained following beneficial effect:
1, realized the recycling of three kinds of elements of nickel ferro-cobalt in the nickel oxide ore hydrochloric acid leachate.
2, it is low to produce the mix product sulfur-bearing of nickeliferous ferro-cobalt, and nickel of high grade can be for producing stainless steel.
Therefore, compare with traditional nickel oxide ore wet processing process, the method from nickel oxide ore recovery nickel ferro-cobalt of the present invention is that a comprehensive utilization of resources efficient is high, and energy consumption is low, technique environmentally friendly and easy to implement.
Embodiment
Below describe through the specific embodiment and the embodiment the present invention in detail.
A kind of technique that reclaims the nickel ferro-cobalt from nickel oxide ore may further comprise the steps:
A, preparation raw material nickel oxide ore
Nickel oxide ore is transported to the raw ore stockyard, nickel oxide ore is broken, ball milling, and granularity is 100 orders-120 orders;
B, nickelous oxide mine chloridization roasting
Admix chlorizating agent and stir by 2%～5% of nickel oxide ore weight ratio.Employed chlorizating agent is wherein one or any several of calcium chloride, ammonium chloride, sodium-chlor, magnesium chloride.The nickel oxide ore of admixing chlorizating agent is carried out chloridizing roasting 30～60 minutes under 900～1000 ℃ of temperature, be cooled to 150～250 ℃ after the roasting;
C, preparation are through the nickel oxide ore hydrochloric acid leachate of chloridizing roasting
The nickel oxide ore through chloridizing roasting that is cooled to 150～250 ℃ is put into leaching vat, and adding concentration is that the hydrochloric acid of 5～8mol/L leaches processing and stirring, and the hydrochloric acid of use is 1.5～3: 1 with the ratio of the weight of breeze; 80～100 ℃ of extraction temperatures of control, extraction time 40～70 minutes; Leach the complete rear plate-and-frame filter press press filtration of using, solid-liquid separation obtains leach liquor and filter residue.
D, production contain the mix product of nickel hydroxide, cobaltous hydroxide, ironic hydroxide
Add neutralizing agent calcium oxide or calcium hydroxide in the leach liquor that in the C step, obtains, under the condition of 60～80 ℃ of temperature, stir and carry out neutralizing treatment, 60～80 minutes reaction times, terminal point PH=7～9.Make the mixture co-precipitation that contains nickel hydroxide, cobaltous hydroxide, ironic hydroxide, use the plate-and-frame filter press press filtration again, output contains the mixture of nickel hydroxide, cobaltous hydroxide, ironic hydroxide.
Below with indefiniteness embodiment technique of the present invention is further described, to help to understand the present invention and advantage thereof.
Embodiment 1
Contain (% by weight): Ni 1.45%, Fe 14.5%, CO 0.08%, MgO 18.5%, SiO 35.7%, CaO 0.3%, Al in the composition of nickel oxide ore
2O
36.08%, Cr 1.02%.
Nickel oxide ore is broken, ball milling, the fineness of the nickel oxide ore behind the ball milling is 100 orders.
The chloridizing roasting condition: press 2% of nickel oxide ore weight and add ammonium chloride, 900 ℃ of maturing temperatures, roasting time 30 minutes is cooled to 150 ℃.
Leaching condition: concentration of hydrochloric acid 6mol/L, with the solvent and solute weight ratio of nickel oxide breeze 2: 1,85 ℃ of extraction temperatures, extraction time 60 minutes stirred linear velocity 4.5m/s.Leaching yield: nickel 96%, cobalt 94%, iron 55%.
The mixture Coprecipitation of nickel ferro-cobalt compound: add calcium hydroxide slurry, neutralization precipitation temperature 60 C, reaction times 60 minutes, control terminal point PH=8.5, obtain the mixture of nickel and cobalt containing iron cpd.
Embodiment 2
Used nickel oxide ore forms and contains (% by weight): Ni 1.65%, Fe 16.3%, Co 0.07%, MgO 15.8%, SiO
2: 41.2%, CaO 0.2%, Al
2O
35.28%, Cr 0.92%.
Nickel oxide ore is broken, ball milling, the fineness of the nickel oxide ore behind the ball milling is 100 orders.
The chloridizing roasting condition: press 5% of nickel oxide ore weight ratio and add ammonium chloride, 950 ℃ of maturing temperatures, roasting time 50 minutes is cooled to 200 ℃.
Leaching condition: concentration of hydrochloric acid 5mol/L, solvent and solute weight ratio 3: 1,85 ℃ of extraction temperatures, extraction time 60 minutes stirs linear velocity 5m/s.Leaching yield: nickel 98%, cobalt 96%, iron 54%.
The mixture Coprecipitation of nickel ferro-cobalt compound: add calcium hydroxide slurry, neutralization precipitation temperature 60 C, reaction times 60 minutes, control terminal point PH=7.5, obtain the mixture of nickel and cobalt containing iron cpd.
Embodiment 3
Used nickel oxide ore forms in (% by weight): Ni 1.82%, Fe 13.5%, CO 0.08%, MgO16.5%, SiO
238.2%, CaO 0.32%, Al
2O
34.57%, Cr 1.15%.
Nickel oxide ore is broken, ball milling, the fineness of the nickel oxide ore behind the ball milling is 120 orders.
The chloridizing roasting condition: press nickel oxide ore weight ratio 3% and add sodium-chlor, 1000 ℃ of maturing temperatures, roasting time 60 minutes is cooled to 250 ℃.
Leaching condition: concentration of hydrochloric acid 5mol/, solvent and solute weight ratio 2.5: 1,90 ℃ of extraction temperatures, extraction time 45 minutes stirs linear velocity 5m/s.Leaching yield: nickel 98.5%, cobalt 96.5%, magnesium 95.5%, iron 56%.
The mixture Coprecipitation of nickel ferro-cobalt compound: add calcium hydroxide slurry, neutralization precipitation temperature 70 C, reaction times 75 minutes, control terminal point pH=9, obtain the mixture of nickel and cobalt containing iron cpd.
Embodiment 4
Used nickel oxide ore forms in (% by weight): Ni 1.95%, Fe 13.8%, CO 0.09%, MgO14.8%, SiO
239.8%, CaO 0.12%, Al
2O
35.6%, Cr 0.96%.
Nickel oxide ore is broken, ball milling, the fineness of the nickel oxide ore behind the ball milling is 120 orders.
The chloridizing roasting condition: press nickel oxide ore weight ratio 5% and add magnesium chloride, 900 ℃ of maturing temperatures, roasting time 60 minutes is cooled to 200 ℃.
Leaching condition: concentration of hydrochloric acid 7mol/L, solvent and solute weight ratio 3: 1,90 ℃ of extraction temperatures, extraction time 60 minutes stirs linear velocity 5m/s.Leaching yield: nickel 99%, cobalt 96%, magnesium 95%, iron 57%.
The mixture Coprecipitation of nickel ferro-cobalt compound: add calcium hydroxide slurry, 75 ℃ of neutralization precipitation temperature, 80 minutes reaction times, control terminal point PH=9, obtain the mixture of nickel and cobalt containing iron cpd.
Claims (5)
1. technique that reclaims the nickel ferro-cobalt from nickel oxide ore may further comprise the steps:
A, preparation raw material nickel oxide ore
Nickel oxide ore is transported to the raw ore stockyard, nickel oxide ore is broken, ball milling;
B, nickelous oxide mine chloridization roasting
In the nickel oxide ore after the A step preparation, admix chlorizating agent and stir.The nickel oxide ore that to admix again chlorizating agent carries out chloridizing roasting, cools off after the roasting;
C, preparation are through the nickel oxide ore hydrochloric acid leachate of chloridizing roasting
Described nickel oxide ore through chloridizing roasting is put into leaching vat, add hydrochloric acid and leach processing; Leach the complete rear pressure filter press filtration of using, make solid-liquid separation;
D, production contain the mix product of nickel hydroxide, cobaltous hydroxide, ironic hydroxide
Add neutralizing agent calcium oxide or calcium hydroxide in the leach liquor that obtains in the C step, stir and carry out neutralizing treatment, make nickel, cobalt, iron cpd co-precipitation, use the plate-and-frame filter press press filtration, output contains the mixture of nickel hydroxide, cobaltous hydroxide, ironic hydroxide.
2. the technique that reclaims the nickel ferro-cobalt from nickel oxide ore according to claim 1 is characterized in that: in the described A step, and nickel oxide ore is broken, ball milling, granularity is 100 orders-120 orders.
3. the technique that from nickel oxide ore, reclaims the nickel ferro-cobalt according to claim 1, it is characterized in that: in the described B step, admix chlorizating agent and stir by 2%～5% of nickel oxide ore weight ratio, employed chlorizating agent is wherein one or any several of calcium chloride, ammonium chloride, sodium-chlor, magnesium chloride; The nickel oxide ore of admixing chlorizating agent is carried out chloridizing roasting 30～60 minutes under 900～1000 ℃ of temperature, be cooled to 150～250 ℃ after the roasting.
4. according to claim 1 or the 3 described techniques that from nickel oxide ore, reclaim the nickel ferro-cobalt, it is characterized in that: in the described C step, the nickel oxide ore through chloridizing roasting that is cooled to 150～250 ℃ is put into leaching vat, adding concentration is that the hydrochloric acid of 5～8mol/L leaches processing and stirring, and the hydrochloric acid of use is 1.5～3: 1 with the ratio of the weight of breeze; 80～100 ℃ of extraction temperatures of control, extraction time 40～70 minutes; Leach the complete rear plate-and-frame filter press press filtration of using, solid-liquid separation obtains leach liquor and filter residue.
5. the technique that from nickel oxide ore, reclaims the nickel ferro-cobalt according to claim 4, it is characterized in that: in the described D step, add neutralizing agent calcium oxide or calcium hydroxide in the leach liquor that in the C step, obtains, under the condition of 60～80 ℃ of temperature, stir and carry out neutralizing treatment, 60～80 minutes reaction times, terminal point PH=7～9; Make the mixture co-precipitation that contains nickel hydroxide, cobaltous hydroxide, ironic hydroxide, use the plate-and-frame filter press press filtration again, output contains the mixture of nickel hydroxide, cobaltous hydroxide, ironic hydroxide.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104232882A (en) * | 2014-09-28 | 2014-12-24 | 毛黎生 | Technology for recovering nickel, cobalt and iron from nickel oxide ores through high-temperature chlorinating volatilization |
| CN104263909A (en) * | 2014-09-28 | 2015-01-07 | 毛黎生 | Process for recovering nickel, cobalt and iron from nickel oxide ores by virtue of roasting and water leaching |
| CN106566934A (en) * | 2016-10-28 | 2017-04-19 | 中国恩菲工程技术有限公司 | Method for processing iron-removed and aluminum-removed liquid |
| CN107419089A (en) * | 2017-04-18 | 2017-12-01 | 彭海洋 | The method of low-grade high impurity ore magnetizing roast removal of impurities |
| CN113860396A (en) * | 2021-09-02 | 2021-12-31 | 格林美股份有限公司 | Method for preparing nickel hydroxide by recovering waste nickel catalyst |
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| CN101550491A (en) * | 2009-05-16 | 2009-10-07 | 谢永巨 | Method for extracting nickel or cobalt from nickel ore with chloridizing roasting-leaching method |
| CN102424431A (en) * | 2011-09-01 | 2012-04-25 | 东北大学 | Method for preparing nickel oxide, magnesium oxide and silicon oxide products from laterite-nickel ore |
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2012
- 2012-04-27 CN CN2012101268672A patent/CN103374656A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101550491A (en) * | 2009-05-16 | 2009-10-07 | 谢永巨 | Method for extracting nickel or cobalt from nickel ore with chloridizing roasting-leaching method |
| CN102424431A (en) * | 2011-09-01 | 2012-04-25 | 东北大学 | Method for preparing nickel oxide, magnesium oxide and silicon oxide products from laterite-nickel ore |
Non-Patent Citations (1)
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104232882A (en) * | 2014-09-28 | 2014-12-24 | 毛黎生 | Technology for recovering nickel, cobalt and iron from nickel oxide ores through high-temperature chlorinating volatilization |
| CN104263909A (en) * | 2014-09-28 | 2015-01-07 | 毛黎生 | Process for recovering nickel, cobalt and iron from nickel oxide ores by virtue of roasting and water leaching |
| CN106566934A (en) * | 2016-10-28 | 2017-04-19 | 中国恩菲工程技术有限公司 | Method for processing iron-removed and aluminum-removed liquid |
| CN107419089A (en) * | 2017-04-18 | 2017-12-01 | 彭海洋 | The method of low-grade high impurity ore magnetizing roast removal of impurities |
| CN113860396A (en) * | 2021-09-02 | 2021-12-31 | 格林美股份有限公司 | Method for preparing nickel hydroxide by recovering waste nickel catalyst |
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Application publication date: 20131030 |