CN1148461C - Process for extracting nickel from nickel sulfide material with low copper content - Google Patents

Process for extracting nickel from nickel sulfide material with low copper content Download PDF

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CN1148461C
CN1148461C CNB011347309A CN01134730A CN1148461C CN 1148461 C CN1148461 C CN 1148461C CN B011347309 A CNB011347309 A CN B011347309A CN 01134730 A CN01134730 A CN 01134730A CN 1148461 C CN1148461 C CN 1148461C
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nickel
extraction
cupric
leaching
sulfide
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CNB011347309A
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CN1352308A (en
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蒋开喜
王海北
刘大星
何良菊
王春
林江顺
崔学仲
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北京矿冶研究总院
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The present invention provides a method for extracting nickel from nickel sulfide material with low copper content, which relates to a method for extracting the nickel from nickel ore concentrate and especially from nickel ore concentrate with low copper content or slow cooling high sulfur grinding and floating separation output in a section of pressure leaching. The present invention is characterized in that pressure leaching is carried out for the nickel ore concentrate under the conditions of oxygen circulation, sulphur or sulfuric acid addition, the temperature of 100 to 180 DEG C, and the oxygen partial pressure of 50 to 300 kPa. The method of the present invention only needs a section of pressure leaching to complete a leaching process of nickel, cobalt and copper, and iron is solidified in slag in the form of iron oxide. A nickel sulfate solution after liquid solid separation can be used for producing pure nickel sulfate or electrolytic nickel, and meanwhile, valuable metals, such as cobalt, copper, etc. are recovered. The present invention has the advantages of simple technology and high production efficiency.

Description

A kind of method of extracting nickel from the low nickel sulfide material of cupric
(1) technical field
A kind ofly extract the method for nickel, relate to a kind ofly,, leach the method for extracting nickel with one section pressure as nickel ore concentrate and the lower nickel matte of cupric from the low nickel sulfide material of cupric from the low nickel sulfide material of cupric.
(2) background technology
Most in the world nickel is that the nickel matte that adopts hydrometallurgical processes to handle the pyrogenic process output is produced at present.The technology that the wet processing nickel matte adopts often has: 1) one section normal pressure leaches and connects the combination that one section pressurization is leached, and enters autoclave by force (forcing) pump after the pulp of normal pressure leached mud, and the pressurization leach liquor returns the normal pressure leaching and purifies.In normal pressure leached, the oxidized precipitation of iron in the pressurization leach liquor entered leached mud, and copper wherein also will be entered leached mud by displacement and hydrolysis, and control is leached terminal point pH about 6.1 usually.The normal pressure leached mud enters pressurization and leaches, and by controlling suitable condition, nickel, cobalt is entered in the leach liquor by leaching, and most copper iron rules are stayed in the leached mud.Obtain copper and all very low leach liquor of iron for normal pressure is leached, pressurization is leached needs control condition, and copper iron is opened a way from leached mud, and at this moment the nickel in the partial vulcanization nickel (as β-nickelous sulfide) in the nickel ore concentrate is difficult to be leached.Rule of thumb, the nickel leaching yield of this selectivity extract technology is generally at 85%-90%.Leached mud Returning smelting batching.2) one section normal pressure leaches the combination that connects two sections pressurizations.In the one section pressurization that increases is leached, copper and mickel in first section pressurization leached mud is as far as possible all leached, and the leach liquor that obtains adopts suitable mode decopper(ing), as insoluble anode electrolysis decopper(ing), method copper removals such as displacement, hydrolysis or sulfide precipitation, liquid returns first section pressurization leaching behind the copper removal.
At United States Patent (USP) 4,093, in 526, adopt one section normal pressure to add two sections pressurizations and leach valuable metals such as from nickel matte, reclaiming nickel.It is to adopt first section pressurization leach liquor to leach nickel matte that first section normal pressure leaches, and can suitably add sulfuric acid as needs.The purpose that normal pressure leaches is the part of nickel that leaches in the nickel matte, the cupric ion of pressurization in the leach liquor can with metallographic phase nickel in the nickel matte and curing three nickel reactants, nickel is leached, and copper is then stayed in the slag with the form of copper or copper hydroxide and is separated with nickel, and the bright sulfur acid nickel solution that obtains advances nickel electrowinning.The normal pressure leached mud advances first section pressure oxidation and leaches, and the pressurization leach liquor advances normal pressure and leaches purification, and leached mud advances second section pressurization and soaks entirely, nickel, cobalt and copper in one section pressurization leached mud are all leached with copper electrolyte, send the copper electrodeposition behind the purification of leaching liquor, be mainly iron in the leached mud, can discard.
At United States Patent (USP) 4,233, in 541, adopt two sections normal pressures to leach to add one section pressurization to leach and handle nickel matte.Its objective is and nickel as far as possible all leached and most copper is stayed in the pressurization leached mud that the slag of this cupric and precious metal can return the copper melting and rectification systems is handled.Above-mentioned technology shortcoming be that technical process is long.
At United States Patent (USP) 6,206, in 951, proposed a kind ofly will be rich in copper nickel matte, or nickel matte is with the treatment process of copper ashes.In first section pressure oxidation leached, nickel was leached, and copper enters slag with alpha chalcocite and lapis divinus form, and bright sulfur acid nickel solution send nickel electrowinning.Leached mud carries out one section oxidation with sulfuric acid again and leaches, and the copper in the slag is become copper sulfate and cupric sulfide, and iron is the oxide compound slag input.The leach liquor of sulfur acid copper returns first section pressure and leaches.Leach with two sections normal pressures and to add the method that one section pressurization leaches and compare, the advantage of this method is to have only 1/16 to be oxidized to acid in the leaching process at most, and the former has 1/6 sulphur to be oxidized to sulfuric acid.But its technology is still the leaching of adopting one section pressurization and one section normal pressure to realize nickel, copper and separates, and its process that reclaims metal is comparatively complicated, the cost height.
(2) summary of the invention
Purpose of the present invention is exactly in the existing technology of extracting nickel from nickel sulfide material, the shortcoming that the technical process that exists is long provides simple and direct, the various metal direct yield of a kind of flow process height, a kind of method of extracting nickel from the low nickel sulfide material of cupric with low cost.
The objective of the invention is to be achieved through the following technical solutions.
A kind of method from the low nickel sulfide material extraction nickel of cupric is characterized in that its process is followed successively by:
A) in nickel ore concentrate, add sulfuric acid and water with the mineral pulp after, preheating ore pulp to 50 ℃-80 ℃; The weight percent of the mineral concentration of ore pulp is 5%-30% after the pulp, and the vitriolic weight percent concentration is 50-90g/l,
B) carry out pressure in leaching still and leach, the total pressure that control is leached is 50-1000kPa, and oxygen partial pressure is 10-300kPa, and temperature is 100-180 ℃, and extraction time is 1-6 hour;
D) with purification of leaching liquor, use earlier the chemical precipitation method copper removal, go out cobalt and remaining copper with Solvent Extraction Separation again and obtain electrolysis production nickel behind the sour nickel solution of bright sulfur.
Method of the present invention is specially adapted to copper content less than 5% nickel ore concentrate.
Acid during leaching also can obtain by add the sulphur rear oxidation in mineral, and add-on is the 5%-30% of nickel ore concentrate weight.The sulphur amount that adds is nickel ore concentrate weight 10%-15% preferably.Vitriolated weight percent concentration 70-90 grams per liter preferably in the ore pulp.
The optimum range of the temperature of leach liquor is 140-160 ℃.Leach total pressure and be preferably 500-1000kPa, oxygen partial pressure is 100-300kPa.
Method of the present invention can adopt pressurized air to leach, and its total pressure is 1000-1300kPa, and oxygen partial pressure is 200-300kPa.
Time that its pressurization is leached is to think good in 2-4 hour.
A kind of method from the low nickel sulfide material extraction nickel of cupric of the present invention adopts chemical precipitation method copper removal from leach liquor, and the precipitation agent of copper is nickelous carbonate or bicarbonate of ammonia.
Adopt solvent extraction to reclaim cobalt from the nickel leach liquor, used extraction agent is dialkyl phosphine acid compounds or two (2,4, a 4-tri-methyl-amyl) phosphonic acids.
Method of the present invention adopts one section pressurization to leach low nickel matte and the nickel ore concentrate of Treatment of Copper.Its its extract technology route is simple and direct, and the thorough leaching of nickel is retained in iron in the nickel ore concentrate and precious metal in the leached mud Returning smelting or alloy vulcanization process simultaneously in realizing high sulfonium nickel ore concentrate.Copper, cobalt and some other assorted very a spot of impurity such as zinc, manganese etc. enter leach liquor in the nickel ore concentrate, remove when solution purification and separate with nickel.Brief, the various metal direct yield of its flowage structure height, cost are low.
(4) description of drawings
Accompanying drawing is a kind of process flow sheet that extracts the nickel method from the low nickel sulfide material of cupric of the present invention.
(5) embodiment
A kind of method from the low nickel sulfide material extraction nickel of cupric, its method are to leach with one section pressurization to extract nickel from nickel matte or nickel ore concentrate.It is with in leaching nickel mineral, and the 5%-30% that presses nickel mineral weight adds sulphur, the water pulp, and pulp density is 5%-20%, and pulp pre-heating is arrived 50-80 ℃.In leaching still ore pulp is carried out pressure and leach, total pressure is 50-1000kPa, and oxygen partial pressure is 10-300kPa, and temperature is 100-180 ℃, and the residence time is 1-6 hour.Most copper in the gained leach liquor adopts chemical precipitation method to remove, and remaining a spot of copper separates with nickel from solvent extration with all cobalts, and a bright sulfur acid of output nickel solution can directly return nickel electrowinning and produce electric nickel, or produce high-purity sulphuric acid nickel.
The raw material that the present invention handles is low nickel matte of cupric and nickel ore concentrate, and copper content is 0-10%.The pressurization of nickel-containing material is leached by one section pressure leaching and is finished.
In the present invention, adopt sulphur or sulfuric acid to prepare burden, the sulphur amount of adding is the 15%-20% of nickel mineral weight, and the best is 16%-18%.The sulfuric acid that adds is the 70-90 grams per liter.
In the present invention, the concentration that leaches ore pulp is 5%-20%, and the best is 10%-15%.
In the present invention, when temperature was 130 ℃, the nickel leaching yield only was 85%.Temperature is higher than 140 when spending, and the nickel leaching yield can reach 99.7%, and the leaching of iron is lower.When temperature is higher, helps iron and enter leached mud.So the temperature of best leach liquor is 140-160 ℃.
In the present invention, when oxygen partial pressure was 100kPa, the leaching yield of nickel had only 68%.When oxygen partial pressure rose to 150kPa, the leaching yield of nickel can reach more than 99%.So the leaching total pressure is 600-800kPa, oxygen partial pressure is 150-250kPa.Also can adopt pressurized air to replace pure oxygen to leach, total pressure is 1000-1300kPa, and oxygen partial pressure is 200-300kPa.
In the present invention, pressurization was leached more than 2 hours, the nickel in the nickel ore concentrate almost all can be leached, and cobalt also can leach simultaneously, and the leaching yield of copper is 86%~96%.Be sufficient reacting, the time that pressurization is leached is 3-4 hour.
In the present invention, adopt chemical precipitation method copper removal from leach liquor, the precipitation agent of copper is a nickelous carbonate.
In the present invention, adopt solvent extraction to reclaim cobalt from the nickel leach liquor, used extraction agent is the dialkyl phosphine acid compounds.The Cyanex 272 (two (2,4,4-tri-methyl-amyl) phosphonic acids) of relatively typical this kind of extractants as producing by the special company of U.S.'s cyanogen (Cytec Industries Inc.).
Advantage of the present invention is the leaching fully of valuable metal nickel in finishing nickel matte in one section pressurization is leached, cobalt, copper.The extract technology structure is very simple, the leaching efficiency height.Nickel sulfate solution after the liquid-solid separation purifies with chemical precipitation method or solvent extration, and purified nickel sulfate solution of output can directly return nickel nickel electrowinning Workshop Production electricity nickel, but also evaporative crystallization is produced high-purity sulphuric acid nickel.Reclaim cobalt and copper simultaneously.Iron and precious metal are fixed in the slag.Leached mud can return the nickel smelting system, and present method is fit to the lower nickel matte of Treatment of Copper, and the nickel matte that cupric is high can advance pressurization and leach earlier through the floating low nickel ore concentrate of output cupric of high-sulfur mill again.This method be one simply, technology efficiently.
With following indefiniteness examples of implementation technology of the present invention is further described, helping understanding the present invention and advantage thereof, and as the qualification to protection domain of the present invention, protection scope of the present invention is determined by claims.
Example 1
The composition of the nickel ore concentrate of used leaching (%): Ni 66.27, and Cu 2.65, and Fe 2.32, Co0, and 85, S 23.75.
The pressurization leaching condition is: get nickel ore concentrate 100g, add sulphur 18g, leaching liquid-solid ratio is 6: 1, and extraction temperature is 140 ℃, oxygen partial pressure 150kPa, and the reaction times is 3 hours.
The leaching result of nickel, cobalt, copper, iron is as follows.
Leaching yield (%)
????Ni ????Co ????Cu ????Fe
????99.88 ????99.75 ????97.99 ????2.32
Example 2
The composition of the nickel ore concentrate of used leaching (%): Ni 66.27, and Cu 2.65, and Fe 2.32, Co0.85, and S 23.75.
The pressurization leaching condition is: get nickel ore concentrate 100g, add vitriol oil 26ml milliliter, leaching liquid-solid ratio is 5: 1, and extraction temperature is 145 ℃, oxygen partial pressure 200kPa, and the reaction times is 3.5 hours.
The leaching result of nickel, cobalt, copper, iron is as follows.
Leaching yield (%)
????Ni ????Co ????Cu ????Fe
????99.54 ????99.47 ????98.62 ????2.47
Example 3
The composition of the nickel ore concentrate of used leaching (%): Ni 66.27, and Cu 2.65, and Fe 2.32, Co0.85, and S 23.75.
The pressurization leaching condition is: get nickel ore concentrate 500g, add vitriol oil 120ml liter, leaching liquid-solid ratio is 5: 1, and extraction temperature is 145 ℃, oxygen partial pressure 250kPa, and the reaction times is 5 hours.
The leaching result of nickel, cobalt, copper, iron is as follows.
Leaching yield (%)
????Ni ????Co ????Cu ????Fe
????99.70 ????98.46 ????93.32 ????3.40
Example 4
The composition of the nickel ore concentrate of used leaching (%): Ni 66.27, and Cu 2.65, and Fe 2.32, Co0.85, and S 23.75.
The pressurization leaching condition is: get nickel ore concentrate 500g, add sulphur 85g, leaching liquid-solid ratio is 6: 1, and extraction temperature is 140 ℃, oxygen partial pressure 150kPa, and the reaction times is 5 hours.
The leaching result of nickel, cobalt, copper, iron is as follows.
Leaching yield (%)
????Ni ????Co ????Cu ????Fe
????99.33 ????97.77 ????87.11 ????2.20
Example 5
The composition of the nickel ore concentrate of used leaching (%): Ni 66.01, and Cu 3.15, and Fe 2.80, Co0.99, and S 22.97.
The pressurization leaching condition is: nickel ore concentrate 750kg/h, add sulfuric acid 450kg/t concentrate, and leaching liquid-solid ratio is 4: 1, and extraction temperature is 145 ℃, and compressed air require is 300m 3/ h, stagnation pressure are 1200kPa, and the reaction times is 4 hours.
The leaching result of nickel, cobalt, copper, iron is as follows.
Leaching yield (%)
????Ni ????Co ????Cu ????Fe
????99.72 ????98.71 ????93.16 ????4.15
Example 6
The composition of the nickel ore concentrate of used leaching (%): Ni 66.01, and Cu 3.15, and Fe 2.80, Co0.99, and S 22.97.
The pressurization leaching condition is: nickel ore concentrate 750kg/h, add sulphur 150kg/f concentrate, and leaching liquid-solid ratio is 4: 1, and extraction temperature is 140 ℃, and compressed air require is 360m 3/ h, stagnation pressure are 1250kPa, and the reaction times is 4 hours.
The leaching result of nickel, cobalt, copper, iron is as follows.
Leaching yield (%)
????Ni ????Co ????Cu ????Fe
????99.82 ????98.65 ????92.13 ????5.02
Typical leach liquor chemistry multielement analysis result is as follows.
Element ??Ni ????Cu ????Fe ????Co ????S ????Pb ????Zn
Content (g/L) ??110.10 ????2.74 ????0.082 ????1.26 ????- ????0.006 ????0.001
Element ??Ca ????Mg ????Si ????Al ????Mn ????As ????Sb
Content (g/L) ??0.10 ????0.07 ????0.16 ????0.13 ????0.0015 ????<0.01 ????<0.01

Claims (12)

1. one kind is extracted the method for nickel from the low nickel sulfide material of cupric, it is characterized in that its process is followed successively by:
A) in nickel ore concentrate, add sulfuric acid and water with the mineral pulp after, preheating ore pulp to 50 ℃-80 ℃, the weight percent of the mineral concentration of ore pulp is 5%-30% after the pulp, the vitriolic weight percent concentration is 50-90g/l,
B) carry out pressure in leaching still and leach, the total pressure that control is leached is 50-1000kPa, and oxygen partial pressure is 10-300kPa, and temperature is 100-180 ℃, and extraction time is 1-6 hour;
D) with purification of leaching liquor, use earlier the chemical precipitation method copper removal, go out cobalt and remaining copper with Solvent Extraction Separation again and obtain electrolysis production nickel behind the sour nickel solution of bright sulfur.
2. a kind of method from the low nickel sulfide material extraction nickel of cupric according to claim 1 is characterized in that copper content is less than 5% in its nickel ore concentrate.
3. a kind of method according to claim 1 from the low nickel sulfide material extraction nickel of cupric, the acid when it is characterized in that leaching obtains by add the sulphur rear oxidation in mineral, and add-on is the 5%-30% of nickel ore concentrate weight.
4. a kind of method from the low nickel sulfide material extraction nickel of cupric according to claim 1, after it is characterized in that adding sulfuric acid, vitriolated weight percent concentration is the 70-90 grams per liter in the ore pulp.
5. according to claim 1 and the described a kind of method of claim 3, it is characterized in that the sulphur amount that adds is the 10%-15% of nickel ore concentrate weight from the low nickel sulfide material extraction nickel of cupric.
6. a kind of method from the low nickel sulfide material extraction nickel of cupric according to claim 1, the temperature that it is characterized in that leach liquor is 140-160 ℃.
7. a kind of method according to claim 1 from the low nickel sulfide material extraction nickel of cupric, it is characterized in that leaching total pressure is 500-1000kPa, oxygen partial pressure is 100-300kPa.
8. a kind of method according to claim 1 from the low nickel sulfide material extraction nickel of cupric, its feature is being to adopt pressurized with compressed air to leach, and total pressure is 1000-1300kPa, and oxygen partial pressure is 200-300kPa.
9. a kind of method from the low nickel sulfide material extraction nickel of cupric according to claim 1, the time of leaching that it is characterized in that pressurizeing is 2-4 hour.
10. a kind of method from the low nickel sulfide material extraction nickel of cupric according to claim 1 is characterized in that adopting chemical precipitation method copper removal from leach liquor, and the precipitation agent of copper is a nickelous carbonate.
11. a kind of method from the low nickel sulfide material extraction nickel of cupric according to claim 1 is characterized in that adopting solvent extraction to reclaim cobalt from the nickel leach liquor, used extraction agent is the dialkyl phosphine acid compounds.
12. a kind of method from the low nickel sulfide material extraction nickel of cupric according to claim 1 is characterized in that adopting solvent extraction to reclaim cobalt from the nickel leach liquor, used extraction agent is two (2,4, the 4-tri-methyl-amyl) phosphonic acids.
CNB011347309A 2001-11-09 2001-11-09 Process for extracting nickel from nickel sulfide material with low copper content CN1148461C (en)

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CN100497680C (en) * 2007-01-19 2009-06-10 昆明贵金属研究所 New method for extracting nickel from enriched ore of nickel sulfide

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CN101328536B (en) * 2007-06-18 2010-06-02 中国恩菲工程技术有限公司 Process for comprehensive recovery of nickel, copper, cobalt, sulfur and magnesium from ore
WO2009129653A1 (en) * 2008-04-23 2009-10-29 Dong Shutong A comprehensive recovery and utilization process for laterite-nickel ore
CN101705371B (en) * 2009-11-20 2011-04-06 北京矿冶研究总院 Method for extracting cobalt in copper cobalt sulfide ore
CN101899568B (en) * 2010-07-23 2012-06-20 陕西华泽镍钴金属有限公司 Method for producing electrolytic nickel by leaching chemically precipitated nickel sulfide with pure oxygen
JP5445777B2 (en) * 2010-07-28 2014-03-19 住友金属鉱山株式会社 Method for producing ferronickel smelting raw material from low-grade nickel oxide ore
CN102703730A (en) * 2012-06-18 2012-10-03 中国恩菲工程技术有限公司 Method for smelting nickel matte by using lateritic nickel ore
CN102851495B (en) * 2012-08-29 2014-02-26 江西自立资源再生有限公司 Technology for producing cathode copper through high-pressure oxygen leaching of copper and nickel contained melting slag
CN104831062B (en) * 2015-03-26 2017-09-15 武汉钢铁(集团)公司 The method that valuable element is extracted using iron concentrate
CN106399682A (en) * 2016-09-23 2017-02-15 中国恩菲工程技术有限公司 Method for extracting valuable metal from copper, cobalt and nickel sulfide
CN108950199A (en) * 2018-07-13 2018-12-07 兰州金川新材料科技股份有限公司 A method of it being used for the nickel and cobalt solution of synthesis of ternary presoma using the preparation of nickel sulfide cobalt ore
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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