CN107630146A - nickel recovery method - Google Patents
nickel recovery method Download PDFInfo
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- CN107630146A CN107630146A CN201710668027.1A CN201710668027A CN107630146A CN 107630146 A CN107630146 A CN 107630146A CN 201710668027 A CN201710668027 A CN 201710668027A CN 107630146 A CN107630146 A CN 107630146A
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Abstract
The invention provides a kind of nickel recovery method.The recovery method includes：Alloying converter mattes are subjected to normal pressure leaching, obtain normal pressure leaching liquid and normal pressure leaching slag, and first time nickel element recovery is carried out to normal pressure leaching liquid；And the mixture of normal pressure leaching slag and converter mattes is subjected to Selectively leaching, to carry out second of nickel element recovery.Converter mattes and alloying converter mattes can not only effectively be handled using the handling process, and due to first handling forming complex alloying converter mattes, remove its a large amount of ferro element contained, the process not consumption acids and alkaline reagent, and with technological process is simple, low cost and other advantages.Then the leached mud obtained after processing and converter mattes are subjected to Selectively leaching jointly.Converter mattes and alloying converter mattes are handled respectively compared to existing, and above-mentioned recovery method has the strong adaptability to material, technological process short and low cost and other advantages.
Description
Technical field
The present invention relates to field of hydrometallurgy, in particular to a kind of nickel recovery method.
Background technology
Mainly there is nickel sulfide soluble anode electric by the process that raw material is processed refining of high nickel matte both at home and abroad at present
Solution technique, sulfuric acid Selectively leaching technique, carbonylation process and potassium cloride technique.
Nickel sulfide anode electrolysis technique is to grow up the sixties in last century, and main manufacturer has Canada at present
The Thompson factory of Inco companies and the Jinchuan Non-ferrous Metals Company in China, Chengdu electrometallurgy factory, Chongqing Ji En smelteries, Jilin Ji grace nickel industry stock
Part Co., Ltd etc..Although there is difference in each factory on specific process detail, generally the technique exist flow it is complicated,
High energy consumption, auxiliary material consumption are high, and nickel yield is low, and precious metal losses are big, and the current efficiency of nickel sulfide anode is low, the net liquid quantity of slag
Greatly, anode is easily passivated, and need to be electrolysed or many drawbacks such as chemical liquid making.
Carbonylation process carries out industrialized production and appears in early 20th century in the world.Carbonylation process passes through the hair of last 100 yearses
Exhibition, the three kinds of techniques produced with normal pressure, middle pressure (5~7MPa), high pressure (22~25MPa) are formed.Carbonylation process
Product structure is substantially similar, including the thousands of kinds of products such as nickel rondelle, ferronickel ball, pure nickel powder, nickel coated powder.Because its product is than other
The product copper containing cobalt of nickel refining method output, lead, zinc order of magnitude lower, and possess the crystalline structure and surface topography of uniqueness,
Therefore it is widely used in the fields such as powder metallurgy, military project high density and materials with high melting point, Precise Alloy, special steel.But the technique is given birth to
Production process can produce carbon monoxide and the carbonyls with hypertoxicity, and whole production process needs to enter in closed system
OK, and to equipment and production operation control require high.Possess the technology of carbonylation metallurgy Refining Nickel in the world at present and realize work
Only Canadian INCO companies and the Russian NORILSK companies of industryization large-scale production.The country is entered using carbonylation process at present
The major vendor of row production is Jinchuan Non-ferrous Metals Company and Jilin Ji grace nickel industry.According to statistics, the total output of carbonyl nickel is annual in the world at present
About 170,000 tons, wherein International nickel Co. Ltd. Inco. Ltd. accounts for more than 80%, has almost monopolized carbonyl nickel market.
The potassium cloride technique of high nickel matte, production application is obtained abroad in the seventies in last century.France in 1978, which strangles, breathes out
Fo Er-Sang Duowei thats factory is with Fe2+/Fe3+For high nickel matte of the more Ni Anbo factories in galvanic couple chlorination refining New Caledonia containing trace copper
Produce electric nickel.Canadian Ying Qiao companies Christian pine refinery is with Cu within 1981+/Cu2+For galvanic couple, soaked with chlorine gas selecting
Go out the high nickel matte of cupro-nickel of the said firm.SUMITOMO CHEMICAL metal mine company new home Bin Niejinglianchang in 1993, electricity is soaked with high nickel matte chlorine
Area method substitutes original high nickel matte anode electrolysis refinery practice.The technique has that technological process is short, electro deposited nickel quality is high, the rate of recovery
The high, advantage such as processing charges is low, power consumption is low.However, because the technique is chloride system, output chlorine and needs in electrolytic deposition process
Return to leaching process to recycle, the requirement to key equipment, material is high, and there is presently no industrial applications in China.In addition, by
The chlorine recycled in technical process is hypertoxicity gas, higher security risk be present.
Sulfuric acid Selectively leaching technique is the advanced technology to grow up in 20th century, by the nickel in high nickel matte in autoclave
Leached with selective copper so as to realize the separation of ambrose alloy.It is characterized in that technological process is short, valuable gold stronger to the adaptability of raw material
Belong to that the rate of recovery is high, and solution is impure very low, removal of impurities load is small, and automaticity is high, do not produced during raw factory waste gas, waste residue and
Waste liquid, it is substantially free of contamination cleaning procedure.The technique at home and abroad has the knowhow of maturation, and obtains preferably
Economic benefit.This Rustenburg nickel refining factory, Zimbabwe guest strangle all in Outokumpu company Ha Jiawaerta nickel refinings factory, South Africa
Smeltery etc. is drawn to use the technique productions electro deposited nickel.Domestic Jinchuan Non-ferrous Metals Company, Fukang, Xinjiang smeltery, Jilin Nickel Industry Co. into
Pressure leaching technology is applied in production by work(.
But in this area, existing research method is primarily directed to single converter mattes.If directly use identical work
When skill is respectively processed to converter mattes and alloying converter mattes, process costs hand over high, technological process length.
The content of the invention
It is a primary object of the present invention to provide a kind of nickel recovery method, yet there are no in the prior art with solution can be simultaneously
The problem of refinery practice of processing converter mattes and alloying converter mattes.
To achieve these goals, the invention provides a kind of nickel recovery method, recovery method to include：By alloying Gao Bing
Nickel carries out normal pressure leaching, obtains normal pressure leaching liquid and normal pressure leaching slag, and carry out first time nickel element recovery to normal pressure leaching liquid；
And the mixture of normal pressure leaching slag and converter mattes is subjected to Selectively leaching, to carry out second of nickel element recovery.
Further, the process of normal pressure leaching includes：In the presence of the first thermal medium and the first leaching agent, by alloying
Part of nickel element oxide in converter mattes is ion, obtains normal pressure leaching liquid；Preferably, during normal pressure leaching, first leaches
The weight of agent and alloying converter mattes ratio is 20~30:1, extraction temperature is 80~90 DEG C, and extraction time is 8~10h, is leached eventually
Point pH value is 2.0~2.5；Preferably, the first thermal medium is steam, and the first leaching agent is sulfuric acid.
Further, the process of Selectively leaching includes：In the presence of the second thermal medium and the second leaching agent, by normal pressure
The mixture of leached mud and converter mattes carries out one section of pressure leaching, obtains first choice leachate and first choice leaches
Slag；And in the presence of the 3rd thermal medium and the 3rd leaching agent, first choice leached mud is subjected to two sections of pressure leachings, obtained
Second Selectively leaching liquid and the second selective leaching are slagged tap；Preferably, during one section of pressure leaching, extraction temperature be 140~
160 DEG C, leaching pressure is 0.8~1.0MPa, and extraction time is 4~6h；Preferably, during two sections of pressure leachings, temperature is leached
Spend for 150~160 DEG C, leaching pressure is 0.8~1.0MPa, and extraction time is 4~6h；Preferably, the second thermal medium and the 3rd
Thermal medium is steam, and the second leaching agent and the 3rd leaching agent are sulfuric acid.
Further, the second leaching agent is divided into Part I and Part II；By the mixed of normal pressure leaching slag and converter mattes
The step of compound one section of pressure leaching of progress, includes：Normal pressure leaching slag is mixed with converter mattes, obtains mixture；By mixture,
After the mixing of the leaching agent of Part I second, one section of normal pressure leaching is carried out, obtains one section of normal pressure leaching liquid and one section of normal pressure leaching slag；
After one section of normal pressure leaching slag, the leaching agent of Part II second and sulphur-fixing agent are mixed, two sections of normal pressure leachings are carried out, obtain leaching ore deposit
Slurry；And it is passed through the second thermal medium to leaching in ore pulp, one section of pressure leaching process is carried out, obtains first choice leachate and the
One selective leaching is slagged tap.
Further, during one section of normal pressure leaching, the weight ratio of the leaching agent of Part I second and mixture for 30~
40:1, extraction temperature is 80~90 DEG C, and extraction time is 6~8h, and it is 6.0~6.5 to leach endpoint pH；Preferably, two sections often
Press in leaching process, the weight of one section of normal pressure leaching slag and the mixture of sulphur-fixing agent is designated as n1, Part II second is leached
The weight of agent is designated as n2, n1/n2=1：8~10,80~90 DEG C, 10~12h of extraction time of extraction temperature, leaching endpoint pH is
1.0~1.5；Preferably, sulphur-fixing agent is cupric oxide.
Further, recovery method also includes：It is that raw material carries out Selectively leaching process to first choice leachate；It is excellent
Selection of land, in first time nickel element removal process, the nickel element in normal pressure leaching liquid is reclaimed using electrodeposition method；Second of nickel element returns
During receipts, the nickel element in one section of normal pressure leaching liquid is reclaimed using electrodeposition method.
Further, before the removal process of first time nickel element is carried out, recovery method is also included normal pressure leaching liquid
The step of carrying out pressurization iron removaling；Preferably, before second of nickel element removal process is carried out, recovery method also includes one section
Normal pressure leaching liquid carries out the step of pressurization iron removaling.
Further, the step of iron removaling of pressurizeing, includes：In the presence of the 4th thermal medium, make normal pressure leaching liquid and/or one
Hydrolysis occurs for the iron ion in section normal pressure leaching liquid, and is separated out in the form of precipitation；The temperature for iron removal of pressurizeing is 180
~190 DEG C, pressure is 1.2~1.5MPa；Preferably, the 4th thermal medium is steam.
Further, after the step of carrying out pressurization iron removaling, recovery method also includes：Remove the normal pressure leaching after pressurization iron removaling
The lead element and cobalt element gone out in liquid, and/or remove lead element and cobalt member in the first choice leachate after pressurization iron removaling
Element.
Further, cobalt element is removed using chemical precipitation method or extraction, it is preferable that using chemical precipitation method or ion
Exchange process removes lead element.
Apply the technical scheme of the present invention, the nickel recovery method that the application provides provide it is a kind of and meanwhile handle converter mattes with
The recovery method of alloying converter mattes.Converter mattes and alloying converter mattes can not only effectively be handled using the handling process, and
And due to first handling forming complex alloying converter mattes, its a large amount of ferro element contained is removed, the process is not
Consumption acids and alkaline reagent, and with technological process is simple, low cost and other advantages.Then by the leached mud obtained after processing and height
Ice nickel carries out Selectively leaching jointly.Converter mattes and alloying converter mattes, above-mentioned recovery method are handled respectively compared to existing
With the strong adaptability to material, technological process is short and low cost and other advantages.
Brief description of the drawings
The Figure of description for forming the part of the application is used for providing a further understanding of the present invention, and of the invention shows
Meaning property embodiment and its illustrate be used for explain the present invention, do not form inappropriate limitation of the present invention.In the accompanying drawings：
Fig. 1 shows the process chart of the nickel recovery method provided according to a kind of typical embodiment of the present invention.
Embodiment
It should be noted that in the case where not conflicting, the feature in embodiment and embodiment in the application can phase
Mutually combination.The present invention is described in detail below in conjunction with embodiment.
As described by background technology, it yet there are no in the prior art while handle converter mattes and the essence of alloying converter mattes
Sweetening process.In order to solve the above-mentioned technical problem, the invention provides a kind of nickel recovery method, the recovery method to include：By alloy
Change converter mattes and carry out normal pressure leaching, obtain normal pressure leaching liquid and normal pressure leaching slag, and a nickel element is carried out to normal pressure leaching liquid
Recovery；And the mixture of normal pressure leaching slag and converter mattes is subjected to Selectively leaching, to carry out second of nickel element recovery.
This application provides a kind of recovery method for handling converter mattes and alloying converter mattes.Alloying converter mattes are in normal pressure
Leach in leaching tanks, the metals such as a large amount of metallization iron, copper, nickel leached into solution, be passed through in normal pressure leaching groove oxygen or
Compressed air is aoxidized, and is passed through steam to maintain to leach required temperature, is obtained normal pressure leaching ore pulp；Normal pressure leaching ore pulp
After concentrator carries out solid-liquor separation, normal pressure leaching slag delivers to converter mattes dosage bunker.
Compared to converter mattes, the composition of alloying converter mattes is increasingly complex, thus first alloying converter mattes are located in advance
Reason.Specifically, alloying converter mattes are subjected to normal pressure leaching, after separation of solid and liquid, obtain normal pressure leaching liquid and normal pressure leaching slag；And
The mixture of normal pressure leaching slag and converter mattes is subjected to Selectively leaching, to reclaim nickel element.
Normal pressure leaching processing first is carried out to forming complex alloying converter mattes in above-mentioned process, alloying is high
Part metals simple substance in ice nickel is converted into metal ion, so as to be transferred in normal pressure leaching liquid, and does not have in alloying converter mattes
With the presence of reaction material as normal pressure leaching slag, and in normal pressure leaching liquid carry out first time nickel element recovery.Then inciting somebody to action
The mixture of normal pressure leaching slag and converter mattes carries out Selectively leaching, to carry out second of nickel element recovery.Using the processing work
Artistic skill is enough targetedly to be handled according to the difference of converter mattes and alloying converter mattes composition, and then is advantageous to improve nickel element
Deng the rate of recovery.Converter mattes and alloying converter mattes are handled respectively compared to existing, and the above method also has fits to material
Ying Xingqiang, technological process be short and low cost and other advantages.
Term " Selectively leaching " refers to by selectively leaching condition in the application, makes main metal ingredient and associated metal point
Not Jin Ru solution or slag, to reach the purpose of initial gross separation.
Term " converter mattes " refers to that nickel ore concentrate smelts the metals such as the nickel formed, copper, cobalt through electricity, converter primary in the application
Sulfide eutectic.
In the application term " alloying converter mattes " refer to the metallic elements such as nickel in converter mattes, copper, iron some with
The form of metal or alloy is present.
In a preferred embodiment, the process of normal pressure leaching includes：In the first thermal medium and the first leaching agent
Under effect, it is ion by the part of nickel element oxide in alloying converter mattes, obtains normal pressure leaching liquid.Preferably, normal pressure leaching
During, the weight ratio of the first leaching agent and alloying converter mattes is 20~30:1, extraction temperature is 80~90 DEG C, extraction time
For 8~10h, it is 2.0~2.5 to leach endpoint pH.The condition of normal pressure leaching process includes but is not limited to above range, and by its
The content for, being advantageous to improve nickel element in normal pressure leaching liquid within the above range is limited, and then improves the rate of recovery of nickel element.It is excellent
It is steam to select the first thermal medium, and the first leaching agent is sulfuric acid.
The recovery method of converter mattes and alloying converter mattes is handled while the application provides that cost is low, nickel element recovery
The advantages that rate is high.Above-mentioned Selectively leaching process can use the process conditions that ability is commonly used.In a kind of preferred embodiment
In, the process of Selectively leaching includes：In the presence of the second thermal medium and the second leaching agent, by normal pressure leaching slag and converter mattes
Mixture carry out one section of pressure leaching, obtain first choice leachate and first choice leached mud；In the 3rd thermal medium
In the presence of the 3rd leaching agent, first choice leached mud is subjected to two sections of pressure leachings, obtains the second Selectively leaching liquid
Slagged tap with the second selective leaching.
Metal phase in converter mattes further leaches, a small amount of Ni3S2Also leach in the lump.Iron hydrolytic precipitation in solution enters
Copper in leached mud, solution, which is replaced and hydrolyzed, also enters leached mud, leaches endpoint pH control 6~6.5 or so.Leaching tanks
Domestic demand is passed through thermal medium (steam) and heated, to maintain the temperature required for leaching.
It is preferred that one section of normal pressure leaching slag of converter mattes, sulphur-fixing agent (cupric oxide calcining), nickel electrodeposition anolyte mix in slurrying tank
Afterwards, two sections of normal pressure leachings are carried out, further leach alloy and a small amount of Ni in raw material3S2.Hydrolyzed in one section of normal pressure leaching process
Iron copper etc. is in this in-process by dissolution again.Leaching tanks domestic demand is passed through oxygen or compressed air oxidation, is passed through steam to maintain to soak
Go out required temperature.
Preferably, during one section of pressure leaching, extraction temperature is 140~160 DEG C, and leaching pressure is 0.8~1.0MPa,
Extraction time is 4~6h.
Preferably, during two sections of pressure leachings, extraction temperature is 150~160 DEG C, and leaching pressure is 0.8~1.0MPa,
Extraction time is 4~6h.Preferably, steam is passed through in Selectively leaching system to ensure one section of pressure leaching and two sections of pressurizations
The treatment temperature of leaching.Be advantageous to further carry from the concrete technology progress Selectively leaching of the process of above-mentioned Selectively leaching
The rate of recovery of high nickel element.It is preferred that the second thermal medium and the 3rd thermal medium are steam, the second leaching agent and the 3rd leaching agent are equal
Sulfuric acid.
Preferably, the second leaching agent is divided into Part I and Part II；By the mixing of normal pressure leaching slag and converter mattes
The step of thing one section of pressure leaching of progress, includes：Normal pressure leaching slag is mixed with converter mattes, obtains mixture；By mixture,
After a part of second leaching agent mixing, one section of normal pressure leaching is carried out, obtains one section of normal pressure leaching liquid and one section of normal pressure leaching slag；Will
After one section of normal pressure leaching slag, the leaching agent of Part II second and sulphur-fixing agent mixing, two sections of normal pressure leachings are carried out, obtain leaching ore pulp
(copper sulfide) is precipitated with sulfur-bearing；And the second thermal medium is passed through in ore pulp to leaching, one section of pressure leaching process is carried out, obtains first
Selectively leaching liquid and first choice leached mud.
Before carrying out Selectively leaching process, element sulphur is first removed, is advantageous to improve the rate of recovery of nickel element.
In a preferred embodiment, during one section of normal pressure leaching, the leaching agent of Part I second and mixture
Weight ratio be 30~40:1, extraction temperature is 80~90 DEG C, and extraction time is 6~8h, and it is 6.0~6.5 to leach endpoint pH.
Preferably, the weight of one section of normal pressure leaching slag and the mixture of sulphur-fixing agent is designated as n1, by the leaching agent of Part II second
Weight is designated as n2, n1/n2=8~10:1,80~90 DEG C, 10~12h of extraction time of extraction temperature, leach endpoint pH be 1.0~
1.5；It is preferred that sulphur-fixing agent is cupric oxide.
The process conditions of one section of normal pressure leaching process are limited and are advantageous to the clearance for improving element sulphur within the above range,
And then improve the rate of recovery of nickel element.One section of normal pressure leaching slag and sulphur-fixing agent and the second leaching agent are carried out into two sections of normal pressures simultaneously to soak
Go out, the element sulphur in one section of normal pressure leaching slag can be removed.This method need not by the way that element sulphur is first converted into sulfate radical,
The mode for removing sulfate radical again removes element sulphur.As can be seen here, above-mentioned process for sulfur removal has that technological process is simple, cost is low and useless
The features such as water discharge rate is low.Preferably, after one section of pressure leaching slag, the second leaching agent mix in slurrying tank, ore pulp is formed.Will
Above-mentioned ore pulp is pumped into ore pulp heat exchange device by two sections of pressurizations and preheated, and the ore pulp after preheating carries out two in two sections of autoclaves
Section pressure leaching.Steam (to maintain required temperature) and oxygen (thermal medium) are passed through in autoclave.By controlling appropriate bar
Part, remaining nickel, cobalt is set to be leached into leachate, iron and copper still suppress in leached mud.Ore pulp after leaching is in flash tank
Interior decompression cooling, the indirect steam of the interior generation of flash tank are similar with the processing of above-mentioned flash-off steam.Two sections of pressurization leachings in flash tank
Go out ore pulp and carry out solid-liquor separation, obtain leached mud (vulcanizing copper ashes) and leachate.Leached mud is delivered into oxidizing roasting, leachate
Return to one section of pressure leaching.
The element sulphur in one section of normal pressure leaching slag is removed using sulphur-fixing agent, the leaching ore pulp of formation.Then ore pulp is leached
The second selective leaching is obtained by one section of pressure leaching and two sections of pressure leachings to slag tap.Above-mentioned second selective leaching is slagged tap progress
Oxidizing roasting obtains cupric oxide calcining so that contained sulphur to be removed.The roasting technique of use can be rotary kiln baking or boiling
Stove is calcined, and about 500~950 DEG C of sintering temperature, desulfurization degree is more than 95wt%.Sulfur dioxide caused by roasting can be used for relieving haperacidity or system
Sulphur.Sulfur content in raw material, a certain amount of cupric oxide calcining is returned to two sections of normal pressure leaching processes.Surplus cupric oxide roasts
Sand can be sold as product or further handle to reclaim valuable metal therein.
In a preferred embodiment, above-mentioned recovery method also includes using first choice leachate as raw material, enters
Row Selectively leaching process.Preferably, in first time nickel element removal process, the nickel in normal pressure leaching liquid is reclaimed using electrodeposition method
Element；In second of nickel element removal process, the nickel element in one section of normal pressure leaching liquid is reclaimed using electrodeposition method.Pass through electrodeposition method
Be advantageous to that the higher metallic nickel of purity is made.The anolyte of electrolytic deposition process can be used as the first leaching agent and/or the second leaching agent
Used.
In a preferred embodiment, before the removal process of first time nickel element is carried out, recovery method also wraps
Include the step of normal pressure leaching liquid is subjected to pressurization iron removaling；Preferably, before second of nickel element removal process is carried out, recovery side
The step of method also includes one section of normal pressure leaching liquid carrying out pressurization iron removaling.
Contain substantial amounts of ferro element in alloying converter mattes, iron removaling processing of pressurizeing is carried out to normal pressure leaching liquid, it is normal to remove
The ferro element in leachate is pressed, is advantageous to improve the purity and the rate of recovery of the nickel element that recovery obtains.The process does not disappear simultaneously
Consume acid and alkaline reagent, and with technological process is simple, low cost and other advantages.
In a preferred embodiment, before the removal process of first time nickel element, normal pressure leaching liquid is carried out
Pressurization iron removaling, the process of the pressurization iron removaling include：In the presence of the 4th thermal medium, the iron ion in normal pressure leaching liquid occurs
Hydrolysis, and removed in the form of precipitation；Before the removal process of second of nickel element, one section of normal pressure leaching liquid is carried out
Pressurization iron removaling, the process of the pressurization iron removaling include：In the presence of the 4th thermal medium, make the iron ion in one section of normal pressure leaching liquid
Generation hydrolysis, and removed in the form of precipitation.It is preferred that normal pressure leaching liquid and/or one section of normal pressure leaching liquid are sent into pressurization iron removaling
In autoclave, the 4th thermal medium (maintain needed for temperature) is passed through, the iron in solution is precipitated into slag in the form of bloodstone, reaches
The purpose of iron removaling.Ore pulp after iron removaling carries out decompression cooling into flash tank, and the indirect steam of flash tank washs in flash-off steam
Wash cooling in device, the tail gas after washing can reach environmental emission standard, is emitted into air.Ore pulp after cooling in flash tank
Send concentrator to carry out solid-liquor separation, obtain normal pressure leaching liquid and scum.Then normal pressure leaching liquid is sent to one section of normal pressure of converter mattes
Leaching process, scum send pyrogenic attack to reclaim valuable metal therein after press filtration.4th thermal medium is steam.
Ferro element in normal pressure leaching liquid is precipitated in the form of bloodstone and yellow potassium iron sail.Scum can be thrown aside as waste residue,
Or the pyrogenic process system of return nickel fibers further reclaims a small amount of nickel contained therein.Preferably, the temperature of press processes is
180~190 DEG C, pressure is 1.2~1.5MPa.It is preferred that normal pressure leaching liquid is set to keep above-mentioned treatment temperature using steam.And it will add
The term restriction of pressure processing procedure is advantageous to improve within the above range the clearance of ferro element.
In a preferred embodiment, after the step of carrying out pressurization iron removaling, above-mentioned recovery method also includes：Remove
The lead element and cobalt element in normal pressure leaching liquid after iron removaling of pressurizeing, and/or the first choice removed after pressurization iron removaling leach
Lead element and cobalt element in liquid.Before the step of preparing metallic nickel using electrodeposition method, material liquid (normal pressure leaching is first removed
Liquid, first choice leachate or the second Selectively leaching liquid) in lead element and cobalt element, be advantageous to further improve electrodeposition
The purity for the metallic nickel that method obtains.Preferably, cobalt element is removed using chemical precipitation method or extraction, using chemical precipitation method or
Ion-exchange removes lead element.Material liquid (nickel sulfate solution) after purification is pumped to nickel electrodeposition workshop and carries out nickel electrodeposition, production
Go out to meet Ni9996 requirement electrolytic nickel product, nickel anode liquid on demand distinguish revert alloy converter mattes leach, two sections often
Pressure leaches, two sections of pressure leachings etc. leach process.
The present invention is described in further detail below in conjunction with specific embodiment, these embodiments are it is not intended that limit this
Invent scope claimed.
Embodiment 1
The main component of alloying converter mattes and converter mattes is shown in Table 1.
Table 1
| Treating capacity | Ni, wt% | Cu, wt% | Co, wt% | Fe, wt% | S, wt% | |
| Converter mattes | 342g | 55.87 | 12.73 | 0.58 | 5.10 | 23.00 |
| Alloying converter mattes | 444g | 52.34 | 5.80 | 1.33 | 32.00 | 7.00 |
Using patent PROCESS FOR TREATMENT above two material of the present invention, as shown in figure 1, detailed process is as follows：
(1) alloying converter mattes and sulfuric acid are subjected to normal pressure leaching, obtain normal pressure leaching liquid and normal pressure leaching slag；Normal pressure soaks
During going out, the weight ratio of sulfuric acid and alloying converter mattes is 25:1,85 DEG C, extraction time 9h of extraction temperature, leach terminal pH
It is worth for 2.0.
(2) alloying converter mattes leachate is subjected to pressurized treatments, to remove ferro element；The temperature of press processes is
185 DEG C, pressure 1.3MPa.
(3) mixture of above-mentioned normal pressure leaching slag and converter mattes and sulfuric acid are subjected to one section of normal pressure leaching, obtain one section often
Press leachate and one section of normal pressure leaching slag；The weight of sulfuric acid and said mixture ratio is 35:1,85 DEG C of extraction temperature, extraction time
7h, it is 6.2 to leach endpoint pH.
(4) one section of normal pressure leaching slag of converter mattes, cupric oxide calcining and sulfuric acid are subjected to two sections of normal pressure leachings, obtain two sections often
Pressure leaches ore pulp；Wherein the mixture of one section of normal pressure leaching slag and cupric oxide, the weight ratio of sulfuric acid are 1:8,85 DEG C of extraction temperature,
Extraction time 11h, it is 1.2 to leach endpoint pH.
(5) two sections of normal pressure leaching ore pulps are subjected to one section of pressure leaching, leachate returns to one section of normal pressure leaching of converter mattes.One
The extraction temperature of section pressure leaching is 150 DEG C, and leaching pressure is 0.8MPa, extraction time 5h.
(6) one section of pressure leaching slag is subjected to two sections of pressure leachings, obtains the second Selectively leaching liquid and the second selectivity
Leached mud.Second Selectively leaching liquid returns to one section of pressure leaching process；The extraction temperature of two sections of pressure leachings is 150 DEG C, leaching
It is 0.9MPa, extraction time 6h to go out pressure.
(7) by the selective leaching of part second slag tap carry out oxidizing roasting obtain cupric oxide calcining, as sulphur-fixing agent.
(8) after normal pressure leaching liquid and the second Selectively leaching liquid being removed into lead and cobalt element, produced using electrodeposition and prepare electricity
Solve nickel.
Copper sulfide slag ingredient, the cupric oxide calcining composition of copper sulfide slag oxidation calcining output of two sections of pressure leaching outputs,
And the scum composition of pressurization iron removaling output is shown in Table 2.
Table 2
| Treating capacity | Ni, wt% | Cu, wt% | Co, wt% | Fe, wt% | S, wt% | |
| Vulcanize copper ashes | 457g | 4.84 | 40 | 0.13 | 16.3 | 22.9 |
| Cupric oxide calcining | 243g | 5.48 | 45.22 | 0.14 | 18.46 | 1.64 |
| Scum | 346g | 2.02 | 0.02 | 0.01 | 37.6 | 2.82 |
The total recovery of nickel can reach 98.3wt%, and the cobalt rate of recovery is 96.5wt%, copper recovery 95.8wt%.
Embodiment 2
With being distinguished as embodiment 1：The composition of alloying converter mattes and converter mattes is different, is specifically shown in Table 3.
Table 3
| Treating capacity | Ni, % | Cu, % | Co, % | Fe% | S, % | |
| Converter mattes | 444g | 55.87 | 12.73 | 0.58 | 5.10 | 23.00 |
| Alloying converter mattes | 335g | 52.34 | 5.80 | 1.33 | 32.00 | 7.00 |
Above two material is handled using above-mentioned recovery method.The copper sulfide slag ingredient of two sections of pressure leaching outputs, vulcanization
Copper ashes aoxidizes the cupric oxide calcining composition of calcining output, and the scum composition of pressurization iron removaling output is shown in Table 4.
Table 4
| Treating capacity | Ni, % | Cu, % | Co, % | Fe% | S, % | |
| Vulcanize copper ashes | 516g | 4.65 | 40.6 | 0.14 | 16.3 | 23.1 |
| Cupric oxide calcining | 289g | 5.24 | 45.8 | 0.16 | 18.4 | 1.67 |
| Scum | 274g | 2.26 | 0.01 | 0.01 | 35.8 | 2.68 |
The total recovery of nickel can reach 98.2wt%, and the cobalt rate of recovery is 96.3wt%, copper recovery 95.6wt%.
Embodiment 3
Difference with embodiment 1 is：During alloying converter mattes are carried out into normal pressure leaching, sulfuric acid is high with alloying
The weight ratio of ice nickel is 15:1, extraction temperature is 70 DEG C, extraction time 11h, and it is 2.8 to leach endpoint pH.
Copper sulfide slag ingredient, the cupric oxide calcining composition of copper sulfide slag oxidation calcining output of two sections of pressure leaching outputs,
And the scum composition of pressurization iron removaling output is shown in Table 5.
Table 5
| Treating capacity | Ni, wt% | Cu, wt% | Co, wt% | Fe, wt% | S, wt% | |
| Vulcanize copper ashes | 457g | 4.94 | 35 | 0.1 | 15.1 | 20.9 |
| Cupric oxide calcining | 243g | 5.55 | 45.22 | 0.14 | 18.46 | 1.64 |
| Scum | 346g | 2.75 | 0.04 | 0.05 | 36.6 | 3.82 |
The total recovery of nickel can reach 98.0wt%, and the cobalt rate of recovery is 96.1wt%, copper recovery 95.8wt%.
Embodiment 4
Difference with embodiment 1 is：To remove the temperature of ferro element process as 170 DEG C, pressure is pressurized treatments
1.0MPa。
Copper sulfide slag ingredient, the cupric oxide calcining composition of copper sulfide slag oxidation calcining output of two sections of pressure leaching outputs,
And the scum composition of pressurization iron removaling output is shown in Table 6.
Table 6
| Treating capacity | Ni, wt% | Cu, wt% | Co, wt% | Fe, wt% | S, wt% | |
| Vulcanize copper ashes | 457g | 4.99 | 35 | 0.1 | 15.1 | 20.9 |
| Cupric oxide calcining | 243g | 5.61 | 45.22 | 0.14 | 18.46 | 1.64 |
| Scum | 346g | 2.55 | 0.03 | 0.04 | 35.8 | 3.55 |
The total recovery of nickel can reach 97.5wt%, and the cobalt rate of recovery is 94.3wt%, copper recovery 93.7wt%.
Embodiment 5
Difference with embodiment 1 is：During one section of normal pressure leaching, the weight ratio of sulfuric acid and said mixture is 20:
1, extraction temperature is 95 DEG C, extraction time 7h, and it is 6.6 to leach endpoint pH.
Copper sulfide slag ingredient, the cupric oxide calcining composition of copper sulfide slag oxidation calcining output of two sections of pressure leaching outputs,
And the scum composition of pressurization iron removaling output is shown in Table 7.
Table 7
| Treating capacity | Ni, wt% | Cu, wt% | Co, wt% | Fe, wt% | S, wt% | |
| Vulcanize copper ashes | 457g | 4.87 | 42 | 0.1 | 17.1 | 20.9 |
| Cupric oxide calcining | 243g | 5.92 | 45.22 | 0.14 | 18.46 | 1.64 |
| Scum | 346g | 2.75 | 0.04 | 0.05 | 36.6 | 3.82 |
The total recovery of nickel can reach 97.0wt%, and the cobalt rate of recovery is 95.2wt%, copper recovery 94.8wt%.
Embodiment 6
Difference with embodiment 1 is：During two sections of normal pressure leachings, the mixing of one section of normal pressure leaching slag and cupric oxide
Thing, the weight ratio of sulfuric acid are 1:7, extraction temperature is 70 DEG C, extraction time 8h, and it is 1.8 to leach endpoint pH.
Copper sulfide slag ingredient, the cupric oxide calcining composition of copper sulfide slag oxidation calcining output of two sections of pressure leaching outputs,
And the scum composition of pressurization iron removaling output is shown in Table 8.
Table 8
The total recovery of nickel can reach 97.0wt%, and the cobalt rate of recovery is 95.2wt%, copper recovery 93.6wt%.
Embodiment 7
Difference with embodiment 1 is：The extraction temperature of one section of pressure leaching is 130 DEG C, and leaching pressure is 1.1MPa, leaching
It is 3h to go out the time.
Copper sulfide slag ingredient, the cupric oxide calcining composition of copper sulfide slag oxidation calcining output of two sections of pressure leaching outputs,
And the scum composition of pressurization iron removaling output is shown in Table 9.
Table 9
| Treating capacity | Ni, wt% | Cu, wt% | Co, wt% | Fe, wt% | S, wt% | |
| Vulcanize copper ashes | 457g | 5.7 | 38 | 0.1 | 15.4 | 18.2 |
| Cupric oxide calcining | 243g | 6.48 | 45.02 | 0.11 | 17.15 | 1.34 |
| Scum | 346g | 2.75 | 0.02 | 0.01 | 35.8 | 2.17 |
The total recovery of nickel can reach 95.0wt%, and the cobalt rate of recovery is 93.2wt%, copper recovery 91.0wt%.
Embodiment 8
Difference with embodiment 1 is：The extraction temperature of two sections of pressure leachings is 140 DEG C, and leaching pressure is 1.3MPa, leaching
It is 7h to go out the time.
Copper sulfide slag ingredient, the cupric oxide calcining composition of copper sulfide slag oxidation calcining output of two sections of pressure leaching outputs,
And the scum composition of pressurization iron removaling output is shown in Table 10.
Table 10
| Treating capacity | Ni, wt% | Cu, wt% | Co, wt% | Fe, wt% | S, wt% | |
| Vulcanize copper ashes | 457g | 5.30 | 40 | 0.1 | 15.5 | 18.5 |
| Cupric oxide calcining | 243g | 6.68 | 45.13 | 0.10 | 15.33 | 1.2 |
| Scum | 346g | 2.75 | 0.02 | 0.01 | 36.1 | 2.32 |
The total recovery of nickel can reach 94.3wt%, and the cobalt rate of recovery is 93.8wt%, copper recovery 92.6wt%.
Embodiment 9
Difference with embodiment 1 is：It is normal without one section of normal pressure leaching and two sections before one section of pressure leaching is carried out
Press leaching step.
Copper sulfide slag ingredient, the cupric oxide calcining composition of copper sulfide slag oxidation calcining output of two sections of pressure leaching outputs,
And the scum composition of pressurization iron removaling output is shown in Table 11.
Table 11
The total recovery of technological process nickel can reach 93.6wt%, cobalt rate of recovery 90.1wt%, copper recovery 92.0wt%.
Embodiment 10
Difference with embodiment 1 is：The step of normal pressure leaching liquid removes ferro element without pressurization.
The total recovery of technological process nickel can reach 92.6wt%, cobalt rate of recovery 93.2wt%, copper recovery 91.0wt%.
Comparative example 1
With being distinguished as embodiment 1：
Alloying converter mattes are subjected to normal pressure leaching processing processing and pressure leaching processing, obtain the normal of alloying converter mattes
Press the normal pressure leaching liquid of leachate and converter mattes.
In normal pressure leaching processing procedure, the weight ratio of sulfuric acid and alloying converter mattes is 25:1,85 DEG C of extraction temperature, leach
Time 9h, it is 2.0 to leach endpoint pH；
The total recovery of nickel is 80wt%, and the cobalt rate of recovery is 81.0wt%, copper recovery 85.6wt%.
As can be seen from the above description, the above embodiments of the present invention realize following technique effect：
Comparing embodiment 1 to 10 and comparative example 1 are understood, converter mattes are handled while offer using the application and alloying is high
Ice nickel is advantageous to improve the rate of recovery of nickel, cobalt and copper.
Comparing embodiment 1 to 10 understand, will be advantageous to from the preferable process conditions of the application further improve raising nickel,
The rate of recovery of cobalt and copper.
Comparing embodiment 1,5,6 is understood, the removal step of element sulphur is carried out before one section of pressure leaching, is advantageous to improve
Nickel, copper, the rate of recovery of cobalt element.
Comparing embodiment 1 and 9 is understood, after carrying out pressure treating steps to normal pressure leaching liquid, is advantageous to improve nickel, copper, cobalt
The rate of recovery of element.
Converter mattes and alloying Gao Bing can be handled using recovery method provided by the invention simultaneously in a technological process
Two kinds of materials of nickel, and above-mentioned technique can substantially reduce the reagent dosages such as the various soda acids of refining process, drop to the strong adaptability of material
The discharge capacity of low sulfur acid sodium waste water, production cost are low.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.Within the spirit and principles of the invention, that is made any repaiies
Change, equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (10)
1. a kind of nickel recovery method, it is characterised in that the recovery method includes：
Alloying converter mattes are subjected to normal pressure leaching, obtain normal pressure leaching liquid and normal pressure leaching slag, and to the normal pressure leaching liquid
Carry out first time nickel element recovery；And
The mixture of the normal pressure leaching slag and converter mattes is subjected to Selectively leaching, to carry out second of nickel element recovery.
2. recovery method according to claim 1, it is characterised in that the process of the normal pressure leaching includes：
In the presence of the first thermal medium and the first leaching agent, by the part of nickel element oxide in the alloying converter mattes be from
Son, obtain the normal pressure leaching liquid；
Preferably, during the normal pressure leaching, the weight ratios of first leaching agent and the alloying converter mattes for 20~
30:1, extraction temperature is 80~90 DEG C, and extraction time is 8~10h, and it is 2.0~2.5 to leach endpoint pH；
Preferably, first thermal medium is steam, and first leaching agent is sulfuric acid.
3. recovery method according to claim 1 or 2, it is characterised in that the process of the Selectively leaching includes：
In the presence of the second thermal medium and the second leaching agent, the mixture of the normal pressure leaching slag and the converter mattes is carried out
One section of pressure leaching, obtains first choice leachate and first choice leached mud；And
In the presence of the 3rd thermal medium and the 3rd leaching agent, the first choice leached mud is subjected to two sections of pressure leachings,
Obtain the second Selectively leaching liquid and the second selective leaching is slagged tap；
Preferably, during one section of pressure leaching, extraction temperature is 140~160 DEG C, and leaching pressure is 0.8~1.0MPa,
Extraction time is 4~6h；
Preferably, during two sections of pressure leachings, extraction temperature is 150~160 DEG C, and leaching pressure is 0.8~1.0MPa,
Extraction time is 4~6h；
Preferably, second thermal medium and the 3rd thermal medium are steam, second leaching agent and the 3rd leaching
It is sulfuric acid to go out agent.
4. recovery method according to claim 3, it is characterised in that second leaching agent is divided into Part I and
Two parts；The step of mixture of the normal pressure leaching slag and the converter mattes is carried out into one section of pressure leaching includes：
The normal pressure leaching slag is mixed with the converter mattes, obtains mixture；
After second leaching agent described in the mixture, Part I is mixed, one section of normal pressure leaching is carried out, obtains one section of normal pressure leaching
Go out liquid and one section of normal pressure leaching slag；
After second leaching agent described in one section of normal pressure leaching slag, Part II and sulphur-fixing agent are mixed, two sections of normal pressure leachings are carried out
Go out, obtain leaching ore pulp；And
Second thermal medium is passed through into the leaching ore pulp, one section of pressure leaching process is carried out, obtains described first
Selectively leaching liquid and the first choice leached mud.
5. recovery method according to claim 4, it is characterised in that during one section of normal pressure leaching, Part I
The weight ratio of second leaching agent and the mixture is 30~40:1, extraction temperature be 80~90 DEG C, extraction time be 6~
8h, it is 6.0~6.5 to leach endpoint pH；
Preferably, during two sections of normal pressure leachings, by the mixture of one section of normal pressure leaching slag and the sulphur-fixing agent
Weight is designated as n1, the weight of the second leaching agent described in Part II is designated as n2, n1/n2=1：8~10, extraction temperature 80~90
DEG C, 10~12h of extraction time, it is 1.0~1.5 to leach endpoint pH；
Preferably, the sulphur-fixing agent is cupric oxide.
6. the recovery method according to claim 4 or 5, it is characterised in that the recovery method also includes：With described first
Selectively leaching liquid is that raw material carries out the Selectively leaching process；
Preferably, in the first time nickel element removal process, the nickel element in the normal pressure leaching liquid is reclaimed using electrodeposition method；
In second of nickel element removal process, the nickel element in one section of normal pressure leaching liquid is reclaimed using electrodeposition method.
7. recovery method according to claim 6, it is characterised in that carrying out the removal process of the first time nickel element
Before, the step of recovery method also includes the normal pressure leaching liquid carrying out pressurization iron removaling；
Preferably, before second of nickel element removal process is carried out, the recovery method is also included described one section often
The step of pressure leachate carries out pressurization iron removaling.
8. recovery method according to claim 7, it is characterised in that it is described pressurization iron removaling the step of include：In the 4th heat
In the presence of medium, make the iron ion in the normal pressure leaching liquid and/or one section of normal pressure leaching liquid that hydrolysis occur, and
Separated out in the form of precipitation；The temperature of the pressurization iron removal is 180~190 DEG C, and pressure is 1.2~1.5MPa；Preferably,
4th thermal medium is steam.
9. recovery method according to claim 8, it is characterised in that the recovery method also includes：Remove pressurization iron removaling
The lead element and cobalt element in the normal pressure leaching liquid afterwards, and/or the first choice removed after pressurization iron removaling leach
Lead element and cobalt element in liquid.
10. recovery method according to claim 9, it is characterised in that cobalt member is removed using chemical precipitation method or extraction
Element, it is preferable that lead element is removed using chemical precipitation method or ion-exchange.
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| CN112646973A (en) * | 2020-12-09 | 2021-04-13 | 金川集团股份有限公司 | Method for selectively leaching laterite in three stages |
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| CN113584314A (en) * | 2021-07-29 | 2021-11-02 | 湖南中伟新能源科技有限公司 | High nickel matte normal pressure leaching method and nickel sulfate |
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| CN114959300B (en) * | 2022-05-27 | 2024-03-08 | 中国恩菲工程技术有限公司 | Method for comprehensively extracting nickel and copper from high nickel matte |
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