CN107058730A - A kind of method and its system comprehensively utilized to cu-ni sulphide ore - Google Patents
A kind of method and its system comprehensively utilized to cu-ni sulphide ore Download PDFInfo
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- CN107058730A CN107058730A CN201710228509.5A CN201710228509A CN107058730A CN 107058730 A CN107058730 A CN 107058730A CN 201710228509 A CN201710228509 A CN 201710228509A CN 107058730 A CN107058730 A CN 107058730A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0026—Pyrometallurgy
- C22B15/0028—Smelting or converting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0065—Leaching or slurrying
- C22B15/0067—Leaching or slurrying with acids or salts thereof
- C22B15/0071—Leaching or slurrying with acids or salts thereof containing sulfur
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
- C22B23/043—Sulfurated acids or salts thereof
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
- C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
- C22B3/3844—Phosphonic acid, e.g. H2P(O)(OH)2
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention provides a kind of method and its system comprehensively utilized to cu-ni sulphide ore.Methods described includes：1) low nickel matte obtained to cu-ni sulphide ore through matte smelting directly carries out normal pressure Selectively leaching using sulfuric acid, and hydrogen sulfide gas, leachate and leached mud are collected respectively, wherein, the temperature of the normal pressure Selectively leaching is 25 80 DEG C；2) to step 1) leachate carry out removing iron, collect remove liquid and iron dross removing after iron respectively, described to remove liquid after iron and be used for the extraction of nickel and cobalt, the iron dross removing is used to smelt iron；And/or, to step 1) leached mud send copper metallurgy industry to smelt, respectively obtain copper and noble metal.The depth proposed by the present invention that ambrose alloy can be realized to the method that cu-ni sulphide ore is comprehensively utilized is separated, and nickel, copper, cobalt and the noble metal rate of recovery are high, sulphur output in the form of high-purity sulphur, are easy to storage.Present invention process is simple, flow is short, energy consumption is small, cost is low, it is easy to large-scale industrial production.
Description
Technical field
The present invention relates to non-ferrous metallurgy technology field, cu-ni sulphide ore is comprehensively utilized more particularly, to a kind of
Method and its system.
Background technology
Nickel is a kind of important strategy metal, is widely used in national defence, Aero-Space, communications and transportation, petrochemical industry, the energy
Deng field.A considerable amount of nickel minerals are sulphide ores, are associated with copper, cobalt and noble metal (gold, silver and platinum group metal) etc., such as Gansu gold
River copper nickel and Yi 1. at Kalatongke, Xingjiang copper nickel.Therefore also need to consider time of cobalt and noble metal while nickel, copper is extracted
Receive.
The smelting process of traditional cu-ni sulphide ore is, by matte smelting, to make iron, nickel, cobalt and copper with sulfide shape first
Formula is enriched with and forms low nickel matte, and the noble metal of association is also enriched with；Then low nickel matte is bessemerized, by most iron
And sulphur is removed, converter mattes are formed.Cobalt is oxidized easily, therefore often causes the loss of substantial amounts of cobalt to enter in converting process
Enter the slag that blows, (sulfuric acid is because purposes and transportation radius asks while the sulfur dioxide of generation obtains industrial sulphuric acid by acid making system
Inscribe and largely accumulate).Afterwards, the processing method for the converter mattes that blowing is obtained is roughly divided into three classes.
One is, converter mattes carry out the floating separation of mill after slow cooling, respectively obtain low copper nickel sulfide concentrate, low nickel copper sulfide essence
Ore deposit and an alloy.Alloy also needs revulcanization-mill is floating to isolate corresponding low copper nickel sulfide concentrate, low nickel copper sulfide essence
Ore deposit and secondary alloy.Secondary alloy is used for the recovery of noble metal, and low copper nickel sulfide concentrate is used to extract nickel, but divides because mill is floating
From the impurity copper for thoroughly, not also needing to remove carrying subsequently, copper sulfide concentrate is used to carry copper, naturally also has nickel to be taken as impurity
The problem of band, cause smelting procedure quite cumbersome.
Second, converter mattes can be also broadly divided into using sour Selectively leaching technique：Low sour pressure leaching or peracid normal pressure leaching
Go out.Low sour pressure leaching is in the Fukang Smelter application of China.It is reported that Fukang Smelter is soaked using low sour two sections of adverse currents
Go out, be one section of normal pressure leaching (pH >=6.2 for finally giving leachate) first, next to that one section of pressure leaching (finally gives leaching
The pH for going out liquid is 1.8-2.8, oxygen pressure 0.05-0.06MPa).By the sulphur that Cu, Fe≤0.01g/L are obtained after two sections of counterflow leachings
Sour nickel solution, and the cobalt of copper, noble metal, iron and sulphur almost all and 40% in raw material or so stays in nickeliferous 2%-3%'s
In finishing slag.And peracid normal pressure leaching is most early in the loose refinery's application of Christian, the hydrochloric acid (275g/ of the technique high concentration
L leaching agent) is made, the nickeliferous about 120g/L of obtained leaching rich solution, hydrochloric acid 160g/L, also each 2g/L of iron, cobalt, copper.About 3%
Copper is leached, and is largely stayed in slag.Then after solvent extraction and separation iron cobalt copper, evaporating, concentrating and crystallizing nickel chloride product.
Side etc. have studied the dynamics of converter mattes sulfuric acid leaching to Peng less, and also refer to using two grades of reverse leachings of batch (-type) reducing leaching
Copper concentration in liquid.And the Main Ingredients and Appearance Ni of converter mattes2S3With acid reaction during, easily generation is difficult at a lower temperature
β-NiS phases are handled, therefore the peracid normal pressure decomposition technique of converter mattes needs effectively to carry out in the case where temperature is higher than 90 DEG C.
Third, the smelting process of converter mattes also can the leaching of hyperbaric oxygen ammonia.This method is by controlling the free ammonia in solution to contain
Amount and oxygen pressure, make Cu, Ni and Co be changed into Metal amine complex and dissolve, while sulphur is oxidized to sulfate radical, noble metal and iron
Forming slag phase is used to reclaim.Free ammonia control is even more important in leaching process, and concentration is low to cause leaching rate low, excessive concentration meeting again
Formed cobalt high ammino-complex, because its is insoluble and caused by cobalt loss.
Three of the above technical thought can effectively handle converter mattes.But problem is the process that converter mattes are blown into by low nickel matte
Central, substantial amounts of cobalt is entered in blowing slag, and primary recovery is low.In addition, because flow is tediously long, about losing 10% platinum family gold
Category.To reclaim the cobalt lost in blowing slag, someone will blow slag again through pyrogenic attack, the cobalt of loss is reclaimed by reduction melting,
Reduzate main component is the alloy and sulfide of iron-cobalt-nickel, as cobalt ice nickel.But it is due to that cobalt is easily oxidized, content
It is low, excessively disperse in blowing slag, even if by reduction melting, the cobalt of a part can only be reclaimed.In addition, this cobalt ice nickel
Leaching is extremely complex, need to be through three stages acid leach, and first paragraph is mainly the leaching of alloy, in order to prevent the leaching of nickel cobalt, it is necessary in leaching
Hydrogen sulfide is passed through during going out or after leaching or vulcanized sodium is added, the leached mud then formed needs two sections of leachings to obtain again
To cobalt-carrying solution.So, substantial amounts of iron moves in circles in sulphur phase-slag phase, and recovery process is also very cumbersome.
Generally speaking, low nickel matte is blown into converter mattes, though the recovery of cupro-nickel is preferably solved the problems, such as, in association cobalt
And there are serious problems in terms of noble metal recovery.And sulphur is the problem of output is also troubling in the form of sulfuric acid.
Directly processing low nickel matte can avoid the valuable element loss of association such as cobalt and noble metal in above-mentioned converting process
Problem.But the method for existing processing low nickel matte still has inconvenience when reclaiming associated valuable metals.Sulphation such as low nickel matte is roasted
Burning can make nickel cobalt copper be converted into water miscible sulfate, and iron is converted into water-insoluble oxide, and the sulfur dioxide of generation is still used for
Relieving haperacidity.But the platinum group metal of association is retained in scum, special flow is needed to extract again.Low nickel matte can also pass through oxygen pressure
Acidleach is handled, such as Yin Fei and Deng Zhilin etc. has made detailed research.This oxygen leaching is generally required in autoclave
Carry out, but the sulphur of oxidation generation can form retardation film, influence the further leaching of low nickel matte.In addition oxygen leaching can also be generated
A large amount of water-insoluble iron oxide precipitations, noble metal is mingled with it to be caused to reclaim difficult.Although sulphur be transformed into during oxygen leaching
Sulphur, but due to together with being mingled with scum and noble metal, it is still necessary to which further oxidation is to reclaim noble metal.
Generally speaking, existing direct processing low nickel matte has pyrogenic process and the class technique of wet method two.Pyrogenic process can use sulfating roasting,
Then reselection leaches valuable element, and iron oxide is stayed in leached mud, but the noble metal in scum reclaims difficult；Many people are blue or green
Look at wet method, wet method typically uses oxygen leaching, it is necessary to using autoclave and pure oxygen, but equally faces your gold is reclaimed from scum
The problem of category, and sulphur is oxidized to sulphur formation parcel during acid oxygen leaching, and noble metal reclaims the difficulty that remains unchanged.
The content of the invention
(1) technical problem to be solved
The technical problem to be solved in the present invention is can not effectively to reclaim the cobalt of association in existing cu-ni sulphide ore processing method
And noble metal.
(2) technical scheme
In order to solve the above-mentioned technical problem, the invention provides a kind of method comprehensively utilized to cu-ni sulphide ore, including：
1) low nickel matte obtained to cu-ni sulphide ore through matte smelting directly carries out normal pressure Selectively leaching using sulfuric acid, point
Not Shou Ji hydrogen sulfide gas, leachate and leached mud, wherein, the temperature of normal pressure Selectively leaching is 25-80 DEG C；
2) to step 1) leachate carry out remove iron, respectively collect remove iron after liquid and iron dross removing, except after iron liquid be used for nickel and
The extraction of cobalt, iron dross removing is used to smelt iron；
And/or, to step 1) leached mud send copper metallurgy industry to smelt, respectively obtain copper and noble metal.
In the present invention, directly processing cu-ni sulphide ore can avoid low nickel matte through the low nickel matte obtained by matte smelting after
In sequence tradition converting process technique the problem of the association such as cobalt and noble metal valuable element loss.
Use sulfuric acid direct to low nickel matte carries out normal pressure Selectively leaching, and under the concentration and liquid-solid ratio, ferronickel is dissolved in
In sulfuric acid solution, and reaction generation hydrogen sulfide gas completely, now, cuprous sulfide and noble metal are hardly decomposed in low nickel matte,
The depth separation of ambrose alloy can be realized in leaching process.
Copper is the element of very close sulphur, Cu2S solubility product very little, only 10-48.And iron-cobalt-nickel is remote not to the compatibility of sulphur
And copper, ferrous sulfide (FeS), nickel sulfide (α-NiS), the solubility product of cobalt sulfide (CoS) they are respectively 10-18、10-18With 10-21.Cause
As long as this is expected that solution has suitable acidity, it is likely that allow the sulfide of iron-cobalt-nickel to be decomposed and realize leaching, sulphur turns
Become hydrogen sulfide and be volatized into gas phase, cuprous sulfide does not leach and solid phase is stayed in together with noble metal.Sulphur is raw during acidleach
Into H2S volatilize, separated with leached mud, no longer disturb noble metal reclaim, can also special disposal reclaim high-quality solid sulphur.
In addition, in the method for the invention, eliminating the converting process to low nickel matte in common methods, effectively prevent
The loss of the cobalt caused in converting process.Meanwhile, copper and noble metal are effectively stayed in into leached mud using above-mentioned leaching step, then
Send copper metallurgy industry to smelt the leached mud, now noble metal moves towards single, can effectively reclaim, improve companion in cu-ni sulphide ore
Raw cobalt and the platinum group metal rate of recovery.
For the problem of outlet of the sulphur that solves long-standing problem nickel sulfide ore enterprise, the present invention is by low nickel matte in sulfuric acid leaching mistake
Hydrogen sulfide gas produced by journey is used to prepare sulphur, is more easy to compared with situation of the sulphur in conventional method to the sulfuric acid prepared
In storage and transport.
Low nickel matte is mainly derived from cupro-nickel vulcanised ore concentrate, and main component is Ni5Fe4S8, in addition to nickel simultaneously rich in copper, cobalt and
A large amount of platinum families need to reclaim, in a preferred embodiment of the invention, and low nickel matte is that cu-ni sulphide ore is made through matte smelting,
I.e. method of the invention is more suitable for decomposition and extraction of the cu-ni sulphide ore through low nickel matte made from matte smelting.
At 25-80 DEG C, it is anti-that double decomposition occurs in sulfuric acid solution through low nickel matte made from matte smelting for cu-ni sulphide ore
Should, ferronickel cobalt is dissolved in water, and generates hydrogen sulfide gas, and reaction is very thorough, meanwhile, under the sulfuric acid of the temperature, low nickel matte
In cuprous sulfide hardly decompose, can be realized in leaching process cupro-nickel depth separation, improve the rate of recovery, broken with live
The situation of effective extraction of each element in mineral could be realized in work using more than 90 DEG C of high temperature, the energy has been saved, has also dropped
The risk that low operating personnel may receive.
In a preferred embodiment of the invention, those skilled in the art can select leaching according to actual needs
After step, leachate is carried out except iron send copper metallurgy industry to smelt or both carried out removing iron or right to leachate to leached mud
Leached mud send copper metallurgy industry to smelt, and is preferably, both leachate is carried out to remove iron, for reclaiming nickel, cobalt and/or iron,
Copper metallurgy industry is sent to smelt leached mud, for reclaiming copper and noble metal.
, can be by the titanium dioxide generated in matte smelting for the problem of outlet of the sulphur that solves long-standing problem nickel sulfide ore enterprise
The reaction completely of the sulphur hydrogen sulfide gas produced during sulfuric acid leaching with low nickel matte prepares sulphur, is readily transported and stores up
Deposit, and will remaining sulfur dioxide import sulfate system in be converted into above-mentioned steps 1) in carry out normal pressure Selectively leaching used
Sulfuric acid.Wherein, the sulfur dioxide consumption that sulphur is made is 1/2nd of hydrogen sulfide mole.
In order that step 1) in leaching it is more complete so that ambrose alloy is kept completely separate, in a preferred embodiment
In, step 1) in sulfuric acid concentration be 1mol/L-6mol/L, the temperature of normal pressure Selectively leaching is 25-80 DEG C, normal pressure selective leaching
Go out the time for 0.5-5h.
More preferably, step 1) in sulfuric acid concentration be 3mol/L-4mol/L, the normal pressure Selectively leaching time be 0.5-
2h, extraction temperature is 50-70 DEG C, and liquid-solid ratio is 5:1-10:1.
In the present invention, can be to step 1) leachate carry out removing iron using method for removing iron commonly used in the art, be
Except iron and the rate of recovery of nickel cobalt preferably can not be influenceed, in a preferred embodiment of the invention, it is preferred to use pin iron
Ore deposit method or hematite process.
Step 1 in the present invention) leachate in solution copper content be less than 0.008g/L, preferably smaller than 0.003g/L, this
When, iron mainly in ferrous ion form exist, without again through reduction can direct oxidation formed goethite remove, i.e., it is excellent at one
Select in embodiment, the pH of leachate can be adjusted to 3-7, then pass to the gas rich in oxygen, obtain except liquid after iron and remove
Scum.
Specifically can be by step 1) in the pH of leachate be adjusted to 4-7, be placed in enclosed high pressure kettle, logical pure oxygen is simultaneously warming up to 220
DEG C, iron is removed in bloodstone form, obtains removing liquid and iron dross removing after iron.
Can also be to step 1) in leachate be passed through air or oxygen-enriched air, while maintain solution pH be 3-4, you can will
Iron is removed as goethite, obtains removing liquid and iron dross removing after iron.
Obtained scum can be fired into iron ore concentrate, for smelting iron.
Obtain removing liquid after iron after iron when removing leachate, method commonly used in the art can be used to realize carrying for nickel and cobalt
Take, in order to fully achieve the extraction of nickel and cobalt in the present invention, in a preferred embodiment, the pH except liquid after iron is adjusted to
4.0-5.5 is removed backward adds extractant in liquid after iron, extract and separate obtains cobalt-carrying solution and solution containing nickel, then by solution containing nickel
PH is adjusted to the extraction that 5.5-7.0 carries out nickel using extractant；
Wherein, the extractant is P507 kerosin or Cyanex272 kerosin, and volume fraction is 10-
50%.In above-mentioned extractant, kerosene is diluent.
Wherein, P507 is di-2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester, and Cyanex272 is two (2,4,4- trimethyls penta
Base) hypophosphorous acid.
When extractant is P507 kerosin, the pH except liquid after iron is adjusted to 4.0-5.0, then add in liquid to after except iron
Enter extractant, extract cobalt with extractant, extract and separate obtains cobalt-carrying solution and solution containing nickel, then the pH of solution containing nickel is adjusted to
5.5-6.5, uses extractant extraction of nickel, hydrochloric acid back extraction obtains nickel chloride solution, for preparing nickel product.Wherein, by cobalt-carrying solution
Cobalt chloride solution is obtained with hydrochloric acid back extraction, for preparing cobalt product.
When extractant is Cyanex272 kerosin, the pH except liquid after iron is adjusted to 5.0-5.5, then to after except iron
Extractant is added in liquid, extract and separate obtains cobalt-carrying solution and solution containing nickel, then the pH of solution containing nickel is adjusted into 6.5-7.0, used
Extractant extraction of nickel, sulfuric acid back extraction obtains nickel sulfate solution, for preparing nickel sulfate product.Wherein, by cobalt-carrying solution sulfuric acid
Back extraction obtains cobalt sulfate solution, for preparing cobaltous sulfate product.
In a preferred embodiment of the invention, copper can be obtained and expensive using Copper making method conventional in the art
Metal, in order that copper and noble metal are kept completely separate, in a preferred embodiment of the invention, the extracting method of copper and noble metal
Preferably：
By step 1) leached mud respectively obtain refined copper and enriching noble metals through bessemerizing obtained blister copper, then through electrolysis
The earth of positive pole, the earth of positive pole of enriching noble metals is used to extract noble metal.
Or, by step 1) the oxidized roasting of leached mud after use Ore Leaching, the leachate and richness of enriching Cu are collected respectively
Collect the leached mud of noble metal, the leached mud of enriching noble metals is used to extract noble metal.
Or, by step 1) leached mud carry out oxygen leaching, respectively collect the leachate and enriching noble metals of enriching Cu
Leached mud, the leached mud of enriching noble metals is used to extract noble metal.
The leaching rate of nickel, iron, cobalt is more than 99% obtained by the method for the present invention, and cobalt and noble metal have been obtained effectively
Reclaim, the rate of recovery of copper is up to more than 98%, and the rate of recovery of noble metal is up to more than 95%.
According to a further aspect of the present invention, a kind of system comprehensively utilized to cu-ni sulphide ore is additionally provided, including：
Normal pressure Selectively leaching device, for carrying out normal pressure Selectively leaching to the direct use sulfuric acid of low nickel matte, is received respectively
Collect hydrogen sulfide gas, leachate and leached mud；
Deironing apparatus, the leachate for will be obtained in normal pressure Selectively leaching device carries out removing iron；
The extraction element of nickel and cobalt, liquid, the extraction for nickel and cobalt after iron are removed for collecting in deironing apparatus；
Iron-smelting device, for handling the iron dross removing in deironing apparatus, for smelting iron；
And/or, Copper making device, the leached mud for will be obtained in normal pressure Selectively leaching device carries out Copper making, point
Copper and noble metal are not obtained.
After leaching, Copper making device can be set according to actual needs.
Also include within the system：
Matte smelting device, for providing low nickel matte into normal pressure Selectively leaching device, wherein, low nickel matte is cupro-nickel sulphur
Change ore deposit to be made through matte smelting；
Sulphur preparation facilities, for the sulfur dioxide that makes to produce in matte smelting device with normal pressure Selectively leaching device
Produce hydrogen sulfide gas reaction completely and sulphur is made；
Sulfuric acid preparation facilities, for the remaining sulfur dioxide produced in matte smelting device to be converted into sulfuric acid, and by its
It is supplied to the normal pressure Selectively leaching device.
Also include temperature control device in the normal pressure Selectively leaching device, for by the temperature of normal pressure Selectively leaching
Control is at 25-80 DEG C, so as to improve the comprehensive utilization to cu-ni sulphide ore.
The method of the present invention preferably uses the system of the present invention to realize.
The method and its system of cu-ni sulphide ore comprehensive utilization proposed by the present invention are to cu-ni sulphide ore through matte smelting institute
Low nickel matte carries out at 25-80 DEG C nickel, cobalt and iron in normal pressure Selectively leaching, low nickel matte directly with sulfuric acid by sour decomposition
Enter solution afterwards, leachate is through except the extraction of nickel, cobalt is used for after iron, iron dross removing is used to smelt iron；Copper in low nickel matte is to vulcanize Asia
Copper form is retained in leached mud together with noble metal, enters Copper making, reclaims copper and noble metal.This method flow is short, efficiency high, no
The depth separation of ambrose alloy can be only realized, the rate of recovery for greatly improving cobalt and noble metal is also helped, is a kind of clean and effective
Element comprehensive utilization process, it is easy to large-scale industrial production.
Brief description of the drawings
Fig. 1 is according to the schematic flow sheet comprehensively utilized in the embodiment of the present invention 1 to cu-ni sulphide ore.
Embodiment
With reference to the accompanying drawings and examples, the embodiment to the present invention is described in further detail.Implement below
Example is used to illustrate the present invention, but is not limited to the scope of the present invention.
Embodiment 1
As shown in figure 1, in the present embodiment, cu-ni sulphide ore obtains low nickel matte, essential element content after matte smelting：Ni
20.21%, Cu 10.52%, Fe 37.44%, Co 0.78%, noble metal about 10g/t.
As raw material, using 4mol/L sulfuric acid solution normal pressure leaching, liquid-solid ratio is 10：1,80 DEG C of reaction temperature, instead
Answer 0.5h.Iron, cobalt, nickel are leached into solution in low nickel matte, and almost all copper and concentration of precious metal are in the leaching of cuprous sulfide
In slag, the separation of copper and nickel cobalt is realized.Filter copper content in resulting solution and be less than 0.005g/L, iron is in mainly ferrous ion
Form is present, and without direct blowing air is aoxidized through reduction again, while maintaining pH value of solution in 3-5, makes iron heavy with goethite
Form sediment and remove, gained scum is fired into iron ore concentrate, available for smelting iron.Except liquid adjusts pH to 4 after iron, cobalt is extracted with P507, hydrochloric acid is used
Back extraction obtains cobalt chloride solution, for preparing cobalt product.PH value of solution is adjusted again to 5.5, P507 extraction of nickel is used, and hydrochloric acid back extraction is obtained
Nickel chloride solution, for preparing nickel product.
Solid phase filter residue is the cuprous sulfide for being enriched noble metal, and main component is：Ni 0.45%, Cu 75.2%, Fe
0.78%, Co ＜ 0.01%, noble metal about 70g/t (leaching rate of equivalent ferronickel cobalt is more than 99%), are directly bessemerized
Blister copper is prepared, blister copper obtains refined copper through electrorefining again, and noble metal is then enriched in the earth of positive pole, send noble metal systems to reclaim, its
In, the rate of recovery of copper is up to more than 98%, and the rate of recovery of noble metal is up to more than 95%.A part of titanium dioxide of matte smelting process
Sulphur prepares sulphur with hydrogen sulfide reaction, and its consumption is 1/2nd of hydrogen sulfide mole；Remaining sulfur dioxide send sulfuric acid system
System extracting sulfuric acid, is used as the leaching agent for decomposing low nickel matte.
Embodiment 2
Cu-ni sulphide ore obtains low nickel matte, essential element content after matte smelting：Ni 13.25%, Cu 8.32%, Fe
38.44%, Co 0.64%.
As raw material, using 6mol/L sulfuric acid solution normal pressure leaching, liquid-solid ratio is 2：1,65 DEG C of reaction temperature, reaction
1h.Iron, cobalt, nickel almost all are leached into solution in low nickel matte, and copper segregation realizes the separation of copper and nickel cobalt in slag.
Filter copper content in resulting solution and be less than 0.006g/L, iron mainly exists in ferrous ion form, and adjustment pH value of solution is 5-7,
It is subsequently placed in enclosed high pressure kettle, logical pure oxygen is simultaneously warming up to 180 DEG C, by iron with the removing of bloodstone form.Except liquid adjusts pH after iron
To 5, cobalt is extracted with P507, cobalt chloride solution is obtained with hydrochloric acid back extraction, for preparing cobalt product.PH value of solution is adjusted again to 6.5, is used
P507 extraction of nickel, hydrochloric acid back extraction obtains nickel chloride solution, for preparing nickel product.
Solid phase filter residue is copper concentrate, and main component is：Ni 0.15%, Cu 73.2%, Fe 0.85%, Co ＜ 0.008%
(leaching rate of equivalent ferronickel cobalt is more than 99%), uses sulfuric acid leaching, obtains copper-bath and leaching after oxidized roasting
Slag, wherein, the rate of recovery of copper is up to more than 98%.Copper-bath is used for copper processed.A part of titanium dioxide of matte smelting process
Sulphur prepares sulphur with hydrogen sulfide reaction, and its consumption is 1/2nd of hydrogen sulfide mole；Remaining sulfur dioxide send sulfuric acid system
System extracting sulfuric acid, is used as the leaching agent for decomposing low nickel matte.
Embodiment 3
Cu-ni sulphide ore obtains low nickel matte, essential element content after matte smelting：Ni 16.55%, Cu 10.32%,
Fe 33.44%, Co 0.34%, about 8.9 grams of tons of noble metal.
As raw material, using 1mol/L sulfuric acid solution normal pressure leaching, liquid-solid ratio is 20：1,25 DEG C of reaction temperature, instead
Answer 5h.Iron, cobalt, nickel almost all are leached into solution in low nickel matte, and copper and concentration of precious metal realize copper and nickel in slag
The separation of cobalt.Filter copper content in resulting solution and be less than 0.008g/L, iron mainly exists in ferrous ion form, without passing through again
Reduction, the oxygen-enriched air that 30%-60% can be directly led at ambient pressure is aoxidized, and maintains pH value of solution in 4-6, makes iron with pin iron
Ore deposit precipitation is removed, and gained scum is fired into iron ore concentrate, available for smelting iron.Except liquid after iron, pH to 5.0 is adjusted, is extracted with Cyanex272
Cobalt is taken, cobalt sulfate solution is obtained with sulfuric acid back extraction, for preparing cobaltous sulfate product；Then adjustment pH value of solution is to 6.5, then uses
Cyanex272 extraction of nickel, sulfuric acid back extraction obtains nickel sulfate solution, for preparing nickel sulfate product.
Solid phase filter residue is the copper concentrate for being enriched noble metal, and main component is：Ni 0.16%, Cu76.2%, Fe
0.65%, Co ＜ 0.01% (leaching rate of equivalent ferronickel cobalt is more than 99%), about 65 grams of tons of noble metal.Using autoclave oxygen
Pressure is leached, and obtaining copper-containing solution is used for copper processed, and leached mud is then used to reclaim noble metal, wherein, the rate of recovery of copper up to 98% with
On, the rate of recovery of noble metal is up to more than 95%.A part of sulfur dioxide of matte smelting process prepares sulphur with hydrogen sulfide reaction,
Its consumption is 1/2nd of hydrogen sulfide mole；Remaining sulfur dioxide send sulfate system extracting sulfuric acid, is used as the low ice of decomposition
The leaching agent of nickel.
Embodiment 4
Cu-ni sulphide ore obtains low nickel matte, essential element content after matte smelting：Ni 12.55%, Cu 8.32%, Fe
39.44%, Co 0.24%, about 7.5 grams of tons of noble metal.
As raw material, using 3mol/L sulfuric acid solution normal pressure leaching, liquid-solid ratio is 5：1,50 DEG C of reaction temperature, reaction
2h.Iron, cobalt, nickel almost all are leached into solution in low nickel matte, and copper and concentration of precious metal realize copper and nickel cobalt in slag
Separation.
Filter copper content in resulting solution and be less than 0.003g/L, iron mainly exists in ferrous ion form, adjusts solution
PH is subsequently placed in enclosed high pressure kettle in 4-6, and logical pure oxygen is simultaneously warming up to 220 DEG C, by iron with the removing of bloodstone form.After iron
Liquid, adjusts pH to 5.5, and cobalt is extracted with Cyanex272, cobalt sulfate solution is obtained with sulfuric acid back extraction, for preparing cobaltous sulfate product；
Then adjustment pH value of solution is to 7.0, then uses Cyanex272 extraction of nickel, and sulfuric acid back extraction obtains nickel sulfate solution, for preparing nickel sulfate
Product.
Solid phase filter residue is the copper concentrate for being enriched noble metal, and main component is：Ni 0.12%, Cu 72.8%, Fe
0.45%, Co ＜ 0.005% (leaching rate of equivalent ferronickel cobalt is more than 99%), about 68 grams of tons of noble metal.Using autoclave
Oxygen leaching, obtaining copper-containing solution is used for copper processed, and leached mud is then used to reclaim noble metal, wherein, the rate of recovery of copper is up to 98%
More than, the rate of recovery of noble metal is up to more than 95%.A part of sulfur dioxide of matte smelting process prepares sulphur with hydrogen sulfide reaction
Sulphur, its consumption is 1/2nd of hydrogen sulfide mole；Remaining sulfur dioxide send sulfate system extracting sulfuric acid, low as decomposing
The leaching agent of ice nickel.
Finally, method of the invention is only preferably embodiment, is not intended to limit the scope of the present invention.It is all
Within the spirit and principles in the present invention, any modification, equivalent substitution and improvements made etc. should be included in the protection of the present invention
Within the scope of.
Claims (10)
1. a kind of method comprehensively utilized to cu-ni sulphide ore, including：
1) low nickel matte obtained to cu-ni sulphide ore through matte smelting directly carries out normal pressure Selectively leaching using sulfuric acid, receives respectively
Collect hydrogen sulfide gas, leachate and leached mud, wherein, the temperature of the normal pressure Selectively leaching is 25-80 DEG C；
2) to step 1) leachate carry out remove iron, respectively collect remove iron after liquid and iron dross removing, it is described remove iron after liquid be used for nickel and
The extraction of cobalt, the iron dross removing is used to smelt iron；
And/or, to step 1) leached mud send copper metallurgy industry to smelt, respectively obtain copper and noble metal.
2. according to the method described in claim 1, it is characterised in that the sulfur dioxide produced in the matte smelting and step 1)
In stink damp precursor reactant prepare sulphur, and remaining sulfur dioxide is converted into step 1) in carry out normal pressure Selectively leaching
Used sulfuric acid.
3. method according to claim 1 or 2, it is characterised in that the step 1) described in sulfuric acid concentration be 1mol/L-
6mol/L, the liquid-solid ratio of normal pressure Selectively leaching is 2:1-20:1, the normal pressure Selectively leaching time is 0.5-5h.
4. method according to claim 3, it is characterised in that the step 1) in sulfuric acid concentration be 3mol/L-4mol/L,
The normal pressure Selectively leaching time is 0.5-2h, and extraction temperature is 50-70 DEG C, and liquid-solid ratio is 5:1-10:1.
5. the method according to any one of claim 1-4, it is characterised in that the step 2) in step 1) in leach
Liquid is carried out except iron is specially：
Leachate pH to 3-7 is adjusted, the gas rich in oxygen is then passed to, obtains removing liquid and iron dross removing after iron.
6. the method according to any one of claim 1-5, it is characterised in that the step 2) described in remove liquid after iron and use
It is specially in the extraction of nickel and cobalt：
Liquid pH after iron will be removed to be adjusted to after 4.0-5.5, extractant is added in liquid to after except iron, extract and separate obtains cobalt-carrying solution and contained
Nickel solution, then the pH of solution containing nickel is adjusted to the extraction that 5.5-7.0 carries out nickel using the extractant；
Wherein, the extractant is P507 kerosin or Cyanex272 kerosin, and volume fraction is 10-50%.
7. the method according to any one of claim 1-6, it is characterised in that the extracting method tool of the copper and noble metal
Body is：
By step 1) leached mud through bessemerizing obtained blister copper, then respectively obtain through electrolysis the anode of refined copper and enriching noble metals
Mud, the earth of positive pole of enriching noble metals is used to extract noble metal；
Or, by step 1) the oxidized roasting of leached mud after use Ore Leaching, the leachate of enriching Cu is collected respectively and is enriched with expensive
The leached mud of metal, the leached mud of enriching noble metals is used to extract noble metal；
Or, by step 1) leached mud carry out oxygen leaching, the leaching of the leachate and enriching noble metals of enriching Cu is collected respectively
Slag, the leached mud of enriching noble metals is used to extract noble metal.
8. a kind of system comprehensively utilized to cu-ni sulphide ore, including：
Normal pressure Selectively leaching device, for carrying out normal pressure Selectively leaching to the direct use sulfuric acid of low nickel matte, collects sulphur respectively
Change hydrogen, leachate and leached mud；
Deironing apparatus, the leachate for will be obtained in normal pressure Selectively leaching device carries out removing iron；
The extraction element of nickel and cobalt, liquid, the extraction for nickel and cobalt after iron are removed for collecting in deironing apparatus；
Iron-smelting device, for handling the iron dross removing in deironing apparatus, for smelting iron；
And/or, Copper making device, the leached mud for will be obtained in normal pressure Selectively leaching device carries out Copper making, respectively
To copper and noble metal.
9. system according to claim 8, it is characterised in that also include：
Matte smelting device, provides low nickel matte, institute for handling cu-ni sulphide ore, and into the normal pressure Selectively leaching device
Low nickel matte is stated to be made through matte smelting for cu-ni sulphide ore；
Sulphur preparation facilities, sulfur dioxide and the normal pressure Selectively leaching for making to produce in the matte smelting device are filled
Put middle generation stink damp precursor reactant and sulphur is made；
Sulfuric acid preparation facilities, for the part sulfur dioxide produced in the matte smelting device to be converted into sulfuric acid, and by its
It is supplied to the normal pressure Selectively leaching device.
10. system according to claim 8 or claim 9, it is characterised in that also include temperature in the normal pressure Selectively leaching device
Spend regulation device, for by the temperature control of the normal pressure Selectively leaching at 25-80 DEG C.
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| CN201710228509.5A CN107058730B (en) | 2017-04-10 | 2017-04-10 | A kind of method and its system to cu-ni sulphide ore comprehensive utilization |
| CA3049827A CA3049827C (en) | 2017-04-10 | 2018-04-08 | Method and system for comprehensive recovery and utilization of copper-nickel sulfide ore |
| AU2018252056A AU2018252056B2 (en) | 2017-04-10 | 2018-04-08 | Method for comprehensively recycling copper-nickel sulfide ore and system thereof |
| FI20195705A FI20195705A1 (en) | 2017-04-10 | 2018-04-08 | Method for comprehensively recycling copper-nickel sulfide ore and system thereof |
| RU2019121486A RU2741429C1 (en) | 2017-04-10 | 2018-04-08 | Method and system for complete reprocessing of copper-nickel sulphide ore |
| PCT/CN2018/082209 WO2018188537A1 (en) | 2017-04-10 | 2018-04-08 | Method for comprehensively recycling copper-nickel sulfide ore and system thereof |
| ZA201904337A ZA201904337B (en) | 2017-04-10 | 2019-07-01 | Method for comprehensively recycling copper-nickel sulfide ore and system thereof |
| US16/529,729 US11459636B2 (en) | 2017-04-10 | 2019-08-01 | Method and system for comprehensive recovery and utilization of copper-nickel sulfide ore |
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