CN108441649A - A kind of method of chemical precipitation nickel sulfide material extraction nickel - Google Patents
A kind of method of chemical precipitation nickel sulfide material extraction nickel Download PDFInfo
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- CN108441649A CN108441649A CN201810260145.3A CN201810260145A CN108441649A CN 108441649 A CN108441649 A CN 108441649A CN 201810260145 A CN201810260145 A CN 201810260145A CN 108441649 A CN108441649 A CN 108441649A
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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
- C22B23/0423—Halogenated 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
- 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
- C22B3/04—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
- 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
- C22B3/10—Hydrochloric acid, other halogenated 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
- C22B3/3846—Phosphoric acid, e.g. (O)P(OH)3
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
A kind of method of chemical precipitation nickel sulfide material extraction nickel.In alkalescent system, the nickel sulfide in nickel sulfide material slurry generates nickel chloride with sodium hypochlorite reaction；And the nickel hydroxide that the nickel sulfate in nickel sulfide material slurry generates generates nickelic hydroxide with sodium hypochlorite reaction, nickelic hydroxide has the oxidation effectiveness that strong oxidation performance accelerates nickel sulfide；Ore pulp is molten through sulfuric acid or hydrochloric acid acid after the completion of alkaline oxygenated, and unreacted is completely vulcanized to material and nickelic hydroxide and is reacted leaching nickel；Leachate obtains high-purity sulphuric acid nickel solution after chemistry and abstraction impurity removal, and nickel sulfate product can be obtained by evaporative crystallization after oil removing or be sent to electrolytic nickel.The method of the present invention is generated without the pernicious gases such as sulfur dioxide and hydrogen sulfide gas, is more advantageous to environmental protection and production operation, and low cost, low stain, comprehensive reutilization effect are good.
Description
Technical field
The present invention relates to non-ferrous metal technical field of wet metallurgy, the nickel sulfide material of specially a kind of chemical precipitation extracts
The method of nickel.
Background technology
Nickel metal has the performances such as excellent energy storage, anti-corrosion, wear-resisting, high temperature resistant and high intensity, is widely used, has become
The grand strategy goods and materials of the national economic development.But China belongs to nickel ore resource and compares one of country of shortage, mostly by into
Mouthful.Nickel sulfide material is exactly one such, it is mainly derived from low grade nickel ore or the leachate of nickel secondary resource recycling is logical
Cross addition vulcanizing agent enriching nickel, precipitation gained metal sulfide.
Currently, some enterprises are roasted the nickel sulfide material for precipitating gained using pyrogenic process, sintering oxidation nickel is obtained, subsequently again
Reduction ammonia-leaching or acidleach are carried out, can be obtained nickel Related product through processing after leachate removal of impurities.There are high energy consumption, streams for this method
Journey is long, of high cost and process has the pernicious gases such as hydrogen sulfide, sulfur dioxide to generate needs mating related environmental protection equipment, enterprise competitiveness
It is smaller.
《China YouSe is metallurgical》3rd phase in 1984 is entitled, and " AMAX chlorides refine method and are recycled from mixed sulphide precipitation
Nickel and cobalt ", which is pointed out to pre-process nickel sulfide material by hydrogen reduction, dead roast or matte smelting, converts sulphur therein to vulcanization
Then pretreated material is carried out salt Ore Leaching, follow-up mating related purification and impurity removal process, refining by hydrogen or sulfur dioxide again
After product nickel can be obtained.Not only energy consumption is larger for such method, long flow path, equipment are more and the technical process control parameter is more, ring
The shortcomings of packing pressure is big, it is difficult to realize enterprise getting profit.
101899568 B of patent announcement CN disclose a kind of nickel sulfide pure oxygen producing electrolytic nickel by leaching of chemical precipitation
Method carry out electricity after one section of leachate removal of impurities by the nickel sulfide of chemical precipitation and sulfuric acid solution through one section of oxygen normal pressure leaching
Solution produces electrolytic nickel and anolyte；One section is leached filter residue and mixes two sections of hyperbaric oxygen leachings of progress after secondary pulp with anolyte, is leached
Obtained leaching filtrate is returned to be used into a pulp；Have that low energy consumption, metal recovery rate height etc. relative to the traditional handicraft technique
Advantage, but there are equipment investments it is high, technical operation is complicated, high to personnel qualifications the shortcomings of, while first segment normal pressure sulfuric acid
Leaching, which will produce a certain amount of hydrogen sulfide gas, needs mating relevant device.
Number of patent application 200780020137.1 provides one group of Wet-process metallurgy method, by its can in environment temperature and
The nickel of dissolving is recycled under low system pressure from water.The continuation method of precipitating nickel ions from water-bearing mother liquor includes, including 0
~50 DEG C of Contact Temperature, the contact of 0.5~1.5 atmospheric pressure and 6~9 contact pH contactor under the conditions of, make this
Mother liquor is contacted with the sulfide of dissolving in contactor, and solid nickel sulphide is detached from the pregnant solution, thus provides sulphur
Change nickel mud and barren water solution, wherein the nickel sulphide sludge is at least 5 microns of average nickel sulfide size and this is without mineral water
Solution has the dissolving nickel concentration less than 10ppm, and at least part nickel sulphide sludge is recycled to contactor.It is disclosed
The intermediate processing of nickel sulfide, and the invention reside in being extracted to the nickel in nickel sulfide material, thus with difference of the present invention.
Number of patent application 201010235078.3 proposes a kind of nickel sulfide pure oxygen producing electrolytic nickel by leaching of chemical precipitation
Method carries out the nickel sulfide of chemical precipitation and high pressure leaching liquid (8~10) in mass ratio: 1 mixing pulp, the material after pulp
One section of normal pressure leaching is electrolysed after one section of leachate removal of impurities, produces electrolytic nickel and anolyte, and one section is leached filter residue and anolyte
It mixes and carries out two sections of high pressures after secondary pulp and further leach obtained leaching filtrate to return into pulp use；The production technology
The utilization of resources is extensive, and process route is simple, and investment is small, and low energy consumption, free from environmental pollution, and nickel cobalt leaching rate is high, easy to operate, production
It is at low cost, it produces electrolytic nickel for nickel sulfide concentrate and provides extremely effective and affordable approach.It is disclosed using two
The process nickel sulfide material that section leaches, first segment are that normal pressure leads to oxygen sulfuric acid leaching, and second segment leaches for hyperbaric oxygen, with this
Invention is the difference in the presence of essence.
Number of patent application 201310717587.3 proposes a kind of method of the coprecipitated nickel hydroxide from the aqueous solution containing nickel ion, including
In 0~50 DEG C of Contact Temperature, environmental pressure be under 0.5~1.5 atmospheric pressure carry out solution ph adjustment, sulfide precipitation,
It is separated by solid-liquid separation, exhaust gas recycles.Reach setting value by adjusting mother liquor pH value, is slowly added to vulcanizing agent, while making reaction system
PH value remain unchanged or slowly varying, the nickel sulfide product being enriched with, the hydrogen sulfide gas generated in reaction process is logical
Absorption plant absorption is crossed, prevents from revealing, while can be with cycling and reutilization.The present invention passes through during adjusting, controlling sulfide precipitation
The variation of pH values prevents the foreign ions such as iron, magnesium, aluminium, manganese hydrolysis hydrate from entering in sulfide, improves point of nickel
From rate and the rate of recovery, the rate of recovery of nickel can reach 99.5% or more, and nickel sulfide product settling velocity is fast, be easy filtering.It is nothing
Patent is weighed, and the intermediate processing that this method is nickel sulfide, it is different from the extracting method of the present invention.
Number of patent application 201310119086.5 proposes the processing side of recycling nickel, chromium, iron in a kind of waste residue from Stainless Steel Plant
Nitration mixture is added in Stainless Steel Plant's waste residue, leaches nickel, chromium, the iron in the waste residue, be separated by filtration out pickle liquor and acidleach by method
Slag；Vulcanized sodium is added under room temperature into pickle liquor, is separated by solid-liquid separation after reaction and obtains nickel sulfide and filtered fluid；Filtered fluid is added
Heat, while sodium hydroxide solution and hydrogenperoxide steam generator are added, trivalent chromium conversion is stopped at Cr VI using alkali leaching oxidizing process
In supernatant, and ferric iron is converted to ferric hydroxide precipitate, is separated by solid-liquid separation, can obtain chromium acid sodium solution, chromium is recycled, hydrogen-oxygen
Smelting utilization can be melted down by changing iron precipitate.Acid leaching residue agricultural can be filled by natural air drying.Do not have in whole process of the present invention
Any pollutant is generated, is recycled completely and recycling, and is simple for process easy to operate, at low cost, it can effectively solution be never
Residue contamination problem in rust steel production, has higher economic benefit and environmental benefit.It is leached for Stainless Steel Plant's waste residue, leaching
Go out liquid and uses vulcanized sodium precipitate nickel sulphides, it is follow-up to be related to the extract technology of nickel sulfide, it is not related to nickel element in nickel sulfide
There is the difference of essence with the present invention in extracting method.
Number of patent application 200510010907.7 proposes a kind of wet-treating side extracting nickel from iron containing nickel sulfide material
Method.It is by the iron containing nickel sulfide material (Fe of chemical precipitation output:5~25%, Ni:8~30%) pulp and the pre- place of oxidation are carried out
After reason, using the method for pressurization, oxygenation and additive, effectively leaches nickel cobalt and inhibit the leaching of iron, 95% or more nickel is soaked
Go out, most iron (70% or more) is inhibited in the form of ferrovanadium and oxide in leached mud, reduces the reagent of purification deferrization
Consumption and the scum quantity of slag, the nickel for reducing purification removing impurities process loses, and after the purified removing iron of infusion solution and other impurity, uses
Sodium hydroxide sinks nickel to remove sodium, magnesium, potassium, and sulfuric acid dissolution nickel hydroxide, obtains pure nickel sulfate solution after extraction and recovery cobalt later.
The concentrated crystallization output of nickel sulfate solution meets the nickel sulfate of national standard, or meets the electric nickel product of national standard through electrodeposition output.It is
Nickel minerals is after sulfuric acid leaching, after leachate is using high ferro nickel sulfide drying obtained by sulfide precipitation, using high pressure addition ammonium sulfate and
Wooden calcium sulfate and logical oxygen leaching；It is different from technique of the present invention.
To sum up, the nickel sulfide material of current technology processing chemical precipitation, mainly using pyrogenic process roasting or melting, which holds
It is also easy to produce sulfur dioxide and hydrogen sulfide gas overflows, aggravating working environment needs mating respective absorption equipment.And pass through wet-treating
Nickel sulfide material generally leads to oxygen-Ore Leaching technique using high pressure, and that there are equipment investments is high for the technique, technical operation is complicated, to people
Member's competency profiling is high, and nickel sulfide can rapidly be reacted with sulfuric acid under high pressure generates hydrogen sulfide, pressure multiplier, it is more difficult to control, have certain
Security risk.
Invention content
The purpose of the present invention is to provide the good chemical precipitation sulphur of a kind of low cost, low stain, comprehensive reutilization effect
Change the method for nickel materials extraction nickel, to solve the problems mentioned in the above background technology.
To achieve the above object, the present invention provides the following technical solutions：A kind of chemical precipitation nickel sulfide material extraction nickel
Method includes the following steps：
S1：Reactive tank is added in the nickel sulfide material of chemical precipitation, water is added to size mixing；After mixing, with certain speed
Sodium hypochlorite, heating stirring 5-9h is added；
S2：Sulfuric acid or hydrochloric acid are added into slurry obtained by S1, carries out heating stirring leaching, the slurry after the completion of reacting carries out
It is separated by solid-liquid separation, obtains leachate and leached mud；
S3：Antalkali is added in leachate into S2, and acquired solution pH in S2 is adjusted to 3.5-4.5；Filtering
Afterwards, it presses and compares 1:1 carries out multi-stage counter current extraction removal of impurities with saponification P204- kerosene extraction systems, and load is organic anti-through sulfuric acid solution
The nickel sulfate solution that can be obtained high concentration after extraction can be obtained nickel product after oil removing by evaporative crystallization or electrolysis.
Preferably, sodium hydroxide is added during adding water to size mixing in the step S1, its pH is adjusted to 8.0-9.5, and
Sodium hypochlorite divides 3-6 addition, the total amount of the sodium hypochlorite of addition to be the 2.5-3.5 of the middle nickel total amount of input nickel sulfide material
Times, liquid-solid ratio 4:1-7:1, temperature is 30-50 DEG C, mixing speed 200-400r/min.
Preferably, it is added after hydrochloric acid or sulfuric acid that initial hydrogen ion concentration is 1.5- in reaction kettle in the step S2
3.0mol/L, control extraction temperature are 80-98 DEG C, mixing speed 250-400r/min, extraction time 3-7h and work as leached mud
Middle nickel content >=0.1wt% return to step S1 sizes mixing, nickel content<0.1wt% send cinder field to be uniformly processed.
Preferably, the solution containing trace cobalt, zinc, iron, aluminium, calcium plasma obtained by abstraction impurity removal can pass through in the step S3
Existing maturation process processing, recycling.
Compared with prior art, the present invention uses alkaline oxygenated processing nickel sulfide material, and the processing procedure is without sulfur dioxide
It is generated with pernicious gases such as hydrogen sulfide gas, is more advantageous to environmental protection and production operation；The present invention leaches vulcanization using normal pressure system
Nickel materials also obtain higher metal while capable of preparing the nickel sulfate hexahydrate crystal of high-purity by chemical subtraction and abstraction impurity removal
The rate of recovery, cobalt and zinc can be sold by vulcanizing alkali precipitation enrichment as byproduct.Therefore, the present invention has in actual production
It is widely applied space, is carried in the good chemical precipitation nickel sulfide material of a kind of low cost, low stain, comprehensive reutilization effect
The method for taking nickel, cobalt.
Description of the drawings
Fig. 1 is the integrated artistic flow chart of the present invention.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes.Obviously, described embodiment is only section Example of the present invention, instead of all the embodiments.Based on this
The embodiment of invention, every other real shallow lake obtained by those of ordinary skill in the art without making creative efforts
Example is applied, shall fall within the protection scope of the present invention.
Refering to fig. 1, a kind of method for the nickel sulfide material extraction nickel that chemistry is heavy of the present invention, includes the following steps：
The first step：Reactive tank is added in the nickel sulfide material of chemical precipitation, water is added to size mixing；After mixing, with certain
Sodium hypochlorite, heating stirring 5-9h is added in speed；Wherein, one sodium oxide molybdena of hydrogen is added during adding water to size mixing to be adjusted to its pH
8.0-9.5, and sodium hypochlorite divides 3-6 addition, the total amount of the sodium hypochlorite of addition total for the middle nickel of input nickel sulfide material
2.5-3.5 times of amount, liquid-solid ratio 4:1-7:1, temperature is 30-50 DEG C, mixing speed 200-400r/min；
Second step：Sulfuric acid or hydrochloric acid are added into slurry obtained by step 1, heating stirring leaching is carried out, after the completion of reacting
Slurry is separated by solid-liquid separation, and leachate and leached mud are obtained；Wherein, it is added after hydrochloric acid or sulfuric acid that initial hydrogen ion is dense in reaction kettle
Degree is 1.5-3.0mol/L, and control extraction temperature is 80-98 DEG C, mixing speed 250-400r/min, extraction time 3-7h,
When nickel content >=0.1wt% return to step S1 sizes mixing in leached mud, nickel content<0.1wt% send cinder field to be uniformly processed；
Third walks：Antalkali is added in leachate into step 2, and step 2 acquired solution pH is adjusted to 3.5-
4.5；After filtering, by compared to 1:1 carries out multi-stage counter current extraction removal of impurities with saponification P204- kerosene extraction systems, and load is organic through sulphur
The nickel sulfate solution that can be obtained high concentration after acid solution back extraction can be obtained nickel production after oil removing by evaporative crystallization or electrolysis
Solution containing trace cobalt, zinc, iron, aluminium, calcium plasma obtained by product, wherein abstraction impurity removal can be handled by existing maturation process, be returned
It receives.
Operation principle：The method that this chemical precipitation nickel sulfide material extracts nickel, in alkalescent system, nickel sulfide material slurry
Nickel sulfide in body generates nickel chloride with sodium hypochlorite reaction；And the nickel hydroxide that the nickel sulfate in nickel sulfide material slurry generates
Nickelic hydroxide is generated with sodium hypochlorite reaction, nickelic hydroxide has the oxidation effectiveness that strong oxidation performance accelerates nickel sulfide；Alkali
Property oxidation after the completion of ore pulp it is molten through sulfuric acid or hydrochloric acid acid, unreacted is completely vulcanized to material and nickelic hydroxide and is reacted leaching
Go out nickel；Leachate obtains high-purity sulphuric acid nickel solution after chemistry and abstraction impurity removal, and sulfuric acid can be obtained by evaporative crystallization after oil removing
Nickel product is sent to electrolytic nickel；Wherein, the main chemical reactions equation of generation is：
2NiS+6NaClO+6H2O→Ni(OH)3+S+6NaCl
Me (Ni, Co, Fe) S+4NaClO → 4NaCl+Me (Co2+, Cu2+, Fe2+)SO4
2Ni(OH)3+NiS+6H+→3Ni2++S+6H2O
It is described based on above-described embodiment and operation principle, following specific embodiment is provided：
Embodiment 1：
By the nickel sulfide material of chemical precipitation (containing Ni 48.92%, Co 0.24%, Ca 0.41%, Fe 3.19%, Al
0.02%, S 27.42%) input reactive tank, by liquid-solid ratio 4:1 adds water to size mixing, and mixing speed is 400 r/min, and hydrogen is added
Its pH is adjusted to 8.0 by sodium oxide molybdena；After the completion of sizing mixing, the sodium hypochlorite being added three times, total amount is input nickel sulfide material
3.5 times of middle nickel total amount, temperature is 30 DEG C, reaction time 5h；After the completion of reaction, initial hydrogen in reaction kettle after addition sulfuric acid
Ion concentration is 1.5mol/L, and control extraction temperature is 80 DEG C, mixing speed 400r/min, extraction time 7h；Filtering, obtains
To leachate and leached mud；Leached mud return is sized mixing；The pH of leachate is adjusted to 3.5-4.0；After filtering, by compared to 1:1 with
Soda soap P204 (containing 75% kerosene), extraction system carried out multi-stage counter current extraction removal of impurities, and nickel-loaded is organic anti-through 2mol/L sulfuric acid solutions
Nickel sulfate product can be obtained by evaporative crystallization after oil removing in the nickel sulfate solution that can be obtained high concentration after extraction；Abstraction impurity removal is washed
Water send outer sewage workshop to handle by the way that soluble akali sulphide enriched in cobalt and zinc, filtering, filtrate is added.
Embodiment 2：
By the nickel sulfide material of chemical precipitation (containing Ni 48.92%, Co 0.24%, Ca 0.41%, Fe 3.19%, Al
0.02%, S 27.42%) input reactive tank, by liquid-solid ratio 7:1 adds water to size mixing, and mixing speed is 200 r/min, and hydrogen is added
Its pH is adjusted to 9.5 by sodium oxide molybdena；After the completion of sizing mixing, the sodium hypochlorite of point 6 additions, total amount is input nickel sulfide material
2.5 times of middle nickel total amount, temperature is 50 DEG C, reaction time 9h；After the completion of reaction, initial hydrogen in reaction kettle after addition hydrochloric acid
Ion concentration is 3.0mol/L, and control extraction temperature is 98 DEG C, mixing speed 250r/min, extraction time 3h；Filtering, obtains
To leachate and leached mud；Nickel content is 0.08wt% in slag after testing, that is, outer cinder field is sent to be uniformly processed；By leachate
PH is adjusted to 4.0；After filtering, by compared to 1:1 carries out multi-stage counter current extraction with nickel soap P204 (containing 75% kerosene) extraction system removes
Miscellaneous, nickel-loaded organic nickel sulfate solution that can be obtained high concentration after the back extraction of 2mol/L sulfuric acid solutions passes through evaporation after oil removing
Nickel sulfate product can be obtained in crystallization；Abstraction impurity removal wash water is by being added soluble akali sulphide enriched in cobalt and zinc, and filtering, filtrate is sent outer
Sewage workshop is handled.
Embodiment 3：
By the nickel sulfide material of chemical precipitation (containing Ni 51.04%, Co 0.12%, Ca 0.35%, Fe 2.07%, Al
0.15%, S 28.46%) input reactive tank, by liquid-solid ratio 5:1 adds water to size mixing, and mixing speed is 300 r/min, and hydrogen is added
Its pH is adjusted to 9.0 by sodium oxide molybdena；After the completion of sizing mixing, the sodium hypochlorite of point 4 additions, total amount is input nickel sulfide material
3.0 times of middle nickel total amount, temperature is 40 DEG C, reaction time 7h；After the completion of reaction, initial hydrogen in reaction kettle after addition hydrochloric acid
Ion concentration is 2.5mol/L, and control extraction temperature is 90 DEG C, mixing speed 300r/min, extraction time 3h；Filtering, obtains
To leachate and leached mud；Nickel content is 0.38wt% in slag after testing, and return is sized mixing；The pH of leachate is adjusted to
4.0；After filtering, by compared to 1:1 carries out multi-stage counter current extraction removal of impurities, nickel-loaded with nickel soap P204 (containing 75% kerosene) extraction system
Organic nickel chloride solution that can be obtained high concentration after the back extraction of 4mol/L hydrochloric acid solutions, it is available by evaporative crystallization after oil removing
Nickel chloride product；Abstraction impurity removal wash water is sent by the way that soluble akali sulphide enriched in cobalt and zinc, filtering, filtrate is added at outer sewage workshop
Reason.
Embodiment 4：
By the nickel sulfide material of chemical precipitation (containing Ni 46.04%, Co 0.46%, Ca 0.60%, Fe 2.77%, Al
0.09%, S 26.46%) input reactive tank, by liquid-solid ratio 6:1 adds water to size mixing, and mixing speed is 350 r/min, and hydrogen is added
Its pH is adjusted to 9.5 by sodium oxide molybdena；After the completion of sizing mixing, the sodium hypochlorite of point 4 additions, total amount is input nickel sulfide material
3.0 times of middle nickel total amount, temperature is 40 DEG C, reaction time 7h；After the completion of reaction, initial hydrogen in reaction kettle after addition sulfuric acid
Ion concentration is 2.0mol/L, and control extraction temperature is 95 DEG C, mixing speed 300r/min, extraction time 5h；Filtering, obtains
To leachate and leached mud；Nickel content is 0.06wt% in slag after testing, that is, outer cinder field is sent to be uniformly processed；By leachate
PH is adjusted to 4.0；After filtering, by compared to 1:1 carries out multi-stage counter current extraction with soda soap P204 (containing 75% kerosene) extraction system removes
Miscellaneous, nickel-loaded organic nickel sulfate solution that can be obtained high concentration after the back extraction of 2mol/L sulfuric acid solutions passes through evaporation after oil removing
Nickel sulfate product can be obtained in crystallization；Abstraction impurity removal wash water is by being added soluble akali sulphide enriched in cobalt and zinc, and filtering, filtrate is sent outer
Sewage workshop is handled.
In summary：The method of the nickel sulfide material extraction nickel of this chemical precipitation uses alkaline oxygenated processing nickel sulfide object
Material, the process are generated without the pernicious gases such as sulfur dioxide and hydrogen sulfide gas, are more advantageous to environmental protection and production operation；In addition this hair
It is bright that nickel sulfide material is leached using normal pressure system, the nickel sulfate hexahydrate crystal of high-purity can be prepared by chemical subtraction and abstraction impurity removal
While also obtain higher metal recovery rate, cobalt and zinc can be sold, the party by vulcanizing alkali precipitation enrichment as byproduct
Method is widely used space in actual production.
Claims (4)
1. a kind of method of chemical precipitation nickel sulfide material extraction nickel, which is characterized in that include the following steps：
S1：Reactive tank is added in the nickel sulfide material of chemical precipitation, water is added to size mixing；After mixing, it is added with certain speed
Sodium hypochlorite, heating stirring 5-9h；
S2：Sulfuric acid or hydrochloric acid are added into slurry obtained by S1, carries out heating stirring leaching, the slurry after the completion of reacting carries out solid-liquid
Separation, obtains leachate and leached mud；
S3：Antalkali is added in leachate into S2, and acquired solution pH in S2 is adjusted to 3.5-4.5；After filtering, by phase
Than 1:1 carries out multi-stage counter current extraction removal of impurities with saponification P204- kerosene extraction systems, and load is organic after sulfuric acid solution is stripped
The nickel sulfate solution of high concentration is obtained, nickel product can be obtained by evaporative crystallization or electrolysis after oil removing.
2. the method for chemical precipitation nickel sulfide material extraction nickel as described in claim 1, which is characterized in that in the step S1
Sodium hydroxide is added during adding water to size mixing, its pH is adjusted to 8.0-9.5, and sodium hypochlorite divides 3-6 addition, time of addition
The total amount of sodium chlorate is 2.5-3.5 times of the middle nickel total amount of input nickel sulfide material, liquid-solid ratio 4:1-7:1, temperature 30-50
DEG C, mixing speed 200-400r/min.
3. the method for chemical precipitation nickel sulfide material extraction nickel as described in claim 1, which is characterized in that in the step S2
Initial hydrogen ion concentration is 1.5-3.0mol/L in reaction kettle after addition hydrochloric acid or sulfuric acid, and control extraction temperature is 80-98 DEG C, is stirred
It is 250-400r/min, extraction time 3-7h to mix speed, when nickel content >=0.1wt% return to step S1 sizes mixing in leached mud,
Nickel content<0.1wt% send cinder field to be uniformly processed.
4. a kind of method of chemical precipitation nickel sulfide material extraction nickel as described in claim 1, which is characterized in that the step
Solution in S3 containing trace cobalt, zinc, iron, aluminium, calcium plasma obtained by abstraction impurity removal can pass through the processing of existing maturation process, recycling.
Priority Applications (1)
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109081475A (en) * | 2018-09-30 | 2018-12-25 | 荆门市格林美新材料有限公司 | A kind of comprehensive resource processing unit for the raffinate that cobalt nickel leaching process generates |
| CN114230038A (en) * | 2021-12-14 | 2022-03-25 | 浙江中金格派锂电产业股份有限公司 | Process for separating and recovering nickel and cobalt from cobalt raffinate wastewater |
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| JPS5240403A (en) * | 1975-09-27 | 1977-03-29 | Nippon Mining Co Ltd | Process for leaching metallic sulfide |
| CN102560102A (en) * | 2012-01-18 | 2012-07-11 | 长沙矿冶研究院有限责任公司 | Method for leaching nickel and molybdenum from nickel-molybdenum ores by catalytic oxidation |
| CN104911359A (en) * | 2015-06-29 | 2015-09-16 | 北京科技大学 | Process method for extracting cobalt and nickel from manganese waste slag |
| CN105274332A (en) * | 2015-11-20 | 2016-01-27 | 金川集团股份有限公司 | Isolation technology and process for extracting Ni and Co from nickel-containing high-cobalt hydroxide |
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| JPS5240403A (en) * | 1975-09-27 | 1977-03-29 | Nippon Mining Co Ltd | Process for leaching metallic sulfide |
| CN102560102A (en) * | 2012-01-18 | 2012-07-11 | 长沙矿冶研究院有限责任公司 | Method for leaching nickel and molybdenum from nickel-molybdenum ores by catalytic oxidation |
| CN104911359A (en) * | 2015-06-29 | 2015-09-16 | 北京科技大学 | Process method for extracting cobalt and nickel from manganese waste slag |
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| CN109081475A (en) * | 2018-09-30 | 2018-12-25 | 荆门市格林美新材料有限公司 | A kind of comprehensive resource processing unit for the raffinate that cobalt nickel leaching process generates |
| CN114230038A (en) * | 2021-12-14 | 2022-03-25 | 浙江中金格派锂电产业股份有限公司 | Process for separating and recovering nickel and cobalt from cobalt raffinate wastewater |
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| CN108441649B (en) | 2020-08-28 |
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