CN105714119A - Method for recovering nickel from calcium-magnesium slag through ion exchange solution - Google Patents
Method for recovering nickel from calcium-magnesium slag through ion exchange solution Download PDFInfo
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- CN105714119A CN105714119A CN201610215549.1A CN201610215549A CN105714119A CN 105714119 A CN105714119 A CN 105714119A CN 201610215549 A CN201610215549 A CN 201610215549A CN 105714119 A CN105714119 A CN 105714119A
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- nickel
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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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
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
- C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
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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
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
- C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
- C22B23/0469—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods by chemical substitution, e.g. by cementation
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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
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- General Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Processing Of Solid Wastes (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for recovering nickel from calcium-magnesium slag through an ion exchange solution. The method mainly comprises the steps of preparation of the ion exchange solution, ion exchange reaction, filtration, washing, increase of concentration of the nickel in a filtrate, filtrate detection, replacement recovery of the nickel and the like. The method has the advantages that raw materials adopted by the method are cheap, the process and technique are simple, reaction is mild, operation is simple and convenient, and large-scale production is easy to achieve. In addition, the recovery process is free of pollution, and the requirement of the national environmental protection policy is met. A nickel chloride recovery solution can be used as a raw material for producing ferronickel products after being repeatedly used, or the nickel chloride recovery solution is recovered and processed through Na2S to generate NiS which directly enters a pyrogenic process system, and the calcium-magnesium slag subjected to ion exchange is almost free of the nickel after being washed, so that the requirement of waste slag is met, the production cost is reduced, and the comprehensive utilization level of resources is increased. The method is perfectly combined with existing nickel sulfate production techniques, does not influence present production, and is simple in flow process, low in production cost and good in environment protection effect.
Description
Technical field
The invention belongs to the process of resource and environment technology and solid waste and technical field of comprehensive utilization, be specifically related to a kind of method that ion exchanged soln reclaims nickel from nickeliferous calcium and magnesium slag.
Background technology
At present, in the enterprise that nickel sulfate produces, nickel raw material passes through sulfuric acid leaching, after sodium jarosite deironing, then carries out P204The metals such as extract and separate copper zinc-manganese, raffinate passes through P507After Separation of nickel and cobalt, re-evaporation crystallization produces nickel sulfate product, P204The calcium ions and magnesium ions in solution is must be driven off, it is prevented that calcium and magnesium produces the crystallization of calcium sulfate, magnesium sulfate in extraction process, and blocking pipeline hinders production properly functioning before extraction.
Each big business all remove the calcium ions and magnesium ions in the nickel sulfate solution of nickeliferous 50-60g/L with sodium fluoride, due to removing calcium and magnesium in the nickel sulfate solution of high concentration, the lattice that small part nickel ion enters sodium fluoride and Afluon (Asta) is made to define displacement compound and interstitial compound, thus defining nickeliferous calcium fluoride slag and Afluon (Asta) slag, calcium fluoride slag and Afluon (Asta) slag are also calcium and magnesium slag.
Pass through diluted acid at present, the conventional method washings such as ammonia, all the nickel of the 2-3% contained in calcium and magnesium slag cannot be reclaimed, recovery nickel is reacted by concentrated acid and calcium and magnesium slag, course of reaction generates severe toxicity fluohydric acid gas contaminated environment etching apparatus again, and the peracid solution containing nickel of follow-up generation cannot low cost reclaim, pass through pyrogenic attack, calcium magnesium element circulates in system always, energy consumption is high, cost is high, and waste gas both contaminated environment that production process produces, etching apparatus again, the enterprise producing nickel sulfate at present has all stored up substantial amounts of calcium and magnesium slag mostly, large enterprise will produce the calcium and magnesium slag of kiloton every year, valuable metal nickel therein contains 2-3%, reclaim grade 0.5% according to nickel to calculate, these calcium and magnesium slags cannot abandon, the needs of depositing of a large amount of calcium and magnesium slags take a large amount of place, simultaneously because calcium and magnesium solid impurity particle is tiny, wind easily forms a large amount of dust polluting environment, cause the wasting of resources, the so how metallic nickel in the recovery calcium and magnesium slag of low-cost and pollution-less, solve calcium and magnesium slag muck and send one's regards to the emphasis that topic is the research of current each big business.
Summary of the invention
It is an object of the invention to provide a kind of method that ion exchanged soln reclaims nickel from nickeliferous calcium and magnesium slag, the nickel of the 2-3% to solve in prior art in calcium and magnesium slag is difficult to reclaim, reclaim energy consumption height, cost height, produce waste gas both contaminated environment that removal process produces, etching apparatus again, calcium and magnesium slag muck is put and is taken a large amount of place, the problem easily causing environmental pollution and the wasting of resources.
For reaching above-mentioned purpose, the technical scheme is that a kind of method that ion exchanged soln reclaims nickel from nickeliferous calcium and magnesium slag, comprise the following steps:
A prepared by () ion exchanged soln: extracting concentration is the magnesium chloride solution of 5-100g/L and puts in reaction vessel, blender of starting shooting, and heats, and treats that solution temperature reaches 70-80 DEG C；
(b) ion-exchange reactions: being added in ion exchanged soln by calcium and magnesium slag and carry out ion exchange, the solid-to-liquid ratio of calcium and magnesium slag and ion exchanged soln is 1:4, and the response time is 2-5h, and reaction temperature is 50-85 DEG C；
C () filters, washing: after ion-exchange reactions terminates, by solution heat filtering, and washing with wash water, the filtrate after filtration is stand-by, and filtering residue is individually in heaps after drying；
D () improves the concentration of nickel in filtrate: add ion exchanged soln according to the concentration of the ion exchanged soln of step (a) in filtrate, and with wash water, filtrate volume is adjusted to the volume of step (b) intermediate ion exchange solution, repeat the operation of step (b)-(c), until the concentration of nickel is close to desired value in filtrate；
E () filtrate is detected: the concentration of nickel in detection filtrate；
F the displacement of () nickel is reclaimed: the nickel reclaimed in filtrate by adding fine iron powder to replace in filtrate, and as producing the raw material of ferro-nickel product.
Preferably, with the pH value of the ion exchanged soln in hydrochloric acid rate-determining steps (a) and (d) at 1-3.
Preferably, the content of the magnesium chloride in the ion exchanged soln of step (b) is 8-15 times of nickel content in the calcium and magnesium slag added.
Preferably, in step (a), the rotating speed of blender is 150-250r/min.
Preferably, the filtering residue in step (c) is the calcium and magnesium slag being substantially free of nickel, reaches waste requirement after washing, and the filtrate in step (c) is nickel chloride solution.
Preferably, step (c) is distilled water with the wash water in (d).
Preferably, step (d) repeatable operation 6-8 time.
Preferably, in step (e) filtrate, the concentration of nickel is 30-50g/L.
Preferably, step (f) can also be used with Na2S solution reclaims the nickel in filtrate, generates NiS and is directly entered the process of pyrogenic process system.
It is an advantage of the current invention that: the method for the present invention is that the method exchanged by cation reclaims the nickel of 2-3% in calcium and magnesium slag; the raw material that the method provides is cheap; process is simple; reaction temperature and, easy and simple to handle, it is easy to accomplish large-scale production; and removal process non-environmental-pollution; meet the environmental protection policy of country, Nickel dichloride. recovered liquid repeatedly reuse after can as the raw material producing ferro-nickel product, or through Na2S recycling generates NiS and is directly entered pyrogenic process system, calcium and magnesium slag after ion exchange is substantially free of nickel after washing, reach the requirement of waste, reducing production cost, improve the level of comprehensive utilization of resource, this method is perfectly combined with existing nickel sulfate production technology, existing production is not impacted, flow process is simple, and production cost is low, and environment protecting is good.
Accompanying drawing explanation
Fig. 1 is the process chart of the present invention.
Detailed description of the invention
Illustrate that the invention will be further described with embodiment below in conjunction with accompanying drawing.
Embodiment 1
Extracting concentration is the magnesium chloride solution 200mL of 50g/L, the pH ≈ 2 of ion exchanged soln is controlled with hydrochloric acid, open blender, the rotating speed arranging blender is 200r/min, and heat, when solution temperature reaches 75 DEG C, calcium and magnesium slag by nickeliferous for 50g 2.26% adds ion exchanged soln, and ensure that the content of the magnesium chloride in ion exchanged soln is in the calcium and magnesium slag added 10 times of nickel content, insulation reaction 4h, reaction temperature is 70 DEG C, after reaction terminates, by solution heat filtering, and wash with distilled water, filtrate after filtration is stand-by, filtering residue is individually in heaps after drying, by detect nickel content in filtering residue is 0.12%, filtering residue reaches waste requirement and directly discards, filtrate is added 1.4g magnesium chloride, with distilled water, the volume of filtrate is regulated to 200mL continuation leaching again, after repeat the above steps 6 times, the nickel content measured in filtrate is after 32.25g/L, stopped reaction, the nickel reclaimed in filtrate by adding fine iron powder to replace in filtrate, and as producing the raw material of ferro-nickel product, or use Na2S solution reclaims the nickel in filtrate, and in the solution after recovery, the content of nickel is directly entered the process of pyrogenic process system less than 0.001g/L, the NiS of generation.
The raw material that the method provides is cheap, and process is simple, reaction temperature and; easy and simple to handle, it is easy to accomplish large-scale production, and removal process non-environmental-pollution; meeting the environmental protection policy of country, the calcium and magnesium slag after ion exchange is substantially free of nickel after washing, has reached the requirement of waste; reducing production cost, improve the level of comprehensive utilization of resource, this method is perfectly combined with existing nickel sulfate production technology; existing production is not impacted; flow process is simple, and production cost is low, and environment protecting is good.
Embodiment 2
Extracting concentration is the magnesium chloride solution 400mL of 45g/L, the pH ≈ 2 of ion exchanged soln is controlled with hydrochloric acid, open blender, the rotating speed arranging blender is 180r/min, and heat, when solution temperature reaches 73 DEG C, calcium and magnesium slag by nickeliferous for 100g 2.26% adds ion exchanged soln, and ensure that the content of the magnesium chloride in ion exchanged soln is in the calcium and magnesium slag added 8 times of nickel content, insulation reaction 3.5h, reaction temperature is 65 DEG C, after reaction terminates, by solution heat filtering, and wash with distilled water, filtrate after filtration is stand-by, filtering residue is individually in heaps after drying, by detect nickel content in filtering residue is 0.15%, filtering residue reaches waste requirement and directly discards, filtrate is added 2.8g magnesium chloride, with distilled water, the volume of filtrate is regulated to 400mL continuation leaching again, after repeat the above steps 6 times, the nickel content measured in filtrate is after 31.65g/L, stopped reaction, the nickel reclaimed in filtrate by adding fine iron powder to replace in filtrate, and as producing the raw material of ferro-nickel product, or use Na2S solution reclaims the nickel in filtrate, and in the solution after recovery, the content of nickel is directly entered the process of pyrogenic process system less than 0.001g/L, the NiS of generation.
Embodiment 3
Extracting concentration is the magnesium chloride solution 2000mL of 55g/L, the pH ≈ 2 of ion exchanged soln is controlled with hydrochloric acid, open blender, the rotating speed arranging blender is 220r/min, and heat, when solution temperature reaches 78 DEG C, calcium and magnesium slag by nickeliferous for 500g 2.26% adds ion exchanged soln, and ensure that the content of the magnesium chloride in ion exchanged soln is in the calcium and magnesium slag added 12 times of nickel content, insulation reaction 4.5h, reaction temperature is 75 DEG C, after reaction terminates, by solution heat filtering, and wash with distilled water, filtrate after filtration is stand-by, filtering residue is individually in heaps after drying, by detect nickel content in filtering residue is 0.12%, filtering residue reaches waste requirement and directly discards, filtrate is added 14g magnesium chloride, with distilled water, the volume of filtrate is regulated to 2000mL continuation leaching again, after repeat the above steps 7 times, the nickel content measured in filtrate is after 32.1g/L, stopped reaction, the nickel reclaimed in filtrate by adding fine iron powder to replace in filtrate, and as producing the raw material of ferro-nickel product, or use Na2S solution reclaims the nickel in filtrate, and in the solution after recovery, the content of nickel is directly entered the process of pyrogenic process system less than 0.001g/L, the NiS of generation.
Embodiment 4
Extracting concentration is the magnesium chloride solution 4000mL of 60g/L, the pH ≈ 2 of ion exchanged soln is controlled with hydrochloric acid, open blender, the rotating speed arranging blender is 250r/min, and heat, when solution temperature reaches 70 DEG C, calcium and magnesium slag by nickeliferous for 1000g 2.26% adds ion exchanged soln, and ensure that the content of the magnesium chloride in ion exchanged soln is 15 times of insulation reaction 5h of nickel content in the calcium and magnesium slag added, reaction temperature is 80 DEG C, after reaction terminates, by solution heat filtering, and wash with distilled water, filtrate after filtration is stand-by, filtering residue is individually in heaps after drying, by detect nickel content in filtering residue is 0.11%, filtering residue reaches waste requirement and directly discards, filtrate is added 28g magnesium chloride, with distilled water, the volume of filtrate is regulated to 4000mL continuation leaching again, after repeat the above steps 7 times, the nickel content measured in filtrate is after 31.95g/L, stopped reaction, the nickel reclaimed in filtrate by adding fine iron powder to replace in filtrate, and as producing the raw material of ferro-nickel product, or use Na2S solution reclaims the nickel in filtrate, and in the solution after recovery, the content of nickel is directly entered the process of pyrogenic process system less than 0.001g/L, the NiS of generation.
Above-described is only the preferred embodiments of the present invention; technical scheme is not limited thereto; should be understood that to those skilled in the art; under technology provided by the present invention is enlightened; known general knowledge as this area; other equivalent modifications and improvement can also be made, also should be regarded as protection scope of the present invention.
Claims (9)
1. the method reclaiming nickel with ion exchanged soln from nickeliferous calcium and magnesium slag, it is characterised in that: comprise the following steps:
A prepared by () ion exchanged soln: extracting concentration is the magnesium chloride solution of 5-100g/L and puts in reaction vessel, blender of starting shooting, and heats, and treats that solution temperature reaches 70-80 DEG C；
(b) ion-exchange reactions: being added in ion exchanged soln by calcium and magnesium slag and carry out ion exchange, the solid-to-liquid ratio of calcium and magnesium slag and ion exchanged soln is 1:4, and the response time is 2-5h, and reaction temperature is 50-85 DEG C；
C () filters, washing: after ion-exchange reactions terminates, by solution heat filtering, and washing with wash water, the filtrate after filtration is stand-by, and filtering residue is individually in heaps after drying；
D () improves the concentration of nickel in filtrate: add ion exchanged soln according to the concentration of the ion exchanged soln of step (a) in filtrate, and with wash water, filtrate volume is adjusted to the volume of step (b) intermediate ion exchange solution, repeat the operation of step (b)-(c), until the concentration of nickel is close to desired value in filtrate；
E () filtrate is detected: the concentration of nickel in detection filtrate；
F the displacement of () nickel is reclaimed: the nickel reclaimed in filtrate by adding fine iron powder to replace in filtrate, and as producing the raw material of ferro-nickel product.
2. the method that a kind of ion exchanged soln as claimed in claim 1 reclaims nickel from nickeliferous calcium and magnesium slag, it is characterised in that: with the pH value of the ion exchanged soln in hydrochloric acid rate-determining steps (a) and (d) at 1-3.
3. the method that a kind of ion exchanged soln as claimed in claim 2 reclaims nickel from nickeliferous calcium and magnesium slag, it is characterised in that: the content of the magnesium chloride in the ion exchanged soln of described step (b) is 8-15 times of nickel content in the calcium and magnesium slag added.
4. the method that a kind of ion exchanged soln as claimed in claim 3 reclaims nickel from nickeliferous calcium and magnesium slag, it is characterised in that: in described step (a), the rotating speed of blender is 150-250r/min.
5. the method that a kind of ion exchanged soln as claimed in claim 4 reclaims nickel from nickeliferous calcium and magnesium slag, it is characterized in that: the filtering residue in described step (c) is the calcium and magnesium slag being substantially free of nickel, reaching waste requirement after washing, the filtrate in described step (c) is nickel chloride solution.
6. the method that a kind of ion exchanged soln as claimed in claim 5 reclaims nickel from nickeliferous calcium and magnesium slag, it is characterised in that: the wash water in described step (c) and (d) is distilled water.
7. the method that a kind of ion exchanged soln as claimed in claim 6 reclaims nickel from nickeliferous calcium and magnesium slag, it is characterised in that: described step (d) repeatable operation 6-8 time.
8. the method that a kind of ion exchanged soln as claimed in claim 7 reclaims nickel from nickeliferous calcium and magnesium slag, it is characterised in that: in described step (e) filtrate, the concentration of nickel is 30-50g/L.
9. the method that a kind of ion exchanged soln as described in claim as any in claim 1-8 reclaims nickel from nickeliferous calcium and magnesium slag, it is characterised in that: described step (f) can also be used with Na2S solution reclaims the nickel in filtrate, generates NiS and is directly entered the process of pyrogenic process system.
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| CN201610215549.1A CN105714119B (en) | 2016-04-08 | 2016-04-08 | A kind of method for recycling nickel from nickeliferous calcium and magnesium slag with ion exchanged soln |
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| CN201610215549.1A CN105714119B (en) | 2016-04-08 | 2016-04-08 | A kind of method for recycling nickel from nickeliferous calcium and magnesium slag with ion exchanged soln |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106282576A (en) * | 2016-08-29 | 2017-01-04 | 金川集团股份有限公司 | A kind of reclaim the method for nickel in calcium and magnesium slag |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106282576A (en) * | 2016-08-29 | 2017-01-04 | 金川集团股份有限公司 | A kind of reclaim the method for nickel in calcium and magnesium slag |
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