CN106191442A - A kind of method of nickel solution deeply purifying and removing silicon - Google Patents
A kind of method of nickel solution deeply purifying and removing silicon Download PDFInfo
- Publication number
- CN106191442A CN106191442A CN201610709019.2A CN201610709019A CN106191442A CN 106191442 A CN106191442 A CN 106191442A CN 201610709019 A CN201610709019 A CN 201610709019A CN 106191442 A CN106191442 A CN 106191442A
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- China
- Prior art keywords
- nickel
- solution
- hydroxide
- value
- slag
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Classifications
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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
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
-
- 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
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/20—Obtaining zinc otherwise than by distilling
- C22B19/26—Refining solutions containing zinc values, e.g. obtained by leaching zinc ores
-
- 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
A kind of method of nickel solution deeply purifying and removing silicon relates to solution impurity removing technology field, including: solution heating, regulation pH value, 3 steps of reactants separate.The nickel hydroxide slag that reactants separate step obtains can be used for regulating in pH value step, and the nickel hydroxide slag produced first can be recycled for multiple times 34 times.This method is particularly suited for nickel sulfate, Nickel dichloride., the mixed solution nickel sulfate cobalt liquor of nickel sulfate and Nickel dichloride. or sulphuric acid nickel cobalt and Nickel dichloride. mixed solution, and nickel total concentration is 15 ~ 75g/L, and silicone content is 0.1 ~ 1g/L.
Description
Technical field
The present invention relates to solution impurity removing technology field, a kind of method of nickel solution deeply purifying and removing silicon.
Background technology
The nickel solution obtained in nickel hydrometallurgy, wherein contains the impurity such as cobalt, calcium, magnesium, lead, silicon, generally utilizes extraction
Cobalt, calcium, magnesium, lead carried out after remove impurity targetedly for nickel plate and the preparation of nickel salt crystal with the sedimentation method, but impurity silicon is not had
Having and process technique accordingly, the silicone content in system maintains between 0.5～1g/L.Along with nickel salt product at lithium ion battery just
Continuous application in the material of pole, the requirement to its impurity content is more and more higher, especially impurity silicon, due in production process not
Can avoid being introduced back into, therefore silicone content in raw material be required higher.
About the research of degree of depth silicon removing method in solution, it is concentrated mainly on removing of sodium aluminate solution in aluminum oxide production process
Silicon study, it is known that Chinese patent have CN1569639, CN101857254, CN101891227A, CN102923745A,
CN102951667A, CN103739010A and CN103803614A, mainly disclose the different desiliconization agent of use at sodium aluminate solution
Middle normal pressure or pressurization are except the method for silicon.
The method that Chinese patent CN1569639 and CN101857254 is processed by seed activation or add red mud, by aluminum
Dioxide-containing silica in acid sodium solution is reduced to about 1g/L.CN101891227A and CN103739010A uses basic industry
In Friedel salt (the 3CaO Al for preparing of garbage2O3·CaCl2·10H2Or the standby magnesium of the making from brine of magnesium chloride containing O)
Aluminum hydrotalcite (Mg6Al2(OH)16CO3·4H2O) as desiliconization agent, it is possible to the silicon dioxide by least 60% or 80% is from aluminic acid
Sodium solution removes, while deep desilication, achieves the recycling of waste resource.CN102923745A utilize calcium oxide and
EDTA carries out the pressurization degree of depth and removes the silicon in sodium aluminate solution and ferrum, makes silicon concentration in solution be less than 0.67mg/L.Concentration of iron is less than
0.1mg/L.CN102951667A then uses flyash as Desilication seed, adds in sodium silicate solution and carries out normal pressure or middle pressure-off
Silicon, can bring up to 110～1000 by the A/S in sodium aluminate solution from 15～25, and after desiliconization, isolated flyash can be as former
Material dispensing produces aluminium oxide.
Chinese patent CN103803614A discloses and a kind of utilizes Ludox method of deep desilication in acid system, should
Method utilizes the silicate of solubility and acid reaction to obtain Ludox, Ludox is added pending acid solution continues into
Row reaction, then sedimentation, solid-liquid separation after flocculating by cationic flocculant, silicone content can be down to less than 0.001%.
Additionally, Mo Dingcheng et al. is at " China YouSe Acta Metallurgica Sinica " Vol.4NO.4,1994,38～40 describe a kind of height
The method of desiliconization in silicon solution of zinc sulfate, utilizes ferrum and powdered carbon to process the impurity silicon in high silicate solution, and enters experimental condition
Row optimizes, and under the optimum test condition of optimization, silicone content is reduced to below 0.2g/L by original about 23g/L, except silicon rate reaches
To more than 99%, the response rate of main metallic zinc reaches about 98%.Its principle is to utilize the electrochemical properties of this system, ferrum and charcoal
The potential difference of grain generation about 1.2v in aqueous is conducive to the deposition of colloidal silicon, additionally, ferrum and acid reaction under acid condition
Generate Fe2+And Fe3+, when the ph is increased, the Fe (OH) of generation2With Fe (OH)3Play absorption and the effect of bonding bridge formation simultaneously,
The silica gel generated condenses, and reaches the purpose of desiliconization.
Above-mentioned patent and article are removed the method removing mainly for the impurity silicon in other system height silicon solution of silicon, nickel
In solution, the degree of depth have not been reported except the method for silicon, and in the solution after said method remove impurity, silicone content is still at more than 0.2g/L, should
Class method can not reach the purpose of deep desilication；When using above-mentioned desiliconizing agent, can be introduced other to some extent in solution miscellaneous
Matter ion, especially ferrum, other magnetic foreign bodies such as ferrum are required strict, will certainly increase follow-up remove impurity burden by battery material,
Increase processing cost.
Summary of the invention
The technical problem to be solved is to provide a kind of method of nickel solution deeply purifying and removing silicon, existing to solve
Technology lacks the problem of degree of depth silicon removing method in nickel solution.
The present invention solves the technical scheme of technical problem: a kind of method of nickel solution deeply purifying and removing silicon includes: solution
Heating, regulation pH value, 3 steps of reactants separate.
Solution heats: the solution that will be enriched in nickel is placed in container, is heated to 50～80 DEG C.
Regulation pH value: enter appropriate alkaline matter, alkaline matter adition process is with uniform stirring, until solution pH value keeps
Between 4～6, depending on concrete numerical value is according to solution concrete condition, after solution PH reaches predetermined value, when continuing stirring one section
Between, mixing time is 1～10 hour；Described alkaline matter is sodium hydroxide solution or concentration 100-of concentration 100-400g/L
400g/L sodium hydroxide solution and the mixture of nickel hydroxide.
Reactants separate: the material operated through step B is carried out solid-liquid separation, the nickel solution after being purified and hydrogen
Nickel oxide slag；Solid-liquid separation can use sucking filtration to separate or filter pressing separates；Nickel solution silicone content after purification is less than 0.005g/L.
The nickel hydroxide slag that step C obtains can be used in step B, and the nickel hydroxide slag produced first can be recycled for multiple times
3-4 time.
This method be particularly suited for nickel sulfate, Nickel dichloride., the mixed solution nickel sulfate cobalt liquor of nickel sulfate and Nickel dichloride. or
Sulphuric acid nickel cobalt and Nickel dichloride. mixed solution, nickel total concentration is 15～75g/L, and silicone content is 0.1～1g/L.
The beneficial effects of the present invention is: present invention process is simple, and overall process is carried out at ambient pressure, the most too high to temperature
Requirement, save the energy, this technique impurity-eliminating effect is good simultaneously, and after remove impurity, solution silicone content is less than 0.005g/L, solves nickel
In solution, the degree of depth is except a difficult problem for silicon.Except only adding sodium hydroxide solution or sodium hydroxide solution and nickel hydroxide during silicon
Mixture, also ensures that the response rate that valuable metal is higher simultaneously, and after remove impurity, pH value of solution is stable, beneficially the carrying out of subsequent processing,
Industrialization can be realized produce continuously.Except the nickel hydroxide produced after silicon can reuse, save sodium hydroxide solution reduction
Cost.
Accompanying drawing explanation
Fig. 1 is present invention process flow chart.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1.
Weighing sodium hydroxide 5g, adds 20mL water and is configured to the sodium hydroxide solution of 250g/L, take siliceous nickel sulfate solution
1L。
Solution heats: is placed in container by siliceous nickel sulfate solution, is heated to 50 DEG C.
Regulation pH value: enter appropriate alkaline matter, alkaline matter adition process is with uniform stirring, until solution pH value keeps
4, when, after solution PH value stabilization, continuing stirring 2 hours.
Reactants separate: the material operated through step B is carried out the sucking filtration that reduces pressure, the nickel solution after being purified and hydrogen
Nickel oxide slag.Nickel hydroxide slag hot pure water 2～3 times i.e. reusable 3～4 times.Nickel hydroxide slag is adding sodium hydroxide
All add in the solution treating remove impurity before solution.
Except before and after silicon, solution index contrast is shown in Table 1.
Table 1 nickel sulfate solution is except solution index contrast before and after silicon
Embodiment 2
Weighing sodium hydroxide 8g, adds 20mL water and is configured to the sodium hydroxide solution of 400g/L, take siliceous nickel chloride solution
2L。
Solution heats: is placed in container by siliceous nickel chloride solution, is heated to 80 DEG C.
Regulation pH value: enter appropriate alkaline matter, alkaline matter adition process is with uniform stirring, until solution pH value keeps
5, when, after solution PH value stabilization, continuing stirring 10 hours.
Reactants separate: the material operated through step B is carried out the sucking filtration that reduces pressure, the nickel solution after being purified and hydrogen
Nickel oxide slag.
Nickel hydroxide slag hot pure water 2～3 times i.e. reusable 3～4 times.Nickel hydroxide slag is molten at addition sodium hydroxide
All add in the solution treating remove impurity before liquid.
Except before and after silicon, solution index contrast is shown in Table 2.
Table Z Nickel dichloride. nickel solution is except solution index contrast before and after silicon
Embodiment 3
Weighing sodium hydroxide 150g, adds 375mL water and is configured to the sodium hydroxide solution of 400g/L, takes siliceous sulphuric acid nickel cobalt
Solution 70L.
Solution heats: siliceous sulphuric acid nickel cobalt is placed in container, is heated to 70 DEG C.
Regulation pH value: enter appropriate alkaline matter, alkaline matter adition process is with uniform stirring, until solution pH value keeps
5.5, when, after solution PH value stabilization, continuing stirring 5 hours.
Reactants separate: the material operated through step B is carried out filter pressing, the nickel solution after being purified and hydroxide
Nickel slag.
Nickel hydroxide slag hot pure water 2～3 times i.e. reusable 3～4 times.Nickel hydroxide slag is molten at addition sodium hydroxide
All add in the solution treating remove impurity before liquid.
Except before and after silicon, solution index contrast is shown in Table 3.
Table 3 nickel sulfate solution is except solution index contrast before and after silicon
Claims (3)
1. the method for a nickel solution deeply purifying and removing silicon, it is characterised in that: described method comprises the technical steps that:
Solution A heats: the solution that will be enriched in nickel is placed in container, is heated to 50 ~ 80 DEG C；
B regulates pH value: enter appropriate alkaline matter, and alkaline matter adition process is with uniform stirring, until solution pH value is maintained at 4
Between ~ 6, depending on concrete numerical value is according to solution concrete condition, after solution PH reaches predetermined value, continue stirring a period of time,
Mixing time is 1 ~ 10 hour；Described alkaline matter is the sodium hydroxide solution of concentration 100-400g/L, nickel hydroxide or concentration
100-400g/L sodium hydroxide solution and the mixture of nickel hydroxide；
C reactants separate: the material operated through step B is carried out solid-liquid separation, the nickel solution after being purified and hydrogen-oxygen
Change nickel slag；Solid-liquid separation can use sucking filtration to separate or filter pressing separates；Nickel solution silicone content after purification is less than 0.005g/L.
2. according to the method for a kind of nickel solution deeply purifying and removing silicon described in right 1, it is characterised in that: described step C obtains
Nickel hydroxide slag can be used in step B, and described nickel hydroxide slag can be recycled for multiple times, and the nickel hydroxide slag produced first can be many
Secondary recycling 3-4 time.
3. according to the method for a kind of nickel solution deeply purifying and removing silicon described in right 1, it is characterised in that: this method is particularly suited for
The mixed solution nickel sulfate cobalt liquor of nickel sulfate, Nickel dichloride., nickel sulfate and Nickel dichloride. or sulphuric acid nickel cobalt and Nickel dichloride. mixed solution,
Nickel total concentration is 15 ~ 75g/L, and silicone content is 0.1 ~ 1g/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610709019.2A CN106191442A (en) | 2016-08-23 | 2016-08-23 | A kind of method of nickel solution deeply purifying and removing silicon |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610709019.2A CN106191442A (en) | 2016-08-23 | 2016-08-23 | A kind of method of nickel solution deeply purifying and removing silicon |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109082526A (en) * | 2018-08-17 | 2018-12-25 | 湖南金凯循环科技有限公司 | The method of silicon is removed in a kind of nickel cobalt manganese lithium solution |
| CN110423898A (en) * | 2019-08-27 | 2019-11-08 | 中国恩菲工程技术有限公司 | Desilication method in lateritic nickel ore leaching process |
| CN110812888A (en) * | 2019-10-23 | 2020-02-21 | 金川集团股份有限公司 | Method for removing silicon by nickel solution adsorption |
| CN110937622A (en) * | 2019-11-12 | 2020-03-31 | 中铝山东有限公司 | Method for preparing 4N gallium oxide from sponge gallium |
| CN112143888A (en) * | 2020-10-14 | 2020-12-29 | 衢州华友钴新材料有限公司 | Method for deeply removing silicon from nickel-cobalt leaching solution |
| CN112209452A (en) * | 2020-10-10 | 2021-01-12 | 广西银亿新材料有限公司 | Method for purifying and removing silicon from nickel-cobalt solution |
Citations (3)
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|---|---|---|---|---|
| US4149875A (en) * | 1978-03-06 | 1979-04-17 | Amax Inc. | Purification of nickel and cobalt metal powders by a caustic wash |
| CN101705377A (en) * | 2009-11-24 | 2010-05-12 | 锦州金业化工冶金技术咨询有限公司 | Method for extracting vanadium from stone coal by wet-process enrichment and pyrogenic-process conversion |
| CN102286661A (en) * | 2011-08-25 | 2011-12-21 | 云南锡业集团（控股）有限责任公司 | Method for direct electrolysis of laterite nickel ore by sulfuric acid leaching |
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2016
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Patent Citations (3)
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| US4149875A (en) * | 1978-03-06 | 1979-04-17 | Amax Inc. | Purification of nickel and cobalt metal powders by a caustic wash |
| CN101705377A (en) * | 2009-11-24 | 2010-05-12 | 锦州金业化工冶金技术咨询有限公司 | Method for extracting vanadium from stone coal by wet-process enrichment and pyrogenic-process conversion |
| CN102286661A (en) * | 2011-08-25 | 2011-12-21 | 云南锡业集团（控股）有限责任公司 | Method for direct electrolysis of laterite nickel ore by sulfuric acid leaching |
Non-Patent Citations (1)
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| 龙 艳: "红土镍矿湿法处理现状及研究", 《湖南有色金属》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109082526A (en) * | 2018-08-17 | 2018-12-25 | 湖南金凯循环科技有限公司 | The method of silicon is removed in a kind of nickel cobalt manganese lithium solution |
| CN110423898A (en) * | 2019-08-27 | 2019-11-08 | 中国恩菲工程技术有限公司 | Desilication method in lateritic nickel ore leaching process |
| CN110423898B (en) * | 2019-08-27 | 2022-03-01 | 中国恩菲工程技术有限公司 | Desiliconization method in laterite nickel ore leaching process |
| CN110812888A (en) * | 2019-10-23 | 2020-02-21 | 金川集团股份有限公司 | Method for removing silicon by nickel solution adsorption |
| CN110937622A (en) * | 2019-11-12 | 2020-03-31 | 中铝山东有限公司 | Method for preparing 4N gallium oxide from sponge gallium |
| CN112209452A (en) * | 2020-10-10 | 2021-01-12 | 广西银亿新材料有限公司 | Method for purifying and removing silicon from nickel-cobalt solution |
| CN112143888A (en) * | 2020-10-14 | 2020-12-29 | 衢州华友钴新材料有限公司 | Method for deeply removing silicon from nickel-cobalt leaching solution |
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Application publication date: 20161207 |