CN109518006A - The minimizing technology of trace cobalt in a kind of nickel chloride solution - Google Patents
The minimizing technology of trace cobalt in a kind of nickel chloride solution Download PDFInfo
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- CN109518006A CN109518006A CN201811279831.1A CN201811279831A CN109518006A CN 109518006 A CN109518006 A CN 109518006A CN 201811279831 A CN201811279831 A CN 201811279831A CN 109518006 A CN109518006 A CN 109518006A
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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
-
- 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
- C22B23/0476—Separation of nickel from cobalt
-
- 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
- C22B3/3842—Phosphinic acid, e.g. H2P(O)(OH)
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/06—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese
- C25C1/08—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese of nickel or cobalt
-
- 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
It is nickel chloride solution by using the molten liquid making of 99.95% nickel plate electricity the present invention provides a kind of minimizing technology of trace cobalt in nickel chloride solution, or is made into nickel chloride solution with commercially available purer nickel chloride crystal；Extraction deeply purifying and removing cobalt, copper, iron are carried out then nickel chloride solution to be mixed to the solvent naphtha of proper ratio with extractant Cyanex272 after；Pure nickel chloride solution is obtained after removal of impurities, cobalt content is reduced to 0.001g/L, meanwhile, copper, iron content are reduced to 0.0001g/L, realize that the same process removes the purpose of three kinds of impurity elements.This method is applied in high purity nickel production, and obtaining nickel plate product purity is 99.999%, and wherein cobalt and copper content are respectively less than 1ppm, and iron content is less than 2ppm.Method of the invention, simple for process, product quality is high, stability is good, and easy to industrialized production, processing capacity is big.Nickel chloride solution after removal of impurities meets the needs of preparing high purity nickel and producing other high-purity nickel products.
Description
Technical field
The invention belongs to non-ferrous metal smelting technologies, and be related to high purity nickel metal prepares solution, and in particular to a kind of
The minimizing technology of trace cobalt in nickel chloride solution.
Background technique
Nickel is silvery white ferromagnetic metal, mainly for the production of stainless steel, high-temperature alloy steel, high-performance special alloy and nickel
Base depositing materials.High purity nickel has extremely strong corrosion resistance, mechanical strength and excellent plasticity, is widely used in large-scale integrated electricity
Road and wiring material, magnetic membrane material and special package material, rocket, radar, aircraft, tank, naval vessels, guided missile, universe fly
The high-tech skills such as machine manufacture, ceramic paint, permanent-magnet material, electronic telecontrol, nuclear industry, long-range control in ship and civilian industry
In art, it is also used to microelectronics industry sputtering target material and ion film plating, evaporation coating, manufacture high purity reagent, standard specimen and advanced alloy
Deng being national defence and civilian valuable source.
The preparation of high purity nickel metal needs the nickel solution of high-purity, and the deep purifying purification technique of nickel solution just becomes preparation
The key of high-purity nickel plate.Impurity element is mainly the metal ions such as cobalt, copper, iron in nickel solution, wherein nickel, cobalt property very phase
Seemingly, it is difficult to separate, the separation especially in the nickel solution of high concentration containing micro cobalt is always the research in nickel cobalt hydrometallurgy
Emphasis, hot and difficult issue.
It is generally more to remove cobalt, extraction, ion-exchange and film using oxydrolysis in Separation of nickel and cobalt technology
A variety of methods such as separation.
Production method about high purity nickel, it is known that patent have China patent CN 102268691A, 1084896 CN,
Japan Patent JP1489642, JP6136584A, JP2007290937A etc..
Chinese patent CN 102268691A discloses a kind of production method of high purity nickel, is electrolysed using nickel salt solution
Nickel is obtained, before electrolysis, pretreatment removes the impurity element in electrolyte, and electrolyte passes sequentially through ion exchange resin and activity
The adsorption treatment that charcoal carries out, the ion exchange resin include at least Diphonix resin and M-4195 resin；It is electrolysed
When, recycle electrolyte constantly between electrolytic cell-ion exchange resin-active carbon-electrolytic cell；After electrolysis, electrolytic nickel
Then vacuum outgas carries out vacuum melting and obtains 99.999% or more high-purity nickel ingot.Ion exchange removes the copper-lead zinc etc. in solution
Ion, except the depth of cobalt is limited, impurity-eliminating effect is undesirable in actual application, is not able to satisfy in actual production to high-purity chlorine
Change the requirement of cobalt liquor.
Chinese patent CN 1084896 prepares high purity nickel salt using ni-type extration resin substitution chromatography, keeps nickeliferous feed liquid logical
After the extration resin chromatographic column containing acid phosphine extractant for having switched to ni-type, the impurity such as the cobalt in nickel salt are separated, obtain purity
High purity nickel salt more than 99.99%, the rate of recovery are greater than 99%.Extractant using acid phosphine extractant such as P507 or 5709, P272,
P554,P204,P5601.Extration resin technique in the invention be not it is very stable, present extration resin makes and uses technology also
It is not very mature, and 4N high purity nickel can only be obtained, high-precision requirement is not achieved.
Japan Patent CN1489642A (JP233036/2001) discloses a kind of technology for preparing 5N high purity nickel, using containing
When nickel solution is electrolysed as electrolyte, it is 2-5 that anolyte, which is adjusted to pH value, and oxidant is added in anolyte
The impurity such as iron, cobalt, copper are precipitated in the form of hydroxide, or logical by the preparation electrolysis removing impurity, or addition Ni foil
Cross the displacement reaction removing impurity further makes after no matter using a kind of or two or more removing impurity of combination in these methods
Impurity is removed with filter, uses the solution after eliminating impurity to carry out electrolysis as catholyte and obtains purity 5N
High purity nickel more than (99.999 weight %).In this method hydrolysis methods except cobalt, copper, the method time of iron it is long, temperature is high, molten
It is even more more difficult to control when liquid measure is big, and the precision controlled is not high, combined method is again more troublesome, and is not easy to reach high-precision
It is required that.
Japan Patent JP6136584A, which discloses chlorine leaching, electroextraction when not increasing new equipment and produces, to be surpassed
High-purity and high purity nickel provides a method.Nickeliferous >=65g/L and the nickel chloride solution containing cobalt≤1.5mg/L are with 70-100ml/h
Speed first electrolytic cell be added obtain high purity nickel, containing cobalt≤0.25mg/L first step electrolysis waste solution it is degassed after make to dissolve chlorine
Second electrolytic cell is added with the speed of 100-150ml/h after≤0.01g/l, adjusting pH value 1.1-1.8 and obtains ultra-pure electricity
Solve nickel.This method is at high cost, and since nickel cobalt property is similar, operating process is not easily controlled, technique be not it is particularly stable, removal of impurities
Depth is not very high.
Japan Patent JP2007290937A, which is provided, purifies impurity element copper, iron, the side of cobalt and zinc in a kind of nickel chloride solution
Method is reached by the way that the water-soluble metal chloride adjustment total cl concn of solution is added in the acid chlorization nickel solution to impure element
To 8.5-10.0 mol/L, concentration of hydrochloric acid≤3 mol/L, nickel chloride solution adjusted is contacted with strong basic anion-exchange resin
It is adsorbed and removed impurity element.The concentration operation that chlorine is adjusted in the invention is upper comparatively laborious, and cobalt cannot be completely formed in solution
Anion, anion exchange resin are limited except the depth of cobalt.3mol/L hydrochloric acid solution acidity is relatively high, is easy special to equipment
Damage, pollutes the environment.
Summary of the invention
In order to solve the deficiency of the above method, the purpose of the present invention is to provide trace cobalts in a kind of removal nickel chloride solution
Method, solution after using removal of impurities for raw material makes the nickel plate product purity of output, and to reach 99.999%, stability good.
The technical solution adopted by the invention is as follows: in a kind of nickel chloride solution trace cobalt minimizing technology, specifically include with
Lower step
Step a. prepares nickel chloride solution: being by the molten liquid making of 99.95% nickel plate electricity or nickel chloride crystal wiring solution-forming concentration
The nickel chloride solution of 100 ~ 220g/L；
Step b. adjusts solution ph: adjustment nickel chloride solution pH value is stand-by to 1.0-1.5；
The processing of step c. extractant: extractant Cyanex272 is mixed with sulfonated kerosene, first uses 300-400g/L hydroxide
Sodium solution carries out soda soap, then carries out nickel soap with nickel chloride solution, obtains the Cyanex272 organic phase of nickel soap；
Step d. abstraction impurity removal: the step b Cyanex272 organic phase for mixing up the nickel chloride solution and step c nickel soap of pH value is mixed
It closes, extracting and purifying removes cobalt, copper and iron simultaneously, and the mass concentration ratio of nickel cobalt reaches 400000 or more in solution after purification.
Preferably, in step a, the nickel chloride solution is that the molten liquid making of nickel plate electricity or nickel chloride crystal are configured to
Nickel chloride solution, wherein the mass concentration of nickel is 100 ~ 220g/L, and the mass concentration of cobalt is 0.001 ~ 0.01g/L.
Preferably, in step c, extractant Cyanex272 is 2 ~ 10% by volume in the Cyanex272 organic phase,
Sulfonated kerosene is 90 ~ 98%, and soda soap saponification rate is 30 ~ 50%.
Preferably, in step d, extraction phase ratio 1:1 extracts 2 ~ 6 grades of series, and purification afterchlorinate nickel solution cobalt content is less than
0.001g/L, copper, iron content are respectively less than 0.0001g/L.
Preferably, in step c, it is molten to be greater than the 5-15g/L nickel chloride that 99.99% nickel chloride is made into purity for the nickel soap
Liquid, nickel soap compare 1:1,2 ~ 4 grades of nickel soap series.
A kind of nickel plate for using nickel chloride solution obtained by the above method to prepare for raw material, using the purified chlorine of step d
Change nickel solution electrodeposition, control condition are carried out in Winning cell are as follows: solution ph be greater than 1,50 ~ 70 DEG C of temperature, current density 30 ~
100A/m2, 1.7 ~ 2.2V of voltage, the electrodeposition period is 4 ~ 7 days, and nickel concentration is 50 ~ 200g/L in electric effusion；Nickel plate is obtained after electrodeposition
Purity is that 99.999%, wherein cobalt and copper content are less than 1ppm, and iron content is less than 2ppm.
The beneficial effects of the present invention are: the present invention is by using the electric molten liquid making of 99.95% nickel plate or commercially available nickel chloride
Crystal is made into nickel chloride solution；Then nickel chloride solution is subjected to extraction deep purifying with nickel soap Cyanex272 organic extractant
Except cobalt, copper, iron；Pure nickel chloride solution is obtained after removal of impurities, cobalt content is reduced to 0.001g/L, meanwhile, copper, iron content reduce
To 0.0001g/L, realize that the same process removes the purpose of three kinds of impurity elements.This method is applied in high purity nickel production, is obtained
Nickel plate product purity is 99.999%, and wherein cobalt and copper content are respectively less than 1ppm, and iron content is less than 2ppm.Method of the invention, work
Skill is simple and easy, and impurity-eliminating effect is good, synchronously completes the deep purifying of the impurity such as cobalt, copper, iron, technical process continuous-stable, easily
In industrialized production, processing capacity is big, it is possible to provide the nickel chloride solution of large-batch high-purity, the nickel chloride solution after removal of impurities meet
The high purity nickel demand of preparation 99.999%, it can also be used to which the other industries high to nickel chloride solution purity requirement, the impurity-removing method is also
In the preparation process that may be used on other high-purity nickel products.
Specific embodiment
Raw material: the molten liquid making of 99.95% nickel plate electricity is nickel chloride solution, and nickel plate product producer is Jinchuan Group Co., Ltd, is produced
Product index is shown in Table 1, and nickel chloride crystal producer is Jin Ke non-ferrous metal Co., Ltd, and product index is shown in Table 2.
1 nickel plate product index of table
2 nickel chloride product index of table
Embodiment 1
The minimizing technology of trace cobalt in a kind of nickel chloride solution, specifically includes the following steps:
Step a. prepares nickel chloride solution: being made into nickel chloride solution using the molten liquid making of 99.95% nickel plate electricity；
Step b. adjusts solution ph: with ammonium hydroxide or sodium hydrate regulator solution pH value 1 or more；
The pretreatment of step c. extractant: extraction organic phase is prepared, extractant Cyanex272 is mixed with sulfonated kerosene, wherein
Cyanex272 extractant is 8%, sulfonated kerosene 92%, and extractant saponification rate is 40%, and the good organic phase of soap first uses pure chlorine
Change nickel and carry out nickel soap, nickel soap is 5-15g/L with chlorination nickel concentration, and nickel soap is comparably 1:1, and nickel soap series is 3 grades；
Step d. abstraction impurity removal: the Cyanex272 organic phase hybrid extraction of the nickel chloride solution for mixing up pH value and nickel soap is removed
Miscellaneous, extraction is comparably 1:1, extracts 3 grades of series, three groups of parallel laboratory tests the results are shown in Table 3.
It purifies afterchlorinate nickel solution cobalt content and is less than 0.001g/L, copper, iron content are respectively less than 0.0001g/L, nickel cobalt quality
Concentration ratio reaches 400000 or more；It is recycled after obtained load organic counter, pickling, saponification.
The purified nickel chloride solution carries out electrodeposition, control condition in Winning cell are as follows: solution ph is greater than 1, temperature
70 DEG C of degree, current density 100A/m2, voltage 2.2V, the electrodeposition period is 7 days, and it is 99.999% that nickel plate purity is obtained after electrodeposition,
Middle cobalt and copper content are less than 1ppm, and iron content is less than 2ppm.
The solution index comparison of 3 nickel chloride solution of table removal of impurities front and back
Solution extracted is subjected to electrodeposition, experiment condition are as follows: pH value of solution=2, temperature 60 C, current density 50A/m2, electrodeposition 6
It, nickel content is 99.9997% in obtained nickel plate, and experimental result is shown in Table 4.
4 high-purity nickel impurity content index of table
Embodiment 2
The minimizing technology of trace cobalt in a kind of nickel chloride solution, specifically includes the following steps:
Step a. prepares nickel chloride solution: using being made into nickel chloride solution after nickel chloride dissolution of crystals；
Step b. adjusts solution ph: with ammonium hydroxide or sodium hydrate regulator solution pH value 1 or more；
The pretreatment of step c. extractant: extraction organic phase is prepared, extractant Cyanex272 is mixed with sulfonated kerosene, wherein
Cyanex272 extractant is 5%, sulfonated kerosene 95%, and extractant saponification rate is 50%, and the good organic phase of soap first uses pure chlorine
Change nickel and carry out nickel soap, nickel soap is 15g/L with chlorination nickel concentration, and nickel soap is comparably 1:1, and nickel soap series is 4 grades；
Step d. abstraction impurity removal: the Cyanex272 organic phase hybrid extraction of the nickel chloride solution for mixing up pH value and nickel soap is removed
Miscellaneous, extraction is comparably 1:1, extracts 5 grades of series, experimental result such as table 5, purification afterchlorinate nickel solution cobalt content is less than 0.001g/
L, copper, iron content are respectively less than 0.0001g/L, and nickel cobalt mass concentration ratio reaches 400000 or more；Obtained load organic counter, acid
Wash, be saponified after be recycled.
The solution index comparison of 5 nickel chloride solution of table removal of impurities front and back
Above-mentioned purification afterchlorinate nickel solution is subjected to electrodeposition, experiment condition are as follows: pH value of solution=4.5, temperature 70 C, current density
80A/m2, electrodeposition 7 days, it was 99.999724% that nickel content in nickel plate is obtained after control condition electrodeposition.Nickel plate purity is 99.999%,
Wherein cobalt and copper content are less than 1ppm, and iron content is less than 2ppm.Experimental result is shown in Table 6.
6 high-purity nickel impurity content index of table
It can be seen that by means of the present invention from above content, purity is that the electric molten or nickel chloride crystal of 99.95% nickel plate is molten
The nickel chloride solution that solution obtains by that can effectively remove impurity cobalt after Cyanex272 extraction after nickel soap, while realizing that copper, iron are miscellaneous
The synchronous removal of matter, obtains the high-purity nickel that purity is 99.999% or more.
The above is presently preferred embodiments of the present invention, all to appoint according to the technical essence of the invention to above embodiments
The simple modification, equivalent change and modification of what form, each falls within protection scope of the present invention.
Claims (7)
1. the minimizing technology of trace cobalt in a kind of nickel chloride solution, it is characterised in that: specifically include following steps
Step a. prepares nickel chloride solution: being by the molten liquid making of 99.95% nickel plate electricity or nickel chloride crystal wiring solution-forming concentration
The nickel chloride solution of 100 ~ 220g/L；
Step b. adjusts solution ph: adjustment nickel chloride solution pH value is stand-by to 1.0-1.5；
The processing of step c. extractant: extractant Cyanex272 is mixed with sulfonated kerosene, first uses 300-400g/L hydroxide
Sodium solution carries out soda soap, then carries out nickel soap with nickel chloride solution, obtains the Cyanex272 organic phase of nickel soap；
Step d. abstraction impurity removal: the step b Cyanex272 organic phase for mixing up the nickel chloride solution and step c nickel soap of pH value is mixed
It closes, extracting and purifying removes cobalt, copper and iron simultaneously, and the mass concentration ratio of nickel cobalt reaches 400000 or more in solution after purification.
2. the minimizing technology of trace cobalt in a kind of nickel chloride solution according to right 1, it is characterised in that: described in step a
Nickel chloride solution be the nickel plate molten liquid making of electricity or the nickel chloride solution that nickel chloride crystal is configured to, the wherein mass concentration of nickel
For 100 ~ 220g/L, the mass concentration of cobalt is 0.001 ~ 0.01g/L.
3. the minimizing technology of trace cobalt in a kind of nickel chloride solution according to right 1, it is characterised in that: described in step c
Cyanex272 organic phase in by volume extractant Cyanex272 be 2 ~ 10%, sulfonated kerosene be 90 ~ 98%, soda soap saponification rate
It is 30 ~ 50%.
4. the minimizing technology of trace cobalt in a kind of nickel chloride solution according to right 1, it is characterised in that: in step d, extraction
Compared to 1:1,2 ~ 6 grades of series are extracted, purification afterchlorinate nickel solution cobalt content is less than 0.001g/L, and copper, iron content are respectively less than
0.0001g/L。
5. the minimizing technology of trace cobalt in a kind of nickel chloride solution according to right 1, it is characterised in that: in step c, institute
Nickel soap is stated, is greater than the 5-15g/L nickel chloride solution that 99.99% nickel chloride is made into purity, nickel soap compares 1:1, nickel soap series 2 ~ 4
Grade.
6. a kind of nickel plate that the nickel chloride solution for using 1 the method for right to obtain is prepared for raw material, it is characterised in that: using step
The rapid purified nickel chloride solution of d carries out electrodeposition, obtains the high-purity nickel of cobalt content 1ppm after electrodeposition, and purity reaches 99.999%,
Copper content is less than 1ppm, and iron content is less than 2ppm.
7. a method of the nickel chloride solution for using any one of right 1-6 the method to obtain prepares nickel plate for raw material, special
Sign is: the purified nickel chloride solution carries out electrodeposition, control condition in Winning cell are as follows: solution ph is greater than 1, temperature
50 ~ 70 DEG C, 30 ~ 100A/m of current density2, 1.7 ~ 2.2V of voltage, the electrodeposition period be 4 ~ 7 days, in electric effusion nickel concentration be 50 ~
200g/L；It is that 99.999%, wherein cobalt and copper content are less than 1ppm that nickel plate purity is obtained after electrodeposition, and iron content is less than 2ppm.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110358915A (en) * | 2019-07-11 | 2019-10-22 | 兰州理工大学 | A kind of method of nickel and cobalt ions in separation electrolytic solution |
| CN112573592A (en) * | 2021-01-30 | 2021-03-30 | 浙江博瓦德新材料科技有限公司 | Preparation method of high-purity nickel protoxide |
| CN113981220A (en) * | 2021-11-05 | 2022-01-28 | 金川集团股份有限公司 | Method for separating nickel and cobalt from low-concentration nickel chloride solution by using C272 |
| CN114058845A (en) * | 2021-11-05 | 2022-02-18 | 金川集团股份有限公司 | Method for combined extraction in nickel chloride solution by utilizing P204 and N235 |
| WO2023213919A1 (en) | 2022-05-05 | 2023-11-09 | Umicore | Process for the oxidative leaching of a metal |
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| CN104313323A (en) * | 2014-10-17 | 2015-01-28 | 金川集团股份有限公司 | Extraction purification method of cobalt nickel hydroxide hydrochloric acid leaching solution |
| CN105349780A (en) * | 2015-11-20 | 2016-02-24 | 兰州金川新材料科技股份有限公司 | Purification method for nickel electric accumulated liquid for manufacturing high-purity nickel plate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110358915A (en) * | 2019-07-11 | 2019-10-22 | 兰州理工大学 | A kind of method of nickel and cobalt ions in separation electrolytic solution |
| CN112573592A (en) * | 2021-01-30 | 2021-03-30 | 浙江博瓦德新材料科技有限公司 | Preparation method of high-purity nickel protoxide |
| CN113981220A (en) * | 2021-11-05 | 2022-01-28 | 金川集团股份有限公司 | Method for separating nickel and cobalt from low-concentration nickel chloride solution by using C272 |
| CN114058845A (en) * | 2021-11-05 | 2022-02-18 | 金川集团股份有限公司 | Method for combined extraction in nickel chloride solution by utilizing P204 and N235 |
| WO2023213919A1 (en) | 2022-05-05 | 2023-11-09 | Umicore | Process for the oxidative leaching of a metal |
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