CN106756013A - A kind of method of the direct nickel cobalt saponification of P204, P507 - Google Patents
A kind of method of the direct nickel cobalt saponification of P204, P507 Download PDFInfo
- Publication number
- CN106756013A CN106756013A CN201611062660.8A CN201611062660A CN106756013A CN 106756013 A CN106756013 A CN 106756013A CN 201611062660 A CN201611062660 A CN 201611062660A CN 106756013 A CN106756013 A CN 106756013A
- Authority
- CN
- China
- Prior art keywords
- nickel
- cobalt
- saponification
- extractant
- acetate
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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
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
- C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
- C22B3/3844—Phosphonic acid, e.g. H2P(O)(OH)2
-
- 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
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses the method for the direct nickel cobalt saponification of a kind of P204, P507.Acetate dissolution nickel cobalt raw material is used first（Nickel cobalt oxide, hydroxide or carbonate）The Acetate Solution of cobalt or nickel is obtained, is then mixed with the Acetate Solution of cobalt or nickel using the extraction organic phase containing P204, P507, that is, obtain acetum after saponification, acetum can return to the Acetate Solution that cobalt or nickel are prepared as acetic acid raw material after saponification.The present invention by extractant and NaOH or ammoniacal liquor without reacting the compound for being transformed into sodium, ammonium first, again by itself and nickel cobalt reactant salt, it is converted into corresponding nickel cobalt soap, but extractant and nickel acetate, cobalt are directly reacted into a step and prepares nickel, cobalt soap, reduce reagent consumption, shorten technological process, reduce cost.The discharge containing sodium or ammonia nitrogen waste water is avoided, is conducive to environmental protection.
Description
Technical field
The invention belongs to hydrometallurgy or chemical field, and in particular to a kind of method of the direct nickel cobalt saponification of P204, P507.
Background technology
Requirement of the compound products of cobalt nickel to purity is higher（Reference pair answers GB《POV cobalt GB/T26523-
2011》,《GB/T 26524-2011 POV nickel》）, use more extracted with the solvent that P204, P507 are main extractant at present
Follow the example of and rough cobalt nickel compound is purified.When current solvent extraction purifying cobalt, nickel compound, need corresponding extraction more
Taking agent carries out corresponding cobalt, nickel transition, will extractant such as P204（H2R2）It is transformed into correspondence nickel or cobalt salt form（NiR2·
XH2R2, CoR2xH2R2）Abstraction impurity removal is carried out again.Existing transformation process is：First by extractant and NaOH or
The ammoniacal liquor reaction corresponding sodium salt of generation or ammonium salt, then react with nickel or cobalt salt, can just obtain correspondence extractant nickel or
Person's cobalt salt form（Abbreviation nickel, cobalt soap）（Bibliography：Purification production [J] the Anhui chemical industry of Jiang Jing POV nickel,
2008, 34(6):32-35.）.Existing process process prepares nickel, cobalt soap two steps of needs and can just obtain correspondence product, there is reagent
Consumption is big, complex technical process, high cost, and produces containing sodium or ammonia nitrogen waste water, is unfavorable for environmental protection.Therefore exploitation one is needed badly
Plant low cost, the method for preparing nickel, cobalt soap of clean environment firendly.
The content of the invention
In view of the shortcomings of the prior art, the invention provides the method for the direct nickel cobalt saponification of a kind of P204, P507, mesh
Be solve the consumption of existing process reagent big, complex technical process, high cost, and produce and contain sodium or ammonia nitrogen waste water, it is unfavorable
In deficiencies such as environmental protection, with process is simple, low cost, pollution isopreference is not formed.
Concretely comprise the following steps：
（1）By 180-220mL concentration for 0.1 ~ 15 mol/L acetum dissolving 50-70 g nickel cobalt raw materials obtain correspondence cobalt or
The Acetate Solution of nickel, temperature is 5 ~ 150 DEG C, and the reaction time is 1 ~ 300 minute, and endpoint pH is 5 ~ 7.5.
（1）It is by volume 1-2 by extractant and diluent:9 ratio is mixed to get extraction organic phase.
（3）By step（1）The Acetate Solution and step of gained cobalt or nickel（2）Gained extraction is organic to be mixed, and obtains soap
Acetum after change；The temperature of reaction is 5 ~ 90 DEG C, and the time is 0.1 ~ 60 minute, and extraction organic phase is molten with the acetate of cobalt or nickel
During liquid saponification, extractant in extraction organic phase（HR is represented）With cobalt acetate in solution or nickel acetate（MeCA is represented）Thing
Mass ratio is：nHR : nMeCA=1:0.1~1:10.
（4）Energy will be through step（3）Acetum return to step after saponification（1）As acetic acid raw material.
The extractant be acid phosphoric acid ester, acidic phosphonate and carboxylic acid extractant in one or more.
One kind in diluent sulfonated kerosene, kerosene, toluene and 260# solvent naphthas.
The nickel cobalt raw material is the one kind in nickel, the oxide of cobalt, hydroxide and carbonate.
There is prior art to compare, the beneficial effects of the invention are as follows：
（1）Compound without extractant and NaOH or ammoniacal liquor reaction to be transformed into sodium, ammonium, directly by extractant and vinegar
Sour nickel, cobalt react a step and prepare nickel, cobalt soap, reduce reagent consumption, shorten technological process, reduce cost.
（2）The discharge containing sodium or ammonia nitrogen waste water is avoided, is conducive to environmental protection.
Brief description of the drawings
Fig. 1 is process chart of the invention.
Specific embodiment
With reference to embodiment, the invention will be further described, and it is right that following examples are intended to illustrate rather than
The further restriction of invention.
Embodiment 1：
(1) it is that 3 mol/L acetums add 60g NiO compounds to be reacted 1 hour at 25 DEG C to 200mL concentration, obtains acetic acid
Nickel solution, pH value is 5.
（2）It is 2 by volume ratio:9 P507 and sulfonated kerosene is mixed to get extraction organic phase.
（3）By 100mL steps（2）The extraction organic phase for obtaining and 30mL steps（1）The nickel acetate solution of gained is mixed into
Row saponification, the temperature of reaction is 30 DEG C, and the time is 10 minutes, after split-phase, analysis shows, nickel saponification rate is in organic phase
53.5%。
Embodiment 2：
(1) it is that 4 mol/L acetums add 50g CoCO to 200mL concentration3Solid reacts 2 hours at 35 DEG C, obtains acetic acid
Cobalt liquor, pH value is 6.
（2）It is 1 by volume ratio:9 P204 and sulfonated kerosene is mixed to get extraction organic phase.
（3）By 100mL steps（2）The extraction organic phase for obtaining and 10mL steps（1）The cobalt acetate solution of gained is mixed into
Row saponification, the temperature of reaction is 60 DEG C, and the time is 3 minutes, after split-phase, analysis shows, nickel saponification rate is in organic phase
53.5%。
Embodiment 3：
（1）It is that 3.5 mol/L acetums add 50g Co (OH) to 200mL concentration2Solid reacts 4 hours at 45 DEG C, obtains
Cobalt acetate solution, pH value is 7.
（2）It is 1 by volume ratio:9 P204 and sulfonated kerosene is mixed to get extraction organic phase.
（3）By 100mL steps（2）The extraction organic phase for obtaining and 10mL steps（1）The cobalt acetate solution of gained is mixed into
Row saponification, the temperature of reaction is 50 DEG C, and the time is 3 minutes, after split-phase, analysis shows, nickel saponification rate is in organic phase
53.5%。
Embodiment 4：
（1）It is that 7 mol/L acetums add 80g Ni (OH) to 200mL concentration2Reacted 6 hours at 25 DEG C, obtain nickel acetate
Solution, pH value is 5.5.
（2）It is 2 by volume ratio:9 P507 and sulfonated kerosene is mixed to get extraction organic phase.
（3）By 100mL steps（2）The extraction organic phase for obtaining and 30mL steps（1）The nickel acetate solution of gained is mixed into
Row saponification, the temperature of reaction is 90 DEG C, and the time is 2 minutes, after split-phase, analysis shows, nickel saponification rate is in organic phase
63.5%。
Embodiment 5：
（1）Acetic acid water will be obtained after the saponification of embodiment 4 and is added to 85 g Ni (OH)2, regulation solution ph is 7.0, is filtered
To nickel acetate solution
(2) it is 2 by volume ratio:9 P507 and sulfonated kerosene is mixed to get extraction organic phase.
(3) by 100mL steps（2）The extraction organic phase for obtaining and 30mL steps（1）The nickel acetate solution of gained is mixed into
Row saponification, the temperature of reaction is 30 DEG C, and the time is 10 minutes, after split-phase, analysis shows, nickel saponification rate is in organic phase
51.2%。
Although combined exemplary embodiment describes the method for the present invention in detail, those skilled in the art should
This is understood, in the case where the spirit and scope that claim is limited are not departed from, embodiment can be modified.
Claims (1)
1. the method for the direct nickel cobalt saponification of a kind of P204, P507, it is characterised in that specific steps are carried out：
（1）By 180-220mL concentration for 0.1 ~ 15 mol/L acetum dissolving 50-70 g nickel cobalt raw materials obtain correspondence cobalt or
The Acetate Solution of nickel, temperature is 5 ~ 150 DEG C, and the reaction time is 1 ~ 300 minute, and endpoint pH is 5 ~ 7.5；
（2）It is by volume 1-2 by extractant and diluent:9 ratio is mixed to get extraction organic phase；
（3）By step（1）The Acetate Solution and step of gained cobalt or nickel（2）Gained extraction is organic to be mixed, after obtaining saponification
Acetum；The temperature of reaction is 5 ~ 90 DEG C, and the time is 0.1 ~ 60 minute, the Acetate Solution soap of extraction organic phase and cobalt or nickel
When changing reaction, extractant is with the amount of substance ratio of cobalt acetate in solution or nickel acetate in extraction organic phase：1:0.1~1:10；
（4）Energy will be through step（3）Acetum return to step after saponification（1）As acetic acid raw material；
The extractant be acid phosphoric acid ester, acidic phosphonate and carboxylic acid extractant in one or more；
One kind in the diluent sulfonated kerosene, kerosene, toluene and 260# solvent naphthas；
The nickel cobalt raw material is the one kind in nickel, the oxide of cobalt, hydroxide and carbonate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611062660.8A CN106756013A (en) | 2016-11-25 | 2016-11-25 | A kind of method of the direct nickel cobalt saponification of P204, P507 |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611062660.8A CN106756013A (en) | 2016-11-25 | 2016-11-25 | A kind of method of the direct nickel cobalt saponification of P204, P507 |
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| CN106756013A true CN106756013A (en) | 2017-05-31 |
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| CN201611062660.8A Pending CN106756013A (en) | 2016-11-25 | 2016-11-25 | A kind of method of the direct nickel cobalt saponification of P204, P507 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108946826A (en) * | 2018-07-31 | 2018-12-07 | 金川集团股份有限公司 | A method of handling copper in nickeliferous cobalt sulfate solution, manganese impurity |
| CN109516623A (en) * | 2018-11-16 | 2019-03-26 | 浙江万盛股份有限公司 | A kind of method of comprehensive utilization of tri butylethyl phosphate waste water |
| CN109912405A (en) * | 2019-03-30 | 2019-06-21 | 赣州逸豪优美科实业有限公司 | A kind of processing purifying technique of cobalt oxalate defective products |
| CN113174485A (en) * | 2021-04-29 | 2021-07-27 | 金川集团镍盐有限公司 | Method for deeply removing calcium and manganese in cobalt sulfate solution |
| CN113355512A (en) * | 2021-06-03 | 2021-09-07 | 华中科技大学 | Pretreatment method and extraction method of di (2-ethylhexyl) phosphate extractant |
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| JPH04304330A (en) * | 1991-03-29 | 1992-10-27 | Sumitomo Metal Mining Co Ltd | Solvent extracting method |
| CN102010999A (en) * | 2010-12-24 | 2011-04-13 | 湖南邦普循环科技有限公司 | Method for separating impurities from cobalt and/or nickel solution by non-saponifiable extraction |
| CN102181665A (en) * | 2011-04-13 | 2011-09-14 | 广西银亿科技矿冶有限公司 | Method for keeping balance of sodium-magnesium-water system in technique for extracting nickel from lateritic nickel ore by wet process |
| CN103740938A (en) * | 2014-01-13 | 2014-04-23 | 合肥融捷金属科技有限公司 | Method for recovering cobalt in cobalt carbonate production wastewater by saponification-free solvent extraction method |
| CN103757260B (en) * | 2014-01-13 | 2015-05-20 | 中国恩菲工程技术有限公司 | Treatment method of nickel-containing eluvial ores |
| CN105907972A (en) * | 2016-05-09 | 2016-08-31 | 芦秀琴 | Method for comprehensively recycling multiple valuable metals from electroplating sludge |
| CN105925804A (en) * | 2016-05-13 | 2016-09-07 | 南昌航空大学 | Nickel saponification method for acidic phosphor extraction agent organic phase |
-
2016
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| JPH04304330A (en) * | 1991-03-29 | 1992-10-27 | Sumitomo Metal Mining Co Ltd | Solvent extracting method |
| CN102010999A (en) * | 2010-12-24 | 2011-04-13 | 湖南邦普循环科技有限公司 | Method for separating impurities from cobalt and/or nickel solution by non-saponifiable extraction |
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Non-Patent Citations (1)
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108946826A (en) * | 2018-07-31 | 2018-12-07 | 金川集团股份有限公司 | A method of handling copper in nickeliferous cobalt sulfate solution, manganese impurity |
| CN109516623A (en) * | 2018-11-16 | 2019-03-26 | 浙江万盛股份有限公司 | A kind of method of comprehensive utilization of tri butylethyl phosphate waste water |
| CN109516623B (en) * | 2018-11-16 | 2021-06-01 | 浙江万盛股份有限公司 | Comprehensive utilization method of tributoxyethyl phosphate wastewater |
| CN109912405A (en) * | 2019-03-30 | 2019-06-21 | 赣州逸豪优美科实业有限公司 | A kind of processing purifying technique of cobalt oxalate defective products |
| CN109912405B (en) * | 2019-03-30 | 2021-12-31 | 赣州逸豪优美科实业有限公司 | Treatment and purification process of cobalt oxalate defective products |
| CN113174485A (en) * | 2021-04-29 | 2021-07-27 | 金川集团镍盐有限公司 | Method for deeply removing calcium and manganese in cobalt sulfate solution |
| CN113355512A (en) * | 2021-06-03 | 2021-09-07 | 华中科技大学 | Pretreatment method and extraction method of di (2-ethylhexyl) phosphate extractant |
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