CN105331809A - Application of annular space type centrifugal extractor to cobalt chloride extraction - Google Patents
Application of annular space type centrifugal extractor to cobalt chloride extraction Download PDFInfo
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- CN105331809A CN105331809A CN201510635825.5A CN201510635825A CN105331809A CN 105331809 A CN105331809 A CN 105331809A CN 201510635825 A CN201510635825 A CN 201510635825A CN 105331809 A CN105331809 A CN 105331809A
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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
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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
- C22B3/02—Apparatus therefor
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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
- C22B3/37—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing boron, silicon, selenium or tellurium
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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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- Inorganic Compounds Of Heavy Metals (AREA)
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Abstract
The invention provides application of an annular space type centrifugal extractor to cobalt chloride extraction. The application sequentially includes the steps of saponification, extraction, complementary extraction, acid pickling and air spinning, back extraction and air spinning, first-level water washing, acid pickling, and second-level water washing, wherein saponification is performed in a first tank and a second tank; the extraction level is two and extraction is performed in a fifth tank and a sixth tank; the complementary extraction level is two and complementary extraction is performed in a third tank and a fourth tank; the acid pickling level is three, acid pickling is performed in a seventh tank, an eighth tank and a ninth tank, the corresponding air spinning level is one, and air spinning is performed in a tenth tank; the back extraction level is three, back extraction is performed in an eleventh tank, a twelfth tank and a thirteenth tank, the corresponding air spinning level is one, and air spinning is performed in a fourteenth tank; and first-level water washing is performed in the fourteenth tank, first-level acid pickling is performed in a fifteenth tank, and second-level water washing is performed in a sixteenth tank. Due to the application, the process control level is improved, the organic input is reduced, a cobalt chloride solution extraction and transformation process is adopted for producing cobaltosic oxide, the process that nitric acid is used for dissolving electrical cobalt is replaced, operation is easy and convenient, generation of nitrogen oxide is avoided, the process is safe and reliable, and environmental pollution is lowered.
Description
Technical field
The invention belongs to technical field of wet metallurgy, relate to phase-splitting transition of solution in the non-ferrous metal industries such as nickel cobalt, separation, be specifically related to the application of a kind of annulus type centrifugal extractor in cobalt chloride extraction.
Background technology
Along with the fast development of battery industry, cobalt acid lithium is as the raw material of lithium battery material, and nearly ten years and even rear Two decades years are that the speed that comparatively prevails of cobalt market is in growth.As the raw material supply base that cobalt acid lithium is produced, employing electrodeposited cobalt is raw material, and the tricobalt tetroxide product of production exists: produce cost high, economic benefit is limited, and nitric acid dissolve environment is poor.Therefore, the replacing of process modification and system reduces costs, improves the Main Means that the market competitiveness takes.Centrifugal extractor is as the efficient extraction equipment of one, although can to purify, be separated containing non-ferrous metals such as cobalts, in liquid phase separation and phase-splitting, tool percentage extraction is low, extraction is not thorough.
Summary of the invention
In order to solve the above-mentioned problems in the prior art, the invention provides the application of a kind of annulus type centrifugal extractor in cobalt chloride extraction.
The technical solution used in the present invention is: the application of a kind of annulus type centrifugal extractor in cobalt chloride extraction, described application is carried out as follows, utilize annulus type centrifugal extractor, carry out saponification adding the organic and sodium hydroxide of P507 for second case, saponification degree is 70%, saponification liquor enters the 5th case, 6th case carries out 2 grades of extractions to the feed liquid of chloride containing cobalt, extraction agent is P507 and the sulfonated kerosene of 1:1 by volume, the organic phase of liquid phase and Supported Co is obtained after extraction, liquid phase returns in the 3rd case and the 4th case, the organic phase of Supported Co enters the 7th case successively, 8th case, 0.3mol/L nitric acid is adopted to carry out 3 grades of impurity washings in 9th case, enter the tenth case sky after washing and get rid of the organic phase and liquid phase that obtain containing cobalt, liquid phase returns the 7th case and continues washing, continue to enter the tenth case sky after washing to get rid of, the liquid phase obtained after final sky gets rid of enters in the 4th case and continues saponification, the organic phase containing cobalt obtained is got rid of to the tenth case sky and enters the 11 case, 12 case, the back extraction nitric acid adding concentration 3mol/L for the 13 casees again carries out 3 grades of reextraction and obtains Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES liquid and the organic phase containing a small amount of cobalt, organic phase containing a small amount of cobalt enters in the 14 casees successively carries out one-stage water wash, pickling in the 15 casees, in the 16 casees after secondary washing removing small part cobalt, organic phase returns the first case, continue for second case to recycle, secondary washing lotion is arranged outward, in addition, in first case, add the organic and sodium hydroxide of P507 carry out saponification, saponification degree is 20%, and saponification liquor enters the 3rd case, the 4th case carries out to the 5th case aqueous phase out and the 7th case aqueous phase out benefits and extracts.
Further, it is 0.3m that the one-stage water wash carried out in the 14 casees controls discharge
3obtain 1 grade of washing lotion and organic phase after/h washing, organic phase enters in the 15 casees and adopts 6mol/L hydrochloric acid control flow to be 0.3m to organic phase
3/ h obtains pickle solution and organic phase, organic phase enter in the 16 casees to organic phase adopt pure water carry out secondary washing control flow be 0.3m
3/ h obtains secondary washing lotion and organic phase.
Further, saponification liquor enters the 3rd case, the 4th case carries out benefit extraction to the 5th case aqueous phase out and the 7th case aqueous phase out, mend and extract the raffinate that obtains, and carry out 1 grade of washing lotion that one-stage water wash obtains in the 14 casees, the pickle solution that in the 15 casees, pickling obtains all reclaims.
Wherein, above-mentioned annulus type centrifugal extractor is Φ 300 glass fiber reinforced plastic centrifugal extractor.
the invention has the beneficial effects as follows:glass fiber reinforced plastic centrifugal extractor of the present invention is successfully applied to the extraction of cobalt liquor, improves technology controlling and process level, decreases organic input amount, reduces initial cost; Adopt cobalt chloride solution abstraction and type-reverting Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES explained hereafter tricobalt tetroxide, the raw materials for production of tricobalt tetroxide and production cost are significantly reduced, improves added value and the market competitiveness of tricobalt tetroxide; Adopt cobalt chloride solution abstraction and type-reverting explained hereafter tricobalt tetroxide, replace nitric acid dissolve electricity cobalt, easy and simple to handle, avoid the generation of oxynitride, make production process safer, site environment is greatly improved, and reduces environmental pollution.
The present invention extracts feed liquid by rational proportion, adjustment extraction, washing progression make cobalt chloride solution make the transition into Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES and sodium hydroxide synthesis is utilized to be prepared into cobaltous hydroxide, calcining cobaltous hydroxide is tricobalt tetroxide, thus reduction production cost, thorough replacement nitric acid dissolve electrodeposited cobalt, eliminates the unsafe factor of nitric acid dissolve process.Annulus type centrifugal extractor is used for cobalt chloride abstraction and type-reverting Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES technique, grope through repetition test and parameter, by analyzing the difference of specific gravity of the organic and aqueous phase of load, shown that best stream compares, saponification degree and feed liquid, nitric acid isoconcentration, after making transition, concentration and index reach expection object.Utilize the annulus type centrifugal extractor of Ф 20-300, saponifying agent is P
507+ sodium hydroxide, the ratio 1:1 of saponification degree 60-70%, P507 and sulfonated kerosene, the concentration 3mol/L of back extraction nitric acid, obtaining Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES concentration can reach more than 85g/L; Centrifugal extractor is in cobalt chloride abstraction and type-reverting cobalt nitrate solution process, and its washing concentration of nitric acid and flow determine the clarity of raffinate containing organic phase after cobalt and back extraction; Be separated in feed separation with phase process thoroughly, working efficiency is high, can carry out the transition of non-ferrous metal and the conversion of system such as nickel cobalt.
Accompanying drawing explanation
Fig. 1. the process flow sheet of the embodiment of the present invention 1;
Fig. 2. tricobalt tetroxide shape appearance figure prepared by the present invention.
Embodiment
embodiment 1
As shown in Figure 1, the application of Φ 300 glass fiber reinforced plastic centrifugal extractor in cobalt chloride extraction: wherein comprise saponification, extraction, benefit extraction successively, acid elution sky gets rid of, sky of stripping gets rid of, 1 grade of washing, pickling and secondary are washed, saponification in first case 1 and second case 2, extraction progression is 2 grades to carry out in the 5th case 5, the 6th case 6, benefit extraction progression is 2 grades to carry out in the 3rd case 3, the 4th case 4, acid elution progression is 3 grades to carry out in the 7th case 7, the 8th case 8, the 9th case 9, and sky gets rid of progression 1 grade to carry out in the tenth case 11; Reextraction progression is 3 grades to carry out in the 11 casees 11, the 12 casees 12, the 13 casees 13, and sky gets rid of in progression 1 grade the 14 casees 4 and carries out; 1 grade of washing is carried out in the 14 casees 14, and 1 grade of pickling is carried out in the 15 casees 15, and 2 grades of washings are carried out in the 16 casees 16.Whole technological process is specific as follows: carry out saponification adding the organic and sodium hydroxide of P507 for second case 2, saponification degree is 70%, saponification liquor enters the 5th case 5, 6th case extracts feed liquid for 6 casees, the organic phase of liquid phase and Supported Co is obtained after extraction, liquid phase returns in the 3rd case 3 and the 4th case 4, 7th case 7 is entered successively to the organic phase of Supported Co, 8th case 8, 0.3mol/L nitric acid is adopted to carry out 3 grades of impurity washings in 9th case 9, enter the tenth case 10 sky after washing and get rid of the organic phase and liquid phase that obtain containing cobalt, load organic phases enters the 11 casees 11, the 12 casees 12, the 13 casees 13, the back extraction nitric acid adding concentration 3mol/L again carries out 3 grades of reextraction and obtains Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES liquid and organic phase (containing small part cobalt), organic phase is again through 1 grade of washing the 14 casees 14, pickling the 15 casees 15, wash the 16 casees 16 for 2 grades, first case 1 is returned after removing small part cobalt, continue to recycle for second case 2, 2 grades of water lotions are arranged outward, in addition, in first case 1, add the organic and sodium hydroxide of P507 carry out saponification, saponification degree is 20%, and saponification liquor enters the 3rd case 3, the 4th case 4 carries out to the 5th case 5 aqueous phase out and the 7th case 7 aqueous phase out benefits and extracts, raffinate, 1 grade of washing lotion, pickle solution centralized recovery.Wherein, it is 0.3m that the one-stage water wash carried out in described the 14 casees controls discharge
3obtain 1 grade of washing lotion and organic phase after/h washing, organic phase enters in the 15 casees and adopts 6mol/L hydrochloric acid control flow to be 0.3m to organic phase
3/ h obtains pickle solution and organic phase, organic phase enter in the 16 casees to organic phase adopt pure water carry out secondary washing control flow be 0.3m
3/ h obtains secondary washing lotion and organic phase.
Table 1 Φ 300 annulus type centrifugal extractor is used for cobalt chloride Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES processing parameter transition
Index before and after transition, and prepare tricobalt tetroxide index in table 2:
Tricobalt tetroxide partial data statistics (g/L, %) produced by table 2 cobalt chloride abstraction and type-reverting Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES
As can be seen from Table 2, utilize annulus type centrifugal extractor that cobalt chloride solution is made the transition into cobalt nitrate solution, and solution index after transition is good, as shown in Figure 2, tricobalt tetroxide quality product prepared by the cobalt nitrate solution of production satisfies the demands; Organic phase returns second stage employ, and raffinate is containing cobalt lower than 0.1g/L, and environment is better, compare electrodeposited cobalt dissolving Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES and prepare tricobalt tetroxide product, product cost obtains and significantly reduces, and by calculating, after transition, yield is more than 98%, meets expection object.
Claims (4)
1. the application of annulus type centrifugal extractor in cobalt chloride extraction, it is characterized in that: described application is carried out as follows, utilize annulus type centrifugal extractor, add the organic and sodium hydroxide of P507 at the second case (2) and carry out saponification, saponification degree is 70%, saponification liquor enters the 5th case (5), 6th case (6) carries out 2 grades of extractions to the feed liquid of chloride containing cobalt, extraction agent is P507 and the sulfonated kerosene of 1:1 by volume, the organic phase of liquid phase and Supported Co is obtained after extraction, liquid phase returns in the 3rd case (3) and the 4th case (4), the organic phase of Supported Co enters the 7th case (7) successively, 8th case (8), 0.3mol/L nitric acid is adopted to carry out 3 grades of impurity washings in 9th case (9), enter the tenth case (10) sky after washing and get rid of the organic phase and liquid phase that obtain containing cobalt, liquid phase returns the 7th case (7) and continues washing, continue to enter the tenth case (10) sky after washing to get rid of, the liquid phase obtained after final sky gets rid of enters in the 4th case (4) and continues saponification, the organic phase containing cobalt obtained is got rid of to the tenth case (10) sky and enters the 11 case (11), 12 case (12), the back extraction nitric acid that 13 case (13) adds concentration 3mol/L again carries out 3 grades of reextraction and obtains Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES liquid and the organic phase containing a small amount of cobalt, organic phase containing a small amount of cobalt enters in the 14 case (14) successively carries out one-stage water wash, pickling in 15 case (15), in 16 case (16) after secondary washing removing small part cobalt, organic phase returns the first case (1), second case (2) continues to recycle, secondary washing lotion is arranged outward, in addition, in the first case (1), add the organic and sodium hydroxide of P507 carry out saponification, saponification degree is 20%, and saponification liquor enters the 3rd case (3), the 4th case (4) carries out benefit extraction to the 5th case (5) aqueous phase out and the 7th case (7) aqueous phase out.
2. the application of a kind of annulus type centrifugal extractor as claimed in claim 1 in cobalt chloride extraction, is characterized in that: it is 0.3m that the one-stage water wash carried out in the 14 case (14) controls discharge
3obtain 1 grade of washing lotion and organic phase after/h washing, organic phase enters in the 15 case (15) and adopts 6mol/L hydrochloric acid control flow to be 0.3m to organic phase
3/ h obtains pickle solution and organic phase, organic phase enter in the 16 case (16) to organic phase adopt pure water carry out secondary washing control flow be 0.3m
3/ h obtains secondary washing lotion and organic phase.
3. the application of a kind of annulus type centrifugal extractor as claimed in claim 1 in cobalt chloride extraction, it is characterized in that: saponification liquor enters the 3rd case (3), the 4th case (4) carries out benefit extraction to the 5th case (5) aqueous phase out and the 7th case (7) aqueous phase out, mend the raffinate extracting and obtain, and the 14 carries out 1 grade of washing lotion that one-stage water wash obtains in case (14), the pickle solution that in the 15 case (15), pickling obtains all reclaims.
4. the application of a kind of annulus type centrifugal extractor as described in any one of claim 1-3 in cobalt chloride extraction, is characterized in that: annulus type centrifugal extractor is Φ 300 glass fiber reinforced plastic centrifugal extractor.
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| CN201510635825.5A CN105331809B (en) | 2015-09-30 | 2015-09-30 | A kind of application of annulus type centrifugal extractor in cobalt chloride extraction |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108060302A (en) * | 2017-12-14 | 2018-05-22 | 滁州学院 | A kind of extractant centrifuges saponification process |
| CN108359811A (en) * | 2018-03-07 | 2018-08-03 | 昆明理工大学 | A method of being stripped cobalt using micro-fluidic technologies |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101275240A (en) * | 2007-12-25 | 2008-10-01 | 金川集团有限公司 | Processing method for anode liquor for electrowinning cobalt |
| JP2011006759A (en) * | 2009-06-29 | 2011-01-13 | Sumitomo Metal Mining Co Ltd | Method for producing cobalt chloride aqueous solution |
| CN102505071A (en) * | 2011-12-29 | 2012-06-20 | 清华大学 | Glass fiber reinforced plastic centrifugal extractor and method for implementing extraction transformation of metal compounds |
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- 2015-09-30 CN CN201510635825.5A patent/CN105331809B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101275240A (en) * | 2007-12-25 | 2008-10-01 | 金川集团有限公司 | Processing method for anode liquor for electrowinning cobalt |
| JP2011006759A (en) * | 2009-06-29 | 2011-01-13 | Sumitomo Metal Mining Co Ltd | Method for producing cobalt chloride aqueous solution |
| CN102505071A (en) * | 2011-12-29 | 2012-06-20 | 清华大学 | Glass fiber reinforced plastic centrifugal extractor and method for implementing extraction transformation of metal compounds |
Non-Patent Citations (1)
| Title |
|---|
| 周炳珍: "用P204和P507脱除含钴废料中的杂质生产高纯度氯化钴", 《有色金属》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108060302A (en) * | 2017-12-14 | 2018-05-22 | 滁州学院 | A kind of extractant centrifuges saponification process |
| CN108359811A (en) * | 2018-03-07 | 2018-08-03 | 昆明理工大学 | A method of being stripped cobalt using micro-fluidic technologies |
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