CN103805783A - Method for purifying nickel-containing solution - Google Patents
Method for purifying nickel-containing solution Download PDFInfo
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- CN103805783A CN103805783A CN201210459876.3A CN201210459876A CN103805783A CN 103805783 A CN103805783 A CN 103805783A CN 201210459876 A CN201210459876 A CN 201210459876A CN 103805783 A CN103805783 A CN 103805783A
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- containing nickel
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Abstract
The invention provides a method for purifying a nickel-containing solution, relating to impurity removal of a nickel-containing solution produced by hydrometallurgy, particularly a method for removing impurities in a nickel-containing electrolyte in an electrolytic nickel production process. The method comprises the following steps: preparing a saponification organic phase containing di(2,4,4-trimethylamyl)hypophosphorous acid (the trade name of the extractant is Cyanex272); and carrying out counter-current extraction on the saponification organic phase and the nickel-containing solution to be purified in a mixing settling tank to lower the contents of iron, zinc, manganese, copper, lead and cobalt in the nickel-containing solution, thereby implementing quick and deep purification of the nickel-containing solution. By using the simple extraction technique stead of the precipitation, extraction, replacement, adsorption and other complex operations in the existing nickel-containing solution impurity removal technique, the method obviously enhance the production efficiency.
Description
Technical field
Purify a method for solution containing nickel, relate in the solution containing nickel removal of impurities, particularly electrolytic nickel production process of hydrometallurgy production, remove the method containing impurity in nickel electrolyte.
Background technology
In the production process of electrolytic nickel, the higher and often variation of the impurity such as copper, cobalt, zinc, manganese in thick nickel anode or nickel salt solution.Along with the carrying out of electrolysis, a large amount of impurity progressively accumulates.If can not be removed in time, can make impurity content exceeding index in electrolytic solution, have a strong impact on the quality of product.Nickel electrolyte purification impurity removal process mostly adopts following methods both at home and abroad at present: deironing adopts neutralizing hydrolysis method, jarosite process and hematite process.Copper removal adopts cementation or extraction process.Except cobalt adopts neutralizing hydrolysis, extraction or " black nickel " oxidizing water solution.Deleading, zinc adopt coprecipitation method, ion exchange method and extraction process.The removal of impurities flow process of for example Jinchuan Non-ferrous Metals Company is: M5640 is extraction agent extraction copper removal, hydrolysis deironing, and 717 resins dezincify, 330 resin deleadings, P507 extraction is except cobalt.
Early stage solution containing nickel purification process adopts P204 extraction route, copper, iron, zinc impurity in solution can only be removed, and cobalt, manganese impurity in raw material cannot be purified to required degree.When as high in copper in stock liquid, cobalt, zinc, manganese, just cannot meet the deep purifying needs of nickel solution, directly affect the quality of nickel product.Patent CN101126127 discloses a kind of nickel sulfate solution and has gone deimpurity method.First adopt yellow modumite method that iron ion is purified and removed the iron ion in solution; By P507 extraction agent extraction for liquid after deironing, copper, cobalt, zinc, manganese impurity are extracted in organic phase, then use 4N dilute hydrochloric acid by copper, cobalt, zinc, manganese back extraction again, strip liquor enters copper system, and raffinate enters subsequent handling.This invention reduces the bits that chemical precipitation method produces, and makes solution obtain deep purifying, has improved metal straight yield and quality product.
But that method as above still exists impurity element to remove kind is few, separation efficiency is not high enough, long flow path, the problems such as complex process.The present invention utilize than P204, P507 more excellent two (2,4,4-tri-methyl-amyl) Hypophosporous Acid, 50 (extraction agent commodity are called Cyanex 272) is extraction agent, in mixer-settler, realize fast, effectively and synchronously removing of Determination of Multi-Impurities by the method for extraction, simplified impurity removing equipment and processing condition.
Summary of the invention
The object of the invention is the deficiency existing in order to overcome prior art, provide one can remove quickly and efficiently de-iron, zinc, manganese, copper, lead, cobalt impurity, reduce foreign matter content, improve the method for solution containing nickel purity, with complicated operations such as the precipitation in the alternative existing solution containing nickel impurity removing technology of simple extraction process, extraction, displacement, absorption.
The object of the invention is to be achieved through the following technical solutions.
First produce and contain two (2,4,4-tri-methyl-amyl) the nickel soap organic phase of Hypophosporous Acid, 50 (extraction agent commodity are called Cyanex 272), then in mixer-settler, saponification organic phase and solution containing nickel to be clean are carried out to counter-current extraction operation, iron, zinc, manganese, copper, lead, cobalt contents in solution containing nickel are reduced jointly, realize the quick and deep purifying of solution containing nickel.
The present invention is characterised in that the extraction agent main component using in extraction process is two (2,4,4-tri-methyl-amyl) Hypophosporous Acid, 50 (extraction agent commodity is called Cyanex 272), and thinner is heptane, octane or sulfonated kerosene.
The present invention is characterised in that in the organic phase that extracting operation uses, the volumetric concentration of extraction agent is 5%-60%.
The present invention is characterised in that the extraction agent that extracting operation uses need to be prepared into the use of saponification form, and its saponification deg is 5%-50%, and the positively charged ion in organic phase is Ni
2+.
The present invention is characterised in that saponification organic phase and solution containing nickel carry out counter-current extraction operation in mixer-settler, and the progression of mixer-settler is 1-50 level.
The present invention is characterised in that and utilizes extracting operation that iron, zinc, manganese, copper, lead, cobalt contents in solution containing nickel are reduced jointly, realizes the quick and deep purifying of solution containing nickel.
The present invention is characterised in that as long as adopt extraction system and the operation of aforementioned statement, even if implement by stages in different spaces or different time, iron, zinc, manganese, copper, lead, the cobalt contents that can realize equally in solution containing nickel reduce jointly, complete the quick and deep purifying of solution containing nickel.
Embodiment
The method of preparing saponification organic phase belongs to the prior art that common extraction industry technology personnel know.Understand for ease of layman, now select a kind of conventional method for saponification and be described below: first by the extraction agent of metered proportions and mixing diluents, obtain common soda soap organic phase by adding the method for NaOH solution saponification.By common soda soap organic phase and containing Ni
2+solution mix and carry out ion-exchange, can obtain containing Ni
2+nickel soap organic phase.
According to the number of foreign matter content and the degree of purification that need to reach, the saponification organic phase preparing is carried out to counter-current extraction operation with solution containing nickel (liquid before extraction) to be clean in mixer-settler, until the foreign matter content in raffinate (solution containing nickel) suits the requirements.
Embodiment 1
Implementation condition: dose volume concentration is 60%, the Cyanex272 nickel soap heptane organic phase of saponification deg 25%.Liquid before extraction as shown in the table and saponification organic phase are carried out to counter-current extraction operation in 3 grades of mixer-settlers, and in the raffinate after purification, foreign matter content is reduced, and test result is as shown in the table.
Solution purification result: liquid, raffinate foreign matter content contrast (unit: mg/L) before extraction
| Solution composition | Iron | Zinc | Manganese | Copper | Plumbous | Cobalt |
| Liquid before extraction | 410 | 10.1 | 31.2 | 220 | 10.5 | 1270 |
| Raffinate | <0.05 | <0.05 | <0.05 | 4.31 | <0.05 | 530 |
Embodiment 2
Implementation condition: dose volume concentration is 5%, the Cyanex272 nickel soap heptane organic phase of saponification deg 50%.Liquid before saponification organic phase and extraction as shown in the table is carried out to counter-current extraction operation in 3 grades of mixer-settlers, and in the raffinate after purification, foreign matter content is reduced, and test result is as shown in the table.
Solution purification result: liquid, raffinate foreign matter content contrast (unit: mg/L) before extraction
| Solution composition | Iron | Zinc | Manganese | Copper | Plumbous | Cobalt |
| Liquid before extraction | 410 | 10.1 | 31.2 | 220 | 10.5 | 1270 |
| Raffinate | <0.05 | <0.05 | <0.05 | 17.7 | <0.05 | 650 |
Embodiment 3
Implementation condition: dose volume concentration is 30%, the Cyanex272 nickel soap sulfonated kerosene organic phase of saponification deg 5%.Liquid before saponification organic phase and extraction as shown in the table is carried out to counter-current extraction operation in 4 grades of mixer-settlers, and in the raffinate after purification, foreign matter content is reduced, and test result is as shown in the table.
Solution purification result: liquid, raffinate foreign matter content contrast (unit: mg/L) before extraction
| Solution composition | Iron | Zinc | Manganese | Copper | Plumbous | Cobalt |
| Liquid before extraction | 410 | 10.1 | 31.2 | 220 | 10.5 | 1270 |
| Raffinate | <0.05 | 0.20 | <0.05 | 3.74 | 2.14 | 600 |
Embodiment 4
Implementation condition: dose volume concentration is 10%, the Cyanex272 nickel soap octane organic phase of saponification deg 25%.Liquid before saponification organic phase and extraction as shown in the table is carried out to counter-current extraction operation in 50 grades of mixer-settlers, and in the raffinate after purification, foreign matter content is reduced, and test result is as shown in the table.
Solution purification result: liquid, raffinate foreign matter content contrast (unit: mg/L) before extraction
| Solution composition | Iron | Zinc | Manganese | Copper | Plumbous | Cobalt |
| Liquid before extraction | 610 | 71.3 | 11.0 | 26.1 | 5.19 | 22.4 |
| Raffinate | <0.05 | <0.05 | <0.05 | <0.05 | <0.05 | 0.19 |
Embodiment 5
Implementation condition: dose volume concentration is 15%, the Cyanex272 nickel soap octane organic phase of saponification deg 20%.Liquid before saponification organic phase and extraction as shown in the table is carried out to counter-current extraction operation in 20 grades of mixer-settlers, and in the raffinate after purification, foreign matter content is reduced, and test result is as shown in the table.
Solution purification result: liquid, raffinate foreign matter content contrast (unit: mg/L) before extraction
| Solution composition | Iron | Zinc | Manganese | Copper | Plumbous | Cobalt |
| Liquid before extraction | 610 | 71.3 | 11.0 | 26.1 | 5.19 | 22.4 |
| Raffinate | <0.05 | <0.05 | <0.05 | <0.05 | <0.05 | 0.21 |
Embodiment 6
Implementation condition: dose volume concentration is 10%, the Cyanex272 nickel soap octane organic phase of saponification deg 45%.Liquid before saponification organic phase and extraction as shown in the table is carried out to counter-current extraction operation in 1 grade of mixer-settler, and in the raffinate after purification, foreign matter content is reduced, and test result is as shown in the table.
Solution purification result: liquid, raffinate foreign matter content contrast (unit: mg/L) before extraction
| Solution composition | Iron | Zinc | Manganese | Copper | Plumbous | Cobalt |
| Liquid before extraction | 18.4 | 21.2 | 3.37 | 1.44 | 5.81 | 12.6 |
| Raffinate | <0.05 | <0.05 | <0.05 | <0.05 | 3.54 | 6.77 |
Embodiment 7
Implementation condition: dose volume concentration is 40%, the Cyanex272 nickel soap sulfonated kerosene organic phase of saponification deg 50%.Liquid before saponification organic phase and extraction as shown in the table is carried out to counter-current extraction operation in 4 grades of mixer-settlers, then raffinate is left standstill and within 1 day, introduce afterwards that new 12 grades of mixer-settlers and volumetric concentration are 33%, the Cyanex272 nickel soap organic phase of saponification deg 30% is carried out counter-current extraction operation, in raffinate after purification, foreign matter content is reduced, and test result is as shown in the table.
Solution purification result: liquid, raffinate foreign matter content contrast (unit: mg/L) before extraction
| Solution composition | Iron | Zinc | Manganese | Copper | Plumbous | Cobalt |
| Liquid before extraction | 1133 | 94.8 | 441 | 6810 | 47.5 | 10200 |
| Raffinate | <0.05 | <0.05 | <0.05 | <0.05 | <0.05 | 0.11 |
Claims (7)
1. one kind purifies the method for solution containing nickel, first produce and contain two (2,4,4-tri-methyl-amyl) the nickel soap organic phase of Hypophosporous Acid, 50 (extraction agent commodity are called Cyanex 272), then in mixer-settler, saponification organic phase and solution containing nickel to be clean are carried out to counter-current extraction operation, iron, zinc, manganese, copper, lead, cobalt contents in solution containing nickel are reduced jointly, realize the quick and deep purifying of solution containing nickel.
2. a kind of method that purifies solution containing nickel according to claim 1, it is characterized in that the extraction agent main component using in extraction process is two (2,4,4-tri-methyl-amyl) Hypophosporous Acid, 50 (extraction agent commodity are called Cyanex 272), thinner is heptane, octane or sulfonated kerosene.
3. a kind of method that purifies solution containing nickel according to claim 1, is characterized in that in saponification organic phase that extracting operation uses, the volumetric concentration of extraction agent is 5%-60%.
4. a kind of method that purifies solution containing nickel according to claim 1, is characterized in that the extraction agent that extracting operation uses need to be prepared into the use of saponification form, and its saponification deg is 5%-50%, and the positively charged ion in organic phase is Ni
2+.
5. a kind of method that purifies solution containing nickel according to claim 1, is characterized in that saponification organic phase and solution containing nickel carry out counter-current extraction operation in mixer-settler, and the progression of mixer-settler is 1-50 level.
6. a kind of method that purifies solution containing nickel according to claim 1, is characterized in that utilizing extracting operation that iron, zinc, manganese, copper, lead, cobalt contents in solution containing nickel are reduced jointly, realizes the quick and deep purifying of solution containing nickel.
7. a kind of method that purifies solution containing nickel according to claim 1, as long as adopt the extraction system and the operation that as above indicate in the 5th claim of 1-, even if in different spaces or different time phase in, iron, zinc, manganese, copper, lead, the cobalt contents that can realize equally in solution containing nickel reduce jointly, complete the quick and deep purifying of solution containing nickel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210459876.3A CN103805783A (en) | 2012-11-15 | 2012-11-15 | Method for purifying nickel-containing solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210459876.3A CN103805783A (en) | 2012-11-15 | 2012-11-15 | Method for purifying nickel-containing solution |
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|---|---|
| CN103805783A true CN103805783A (en) | 2014-05-21 |
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|---|---|---|---|
| CN201210459876.3A Pending CN103805783A (en) | 2012-11-15 | 2012-11-15 | Method for purifying nickel-containing solution |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105200235A (en) * | 2015-07-27 | 2015-12-30 | 江西睿锋环保有限公司 | Method for recycling valuable metal from electroplating sludge to prepare cathode copper and battery level nickel sulfate |
| 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 |
| CN109518006A (en) * | 2018-10-30 | 2019-03-26 | 金川集团股份有限公司 | The minimizing technology of trace cobalt in a kind of nickel chloride solution |
-
2012
- 2012-11-15 CN CN201210459876.3A patent/CN103805783A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 吴涛等: "Cyanex272萃取剂在镍钴分离中的应用实践", 《新疆有色金属》 * |
| 曹康学等: "Cyanex272镍钴分离萃取连续扩大试验总结", 《中国有色冶金》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105200235A (en) * | 2015-07-27 | 2015-12-30 | 江西睿锋环保有限公司 | Method for recycling valuable metal from electroplating sludge to prepare cathode copper and battery level nickel sulfate |
| CN105200235B (en) * | 2015-07-27 | 2017-10-27 | 江西睿锋环保有限公司 | The method that valuable metal prepares tough cathode and LITHIUM BATTERY nickel sulfate is reclaimed from electroplating sludge |
| 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 |
| CN109518006A (en) * | 2018-10-30 | 2019-03-26 | 金川集团股份有限公司 | The minimizing technology of trace cobalt in a kind of nickel chloride solution |
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Application publication date: 20140521 |