CN105274332A - Isolation technology and process for extracting Ni and Co from nickel-containing high-cobalt hydroxide - Google Patents
Isolation technology and process for extracting Ni and Co from nickel-containing high-cobalt hydroxide Download PDFInfo
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- CN105274332A CN105274332A CN201510806234.XA CN201510806234A CN105274332A CN 105274332 A CN105274332 A CN 105274332A CN 201510806234 A CN201510806234 A CN 201510806234A CN 105274332 A CN105274332 A CN 105274332A
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Abstract
The sulfuric acid total leaching process is adopted in an isolation technology and process for extracting nickel and cobalt from nickel-containing high-cobalt hydroxide, so that a high Ni and Co leaching rate is guaranteed. By means of the processes of sulfuric acid leaching, impurity removal, extraction, and Ni-Co isolation, leaching agents rich in metallic nickel and metallic cobalt are obtained, the leaching agents are directly fed into an electro-deposited nickel and electro-deposited cobalt production system, and accordingly metallic nickel and metallic cobalt are isolated and extracted. The obtained leaching agents rich in metallic nickel and metallic cobalt can directly enter the electro-deposited nickel and electro-deposited cobalt production system. In addition, the process for extracting nickel and cobalt from nickel-containing high-cobalt hydroxide is simple, efficient, environment-friendly and suitable for treating nickel-containing high-cobalt hydroxide.
Description
Technical field
A kind of metallurgical technology processing nickel-containing high-cobalt oxyhydroxide.By adopting the technique of sulfuric acid leaching-removal of impurities-extraction-Separation of nickel and cobalt to process, obtain the nickeliferous sulfate liquor being greater than 80g/L, this solution send nickel production system to produce electro deposited nickel product; Obtain the sulfate liquor being greater than 60g/L containing cobalt, send cobalt production system production electrodeposited cobalt product.
Background technology
Jinchuan Group Co., Ltd. is the main nickel of China, cobalt manufacturing enterprise.In recent years, along with the minimizing day by day of global nickelous sulfide resource, on market, the supply of nickelous sulfide raw material reduces year by year, and purchase cost progressively raises.In order to ensure the economical operation at full capacity of electro deposited nickel production line, guarantee company's nickel size of capacity, must adjust raw material mix---and employing nickel hydroxide as a supplement raw material becomes selection the most real at present.
Nickel hydroxide material is one of Jinchuan Group Co., Ltd.'s outsourcing raw material.This material, usually containing impurity such as higher Fe, Mn, Ca, Mg and Al, adopts ordinary method process to there is the problem that technical process is long, metal straight yield is low, tooling cost is high and operating environment is poor.
Summary of the invention
The object of the invention is the deficiency adopting ordinary method process to exist for nickel-containing high-cobalt oxyhydroxide, a kind of metallurgical technology processing nickel-containing high-cobalt oxyhydroxide being provided, making Ni, Co of in nickel-containing high-cobalt oxyhydroxide more than 98% be entered solution by leaching.
Nickel-containing high-cobalt oxyhydroxide composition is as following table
table 1 nickel-containing high-cobalt material oxyhydroxide composition (%):
In outsourcing nickel hydroxide starting material, the content of 10 kinds of foreign metal ions such as cobalt, copper, iron, manganese, chromium, magnesium, aluminium, zinc, calcium and lead is 11.54%, close to 30% of main metallic nickel, belongs to typical high impurity material.
Object of the present invention will extract metallic nickel and cobalt metal two kinds of precious metal materials exactly from outsourcing nickel hydroxide starting material.
The present invention is achieved through the following technical solutions metallic nickel and cobalt metal extracts.
Main technical measures are: adopt the full soaking technology of sulfuric acid, thus ensure that the leaching yield that Ni, Co are higher.By the flow process of sulfuric acid leaching, removal of impurities, extraction, Separation of nickel and cobalt, obtain the leach liquor being enriched metallic nickel, cobalt, these leach liquors are directly knocked down electro deposited nickel, electrodeposited cobalt production system, thus separation and Extraction goes out metallic nickel and cobalt metal.
The technical process of separation and Extraction is as follows:
The first step: control condition pulp.
In slurrying tank, add new water according to the pulp liquid-solid ratio of 1.5 ~ 3:1, then utilize crane that nickel hydroxide cobalt material is winched to charging opening, open material bag and material is added slurrying tank, control slurry time 1 ~ 3h; Return after ageing 30min into next procedure;
Second step: sulfuric acid dissolution, sodium sulphite anhydrous 99.3 reducing leaching
Utilize blower duct to return liquid pipeline to pulp to blow, prevent line clogging.Slow unlatching sulfuric acid valve adds sulfuric acid dissolution to dissolving tank, adds the oxide compound in sodium sulphite anhydrous 99.3 reducing leaching material afterwards, controls reaction end pH value 0.5 ~ 1.5, extraction time 2 ~ 4h; Solution transfer pump is utilized ore pulp to be squeezed into deironing aluminium groove after reaction terminates;
3rd step: iron removal by oxidation, barium carbonate deleading
First, the cone end and groove valve is against the wind opened, air blast Oxidation of Fe
2+a certain amount of hydrogen peroxide is added in reactive tank, react after 10 minutes and start to pass into steam intensification, when solution temperature reaches 85 DEG C, add barium carbonate deleading, then low discharge adds the deironing of NaOH adjusted to ph to 3.5 ~ 4.0, and deironing time 3 ~ 4h, enters Filter Press through Cemented filling when liquid is cooled to 70 DEG C after deironing.Filtrate is as liquid before P204 extraction, and filter residue returns the process of pyrogenic process system;
4th step: P204 abstraction impurity removal
According to the extraction curve of P204, under pH=3.5 condition, it is organic that iron, zinc, calcium, copper, manganese and part of nickel, cobalt enter load simultaneously, organic the washing after cobalt, salt pickling copper, washed metal through sulfuric acid of load realizes regeneration, washed metal acid, wash copper acid and use NaOH precipitation to generate copper manganese mixing slag to pay outward, after washing nickel cobalt, liquid is incorporated to P204 raffinate and enters P507 extraction section.
Organic proportioning: 15%P204+85% sulfonated kerosene
Saponification degree: 50-70%
Wash cobalt acid concentration (mol/L): 0.8-1.5mol/L
Wash copper acid concentration (mol/L): 5.0-6.0mol/L
Washed metal acid concentration (mol/L): 5.0-6.0mol/L
5th step: P507 Separation of nickel and cobalt
P204 raffinate is mainly containing the nickel of about 100g/L and the cobalt of about 3g/L, the main purpose entering P507 is Separation of nickel and cobalt, P507 is organic after saponification, advanced nickel soap, laggard extraction, load is organic washes nickel through sulfuric acid, wash cobalt, realize regeneration after washed metal, and after washing nickel, liquid is incorporated to P507 raffinate (i.e. nickel sulfate solution) and send nickel system, after washing cobalt, liquid (i.e. rose vitriol) send cobalt system, and washed metal acid merges with the acid of P204 washed metal carries out heavy copper manganese.
Organic proportioning: 15%P204+85% sulfonated kerosene
Saponification degree: 50-70%
Wash cobalt acid concentration (mol/L): 0.8-1.5mol/L
Wash copper acid concentration (mol/L): 5.0-6.0mol/L
Washed metal acid concentration (mol/L): 5.0-6.0mol/L.
The present invention adopts the full soaking technology of sulfuric acid, by leaching-removal of impurities-extraction-Separation of nickel and cobalt, thus ensure that the leaching yield that Ni, Co are higher, good separating effect.The present invention obtains being enriched metallic nickel, the leach liquor of cobalt directly can enter electro deposited nickel, electrodeposited cobalt production system.In addition, the present invention is simple efficient, an eco-friendly flow process, is applicable to process nickel-containing high-cobalt oxyhydroxide.
Accompanying drawing explanation
Fig. 1 is principle flow chart.
Embodiment
The present invention adopts the technique of sulfuric acid leaching-removal of impurities-extraction-Separation of nickel and cobalt.
The new water of nickel-containing high-cobalt oxyhydroxide carries out pulp operation, ore pulp after pulp is after normal pressure leaching groove adds sulfuric acid dissolution, undertaken heating up by pump delivery to iron removal trough, the deironing of hydro-oxidation sodium, add barium carbonate deleading, after deironing, liquid plate and frame(type)filter press filters, filter residue returns pyrogenic attack, filtrate enters extraction box as liquid before P204 removal of impurities, and P204 raffinate enters P507 and carries out Separation of nickel and cobalt.Nickel sulfate solution send nickel system, and cobalt sulfate solution send cobalt system.
Example:
The property of raw material that the present invention adopts is in table 1.
The present invention produces result of implementation in table 2,3.
Table 2 leach liquor composition (g/l)
Table 3 leached mud composition (%)
。
Claims (2)
1. one kind is extracted isolation technique and the technique of nickel cobalt in nickel-containing high-cobalt oxyhydroxide, it is characterized in that: by leaching, removal of impurities, extraction, Separation of nickel and cobalt, obtain the leach liquor being enriched metallic nickel, cobalt, directly enter electro deposited nickel, electrodeposited cobalt production system, thus separation and Extraction goes out metallic nickel and cobalt metal.
2. a kind of isolation technique and technique extracting nickel cobalt in nickel-containing high-cobalt oxyhydroxide according to claim 1, is characterized in that: the technical process of separation and Extraction is as follows:
The first step: control condition pulp
In slurrying tank, add new water according to the pulp liquid-solid ratio of 1.5 ~ 3:1, then utilize crane that nickel hydroxide cobalt material is winched to charging opening, open material bag and material is added slurrying tank, control slurry time 1 ~ 3h, return after ageing 30min into next procedure;
Second step: sulfuric acid dissolution, sodium sulphite anhydrous 99.3 reducing leaching
Utilize blower duct to return liquid pipeline to pulp to blow, prevent line clogging, slow unlatching sulfuric acid valve adds sulfuric acid dissolution to dissolving tank, add the oxide compound in sodium sulphite anhydrous 99.3 reducing leaching material afterwards, control reaction end pH value 0.5 ~ 1.5, extraction time 2 ~ 4h, utilizes solution transfer pump ore pulp to be squeezed into deironing aluminium groove after reaction terminates;
3rd step: iron removal by oxidation, barium carbonate deleading
First, the cone end and groove valve is against the wind opened, air blast Oxidation of Fe
2+a certain amount of hydrogen peroxide is added in reactive tank, react after 10 minutes and start to pass into steam intensification, when solution temperature reaches 85 DEG C, add barium carbonate deleading, then low discharge adds the deironing of NaOH adjusted to ph to 3.5 ~ 4.0, deironing time 3 ~ 4h, enter Filter Press through Cemented filling when liquid is cooled to 70 DEG C after deironing, filtrate is as liquid before P204 extraction, and filter residue returns the process of pyrogenic process system;
4th step: P204 abstraction impurity removal
According to the extraction curve of P204, under pH=3.5 condition, it is organic that iron, zinc, calcium, copper, manganese and part of nickel, cobalt enter load simultaneously, organic the washing after cobalt, salt pickling copper, washed metal through sulfuric acid of load realizes regeneration, washed metal acid, wash copper acid and use NaOH precipitation to generate copper manganese mixing slag to pay outward, after washing nickel cobalt, liquid is incorporated to P204 raffinate and enters P507 extraction section;
Organic proportioning: 15%P204+85% sulfonated kerosene
Saponification degree: 50-70%
Wash cobalt acid concentration (mol/L): 0.8-1.5mol/L
Wash copper acid concentration (mol/L): 5.0-6.0mol/L
Washed metal acid concentration (mol/L): 5.0-6.0mol/L
5th step: P507 Separation of nickel and cobalt
P204 raffinate is mainly containing the nickel of about 100g/L and the cobalt of about 3g/L, and the main purpose entering P507 is Separation of nickel and cobalt, and P507 is organic after saponification, advanced nickel soap, laggard extraction, and load is organic washes nickel through sulfuric acid, wash cobalt, realize regeneration after washed metal; After washing nickel, liquid is incorporated to P507 raffinate (i.e. nickel sulfate solution) and send nickel system, and after washing cobalt, liquid (i.e. rose vitriol) send cobalt system; Washed metal acid merges with the acid of P204 washed metal carries out heavy copper manganese,
Organic proportioning: 15%P204+85% sulfonated kerosene
Saponification degree: 50-70%
Wash cobalt acid concentration (mol/L): 0.8-1.5mol/L
Wash copper acid concentration (mol/L): 5.0-6.0mol/L
Washed metal acid concentration (mol/L): 5.0-6.0mol/L.
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Cited By (22)
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| CN105692753A (en) * | 2016-02-26 | 2016-06-22 | 兰州金川新材料科技股份有限公司 | Method for treating wastewater containing cobalt and acid |
| CN105803483A (en) * | 2016-04-06 | 2016-07-27 | 王贺 | Preparation method for electro-deposited nickel and cobalt |
| CN106756069A (en) * | 2017-02-08 | 2017-05-31 | 陕西理工学院 | A kind of method that valuable metal is reclaimed in the waste residue from zinc abstraction |
| CN106756065A (en) * | 2016-12-14 | 2017-05-31 | 江西自立环保科技有限公司 | A kind of method of Recovering Copper ferronickel in matte from fuming furnace |
| CN106745342A (en) * | 2016-11-29 | 2017-05-31 | 吉林吉恩镍业股份有限公司 | The preparation method for producing nickel chloride is leached by raw material sulphuric acid of rough nickel hydroxide |
| CN106755994A (en) * | 2017-01-12 | 2017-05-31 | 江苏凯力克钴业股份有限公司 | A kind of production method for comprehensively utilizing zinc cobalt raw material high |
| CN106834742A (en) * | 2017-02-22 | 2017-06-13 | 桂林理工大学 | It is a kind of to clean the method for extracting nickel cobalt |
| CN107419295A (en) * | 2017-03-24 | 2017-12-01 | 金川集团股份有限公司 | The Electrolysis Extraction Method of manganese ion in a kind of nickel hydroxide hydrochloric acid leachate |
| CN107881341A (en) * | 2017-12-08 | 2018-04-06 | 上海产业技术研究院 | Method of comprehensive utilization based on hydrometallurgical processes middle and high concentration sodium sulfate wastewater |
| CN108070719A (en) * | 2016-11-14 | 2018-05-25 | 陕西瑞凯环保科技有限公司 | A kind of method of Copper making speiss recycling cupro-nickel |
| CN108441649A (en) * | 2018-03-27 | 2018-08-24 | 广东佳纳能源科技有限公司 | A kind of method of chemical precipitation nickel sulfide material extraction nickel |
| CN109592720A (en) * | 2018-11-23 | 2019-04-09 | 湖南中伟新能源科技有限公司 | Ternary precursor solution purification method |
| CN110512080A (en) * | 2019-09-12 | 2019-11-29 | 金川集团股份有限公司 | Valuable metal separation and recovery method in a kind of waste and old nickel cobalt manganese lithium ion battery |
| CN110656253A (en) * | 2018-06-28 | 2020-01-07 | 荆门市格林美新材料有限公司 | Method for recovering nickel hydroxide |
| CN110656252A (en) * | 2018-06-28 | 2020-01-07 | 荆门市格林美新材料有限公司 | Cobalt hydroxide recovery method |
| CN111455174A (en) * | 2020-06-09 | 2020-07-28 | 矿冶科技集团有限公司 | Method for preparing battery-grade nickel sulfate and cobalt sulfate from mixed nickel hydroxide cobalt |
| CN111500862A (en) * | 2020-06-09 | 2020-08-07 | 矿冶科技集团有限公司 | Method for removing iron and aluminum from mixed nickel cobalt hydroxide leachate |
| CN112460032A (en) * | 2020-12-10 | 2021-03-09 | 江西睿锋环保有限公司 | Conveying device for copper-nickel-zinc waste pretreatment process |
| CN114085993A (en) * | 2021-11-10 | 2022-02-25 | 金川集团股份有限公司 | Method for separating calcium, magnesium and manganese in nickel chloride solution by extraction method |
| CN115353152A (en) * | 2022-08-24 | 2022-11-18 | 上海锦源晟新能源材料有限公司 | Battery-grade cobalt sulfate, production process method thereof and battery |
| CN115852151A (en) * | 2023-02-17 | 2023-03-28 | 湖南五创循环科技股份有限公司 | Method for treating waste power battery by electrolytic oxidation of ore pulp |
| CN116377243A (en) * | 2023-03-29 | 2023-07-04 | 中国恩菲工程技术有限公司 | Method for separating nickel, cobalt and manganese from nickel-cobalt hydroxide raw material |
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2015
- 2015-11-20 CN CN201510806234.XA patent/CN105274332A/en active Pending
Cited By (24)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105692753A (en) * | 2016-02-26 | 2016-06-22 | 兰州金川新材料科技股份有限公司 | Method for treating wastewater containing cobalt and acid |
| CN105803483A (en) * | 2016-04-06 | 2016-07-27 | 王贺 | Preparation method for electro-deposited nickel and cobalt |
| CN108070719A (en) * | 2016-11-14 | 2018-05-25 | 陕西瑞凯环保科技有限公司 | A kind of method of Copper making speiss recycling cupro-nickel |
| CN106745342A (en) * | 2016-11-29 | 2017-05-31 | 吉林吉恩镍业股份有限公司 | The preparation method for producing nickel chloride is leached by raw material sulphuric acid of rough nickel hydroxide |
| CN106756065A (en) * | 2016-12-14 | 2017-05-31 | 江西自立环保科技有限公司 | A kind of method of Recovering Copper ferronickel in matte from fuming furnace |
| CN106755994A (en) * | 2017-01-12 | 2017-05-31 | 江苏凯力克钴业股份有限公司 | A kind of production method for comprehensively utilizing zinc cobalt raw material high |
| CN106756069A (en) * | 2017-02-08 | 2017-05-31 | 陕西理工学院 | A kind of method that valuable metal is reclaimed in the waste residue from zinc abstraction |
| CN106834742A (en) * | 2017-02-22 | 2017-06-13 | 桂林理工大学 | It is a kind of to clean the method for extracting nickel cobalt |
| CN107419295A (en) * | 2017-03-24 | 2017-12-01 | 金川集团股份有限公司 | The Electrolysis Extraction Method of manganese ion in a kind of nickel hydroxide hydrochloric acid leachate |
| CN107881341A (en) * | 2017-12-08 | 2018-04-06 | 上海产业技术研究院 | Method of comprehensive utilization based on hydrometallurgical processes middle and high concentration sodium sulfate wastewater |
| CN108441649B (en) * | 2018-03-27 | 2020-08-28 | 广东佳纳能源科技有限公司 | Method for extracting nickel from chemical precipitation nickel sulfide material |
| CN108441649A (en) * | 2018-03-27 | 2018-08-24 | 广东佳纳能源科技有限公司 | A kind of method of chemical precipitation nickel sulfide material extraction nickel |
| CN110656253A (en) * | 2018-06-28 | 2020-01-07 | 荆门市格林美新材料有限公司 | Method for recovering nickel hydroxide |
| CN110656252A (en) * | 2018-06-28 | 2020-01-07 | 荆门市格林美新材料有限公司 | Cobalt hydroxide recovery method |
| CN109592720A (en) * | 2018-11-23 | 2019-04-09 | 湖南中伟新能源科技有限公司 | Ternary precursor solution purification method |
| CN110512080A (en) * | 2019-09-12 | 2019-11-29 | 金川集团股份有限公司 | Valuable metal separation and recovery method in a kind of waste and old nickel cobalt manganese lithium ion battery |
| CN111500862A (en) * | 2020-06-09 | 2020-08-07 | 矿冶科技集团有限公司 | Method for removing iron and aluminum from mixed nickel cobalt hydroxide leachate |
| CN111455174A (en) * | 2020-06-09 | 2020-07-28 | 矿冶科技集团有限公司 | Method for preparing battery-grade nickel sulfate and cobalt sulfate from mixed nickel hydroxide cobalt |
| CN112460032A (en) * | 2020-12-10 | 2021-03-09 | 江西睿锋环保有限公司 | Conveying device for copper-nickel-zinc waste pretreatment process |
| CN114085993A (en) * | 2021-11-10 | 2022-02-25 | 金川集团股份有限公司 | Method for separating calcium, magnesium and manganese in nickel chloride solution by extraction method |
| CN115353152A (en) * | 2022-08-24 | 2022-11-18 | 上海锦源晟新能源材料有限公司 | Battery-grade cobalt sulfate, production process method thereof and battery |
| CN115353152B (en) * | 2022-08-24 | 2024-01-09 | 上海锦源晟新能源材料有限公司 | Battery-grade cobalt sulfate and production process method thereof and battery |
| CN115852151A (en) * | 2023-02-17 | 2023-03-28 | 湖南五创循环科技股份有限公司 | Method for treating waste power battery by electrolytic oxidation of ore pulp |
| CN116377243A (en) * | 2023-03-29 | 2023-07-04 | 中国恩菲工程技术有限公司 | Method for separating nickel, cobalt and manganese from nickel-cobalt hydroxide raw material |
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