CN108588416A - A method of deep oxidation removes iron cobalt from nickel salt - Google Patents

A method of deep oxidation removes iron cobalt from nickel salt Download PDF

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Publication number
CN108588416A
CN108588416A CN201810486116.9A CN201810486116A CN108588416A CN 108588416 A CN108588416 A CN 108588416A CN 201810486116 A CN201810486116 A CN 201810486116A CN 108588416 A CN108588416 A CN 108588416A
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China
Prior art keywords
cobalt
nickel
oxidation
solution
iron
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CN201810486116.9A
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Chinese (zh)
Inventor
胡建辉
赵海涛
刘永平
蒋震清
郑春到
吴新明
赖建林
张玲玲
黄冰
吴晓莉
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Jiangxi Copper Corp Ltd
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Jiangxi Copper Corp Ltd
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Priority to CN201810486116.9A priority Critical patent/CN108588416A/en
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/44Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00Obtaining nickel or cobalt
    • C22B23/04Obtaining nickel or cobalt by wet processes
    • C22B23/0453Treatment or purification of solutions, e.g. obtained by leaching
    • C22B23/0461Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00Obtaining nickel or cobalt
    • C22B23/04Obtaining nickel or cobalt by wet processes
    • C22B23/0476Separation of nickel from cobalt
    • C22B23/0484Separation of nickel from cobalt in acidic type solutions
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/26Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
    • C22B3/38Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
    • C22B3/384Pentavalent phosphorus oxyacids, esters thereof
    • C22B3/3846Phosphoric acid, e.g. (O)P(OH)3
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Catalysts (AREA)

Abstract

The method of iron cobalt in a kind of deep oxidation removing nickel salt of the present invention, this method takes that " nickel sulfate solution after vulcanization decopper(ing) arsenic adjusts that pH value addition catalyst depth cobalt ferric oxide, P204 extractions be miscellaneous, nickel sulfate scavenging solution send nickel product extraction process; makes full use of the super oxidation susceptibility of ozone; ferrous iron cobalt obtains oxidation removal; obtain low ore grade nickel oxidizing slag and deferrization cobalt liquor, be conducive to next step P204 and extract zinc, calcium etc..The beneficial effects of the present invention are:This method is by adding catalyst depth oxidation, its removal efficiency of iron cobalt is up to 90% or more, with obvious effects, obtained iron cobalt slag is high containing cobalt, nickeliferous low, conducive to the direct yield of the recycling and raising nickel of cobalt, since oxidation solution is limpid, not iron content cobalt and other low price elements and organic matter, P204 extractions does not generate third phase, conducive to extraction zinc, extraction calcium, loss of extractant is reduced.

Description

A method of deep oxidation removes iron cobalt from nickel salt
Technical field
The method of the present invention relates to a kind of from nickel salt deep oxidation removing iron cobalt, it is de- especially to adapt to crude nickle sulphate depth Except iron cobalt, the technical matters of high-quality nickel product is produced.
Background technology
Currently, both at home and abroad during high impurity nickel salt removing impurities, routinely removing methods mainly use addition reagent to iron cobalt, Not only consumption is big, and removing impurities is not thorough, and may introduce new impurity, and adverse effect is brought to follow-up removing impurities.
Cost how is reduced, while utilizing the superpower oxidability cobalt ferric oxide of ozone instrument, reduces the oxidation quantity of slag and reduction Oxidizing slag is nickeliferous, greatly improves the rate of recovery of nickel, significant.
Invention content
A kind of purpose of the method for the removing of the deep oxidation from nickel salt iron cobalt of the present invention is for thick nickel salt vulcanization dearsenification, takes off Liquid after copper, iron especially cobalt are difficult to remove, and general oxidant cannot be satisfied requirement, and certain difficulty, nothing are brought to subsequent purification Method generates high-quality nickel series of products.
To achieve the above object, the present invention takes following technical scheme:A kind of deep oxidation from nickel salt removing iron cobalt Method, this method specifically include following steps:
Step 1:Liquid tune pH value is to 3-6 after carrying out vulcanization decopper(ing), dearsenification to nickel salt, while adding a certain amount of catalyst;
Step 2:Enough oxygen is passed through to nickel sulfate solution after addition catalyst potassium permanganate and catechol or wooden sodium sulfonate Agent carries out deep oxidation under certain electrode potential, and deferrization, de- cobalt obtain 1 oxidation solution, as P204 extracting zincs, extraction calcium Material liquid generates low ferronickel cobalt slag conduct and carries nickel raw material, while obtaining oxidated solution as liquid before extraction zinc, extraction calcium;
Step 3:P204 extractions calcium, zinc are carried out to liquid after deferrization cobalt oxidation, nickel deep purifying liquid is obtained and carries out ammonia complexing, catch up with ammonia, it is raw Nickelous carbonate presoma is produced, pyrolytic cracking is sent to produce nickel series of products.
Further, the additive amount of the catalyst in the step 1 is the 0.05-1% of solution weight, and the catalyst is height Potassium manganate and catechol or potassium permanganate and lignosulfonic acid, mass ratio between the two are 1:0.1-0.9.
Further, the oxidant in the step 2 is ozone or perchloric acid.
Further, the reaction time of deep oxidation is every liter of 4.5-5.5 hours solution reaction time in the step 2.
Further, electrode potential is 280-380mv in the step 2.
Further, the iron cobalt removal efficiency in the nickel salt is up to 90% or more.
The beneficial effects of the present invention are:This method by add catalyst depth oxidation, its removal efficiency of iron cobalt up to 90% with On, with obvious effects, obtained iron cobalt slag is high containing cobalt, nickeliferous low, is conducive to the recycling of cobalt and improves the direct yield of nickel, due to oxidation solution Limpid, not iron content cobalt and other low price elements and organic matter, P204 extractions does not generate third phase, is conducive to extraction zinc, extraction calcium, reduces extraction Agent is taken to be lost.After adding catalyst ozone oxidation, remains sulfide and organic matter and iron cobalt is effectively removed, pass through P204 dezincifications, calcium produce high-quality nickel product and provide guarantee.
Description of the drawings
Fig. 1 is a kind of flow diagram of the method for the deep removal iron cobalt from nickel salt of the present invention.
Specific implementation mode
Technical scheme of the present invention is described further below in conjunction with the accompanying drawings.
As shown in Figure 1, a kind of method of the removing of the deep oxidation from nickel salt iron cobalt of the present invention, this method specifically includes following Step:
Step 1:Liquid tune pH value is to 3-6 after carrying out vulcanization decopper(ing), dearsenification to nickel salt, while adding a certain amount of catalyst;
Step 2:Enough oxygen is passed through to nickel sulfate solution after addition catalyst potassium permanganate and catechol or wooden sodium sulfonate Agent carries out deep oxidation under certain electrode potential, and deferrization, de- cobalt obtain 1 oxidation solution, as P204 extracting zincs, extraction calcium Material liquid generates low ferronickel cobalt slag conduct and carries nickel raw material, while obtaining oxidated solution as liquid before extraction zinc, extraction calcium;
Step 3:P204 extractions calcium, zinc are carried out to liquid after deferrization cobalt oxidation, nickel deep purifying liquid is obtained and carries out ammonia complexing, catch up with ammonia, it is raw Nickelous carbonate presoma is produced, pyrolytic cracking is sent to produce nickel series of products.
Further, the additive amount of the catalyst in the step 1 is the 0.05-1% of solution weight, and the catalyst is height Potassium manganate and catechol or potassium permanganate and lignosulfonic acid, mass ratio between the two are 1:0.1-0.9.
Further, the oxidant in the step 2 is ozone or perchloric acid.
Further, the reaction time of deep oxidation is every liter of 4.5-5.5 hours solution reaction time in the step 2.
Further, electrode potential is 280-380mv in the step 2.
Further, the iron cobalt removal efficiency in the nickel salt is up to 90% or more.
Embodiment:
A method of deep oxidation removes iron cobalt from nickel salt, and the present invention is further described with reference to embodiments:
It takes 3L to contain Ni88.13g/L, contains Co0.43g/L, iron content Fe0.88g/L, adjust solution pH value to 3-6, while 4 grams of height are added Potassium manganate, 2 grams of wooden sodium sulfonates or 2 grams of catechols.
The new method carries out ozone deep oxidation to 3L iron content, cobalt nickel salt solution, and electrode potential controls after oxidation 325mv, oxidated solution iron cobalt concentration are respectively less than 0.005g/L, and removal efficiency is more than 98%, and oxidizing slag contains cobalt 21.76%, nickeliferous 8.56%, iron content 44.56%.
The new method carries out P204 extractions calcium, zinc to solution after deferrization, cobalt, and calcium is de- to less than 0.005 from 0.53 g/L G/L, removal efficiency are more than 99%, and zinc is taken off from 1.23 g/L to less than 0.005 g/L, and removal efficiency is more than 99%,.
The new method extracts calcium zinc deep purifying liquid, carries out ammonia complexing, catches up with ammonia, generate high-quality nickelous carbonate presoma, high temperature Sudden strain of a muscle is split, production quality oxide Asia nickel.
One embodiment of the present invention has been described in detail above, but it is not meant to the limit to the scope of the present invention System, content is only the preferred embodiment of the present invention, should not be construed as limiting the practical range of the present invention.Fan Yibenfa All the changes and improvements etc. made by bright application range, should all still fall within the scope of the patent of the present invention.

Claims (6)

1. a kind of method of the removing of the deep oxidation from nickel salt iron cobalt, which is characterized in that this method specifically includes following steps:
Step 1:Liquid tune pH value is to 3-6 after carrying out vulcanization decopper(ing), dearsenification to nickel salt, while adding a certain amount of catalyst;
Step 2:Enough oxygen is passed through to nickel sulfate solution after addition catalyst potassium permanganate and catechol or wooden sodium sulfonate Agent carries out deep oxidation under certain electrode potential, and deferrization, de- cobalt obtain 1 oxidation solution, as P204 extracting zincs, extraction calcium Material liquid generates low ferronickel cobalt slag conduct and carries nickel raw material, while obtaining oxidated solution as liquid before extraction zinc, extraction calcium;
Step 3:P204 extractions calcium, zinc are carried out to liquid after deferrization cobalt oxidation, nickel deep purifying liquid is obtained and carries out ammonia complexing, catch up with ammonia, it is raw Nickelous carbonate presoma is produced, pyrolytic cracking is sent to produce nickel series of products.
2. according to the method described in claim 1, it is characterized in that, the additive amount of the catalyst in the step 1 is solution weight The 0.05-1% of amount, the catalyst are potassium permanganate and catechol or potassium permanganate and lignosulfonic acid, quality between the two Than being 1:0.1-0.9.
3. according to the method described in claim 1, it is characterized in that, the oxidant in the step 2 is ozone or perchloric acid.
4. according to the method described in claim 1, it is characterized in that, the reaction time of deep oxidation is every liter in the step 2 4.5-5.5 hours solution reaction time.
5. according to the method described in claim 1, it is characterized in that, electrode potential is 280-380mv in the step 2.
6. according to the method described in claim 1, it is characterized in that, iron cobalt removal efficiency in the nickel salt is up to 90% or more.
CN201810486116.9A 2018-05-21 2018-05-21 A method of deep oxidation removes iron cobalt from nickel salt Pending CN108588416A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109897955A (en) * 2019-04-17 2019-06-18 江西铜业股份有限公司 A kind of method of nickel sulfate solution deep purifying
CN113512649A (en) * 2021-05-27 2021-10-19 金川集团股份有限公司 Production method for realizing nickel-cobalt separation by utilizing ozone under mixed acid system

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101423897A (en) * 2008-11-26 2009-05-06 东北大学 Method for extracting nickel oxide from lateritic nickel
CN103326088A (en) * 2013-07-04 2013-09-25 厦门钨业股份有限公司 Comprehensive recovery method of waste lithium ion battery
CN103320811A (en) * 2013-06-05 2013-09-25 中南大学 Method for removing impurities from nickel electrolysis anolyte

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101423897A (en) * 2008-11-26 2009-05-06 东北大学 Method for extracting nickel oxide from lateritic nickel
CN103320811A (en) * 2013-06-05 2013-09-25 中南大学 Method for removing impurities from nickel electrolysis anolyte
CN103326088A (en) * 2013-07-04 2013-09-25 厦门钨业股份有限公司 Comprehensive recovery method of waste lithium ion battery

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汪尔康: "《分析化学进展》", 31 October 1994, 南京大学出版社 *
肖若珀: "《砷的提取、环保和应用方向》", 31 December 1992, 广西金属学会 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109897955A (en) * 2019-04-17 2019-06-18 江西铜业股份有限公司 A kind of method of nickel sulfate solution deep purifying
CN113512649A (en) * 2021-05-27 2021-10-19 金川集团股份有限公司 Production method for realizing nickel-cobalt separation by utilizing ozone under mixed acid system

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Address after: 330096 No. 15 Metallurgical Avenue, Guixi City, Yingtan City, Jiangxi Province

Applicant after: Jiangxi Copper Group Co., Ltd.

Address before: 330096 No. 7666, Dong Dong Avenue, Jiangxi, Nanchang

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Application publication date: 20180928