CN107935063A - Utilize the nickel oxide method that directly leaching prepares nickel salt under normal pressure - Google Patents
Utilize the nickel oxide method that directly leaching prepares nickel salt under normal pressure Download PDFInfo
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- CN107935063A CN107935063A CN201711156784.7A CN201711156784A CN107935063A CN 107935063 A CN107935063 A CN 107935063A CN 201711156784 A CN201711156784 A CN 201711156784A CN 107935063 A CN107935063 A CN 107935063A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/10—Sulfates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/08—Halides
- C01G53/09—Chlorides
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Abstract
It is to mix dilution heat of sulfuric acid with nickel oxide the invention discloses the method that a kind of non-pressure process leaching nickel oxide prepares nickel sulfate or nickel chloride, 1 ~ 5h of stirring reaction, increasingly generates greenish yellow solid under the conditions of 50 ~ 100 DEG C；After separation of solid and liquid, greenish yellow solid is first washed with distilled water to faintly acid, then is dissolved with distilled water or concentration for 1 ~ 5% aqueous hydrogen peroxide solution, generates corresponding nickel sulfate solution；Or mix hydrochloric acid solution with nickel oxide, 1 ~ 3h of stirring reaction, increasingly generates green nickel chloride solution under the conditions of 50 ~ 100 DEG C.The nickel content of nickel salt solution prepared by this method is all in more than 110g/L.The present invention is directly reacted under normal pressure by lixiviation process, is obtained nickel sulfate and nickel chloride, is effectively simplified the production procedure of nickel sulfate and nickel chloride, reduces cost；And reduce impurity introducing from source, effectively increase nickel sulfate quality.
Description
Technical field
The present invention relates to a kind of preparation method of nickel salt, more particularly to one kind directly to be prepared using nickel oxide under normal pressure
The method of high-purity sulphuric acid nickel or nickel chloride.
Background technology
Nickel salt is important industrial chemicals.For example, nickel sulfate（NiSO4）As a kind of important industrial chemicals, widely
Applied to fields such as plating, battery, printing and dyeing, medicine, building, national defence；Nickel chloride（NiCl2）Applied to nickel plating, disappearing liquid medicine processed
And make ammonia absorbent etc..The preparation method of nickel sulfate and nickel chloride mainly has chemical method and electrochemical process.Nickel sulfate and chlorine
Changing the traditional mode of production raw material of nickel includes electric nickel, converter mattes, nickeliferous waste and old material and thick nickel hydroxide.The oxide of nickel is aerobic
Change sub- nickel（NiO）, nickelous-nickelic oxide（Ni3O4）And nickel sesquioxide（Ni2O3）Three kinds of forms.Nickel sesquioxide is only in low temperature
Stablize, be heated to 400 ~ 500 DEG C, that is, dissociate into nickelous-nickelic oxide, further improve temperature and eventually become nickel protoxide, in nickel oxygen
The mass fraction of nickel may be up to 78.5% in compound.But rarely has the document that nickel sulfate and nickel chloride are directly prepared with nickel oxide
And patent report.
The content of the invention
It is an object of the invention to provide one kind using nickel oxide under normal pressure direct preparation of high-purity nickel salt nickel sulfate or
The method of nickel chloride.
The method that the present invention prepares high-purity sulphuric acid nickel or nickel chloride, is using nickel oxide as raw material, passes through normal pressure leaching method
Nickel sulfate directly is made and nickel chloride, its specific preparation process are as follows：
1st, the preparation of nickel sulfate
Dilution heat of sulfuric acid is mixed with nickel oxide, 1 ~ 5h of stirring reaction, increasingly generates greenish yellow solid under the conditions of 50 ~ 90 DEG C
（Nickel sulfate and nickel oxide mixture）；After separation of solid and liquid, greenish yellow solid is first washed with distilled water to faintly acid, then uses distilled water
Or the aqueous hydrogen peroxide solution that concentration is 1 ~ 5% dissolves, and generates corresponding nickel sulfate solution.It is yellowish green in order to be fully converted to raw material
Color solid, needs to add concentrated sulfuric acid solution during the reaction.The concentration of sulfuric acid solution is 1.84 ~ 18.4 M, nickel oxide with it is dilute
The mass volume ratio of sulfuric acid solution is 1:6 g/ml.
The equation of nickel oxide and sulfuric acid reaction is as follows：
NiO + H2SO4 = NiSO4 + H2O
Ni2O3 + 2H2SO4 = 2NiSO4 + 2H2O + 1/2O2↑
Ni3O4 + 3H2SO4 = 3NiSO4 + 3H2O + 1/2O2↑
2nd, the preparation of nickel chloride：Hydrochloric acid solution is mixed with nickel oxide, 1 ~ 3h of stirring reaction under the conditions of 50 ~ 90 DEG C, gradually
The green nickel chloride solution of generation.The concentration of hydrochloric acid solution is 1.2 ~ 12 M；The mass volume ratio of nickel oxide and hydrochloric acid solution is
1:6( g/ml)。
Nickel oxide and the equation that hydrochloric acid reacts are as follows：
NiO + 2HCl = NiCl2 + H2O
Ni2O3 + 6HCl = 2NiCl2 + 3H2O + Cl2↑
Ni3O4 + 8HCl = 3NiCl2 + 4H2O + Cl2↑
The nickel oxide is any one in nickel protoxide, nickel oxide, nickelous-nickelic oxide, hydroxy nickel oxide.
After testing, nickel sulfate, nickel chloride leachate above-mentioned using nickel oxide as raw material, prepared by normal pressure leaching method
In, nickel ion content is above 110g/L.
The present invention is directly reacted using nickel oxide and hydrochloric acid/sulfuric acid as raw material, obtains sulfuric acid under normal pressure by lixiviation process
Nickel and nickel chloride, are effectively simplified the production procedure of nickel sulfate and nickel chloride, reduce cost；And reduce from source miscellaneous
Matter introduces, and effectively increases nickel sulfate quality.
Embodiment
Embodiment 1
Take the nickel oxide of 5g to be placed in 250ml beakers, add the sulfuric acid solution of 30ml 1.84M, in the condition that temperature is 50 DEG C
Under, stirring reaction 1h, increasingly generates substantial amounts of greenish yellow solid；Add concentrated sulfuric acid 5ml the reaction was continued 1h；After the completion of reaction, mistake
Filter, filter residue is washed with distilled water to faintly acid, then the nickel sulfate solution to form clarification is dissolved by heating with 30ml distilled water.Unreacted
Black solid material quality be 3.8g, nickel ion content is 30g/L in solution.
Embodiment 2
Take the nickel oxide of 5g to be placed in 250ml beakers, add the sulfuric acid solution of 30ml 5.5M, be 100 DEG C in reaction temperature
Under the conditions of, stirring reaction 1h, increasingly generates substantial amounts of greenish yellow solid；Add concentrated sulfuric acid 4ml the reaction was continued 1h；Reaction is completed
Afterwards, filter, filter residue is washed with distilled water to faintly acid, then dissolves by heating with the aqueous hydrogen peroxide solution of 30ml2% that to form clarification molten
Liquid.Unreacted black solid material quality is 1.7g, and nickel ion content is 80g/L in solution.
Embodiment 3
Take the nickel oxide of 5g to be placed in 250ml beakers, add the sulfuric acid solution of 30ml 9.2M.It it is 80 DEG C in reaction temperature
Under the conditions of, stirring reaction 1h, increasingly generates substantial amounts of greenish yellow solid, adds concentrated sulfuric acid 3ml the reaction was continued 1h.Reaction is completed
Afterwards, remained substantially without black solid raw material, filtering, filter residue is washed with distilled water to faintly acid, and solid residue directly uses 30ml5%
Aqueous hydrogen peroxide solution dissolve by heating to form settled solution.Nickel ion content is 121g/L in solution.
Embodiment 4
Take the nickel oxide of 5g to be placed in 250ml beakers, add the sulfuric acid solution of 30ml12.7M.It is 80 in reaction temperatureoC's
Under the conditions of, stirring reaction 2h, increasingly generates pistac solid.After the completion of reaction, filtering, filter residue is washed with distilled water to weak acid
Property.Solid residue directly dissolves by heating to form settled solution with the aqueous hydrogen peroxide solution of 30ml 3%.Unreacted black solid is former
Material quality is 1.3g.Nickel ion content is 90g/L in solution.
Embodiment 5
Take the nickel oxide of 5g to be placed in 250ml beakers, add the sulfuric acid solution of 30ml 18.4M.Reaction is stirred at 80 DEG C
5h, increasingly generates a small amount of pistac solid.After the completion of reaction, filtering, filter residue is washed with distilled water to faintly acid, then directly
Dissolve by heating to form settled solution with the aqueous hydrogen peroxide solution of 30ml 5%.Unreacted black solid material quality is 3.6g.It is molten
Nickel ion content is 35g/L in liquid.
Embodiment 6
Take the nickel oxide of 5g to be placed in 250ml beakers, add the hydrochloric acid solution of 30ml 1.2M.The stirring reaction 3h at 50 DEG C,
Increasingly generate green nickel chloride solution.Unreacted black solid material quality is 4.6g.Nickel ion content is 9g/L in solution.
Embodiment 7
Take the nickel oxide of 5g to be placed in 250ml beakers, add the hydrochloric acid solution of 30ml 4.8M.It it is 100 DEG C in reaction temperature
Under the conditions of, stirring reaction 2.5h, increasingly generates green nickel chloride solution.Unreacted black solid material quality is 1.5g.It is molten
Nickel ion content is 85g/L in liquid.
Embodiment 8
Take the nickel oxide of 5g to be placed in 250ml beakers, add the hydrochloric acid solution of 30ml 8.4M；The stirring reaction 2h at 80 DEG C,
Increasingly generate green nickel chloride solution.Nickel ion content is 121g/L in solution.
Embodiment 9
Take the nickel oxide of 5g to be placed in 250ml beakers, add the hydrochloric acid solution of 30ml 12M.Reaction is stirred at 80 DEG C
1.5h, increasingly generates green nickel chloride solution.Nickel ion content is 121g/L in solution.
In the various embodiments described above, nickel oxide is commercially available high-purity nickel oxide, its component is as shown in the table：
| Element | Ni | Pb | Cr | Co | Ca | Cd | Cu | Mg | Fe | Na | Zn | Mn |
| Content/% | 77.96 | 0.0006 | 0.0013 | 0.0028 | 0.0032 | 0.0005 | 0.0008 | 0.020 | 0.0070 | 0.055 | 0.0008 | 0.013 |
Claims (6)
1. directly prepare the method for nickel salt under normal pressure using nickel oxide, it is characterised in that：
Dilution heat of sulfuric acid is mixed with nickel oxide, 1 ~ 5h of stirring reaction, increasingly generates yellow green and consolidate under the conditions of 50 ~ 100 DEG C
Body；After separation of solid and liquid, greenish yellow solid is first washed with distilled water to faintly acid, then with distilled water or the hydrogen peroxide water of concentration 1 ~ 5%
Solution dissolves, and generates corresponding nickel sulfate solution；
Or mix hydrochloric acid solution with nickel oxide, 1 ~ 3h of stirring reaction, increasingly generates green chlorination under the conditions of 50 ~ 100 DEG C
Nickel solution.
2. the method for directly preparing nickel salt under normal pressure using nickel oxide as claimed in claim 1, it is characterised in that：In sulfuric acid
, it is necessary to add the concentrated sulfuric acid in the preparation of nickel, the reaction was continued to without starting material left, filtering, filter residue is washed with distilled water to weak substantially
Acidity, then use distilled water or the dissolving of the aqueous hydrogen peroxide solution of concentration 1 ~ 5%, generate corresponding nickel sulfate solution.
3. the method for directly preparing nickel salt under normal pressure using nickel oxide as claimed in claim 1, it is characterised in that：It is described dilute
The concentration of sulfuric acid solution is 1.84 ~ 18.4 M.
4. the method for directly preparing nickel salt under normal pressure using nickel oxide as claimed in claim 3, it is characterised in that：Nickel aoxidizes
The mass volume ratio of thing and dilution heat of sulfuric acid is 1:6 g/ml.
5. the method for directly preparing nickel salt under normal pressure using nickel oxide as claimed in claim 1, it is characterised in that：Hydrochloric acid is molten
The concentration of liquid is 1.2 ~ 12 M；The mass volume ratio of nickel oxide and hydrochloric acid solution is 1:6 g/ml.
6. the method that any one directly prepares nickel salt using nickel oxide under normal pressure as described in claim 1 ~ 5, its feature
It is：The nickel oxide is any one in nickel protoxide, nickel oxide, nickelous-nickelic oxide, hydroxy nickel oxide.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109205687A (en) * | 2018-10-09 | 2019-01-15 | 金川集团股份有限公司 | A method of LITHIUM BATTERY nickel sulfate is prepared by raw material of nickel oxide |
| CN109279666A (en) * | 2018-10-09 | 2019-01-29 | 金川集团股份有限公司 | A method of nickel sulfate solution is produced by raw material of nickel oxide |
| CN109279667A (en) * | 2018-10-09 | 2019-01-29 | 金川集团股份有限公司 | A method of LITHIUM BATTERY nickel sulfate is produced by raw material of nickel oxide |
| CN110092423A (en) * | 2019-04-23 | 2019-08-06 | 金川集团股份有限公司 | A kind of nickel oxide quickly dissolves, the method for nickel soap depickling removal of impurities production nickel sulfate solution |
| CN110104694A (en) * | 2019-04-23 | 2019-08-09 | 金川集团股份有限公司 | A method of nickel chloride solution is prepared using nickel oxide |
| CN110607439A (en) * | 2019-09-12 | 2019-12-24 | 金川集团股份有限公司 | Spherical nickel protoxide sectional oxidation acid leaching treatment method |
| WO2019244527A1 (en) * | 2018-06-21 | 2019-12-26 | 日揮グローバル株式会社 | Method for producing nickel sulfate compound |
| JP2020001996A (en) * | 2018-06-21 | 2020-01-09 | 日揮ホールディングス株式会社 | Method for producing nickel sulfate compound |
| CN112062171A (en) * | 2019-06-10 | 2020-12-11 | 天津市茂联科技有限公司 | Method for separating nickel and magnesium from crude nickel carbonate |
| EP4166508A1 (en) * | 2021-10-04 | 2023-04-19 | Prime Planet Energy & Solutions, Inc. | Method of producing nickel sulfate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101219814A (en) * | 2007-12-25 | 2008-07-16 | 金川集团有限公司 | Nickelous oxide dead catalyst dissolution processing method |
| CN101542781A (en) * | 2005-11-08 | 2009-09-23 | 双向电池公司 | Method of producing a nickel salt solution |
| CN106756051A (en) * | 2016-12-31 | 2017-05-31 | 山东飞源科技有限公司 | The technique that nickel sulfate is reclaimed from nickel slag |
-
2017
- 2017-11-20 CN CN201711156784.7A patent/CN107935063A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101542781A (en) * | 2005-11-08 | 2009-09-23 | 双向电池公司 | Method of producing a nickel salt solution |
| CN101219814A (en) * | 2007-12-25 | 2008-07-16 | 金川集团有限公司 | Nickelous oxide dead catalyst dissolution processing method |
| CN106756051A (en) * | 2016-12-31 | 2017-05-31 | 山东飞源科技有限公司 | The technique that nickel sulfate is reclaimed from nickel slag |
Non-Patent Citations (2)
| Title |
|---|
| 张焱: "用废触媒制备硫酸镍", 《广州化工》 * |
| 韩长日等: "《精细化工品实用生产技术手册 电子与信息化学品制造技术》", 31 October 2001 * |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2019290870B2 (en) * | 2018-06-21 | 2021-04-01 | Jgc Corporation | Nickel sulfate compound manufacturing method |
| WO2019244527A1 (en) * | 2018-06-21 | 2019-12-26 | 日揮グローバル株式会社 | Method for producing nickel sulfate compound |
| JP2020001996A (en) * | 2018-06-21 | 2020-01-09 | 日揮ホールディングス株式会社 | Method for producing nickel sulfate compound |
| JP7042719B2 (en) | 2018-06-21 | 2022-03-28 | 日揮グローバル株式会社 | Method for manufacturing nickel sulfate compound |
| CN109279666A (en) * | 2018-10-09 | 2019-01-29 | 金川集团股份有限公司 | A method of nickel sulfate solution is produced by raw material of nickel oxide |
| CN109279667A (en) * | 2018-10-09 | 2019-01-29 | 金川集团股份有限公司 | A method of LITHIUM BATTERY nickel sulfate is produced by raw material of nickel oxide |
| CN109205687A (en) * | 2018-10-09 | 2019-01-15 | 金川集团股份有限公司 | A method of LITHIUM BATTERY nickel sulfate is prepared by raw material of nickel oxide |
| CN110092423A (en) * | 2019-04-23 | 2019-08-06 | 金川集团股份有限公司 | A kind of nickel oxide quickly dissolves, the method for nickel soap depickling removal of impurities production nickel sulfate solution |
| CN110104694A (en) * | 2019-04-23 | 2019-08-09 | 金川集团股份有限公司 | A method of nickel chloride solution is prepared using nickel oxide |
| CN110092423B (en) * | 2019-04-23 | 2021-06-29 | 金川集团股份有限公司 | Method for producing nickel sulfate solution by quickly dissolving nickel oxide and deacidifying and removing impurities with nickel soap |
| CN112062171A (en) * | 2019-06-10 | 2020-12-11 | 天津市茂联科技有限公司 | Method for separating nickel and magnesium from crude nickel carbonate |
| CN110607439A (en) * | 2019-09-12 | 2019-12-24 | 金川集团股份有限公司 | Spherical nickel protoxide sectional oxidation acid leaching treatment method |
| EP4166508A1 (en) * | 2021-10-04 | 2023-04-19 | Prime Planet Energy & Solutions, Inc. | Method of producing nickel sulfate |
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