CN108423716A - It is a kind of to prepare the method and its nickel salt for refining nickel salt as raw material using reduced nickel powder - Google Patents
It is a kind of to prepare the method and its nickel salt for refining nickel salt as raw material using reduced nickel powder Download PDFInfo
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- CN108423716A CN108423716A CN201810265426.8A CN201810265426A CN108423716A CN 108423716 A CN108423716 A CN 108423716A CN 201810265426 A CN201810265426 A CN 201810265426A CN 108423716 A CN108423716 A CN 108423716A
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- nickel
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- nickel powder
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention belongs to fine inorganic chemicals product technical fields, disclose a kind of method and its nickel salt for being prepared as raw material using reduced nickel powder and refining nickel salt.The method of the present invention includes the following steps：(1) it leaches reduced nickel powder with acid solution and obtains nickel salt solution；(2) hydrogen peroxide is added into nickel salt solution, adjusts pH to 4.0 5.5；(3) it is separated by solid-liquid separation, liquid evaporation crystallization obtains refined nickel salt.The present invention also provides the refined nickel salts that the above method is prepared.Preparation method processing step of the present invention is simple, production process is easy to control, products obtained therefrom purity is high, calcium, magnesium, iron, copper, zinc, the cadmium impurity of the nickel salt product of acquisition are both less than 10ppm, and product can be used for preparing lithium ion battery binary presoma (nickel cobalt hydroxide, nickel manganese hydroxide) and ternary precursor (nickel cobalt manganese hydroxide).The method for refining nickel salt being prepared by raw material of reduced nickel powder the present invention provides a kind of, the preparation to refine nickel salt provides a new approach.
Description
Technical field
The invention belongs to fine inorganic chemicals product technical fields, more particularly to a kind of to prepare essence by raw material of reduced nickel powder
The method and its nickel salt of nickel salt processed.
Background technology
Refined nickel salt can be used for preparing nickeliferous lithium ion battery material presoma.Northeastern University Wang Hong etc. has studied a kind of complete
The method that wet-treating dead catalyst containing nickel prepares nickel sulfate hexahydrate crystal.Using dissolution of raw material-extraction and recovery copper-chemical cleaning method-depth
Spend the technological process of purification-extraction back extraction nickel-condensing crystallizing, the impurity ratio such as Fe, Co, Zn, Cu, Pb of obtained nickel sulfate hexahydrate crystal
It is higher, the not up to standard of refined sulfuric acid nickel, and technological process complexity.It is raw material that Jiang Jing, which has studied with crude nickel sulfate, is passed through
Dissolving, oxidation neutralize except iron, extraction except Fe, Cu, Mg, primary concentration, with nickel fluoride removing calcium and magnesium, secondary concentration, crystallisation by cooling
Processing step, it is final to obtain nickel sulfate, but the Fe impurity contents of the method products obtained therefrom are 17ppm.The method complex process, institute
The standard (5ppm) that product is not up to refined sulfuric acid nickel is obtained, the raw material of lithium ion battery material presoma is cannot function as.
It is that raw material prepares the method for refining nickel salt the present invention provides a kind of reduced nickel powder, the preparation to refine nickel salt provides
One new approach.Preparation method processing step of the present invention is simple, and production process is easy to control, and products obtained therefrom purity is high, can
It is used to prepare nickeliferous lithium ion battery material presoma.
Invention content
In order to overcome above-mentioned prior art preparation to refine in nickel salt technological process length, nickel salt product, impurity content is high, manufactures
The big disadvantage of chemical raw material dosage and deficiency in the process, the primary purpose of the present invention is that providing one kind using reduced nickel powder as raw material
The method for refining nickel salt is prepared, the preparation to refine nickel salt provides a new approach.
Another object of the present invention is to provide the refined nickel salt that the above method is prepared.
The purpose of the present invention is realized by following proposal：
A method of it is prepared as raw material using reduced nickel powder and refines nickel salt, included the following steps：
(1) it leaches reduced nickel powder with acid solution and obtains nickel salt solution；
(2) hydrogen peroxide is added into nickel salt solution, adjusts pH to 4.0-5.5；
(3) it is separated by solid-liquid separation, liquid evaporation crystallization obtains refined nickel salt.
The dosage of the acid is 0.8~1.1 times that nickel powder is completely dissolved quality needed for theory.
The n of the acid solutionH+=3.0~5.0mol/L.
In step (1), the acid can be one kind in sulfuric acid or hydrochloric acid.
In step (1), the reaction temperature of the leaching is 50~100 DEG C.
In step (1), the reduced nickel powder can be the bulk that powdered reduced nickel powder or reduced nickel powder physics are pressed into
Object.
In step (1), air is blasted into leaching container during the leaching, makes the hydrogen volume concentration in container
Less than 4.1%；Or closing leaches container and only stays a gas outlet that the hydrogen volume concentration in device is made to be more than 74.2%.
In the method for the present invention, the essential element content such as table 1 of the reduced nickel powder：
Table 1
In the method for the present invention, step (1) and step (2) can be intermittent or continous way method；
The intermittent concrete operations are：Reduced nickel powder is added in container to leaching, it is 1 that solid-to-liquid ratio, which is added,:7~1:10
Water, be added with stirring acid, react 6~18h；Hydrogen peroxide is added, pH to 4.0-5.5 is adjusted.
The continuous concrete operations are：The container being sequentially communicated using multiple tops is persistently added from first container
Enter acid solution, acid solution overflows to second container through first container, arrives a last container successively；Persistently add into each container
Enter reduced nickel powder；Hydrogen peroxide is added in last container, adjusts pH to 4.0-5.5.
In the continous way, be added reduced nickel powder amount should control it is equal or close with leaching content.
The refined nickel salt that the method for the present invention is prepared is that (molecular formula is refined sulfuric acid nickel：xNiSO4·6H2O·
yNiSO4·7H2O) or refined nickel chloride (molecular formula is：NiCl2·6H2O)；Essential element content such as table 2.
Table 2
Preparation method processing step of the present invention is simple, and production process is easy to control, and products obtained therefrom purity is high, the nickel salt of acquisition
Calcium, magnesium, iron, copper, zinc, the cadmium impurity of product are both less than 10ppm, and product can be used for preparing lithium ion battery binary presoma (nickel
Cobalt hydroxide, nickel manganese hydroxide) and ternary precursor (nickel cobalt manganese hydroxide).The present invention provides one kind with reduced nickel
Powder is that raw material prepares the method for refining nickel salt, and the preparation to refine nickel salt provides a new approach.
Description of the drawings
Fig. 1 and Fig. 2 is the process flow chart of preparation method of the present invention.
Specific implementation mode
With reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
Material involved in the following example can be obtained from commercial channel.
Embodiment 1
Process flow chart is shown in Fig. 1.
(1) concentrated sulfuric acid 200g in 120 grams of container of the reduced nickel powder addition equipped with 1L deionized waters, being added 98% is stirred
Reaction 10h is mixed, air is blasted into leaching container makes the hydrogen volume concentration in container be less than 4.1%；
(2) 30% hydrogen peroxide is added into container, when solution ph rises to 4.5 or so, stopping adds hydrogen peroxide；
(3) be separated by solid-liquid separation 112g/L nickel sulfate solution；
(4) nickel sulfate solution evaporative crystallization obtains refined sulfuric acid nickel product, the constituent content such as table 3 of product.
Embodiment 2
Process flow chart is shown in Fig. 1.
(1) 120 grams of reduced nickel powder is added in the container equipped with 1L deionized waters, 30% hydrochloric acid 495g stirrings is added
12h is reacted, nitrogen is blasted into leaching container makes the hydrogen volume concentration in container be less than 4.1%；
(2) 30% hydrogen peroxide is added into container, when solution ph rises to left and right, stopping plus hydrogen peroxide；
(3) be separated by solid-liquid separation 114g/L nickel chloride solution；
(4) nickel chloride solution evaporative crystallization must refine nickel chloride product, the constituent content such as table 3 of product.
Embodiment 3
Process flow chart is shown in Fig. 2.
(1) have 5 dischargeable capacity 1.0L containers, upper vessel portion is connected with pipeline, be separately added into five containers 420g,
The nickel powder of 105g, 54g, 39g and 15g,
(2) sulfuric acid of 1.59mol/L, flow 0.3L/h are added into first container, solution is passed through from first container
It crosses overflow port and flows to second container, until the 5th container, closed container makes each container only stay a gas outlet, retainer
In hydrogen volume concentration be more than 74.2%；
(3) after solution fills up, detect five containers in nickel content be respectively 71.5g/L, 88.6g/L, 97.4g/L,
The nickel of 71.5g, 17.1g, 8.8g, 6.3g and 2.8g is added in 103.7g/L and 106.5g/L into five containers respectively after detection
Powder；
(4) to the 5th container continue that hydrogen peroxide is added with the speed of 5.0L/h, make the pH value of solution in the 5th container
Between 4.2-5.0；
(5) cross detect nickel in five containers again within five hours content be respectively 73.6g/L, 93.1g/L, 101.7g/L,
105.4g/L and 116.2g/L；Distinguish after detection and 112.0g, 30.0g, 13.0g, 6.0g and 16.0g are added in five containers
Nickel powder；
(6) every five hours, the nickel of 112.0g, 30.0g, 13.0g, 6.0g and 16.0g were added into five containers after
Powder；
The solution of (7) the 5th container outflows is by being separated by solid-liquid separation to obtain nickel sulfate solution；
(8) nickel sulfate solution evaporative crystallization obtains refined sulfuric acid nickel product, the constituent content such as table 3 of product.
Table 3 refines the constituent content of nickel salt
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (10)
1. a kind of preparing the method for refining nickel salt by raw material of reduced nickel powder, it is characterised in that include the following steps：(1) acid solution is used
It leaches reduced nickel powder and obtains nickel salt solution；
(2) hydrogen peroxide is added into nickel salt solution, adjusts pH to 4.0-5.5；
(3) it is separated by solid-liquid separation, liquid evaporation crystallization obtains refined nickel salt.
2. according to claim 1 prepare the method for refining nickel salt by raw material of reduced nickel powder, it is characterised in that：The acid
Dosage be that nickel powder is completely dissolved 0.8~1.1 times of quality needed for theory.
3. according to claim 1 prepare the method for refining nickel salt by raw material of reduced nickel powder, it is characterised in that：The acid
The n of liquidH+=3.0~5.0mol/L.
4. according to claim 1 prepare the method for refining nickel salt by raw material of reduced nickel powder, it is characterised in that：Described
Acid is sulfuric acid or hydrochloric acid.
5. according to claim 1 prepare the method for refining nickel salt by raw material of reduced nickel powder, it is characterised in that：The leaching
The reaction temperature gone out is 50~100 DEG C.
6. according to claim 1 prepare the method for refining nickel salt by raw material of reduced nickel powder, it is characterised in that：Step
(1) in, air is blasted into leaching container during the leaching, the hydrogen volume concentration in container is made to be less than 4.1%；Or
Closing leaches container and only stays a gas outlet that the hydrogen volume concentration in device is made to be more than 74.2%.
7. according to claim 1 prepare the method for refining nickel salt by raw material of reduced nickel powder, it is characterised in that：Step
(1) and step (2) is intermittent or continous way method.
8. according to claim 7 prepare the method for refining nickel salt by raw material of reduced nickel powder, it is characterised in that：Described
The concrete operations for formula of having a rest are：Reduced nickel powder is added in container to leaching, it is 1 that solid-to-liquid ratio, which is added,:7~1:10 water, stirring is lower to be added
Enter acid, reacts 6~18h；Hydrogen peroxide is added, pH to 4.0-5.5 is adjusted.
9. according to claim 7 prepare the method for refining nickel salt by raw material of reduced nickel powder, it is characterised in that：The company
The concrete operations of continuous formula are：The container being sequentially communicated using multiple tops is continuously added into acid solution from first container, and acid solution is through
One receptacle overflow arrives a last container successively to second container；It is continuously added into reduced nickel powder into each container；Most
Hydrogen peroxide is added in container afterwards, adjusts pH to 4.0-5.5.
10. a kind of refined nickel salt, it is characterised in that obtained according to claim 1~9 any one of them preparation method.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810265426.8A CN108423716A (en) | 2018-03-28 | 2018-03-28 | It is a kind of to prepare the method and its nickel salt for refining nickel salt as raw material using reduced nickel powder |
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| CN201810265426.8A CN108423716A (en) | 2018-03-28 | 2018-03-28 | It is a kind of to prepare the method and its nickel salt for refining nickel salt as raw material using reduced nickel powder |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021105365A1 (en) * | 2019-11-27 | 2021-06-03 | Solvay Sa | A process for manufacturing nickel sulphate |
| CN113578235A (en) * | 2021-07-30 | 2021-11-02 | 福建常青新能源科技有限公司 | Production device of nickel sulfate solution |
| CN114014385A (en) * | 2021-10-12 | 2022-02-08 | 广东邦普循环科技有限公司 | Method for preparing nickel oxide by using water quenched nickel |
| CN114314699A (en) * | 2021-12-31 | 2022-04-12 | 金川集团镍盐有限公司 | Iron removal method for nickel pill dissolving solution in chlorination system |
| CN114835176A (en) * | 2022-05-30 | 2022-08-02 | 金川集团镍盐有限公司 | Preparation method of spherical anhydrous nickel chloride product |
| CN115353158A (en) * | 2022-08-11 | 2022-11-18 | 中冶瑞木新能源科技有限公司 | Method for preparing sulfate solution |
| CN115403082A (en) * | 2022-10-11 | 2022-11-29 | 金川集团镍盐有限公司 | Method for producing electroplated nickel chloride by taking electrodeposited nickel as raw material |
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| US20060067874A1 (en) * | 2003-12-04 | 2006-03-30 | Chevrontexaco Technology Ventures Llc | Method of producing a nickel salt solution |
| CN102040252A (en) * | 2009-10-16 | 2011-05-04 | 中科铜都粉体新材料股份有限公司 | Method for producing battery-level refined nickel sulfate with electrolyte |
| JP5904459B2 (en) * | 2011-11-22 | 2016-04-13 | 住友金属鉱山株式会社 | Manufacturing method of high purity nickel sulfate |
| CN106241897A (en) * | 2016-08-27 | 2016-12-21 | 无锡中天固废处置有限公司 | A kind of method that nickel plating Ageing solution prepares metal sulfate nickel, sodium dihydrogen phosphate and sodium sulfate |
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2018
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20060067874A1 (en) * | 2003-12-04 | 2006-03-30 | Chevrontexaco Technology Ventures Llc | Method of producing a nickel salt solution |
| CN102040252A (en) * | 2009-10-16 | 2011-05-04 | 中科铜都粉体新材料股份有限公司 | Method for producing battery-level refined nickel sulfate with electrolyte |
| JP5904459B2 (en) * | 2011-11-22 | 2016-04-13 | 住友金属鉱山株式会社 | Manufacturing method of high purity nickel sulfate |
| CN106241897A (en) * | 2016-08-27 | 2016-12-21 | 无锡中天固废处置有限公司 | A kind of method that nickel plating Ageing solution prepares metal sulfate nickel, sodium dihydrogen phosphate and sodium sulfate |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021105365A1 (en) * | 2019-11-27 | 2021-06-03 | Solvay Sa | A process for manufacturing nickel sulphate |
| CN113578235A (en) * | 2021-07-30 | 2021-11-02 | 福建常青新能源科技有限公司 | Production device of nickel sulfate solution |
| CN114014385A (en) * | 2021-10-12 | 2022-02-08 | 广东邦普循环科技有限公司 | Method for preparing nickel oxide by using water quenched nickel |
| CN114014385B (en) * | 2021-10-12 | 2023-10-17 | 广东邦普循环科技有限公司 | Method for preparing nickel oxide by utilizing water quenched nickel |
| CN114314699A (en) * | 2021-12-31 | 2022-04-12 | 金川集团镍盐有限公司 | Iron removal method for nickel pill dissolving solution in chlorination system |
| CN114835176A (en) * | 2022-05-30 | 2022-08-02 | 金川集团镍盐有限公司 | Preparation method of spherical anhydrous nickel chloride product |
| CN115353158A (en) * | 2022-08-11 | 2022-11-18 | 中冶瑞木新能源科技有限公司 | Method for preparing sulfate solution |
| CN115403082A (en) * | 2022-10-11 | 2022-11-29 | 金川集团镍盐有限公司 | Method for producing electroplated nickel chloride by taking electrodeposited nickel as raw material |
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Application publication date: 20180821 |
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