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CN114835176A - Preparation method of spherical anhydrous nickel chloride product - Google Patents

Preparation method of spherical anhydrous nickel chloride product Download PDF

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Publication number
CN114835176A
CN114835176A CN202210598521.6A CN202210598521A CN114835176A CN 114835176 A CN114835176 A CN 114835176A CN 202210598521 A CN202210598521 A CN 202210598521A CN 114835176 A CN114835176 A CN 114835176A
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CN
China
Prior art keywords
nickel chloride
product
spherical anhydrous
preparing
impurity removal
Prior art date
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Pending
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CN202210598521.6A
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Chinese (zh)
Inventor
龚继宝
麻在生
陈士强
魏焘
苏一会
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Jinchuan Group Nickel Salt Co ltd
Original Assignee
Jinchuan Group Nickel Salt Co ltd
Jinchuan Group Co Ltd
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Priority to CN202210598521.6A priority Critical patent/CN114835176A/en
Publication of CN114835176A publication Critical patent/CN114835176A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00Compounds of nickel
    • C01G53/08Halides; Oxyhalides
    • C01G53/09Chlorides; Oxychlorides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/30Particle morphology extending in three dimensions
    • C01P2004/32Spheres
    • 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)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention relates to a preparation method of a spherical anhydrous nickel chloride product, which comprises the following steps: firstly, dissolving hydrochloric acid: cutting the nickel into small pieces, and dissolving the small pieces in a hydrochloric acid medium to obtain a nickel chloride solution; chemical impurity removal: adding an oxidant into the nickel chloride solution to adjust the pH value, and removing Fe to obtain a nickel chloride solution after impurity removal; thirdly, evaporation and crystallization: evaporating, concentrating and crystallizing the nickel chloride solution after impurity removal to obtain nickel chloride crystals; and fourthly, drying, crushing and screening the nickel chloride crystal in vacuum to obtain a spherical anhydrous nickel chloride product with the granularity of 1.3-3.5 mm. The method has the advantages of strong operability, short process flow, low production cost and high application value, and solves the problems of high production cost, complex process, organic entrainment in products, difficulty in realizing industrial production and the like of the anhydrous nickel chloride.

Description

Preparation method of spherical anhydrous nickel chloride product
Technical Field
The invention relates to the technical field of powder metallurgy, in particular to a preparation method of a spherical anhydrous nickel chloride product.
Background
The anhydrous nickel chloride is mainly used for producing nano-scale superfine nickel powder and chip multilayer ceramic capacitors (MLCC), and the MLCC is used in the fields of smart phones, new energy automobiles and the like. At present, anhydrous nickel chloride is mainly produced by a direct chlorination method of metallic nickel, an oxide decomposition chlorination method, an extraction method of organic solvents such as thionyl chloride and the like, but the method has high requirements on raw materials and reagents, toxic gases and organic solvents are involved in the preparation process, and the experimental risk is high; meanwhile, the method also uses an organic reagent in the preparation process, so that organic matters are easy to be carried into the product, and industrial application is difficult to realize.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a spherical anhydrous nickel chloride product with strong operability, short process flow and low production cost.
In order to solve the problems, the preparation method of the spherical anhydrous nickel chloride product comprises the following steps:
the preparation method comprises the following steps of hydrochloric acid dissolution:
cutting the nickel into small pieces, and dissolving the small pieces in a hydrochloric acid medium to obtain a nickel chloride solution;
chemical impurity removal:
adding an oxidant into the nickel chloride solution to adjust the pH value, and removing Fe to obtain a nickel chloride solution after impurity removal;
the evaporation and crystallization:
evaporating, concentrating and crystallizing the nickel chloride solution after impurity removal to obtain nickel chloride crystals;
and fourthly, drying, crushing and screening the nickel chloride crystal in vacuum to obtain a spherical anhydrous nickel chloride product with the granularity of 1.3-3.5 mm.
The method comprises the steps of cutting the nickel into small pieces of material with the length of 2.5cm by 2.5 cm.
H of hydrochloric acid in the step + =5.0~6.0g/L。
The step II is characterized in that the oxidant is 15% -20% of hydrogen peroxide.
The pH = 3.0-4.0 in the step II.
In the step three, the solution after evaporation contains Ni 2+ =260~300g/L。
And step three, the nickel chloride crystal in the step three is nickel chloride hexahydrate.
The vacuum drying condition in the step four is that the high-pressure protective gas is nitrogen or argon, the temperature is 400-450 ℃, and the pressure of the high-pressure protective gas is 0.8-1.2 MPa.
Compared with the prior art, the invention has the following advantages:
1. the method adopts hydrochloric acid to dissolve electrolytic nickel, oxidize and remove impurities, and evaporate and crystallize to produce nickel chloride crystals, and finally the nickel chloride crystals react through a vacuum drying process to produce high-quality spherical anhydrous nickel chloride semi-finished products, and the high-quality spherical anhydrous nickel chloride semi-finished products are crushed and screened to improve the uniformity of anhydrous nickel chloride particles.
2. The method for producing the high-quality anhydrous nickel chloride product by using the vacuum drying method realizes the purposes of strong operability, short process flow and low production cost, has high application value, and solves the problems of high production cost, complex process, organic entrainment in the product, difficulty in realizing industrial production and the like of the anhydrous nickel chloride.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 is a schematic representation of a semi-finished product in example 3 of the present invention.
Fig. 2 is a schematic representation of the finished product in example 3 of the present invention.
Detailed Description
A method for preparing a spherical anhydrous nickel chloride product comprises the following steps:
firstly, dissolving hydrochloric acid:
cutting the nickel into small pieces of 2.5cm by 2.5cm in H + And (3) dissolving the nickel chloride solution in a hydrochloric acid medium of which the concentration is 5.0-6.0 g/L to obtain a nickel chloride solution.
Chemical impurity removal:
adding an oxidant into the nickel chloride solution to adjust the pH = 3.0-4.0, and removing Fe to obtain a nickel chloride solution after impurity removal; the oxidant is 15% -20% of hydrogen peroxide.
Thirdly, evaporation and crystallization:
evaporating and concentrating the nickel chloride solution after impurity removal by using an evaporator, wherein the concentrated solution after evaporation contains Ni 2+ And = 260-300 g/L. And crystallizing the concentrated solution in a crystallizer to obtain nickel chloride hexahydrate crystals.
Putting the nickel chloride crystal into a vacuum drier, opening a high-pressure protective gas valve, wherein the high-pressure protective gas is nitrogen or argon, the pressure of the high-pressure protective gas is 0.8-1.2 MPa, and drying the nickel chloride crystal in vacuum at 400-450 ℃ for 2.0-5.0 h to ensure that the nickel chloride crystal is dried and dehydrated in a vacuum environment; and (3) crushing and screening the dehydrated semi-finished anhydrous nickel chloride product to obtain a spherical anhydrous nickel chloride product with the granularity of 1.3-3.5 mm.
Example 1 a method for preparing a spherical anhydrous nickel chloride product, comprising the steps of:
firstly, dissolving hydrochloric acid:
cutting the nickel into small pieces of 2.5cm by 2.5cm in H + And (4) dissolving in a hydrochloric acid medium of which the concentration is 5.2g/L to obtain a nickel chloride solution.
Chemical impurity removal:
adding 16% hydrogen peroxide into the nickel chloride solution to adjust the pH value of the solution to be 3.2, and completely removing Fe to obtain the nickel chloride solution after impurity removal.
The evaporation and crystallization:
evaporating and concentrating the nickel chloride solution after impurity removal by using an evaporator, wherein the concentrated solution after evaporation contains Ni 2+ =260.6 g/L. And crystallizing the concentrated solution in a crystallizer to obtain nickel chloride hexahydrate crystals.
Putting the nickel chloride crystal into a vacuum drier, opening a high-pressure protective gas valve, wherein the high-pressure protective gas is nitrogen, the pressure of the high-pressure protective gas is 0.85MPa, and performing vacuum drying at 425 ℃ for 2.5h to ensure that the nickel chloride crystal is dried and dehydrated in a vacuum environment; and (4) crushing and screening the dehydrated semi-finished anhydrous nickel chloride product to obtain a spherical anhydrous nickel chloride product with the granularity of 1.35 mm.
Example 2 a method for preparing a spherical anhydrous nickel chloride product, comprising the steps of:
firstly, dissolving hydrochloric acid:
cutting the nickel into small pieces of 2.5cm by 2.5cmMaterials in H + And (4) dissolving in a hydrochloric acid medium of which the concentration is 5.5g/L to obtain a nickel chloride solution.
Chemical impurity removal:
adding 17% hydrogen peroxide into the nickel chloride solution to adjust the pH =3.5 to completely remove Fe, and obtaining the nickel chloride solution after impurity removal.
The evaporation and crystallization:
evaporating and concentrating the nickel chloride solution after impurity removal by using an evaporator, wherein the concentrated solution after evaporation contains Ni 2+ =275.8 g/L. And (4) crystallizing the concentrated solution in a crystallizer to obtain crystals of nickel chloride hexahydrate.
Putting the nickel chloride crystal into a vacuum drier, opening a high-pressure protective gas valve, wherein the high-pressure protective gas is nitrogen, and drying the nickel chloride crystal at 430 ℃ for 3.0h in vacuum under the pressure of 1.0MPa to obtain an anhydrous nickel chloride semi-finished product; and (4) crushing and screening the dehydrated semi-finished anhydrous nickel chloride product to obtain a spherical anhydrous nickel chloride product with the granularity of 2.57 mm.
Example 3 a method for preparing a spherical anhydrous nickel chloride product, comprising the steps of:
firstly, dissolving hydrochloric acid:
cutting the nickel into small pieces of 2.5cm by 2.5cm in H + And (4) dissolving in hydrochloric acid medium of =6.0g/L to obtain a nickel chloride solution.
Chemical impurity removal:
adding 19.5% hydrogen peroxide into the nickel chloride solution to adjust the pH =3.8 to completely remove Fe, thereby obtaining the nickel chloride solution after impurity removal.
Thirdly, evaporation and crystallization:
evaporating and concentrating the nickel chloride solution after impurity removal by using an evaporator, wherein the concentrated solution after evaporation contains Ni 2+ =297.2 g/L. And crystallizing the concentrated solution in a crystallizer to obtain nickel chloride hexahydrate crystals.
Putting the nickel chloride crystal into a vacuum drier, opening a high-pressure protective gas valve, wherein the high-pressure protective gas is nitrogen, the pressure of the high-pressure protective gas is 1.15MPa, and performing vacuum drying at 450 ℃ for 4.0h to obtain an anhydrous nickel chloride semi-finished product, as shown in fig. 1; and (3) crushing and screening the dehydrated semi-finished anhydrous nickel chloride product to obtain a spherical anhydrous nickel chloride product with the granularity of 3.0 mm, as shown in figure 2.

Claims (8)

1. A method for preparing a spherical anhydrous nickel chloride product comprises the following steps:
firstly, dissolving hydrochloric acid:
cutting the nickel into small pieces, and dissolving the small pieces in a hydrochloric acid medium to obtain a nickel chloride solution;
chemical impurity removal:
adding an oxidant into the nickel chloride solution to adjust the pH value, and removing Fe to obtain a nickel chloride solution after impurity removal;
the evaporation and crystallization:
evaporating, concentrating and crystallizing the nickel chloride solution after impurity removal to obtain nickel chloride crystals;
and fourthly, drying, crushing and screening the nickel chloride crystal in vacuum to obtain a spherical anhydrous nickel chloride product with the granularity of 1.3-3.5 mm.
2. The method of claim 1 for preparing a spherical anhydrous nickel chloride product, wherein: the method comprises the steps of cutting the nickel into small pieces of material with the length of 2.5cm by 2.5 cm.
3. The method of claim 1 for preparing a spherical anhydrous nickel chloride product, wherein: h of hydrochloric acid in the step + =5.0~6.0g/L。
4. The method of claim 1 for preparing a spherical anhydrous nickel chloride product, wherein: the step II is characterized in that the oxidant is 15% -20% of hydrogen peroxide.
5. The method of claim 1 for preparing a spherical anhydrous nickel chloride product, wherein: the pH = 3.0-4.0 in the step II.
6. The method of claim 1 for preparing a spherical anhydrous nickel chloride product, wherein: in the step three, the solution after evaporation contains Ni 2+ =260~300g/L。
7. The method of claim 1 for preparing a spherical anhydrous nickel chloride product, wherein: and step three, the nickel chloride crystal in the step three is nickel chloride hexahydrate.
8. The method of claim 1 for preparing a spherical anhydrous nickel chloride product, wherein: the vacuum drying condition in the step four is that the high-pressure protective gas is nitrogen or argon, the temperature is 400-450 ℃, and the pressure of the high-pressure protective gas is 0.8-1.2 MPa.
CN202210598521.6A 2022-05-30 2022-05-30 Preparation method of spherical anhydrous nickel chloride product Pending CN114835176A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5853692A (en) * 1993-07-02 1998-12-29 Pohang Iron & Steel Co., Ltd. Process for manufacturing high purity nickel chloride by recycling waste nickel anode
CN1596152A (en) * 2001-11-26 2005-03-16 纳幕尔杜邦公司 Preparation method of nickel/phosphorus ligand catalyst for olefin hydrocyanation
JP2005194139A (en) * 2004-01-07 2005-07-21 Fujikura Ltd Method for producing anhydrous nickel chloride
CN102060336A (en) * 2010-11-30 2011-05-18 沈阳鑫劲粉体工程有限责任公司 Method for preparing high-purity anhydrous nickel chloride
CN106395921A (en) * 2016-08-29 2017-02-15 金川集团股份有限公司 Method used for producing nickel chloride products taking waste printing nickel screens as raw materials
TW201730114A (en) * 2016-01-21 2017-09-01 Jx Nippon Mining & Metals Corp Anhydrous nickel chloride and method for producing same
CN108423716A (en) * 2018-03-28 2018-08-21 湖南邦普循环科技有限公司 It is a kind of to prepare the method and its nickel salt for refining nickel salt as raw material using reduced nickel powder
CN112563489A (en) * 2020-12-16 2021-03-26 北方特种能源集团有限公司西安庆华公司 Preparation method of nickel chloride anode for novel thermal battery

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5853692A (en) * 1993-07-02 1998-12-29 Pohang Iron & Steel Co., Ltd. Process for manufacturing high purity nickel chloride by recycling waste nickel anode
CN1596152A (en) * 2001-11-26 2005-03-16 纳幕尔杜邦公司 Preparation method of nickel/phosphorus ligand catalyst for olefin hydrocyanation
JP2005194139A (en) * 2004-01-07 2005-07-21 Fujikura Ltd Method for producing anhydrous nickel chloride
CN102060336A (en) * 2010-11-30 2011-05-18 沈阳鑫劲粉体工程有限责任公司 Method for preparing high-purity anhydrous nickel chloride
TW201730114A (en) * 2016-01-21 2017-09-01 Jx Nippon Mining & Metals Corp Anhydrous nickel chloride and method for producing same
CN106395921A (en) * 2016-08-29 2017-02-15 金川集团股份有限公司 Method used for producing nickel chloride products taking waste printing nickel screens as raw materials
CN108423716A (en) * 2018-03-28 2018-08-21 湖南邦普循环科技有限公司 It is a kind of to prepare the method and its nickel salt for refining nickel salt as raw material using reduced nickel powder
CN112563489A (en) * 2020-12-16 2021-03-26 北方特种能源集团有限公司西安庆华公司 Preparation method of nickel chloride anode for novel thermal battery

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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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Effective date of registration: 20240326

Address after: 737100 No.1 Lanzhou Road, Jinchuan District, Jinchang City, Gansu Province

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Address before: 737100 No.1 Lanzhou Road, Jinchuan District, Jinchang City, Gansu Province

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Application publication date: 20220802

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