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.
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.