Preparation method of electronic-grade nickel protoxide
Nickel suboxide was prepared by reacting sodium carbonate and nickel sulfate solution, centrifuging and washing, and calcining. This method solved the problems of complex preparation process, low purity and environmental unfriendliness in the existing technology, and achieved the preparation of high-purity and easily controllable nickel suboxide.
Patent Information
- Application Number
- CN202511351170.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-09-22
- Publication Date
- 2026-01-13
AI Technical Summary
Existing chemical methods for preparing nickel oxide have problems such as difficulty in washing and filtering the product, precipitant adhesion to the container wall, high temperature and high pressure reaction conditions, environmental unfriendliness, long production cycle and high cost.
Nickel suboxide was prepared by reacting sodium carbonate and nickel sulfate solution, controlling the pH value and flow rate, and then calcining it in a muffle furnace after centrifugation, washing and drying, while maintaining the precursor morphology and controlling the morphology of nickel suboxide.
The prepared nickel oxide has high purity, easily controllable morphology, simple steps, and low energy consumption, meeting the requirements for electronic grade.
Smart Images
Figure CN121317901A_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application belongs to the field of metal powder preparation, and particularly relates to a preparation method of electronic-grade nickel protoxide. BACKGROUND
[0002] Nickel protoxide as a high-tech functional material has a wide application in the field of new energy batteries and electronic technology, and has a broad prospect and important commercial value. The preparation methods of nickel protoxide mainly include physical methods and chemical methods. The nickel powder produced by the physical method has a large particle size and a wide distribution, and even some components may have dendritic segregation and intergranular segregation. The chemical preparation method is widely used in actual production due to its simple operation and easy control. The chemical preparation method is simple in operation, easy to control, and suitable for mass production.
[0003] The chemical methods currently used include coprecipitation method, homogeneous precipitation method, hydrolysis method, hydrothermal method, organic complex precursor method, spray pyrolysis method, sol-gel method, and microemulsion method.
[0004] The coprecipitation method has a low cost, but the product is a colloidal substance, which is difficult to wash and filter. In the preparation of nickel protoxide by the homogeneous precipitation method, the precipitant is easily attached to the surface of the wall and is difficult to remove, which increases the uncertainty of the experiment. The hydrolysis method includes metal alkoxide method and inorganic salt hydrolysis method. The raw material of the former is relatively expensive, because the preparation of metal organic matter is difficult and the cycle is long. In the latter, there is always an incomplete hydrolysis phenomenon in the hydrolysis process of inorganic salt, which leads to the defect of less nickel hydroxide colloid. The hydrothermal method refers to that the solubility of hydroxide is greater than that of the corresponding oxide at high temperature and high pressure, and the oxide can be precipitated from the solution. Although this production method can directly produce nickel protoxide products, the performance requirements of the container are high due to the high temperature and high pressure of the reaction condition. The organic complex precursor method is a method for synthesizing oxide nanocrystalline substances. The stability of the organic complex precursor is not easy to control, and a dispersing agent needs to be added in the synthesis process, which also easily introduces impurities and affects the purity of the product in the later period. Although the spray pyrolysis method is simple, some salt types are easy to produce toxic and harmful gases during thermal decomposition, which is not friendly to the environment. The powder prepared by the sol-gel method has high purity, but the gel process is slow and the production cycle is long. In the process of preparing nickel protoxide by the microemulsion method, the consumption of drugs is large, and the cost is high. SUMMARY
[0005] In order to solve the above technical problems, the present application provides a preparation method of nickel protoxide which basically maintains the morphology of the original precursor. The prepared nickel protoxide has high purity, the morphology is easy to control, the steps are simple, and the energy consumption is low.
[0006] Therefore, the present application adopts the following technical solutions: A method for preparing electronic-grade nickel suboxide includes the following steps: (1) Solution preparation: Prepare sodium carbonate and nickel sulfate solutions with the required wave ratio; (2) Synthesis: Sodium carbonate and nickel sulfate are introduced into a reaction vessel to react. Samples are taken at different times during the reaction to measure the pH of the solution; (3) Washing: The product generated by the reaction is transferred to a centrifuge for washing to remove sulfate ions and sodium ions from the sodium carbonate slurry; (4) Drying: The sodium carbonate slurry after washing and centrifugation is dried to obtain the precursor nickel carbonate; (5) Calcination: The obtained precursor is placed in a muffle furnace and calcined, and then allowed to cool naturally to obtain nickel oxide.
[0007] Furthermore, in step (1), the measuring instrument for the wave ratio is a wave ratio meter. The wave ratio of sodium carbonate is 1.312, and the wave ratio of nickel sulfate is 1.632. During the wave ratio measurement, the solution temperature is 30℃.
[0008] Furthermore, in step (1), the two solutions are prepared, wherein the nickel sulfate solution is at room temperature and the sodium carbonate solution is at 75°C.
[0009] Further, in step (2), the flow rate ratio of sodium carbonate and nickel sulfate is 2:1. The pH of the solution is measured every half hour. The pH measurement is carried out at 55°C. The flow rate of the two reaction liquids is controlled by the pH value. The reaction time of the two liquids in the reactor is 3.5h.
[0010] Furthermore, step (3) washing is carried out in a centrifuge for 3 hours.
[0011] Furthermore, in the washing process described in step (3), the conductivity of the washing liquid is required to be less than or equal to 400 mS / cm.
[0012] Furthermore, in step (4), during the drying process of the sodium carbonate slurry, the inlet air temperature is 150°C and the outlet air temperature is 50°C.
[0013] Furthermore, in step (5), the calcination temperature in the muffle furnace is 1000℃ and the calcination time is 3h.
[0014] The beneficial effect of this invention is that the morphology of nickel oxide is basically consistent with that of the precursor, and the morphology of nickel oxide can be controlled by synthesizing the morphology of the precursor. Attached Figure Description
[0015] Figure 1 This is a process flow diagram of the present invention; Figure 2 This is a scanning electron microscope image of nickel carbonate, the precursor of Example 1 of the present invention; Figure 3 This is the XRD pattern of nickel suboxide in Example 2 of the present invention; Figure 4 This is a scanning electron microscope image of nickel suboxide from Example 3 of the present invention. Detailed Implementation
[0016] In the following example, the wave ratio of sodium carbonate is 1.312 and the wave ratio of nickel sulfate is 1.632. The two solutions are introduced into the reactor at a flow rate of 2:1. The nickel carbonate slurry produced by the reaction is centrifuged, washed and dried to obtain solid nickel carbonate. The solid nickel carbonate is then calcined and naturally cooled to obtain electronic grade nickel oxide.
[0017] Example 1 (1) Prepare a sodium carbonate solution with a wave ratio of 1.312 and a nickel sulfate solution with a wave ratio of 1.632, wherein the sodium carbonate solution is at a temperature of 75°C and the nickel sulfate solution is at room temperature.
[0018] (2) The two solutions are introduced into the reactor at a flow rate of 2:1 to allow for a full reaction.
[0019] (3) The nickel carbonate slurry obtained from the reaction was transferred to a centrifuge for washing and drying, with an electrical conductivity of 380 mS / cm.
[0020] (4) Nickel carbonate can be calcined at 1000℃ for 3 hours and then naturally cooled to obtain nickel oxide product.
[0021] Example 2 (1) Prepare a sodium carbonate solution with a wave ratio of 1.312 and a nickel sulfate solution with a wave ratio of 1.632, wherein the sodium carbonate solution is at a temperature of 75°C and the nickel sulfate solution is at room temperature.
[0022] (2) The two solutions are introduced into the reactor at a flow rate of 2:1 to allow for a full reaction.
[0023] (3) The nickel carbonate slurry obtained from the reaction was transferred to a centrifuge for washing and drying, with an electrical conductivity of 230 mS / cm.
[0024] (4) Nickel carbonate can be calcined at 1000℃ for 3 hours and then naturally cooled to obtain nickel oxide product.
[0025] Example 3 (1) Prepare a sodium carbonate solution with a wave ratio of 1.312 and a nickel sulfate solution with a wave ratio of 1.632, wherein the sodium carbonate solution is at a temperature of 75°C and the nickel sulfate solution is at room temperature.
[0026] (2) The two solutions are introduced into the reactor at a flow rate of 2:1 to allow for a full reaction.
[0027] (3) The nickel carbonate slurry obtained from the reaction was transferred to a centrifuge for washing and drying, with an electrical conductivity of 230 mS / cm.
[0028] (4) Nickel carbonate can be calcined at 1000℃ for 6 hours and then naturally cooled to obtain nickel oxide.
Claims
1. A method for preparing electronic-grade nickel suboxide, characterized in that, Includes the following steps: (1) Solution preparation: Prepare sodium carbonate and nickel sulfate solutions with the required wave ratio; (2) Synthesis: Sodium carbonate and nickel sulfate are introduced into a reaction vessel to react. Samples are taken at different times during the reaction to measure the pH of the solution; (3) Washing: The product generated by the reaction is transferred to a centrifuge for washing to remove sulfate ions and sodium ions from the sodium carbonate slurry; (4) Drying: The sodium carbonate slurry after washing and centrifugation is dried to obtain the precursor nickel carbonate; (5) Calcination: The obtained precursor is placed in a muffle furnace and calcined, and then allowed to cool naturally to obtain nickel oxide.
2. The method for preparing electronic-grade nickel suboxide according to claim 1, characterized in that, In step (1), the measuring instrument for the wave ratio is a wave ratio meter. The wave ratio of sodium carbonate is 1.312 and the wave ratio of nickel sulfate is 1.
632. During the wave ratio measurement, the solution temperature is 30℃.
3. The method for preparing electronic-grade nickel suboxide according to claim 1, characterized in that, The two solutions prepared in step (1) are nickel sulfate solution at room temperature and sodium carbonate solution at 75°C.
4. The method for preparing electronic-grade nickel suboxide according to claim 1, characterized in that, Step (2) The flow rate ratio of sodium carbonate and nickel sulfate is 2:
1. The pH of the solution is measured every half hour. The pH measurement is carried out at 55℃. The flow rate of the two reaction liquids is controlled by the pH value. The reaction time of the two liquids in the reactor is 3.5h.
5. The method for preparing electronic-grade nickel suboxide according to claim 1, characterized in that, Step (3) Washing is carried out in a centrifuge for 3 hours.
6. The method for preparing electronic-grade nickel suboxide according to claim 1, characterized in that, In the washing process described in step (3), the conductivity of the washing liquid is required to be less than or equal to 400 mS / cm.
7. The method for preparing electronic-grade nickel suboxide according to claim 1, characterized in that, In step (4), during the drying process of sodium carbonate slurry, the inlet air temperature is 150℃ and the outlet air temperature is 50℃.
8. The method for preparing electronic-grade nickel suboxide according to claim 1, characterized in that, Step (5) Calcination in a muffle furnace at a temperature of 1000℃ for 3 hours.