Method for reducing chlorine ion content in nickel protoxide product

Abstract

The invention relates to a method for reducing the content of chloride ions in a nickel protoxide product, which comprises the following steps: (1) screening and crushing coarse nickel protoxide with the chlorine content of 0.5-1.0% to obtain crushed nickel protoxide; (2) putting the crushed nickel protoxide into a slurrying kettle, adding pure water, stirring, slurrying and washing to obtain a mixture; (3) adding pure water into the mixture, and carrying out centrifugal separation to respectively obtain a water phase containing chloride ions and a solid; supplementing a water phase containing chloride ions to the tail gas leaching tower; and (4) drying the solid to constant weight, and detecting the finished product to obtain the nickel protoxide product with the chloride ion content of less than or equal to 0.03%. The process is simple, impurities cannot be introduced in the impurity removal process, the impurity removal cost is low, the economical efficiency is high, and the method is suitable for industrial production. After the method is adopted, a nickel protoxide product with the chlorine ion content being smaller than or equal to 0.03% can be obtained.

Description

Technical Field

[0001] The present invention relates to the technical field of hydrometallurgy, and particularly relates to a method for reducing the chloride ion content in nickelous oxide products. Background Art

[0002] Nickelous oxide is an important chemical raw material, which is widely used in industries such as batteries, ceramics, and glass. However, during the production process, nickelous oxide products often contain a certain amount of chloride ions, which not only affects the purity and performance of the products, but also has an adverse impact on subsequent applications. Traditional methods for removing chloride ions have problems such as incomplete removal effect, high treatment cost, and easy generation of secondary pollution.

[0003] Therefore, it is of great significance to develop an efficient, economical, and environmentally friendly method for reducing chloride ions in nickelous oxide products. Summary of the Invention

[0004] The technical problem to be solved by the present invention is to provide a simple and low-cost method for reducing the chloride ion content in nickelous oxide products.

[0005] To solve the above problems, a method for reducing the chloride ion content in nickelous oxide products according to the present invention includes the following steps: ⑴ Coarse nickelous oxide with a chlorine content of 0.5 - 1.0% is sieved and crushed to obtain crushed nickelous oxide with a particle size D50 = 2.0 - 5.0 μm; ⑵ The crushed nickelous oxide is put into a pulping kettle, pure water is added, and after stirring, pulping and washing, a mixture is obtained; ⑶ Pure water is added to the mixture, and after centrifugal separation, an aqueous phase containing chloride ions and a solid are respectively obtained; the aqueous phase containing chloride ions is supplemented to the tail gas scrubbing tower; ⑷ The solid is dried to a constant weight and then subjected to finished product inspection to obtain a nickelous oxide product with a chloride ion content ≤ 0.03%.

[0006] The screening accuracy in step ⑴ is 300 - 500 meshes.

[0007] The conditions for stirring, pulping and washing in step ⑵ refer to a solid-liquid mass ratio of 1:5 - 1:10, a feeding time of 60 - 90 min / kettle, a temperature of 65 - 80°C, a stirring rate of 55 - 90 r / min, and a time of 1.0 - 3.0 h.

[0008] In the centrifugal separation process in step ⑶, feeding is carried out in two times. The first feeding time is 10 - 15 min. When the centrifugal process runs stably at high speed, the second feeding is carried out, and the feeding time is controlled at 10 - 15 min.

[0009] In the centrifugal separation process in step (3), the flow rate of pure water is controlled at 12-15 m 3 / h, and the time is controlled at 6-10 min.

[0010] In step (4), the drying temperature is 400-600 °C.

[0011] The present invention has the following advantages compared with the prior art: 1. The present invention can effectively remove chloride ions in nickelous oxide products only through steps such as screening, crushing, pulping and washing, centrifugal separation and drying, thereby improving the purity and quality of the products.

[0012] 2. The method of the present invention has a simple process, will not introduce impurities due to the impurity removal process, has a low impurity removal cost, strong economy, and is suitable for industrial production.

[0013] 3. After adopting the method of the present invention, nickelous oxide products with a chloride ion content ≤ 0.03% can be obtained. Description of the Drawings

[0014] The following further details the specific embodiments of the present invention with reference to the drawings.

[0015] Figure 1 is a flow chart of the present invention. Specific Embodiments

[0016] As Figure 1 shown, a method for reducing the chloride ion content in nickelous oxide products includes the following steps: (1) Screening the crude nickelous oxide with a chlorine content of 0.5-1.0% to remove large particle impurities, making the particle size distribution uniform, and the screening accuracy is 300-500 mesh. After screening, the crude nickelous oxide is crushed to further refine its particle size and improve the processing efficiency, that is, the crushed nickelous oxide with a particle size D50 = 2.0-5.0 μm is obtained.

[0017] ⑵ The crushed nickelous oxide is put into a pulping kettle, pure water is added, the solid-liquid mass ratio (g / g) is 1:5-1:10, the feeding time is 60-90 min / kettle, and it is stirred and pulped and washed at 65-80 °C at a stirring rate of 55-90 r / min for 1.0-3.0 h. By stirring, the chloride ions are desorbed from the surface of the nickelous oxide and dissolved in the water to obtain a mixture.

[0018] ⑶ Pure water is added to the mixture, and after centrifugal separation, an aqueous phase containing chloride ions and a solid are obtained respectively. The aqueous phase containing chloride ions is replenished to the tail gas scrubbing tower, and there is no waste water discharged.

[0019] Among them: During the centrifugal separation process, feeding is carried out in two times. The first feeding time is 10 - 15 minutes. When the centrifugal process runs stably at high speed, the second feeding is carried out, and the feeding time is controlled within 10 - 15 minutes. During the centrifugal separation process, the flow rate of pure water is controlled at 12 - 15 m 3 / h, and the time is controlled within 6 - 10 minutes.

[0020] (4) Put the solid into a drying device and dry it at 400 - 600 °C until constant weight to remove excess moisture. Then, conduct finished product inspection on the dried nickelous oxide to detect the content of chloride ions and ensure that it meets relevant standards and requirements, thus obtaining a nickelous oxide product with a chloride ion content ≤ 0.03%.

[0021] Example 1 (1) Crude nickelous oxide: Prepare a crude nickelous oxide product containing chloride ions, with a chlorine content of 0.8%. Use these crude nickelous oxides as the initial raw materials for treatment.

[0022] (2) Screening: Use a vibrating screen to screen the crude nickelous oxide product to remove large particle impurities, make the particle size distribution uniform, and the screening accuracy is 400 mesh.

[0023] (3) Crushing: Feed the screened crude nickelous oxide product into a ball mill for crushing to further refine its particle size. The D50 of the crushed particle size is 3.5 μm.

[0024] (4) Pulping and washing: Put the crushed nickelous oxide product into a pulping kettle, add pure water, and carry out stirring for pulping and washing. During the pulping and washing process, the solid-liquid ratio (g / g) is controlled at 1:7, and the feeding time is controlled at 75 minutes per kettle. The temperature during the pulping and washing process is 70 °C. Through stirring, the chloride ions are desorbed from the surface of nickelous oxide and dissolved in water.

[0025] (5) Centrifugal separation: Feed the mixture after pulping and washing into a centrifuge for centrifugal separation to remove the water phase containing chloride ions. During the centrifugal separation process, feeding is carried out in two times. The first feeding time is 12 minutes. After the centrifuge runs stably at high speed, the second feeding is carried out, and the feeding time is controlled at 12 minutes. During the centrifugal separation process, the flow rate of pure water is controlled at 13 m 3 / h, and the time is controlled at 8 minutes. The water phase containing chloride radicals generated during the centrifugal separation process is supplemented to the tail gas scrubbing tower to achieve no external discharge of waste water.

[0026] (6) Drying: Feed the solid nickelous oxide product after centrifugal separation into a drying device for drying treatment to remove excess moisture. During the drying process, the temperature is controlled at 500 °C, and the drying time is determined according to the water content of the material.

[0027] (7)Final product inspection: The dried nickelous oxide product is subjected to quality inspection to detect the chloride ion content. The chloride radical content in the final product of nickelous oxide is 0.02%, meeting the nickelous oxide industry standard YS / T 277-2016.

[0028] Example 2 (1)Crude nickelous oxide: Prepare a crude nickelous oxide product containing chloride ions with a chlorine content of 0.5%. These crude nickelous oxides are used as the initial raw materials for treatment.

[0029] (2)Screening: Use a vibrating screen to screen the crude nickelous oxide product to remove large particle impurities, making the particle size distribution uniform. The screening accuracy is 300 mesh.

[0030] (3)Crushing: Feed the screened crude nickelous oxide product into a ball mill for crushing to further refine its particle size. The particle size D50 after crushing is 2.0 μm.

[0031] (4)Slurrying and washing: Put the crushed nickelous oxide product into a slurring kettle, add pure water, and stir for slurring and washing. During the slurring and washing process, the solid-liquid ratio (g / g) is controlled at 1:5, and the feeding time is controlled at 60 min / kettle. The temperature during the slurring and washing process is 65 °C. Through stirring, the chloride ions are desorbed from the surface of nickelous oxide and dissolved in water.

[0032] (5)Centrifugal separation: Feed the mixture after slurring and washing into a centrifuge for centrifugal separation to remove the water phase containing chloride ions. During the centrifugal separation process, feeding is carried out in two steps. The first feeding time is 10 min. After the centrifuge runs stably at high speed, the second feeding is carried out, and the feeding time is controlled at 10 min. The flow rate of pure water during the centrifugal separation process is controlled at 12 m 3 / h, and the time is controlled at 6.0 min. The water phase containing chloride radicals generated during the centrifugal separation process is supplemented to the tail gas scrubbing tower to achieve no wastewater discharge.

[0033] (6)Drying: Feed the solid nickelous oxide product after centrifugal separation into a drying device for drying treatment to remove excess moisture. The temperature during the drying process is controlled at 400 °C, and the drying time is determined according to the water content of the material.

[0034] (7)Final product inspection: The dried nickelous oxide product is subjected to quality inspection to detect the chloride ion content. The chloride radical content in the final product of nickelous oxide is 0.03%, meeting the nickelous oxide industry standard YS / T 277-2016.

[0035] Example 3 (1)Crude nickelous oxide: Prepare a crude nickelous oxide product containing chloride ions with a chlorine content of 0.75%. These crude nickelous oxides are used as the initial raw materials for treatment.

[0036] (2) Screening: Use a vibrating screen to screen the crude nickelous oxide product to remove large particle impurities, make the particle size distribution uniform, and the screening precision is 350 mesh.

[0037] (3) Crushing: Feed the screened crude nickelous oxide product into a ball mill for crushing to further refine its particle size. The D50 of the crushed product is 4.0 μm.

[0038] (4) Pulping and washing: Put the crushed nickelous oxide product into a pulping kettle, add pure water, and carry out stirring, pulping and washing. During the pulping and washing process, the solid-liquid ratio (g / g) is controlled at 1:8, and the feeding time is controlled at 70 min / kettle. The temperature during the pulping and washing process is 78 °C. Through stirring, the chloride ions are desorbed from the surface of nickelous oxide and dissolved in water.

[0039] (5) Centrifugal separation: Feed the mixture after pulping and washing into a centrifuge for centrifugal separation to remove the water phase containing chloride ions. During the centrifugal separation process, feeding is carried out in two times. The first feeding time is 13 min. After the centrifuge runs stably at high speed, the second feeding is carried out, and the feeding time is controlled at 13 min. During the centrifugal separation process, the flow rate of pure water is controlled at 14 m 3 / h, and the time is controlled at 9 min. The water phase containing chloride radicals generated during the centrifugal separation process is supplemented to the tail gas scrubbing tower to achieve no waste water discharge.

[0040] (6) Drying: Feed the solid nickelous oxide product after centrifugal separation into a drying device for drying treatment to remove excess water. During the drying process, the temperature is controlled at 450 °C, and the drying time is determined according to the water content of the material.

[0041] (7) Final product inspection: Conduct quality inspection on the dried nickelous oxide product to detect the chloride ion content. The chloride radical content in the final product nickelous oxide is 0.027%, meeting the nickelous oxide industry standard YS / T 277-2016.

[0042] Example 4 (1) Crude nickelous oxide: Prepare a crude nickelous oxide product containing chloride ions with a chlorine content of 1.0%. Use these crude nickelous oxides as the initial raw materials for treatment.

[0043] (2) Screening: Use a vibrating screen to screen the crude nickelous oxide product to remove large particle impurities, make the particle size distribution uniform, and the screening precision is 500 mesh.

[0044] (3) Crushing: Feed the screened crude nickelous oxide product into a ball mill for crushing to further refine its particle size. The D50 of the crushed product is 5.0 μm.

[0045] (4)Slurry washing: Put the crushed nickelous oxide product into a slurry kettle, add pure water, and stir for slurry washing. During the slurry washing process, the solid-liquid ratio (g / g) is controlled at 1:10, and the feeding time is controlled at 90 min / kettle. The temperature during the slurry washing process is 77 °C. Through stirring, chloride ions are desorbed from the surface of nickelous oxide and dissolved in water.

[0046] (5)Centrifugal separation: Feed the mixture after slurry washing into a centrifuge for centrifugal separation to remove the aqueous phase containing chloride ions. During the centrifugal separation process, feeding is carried out in two times. The first feeding time is 15 min. After the centrifuge runs stably at high speed, the second feeding is carried out, and the feeding time is controlled at 15 min. During the centrifugal separation process, the flow rate of pure water is controlled at 15 m 3 / h, and the time is controlled at 10 min. The aqueous phase containing chloride radicals generated during the centrifugal separation process is supplemented to the tail gas scrubbing tower to achieve zero wastewater discharge.

[0047] (6)Drying: Feed the solid nickelous oxide product after centrifugal separation into a drying device for drying treatment to remove excess moisture. The temperature during the drying process is controlled at 600 °C, and the drying time is determined according to the water content of the material.

[0048] (7)Final product inspection: Conduct quality inspection on the dried nickelous oxide product to detect the chloride ion content. The chloride radical content in the final product nickelous oxide is 0.030%, meeting the nickelous oxide industry standard YS / T 277-2016.

[0049] Example 5 (1)Crude nickelous oxide: Prepare a crude nickelous oxide product containing chloride ions with a chlorine content of 0.95%. Use these crude nickelous oxides as the initial raw materials for treatment.

[0050] (2)Screening: Use a vibrating screen to screen the crude nickelous oxide product to remove large particle impurities, make the particle size distribution uniform, and the screening accuracy is 400 mesh.

[0051] (3)Crushing: Feed the screened crude nickelous oxide product into a ball mill for crushing to further refine its particle size. The D50 of the crushed particle size is 4.25 μm.

[0052] (4)Slurry washing: Put the crushed nickelous oxide product into a slurry kettle, add pure water, and stir for slurry washing. During the slurry washing process, the solid-liquid ratio (g / g) is controlled at 1:9, and the feeding time is controlled at 87 min / kettle. The temperature during the slurry washing process is 79 °C. Through stirring, chloride ions are desorbed from the surface of nickelous oxide and dissolved in water.

[0053] (5) Centrifugal separation: Feed the mixture after pulping and washing into a centrifuge for centrifugal separation to remove the aqueous phase containing chloride ions. During the centrifugal separation process, feeding is carried out in two steps. The first feeding time is 13 minutes. After the centrifuge runs stably at high speed, the second feeding is carried out, and the feeding time is controlled within 13 minutes. During the centrifugal separation process, the flow rate of pure water is controlled at 12 m 3 / h, and the time is controlled within 8 minutes. The aqueous phase containing chloride radicals generated during the centrifugal separation process is supplemented to the tail gas scrubbing tower to achieve zero wastewater discharge.

[0054] (6) Drying: Feed the solid nickel oxide product after centrifugal separation into a drying device for drying treatment to remove excess moisture. During the drying process, the temperature is controlled at 550 °C, and the drying time is determined according to the water content of the material.

[0055] (7) Final product inspection: The dried nickel oxide product is subjected to quality inspection to detect the chloride ion content. The chloride radical content in the final product nickel oxide is 0.015%, which meets the nickel oxide industry standard YS / T 277-2016.

Claims

1. A method for reducing the chloride ion content in nickelous oxide products, comprising the following steps: ⑴ After screening and crushing the crude nickelous oxide with a chlorine content of 0.5 - 1.0%, nickelous oxide after crushing with a particle size D50 = 2.0 - 5.0 μm is obtained; ⑵ The nickelous oxide after crushing is put into a pulping kettle, pure water is added, and after stirring, pulping and washing, a mixture is obtained; ⑶ Pure water is added to the mixture, and after centrifugal separation, an aqueous phase containing chloride ions and a solid are respectively obtained; the aqueous phase containing chloride ions is supplemented to the tail gas scrubbing tower; ⑷ After the solid is dried to a constant weight and subjected to finished product inspection, a nickelous oxide product with a chloride ion content ≤ 0.03% is obtained.

2. The method for reducing the chloride ion content in nickelous oxide products according to claim 1, wherein: The precision of screening in step ⑴ is 300 - 500 meshes.

3. A method for reducing the chloride ion content in nickelous oxide products as claimed in claim 1, characterized in that: The conditions for stirring, pulping and washing in step ⑵ refer to a solid-liquid mass ratio of 1:5 - 1:10, a feeding time of 60 - 90 min / kettle, a temperature of 65 - 80 °C, a stirring rate of 55 - 90 r / min, and a time of 1.0 - 3.0 h.

4. A method for reducing the chloride ion content in nickelous oxide products according to claim 1, characterized in that: In the centrifugal separation process in step ⑶, feeding is carried out in two times. The first feeding time is 10 - 15 min. When the centrifugal process runs stably at high speed, the second feeding is carried out, and the feeding time is controlled at 10 - 15 min.

5. A method for reducing the chloride ion content in nickelous oxide products as described in claim 1, characterized in that: In the centrifugal separation process in step (3), the flow rate of pure water is controlled at 12 - 15 m 3 / h, and the time is controlled at 6 - 10 min.

6. A method for reducing the chloride ion content in nickelous oxide products as described in claim 1, characterized in that: The drying temperature in step ⑷ is 400 - 600 °C.

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