Comprehensive utilization method of cobalt-nickel raffinate
By removing oil and deduplication of cobalt nickel raffinate, and mixing it with organic solvents and phosphorus-containing solution to generate ammonium magnesium phosphate, the problems of waste residue accumulation and magnesium resource utilization in cobalt nickel raffinate treatment are solved, and the problem of waste residue accumulation and magnesium resource utilization is achieved. Efficient recycling and resource utilization of magnesium and ammonium.
Patent Information
- Application Number
- CN202411531995.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-30
- Publication Date
- 2025-02-25
AI Technical Summary
During the treatment of existing cobalt nickel raffinate, waste residue accumulates severely, and the resource utilization of magnesium cannot be achieved.
After deoiling the cobalt raffinate and nickel raffinate, mixing them in a certain proportion and deduplication, then mixing them with organic solvents and phosphorus-containing solutions to adjust the pH to alkalinity, and produce precipitation, and performing The solid-liquid separation was obtained to obtain magnesium ammonium phosphate and magnesium precipitate.
The magnesium in the wastewater was opened and the ammonium and magnesium in the wastewater were recovered while reducing waste residue accumulation. 70-80% ammonium and 99% magnesium were converted into economically valuable ammonium magnesium phosphate, and the resource utilization was successful.
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Figure CN119504053A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of wastewater treatment, and in particular relates to a method for comprehensive utilization of cobalt-nickel raffinate. Background Art
[0002] During the smelting of cobalt and nickel, the raffinate will be produced during the saponification process. Among them, the raffinate of the nickel finished product line mainly contains Na + 、Ni 2+ 、SO4 2- and NH4 + The cobalt finished product line raffinate mainly contains Na + 、Co 2+ 、SO4 2- And Ni 2+ Mg 2+ The usual treatment method for the raffinate of the cobalt finished product line is to add liquid alkali for flocculation and precipitation to recover valuable metals. In this process, 50-70% of magnesium will be co-precipitated with the valuable metals. When the recycled material is returned to production for reuse, Mg will circulate in the system and continue to be enriched, which will eventually affect the raffinate efficiency and increase the raffinate cost. Therefore, it is very necessary to develop a process to remove magnesium from the raffinate. Summary of the invention
[0003] In order to overcome the above-mentioned defects of the prior art, the purpose of the present invention is to provide a method for comprehensive utilization of cobalt-nickel raffinate, so as to solve the technical problems of serious waste residue accumulation and inability to realize resource utilization of magnesium in the existing cobalt-nickel raffinate treatment process.
[0004] To achieve the above object, the present invention is implemented through the following technical solutions: The present invention provides a method for comprehensive utilization of cobalt-nickel raffinate, comprising the following steps: (1) deoiling the cobalt raffinate and the nickel raffinate respectively to obtain a deoiled cobalt raffinate and a deoiled nickel raffinate; (2) mixing the deoiled nickel raffinate and the deoiled cobalt raffinate at a molar ratio of ammonium to magnesium of (1-1.2):1 to obtain a mixed liquid; (3) performing a weight-removing treatment on the mixed liquid to obtain a weight-removed liquid and a weight-removed residue; (4) The deweighted liquid is mixed with an organic solvent and a phosphorus-containing solution, and then the pH of the mixed liquid is adjusted to alkaline. After a precipitate is produced by reaction, solid-liquid separation is performed to obtain magnesium ammonium phosphate and a magnesium precipitate liquid.
[0005] Preferably, in step (1), the oil removal treatment process comprises: allowing the cobalt raffinate or the nickel raffinate to stand and then separating the liquids to obtain an oil phase and an aqueous phase; using activated carbon to adsorb the aqueous phase, and after solid-liquid separation, obtaining a deoiled cobalt raffinate or a deoiled nickel raffinate.
[0006] Preferably, in step (3), the de-weighting treatment process includes coarse de-weighting and fine de-weighting; wherein the coarse de-weighting process includes: mixing the mixed liquid with sulfide, reacting at a temperature of 60-80°C, and obtaining coarse de-weighting slag and coarse de-weighting liquid after solid-liquid separation; and the fine de-weighting process includes: using D851 or D852 resin to adsorb the coarse de-weighting liquid to obtain a fine de-weighting liquid.
[0007] Preferably, in the rough deweighting process, the amount of sulfide used is 1.5-2.5 times the total mass of cobalt and nickel in the mixed liquid; the sulfide is one or more of sodium sulfide and ammonium sulfide; in the fine deweighting process, the adsorption conditions include: the flow rate of the liquid after rough deweighting is 2-4BV, the pH of the liquid after rough deweighting is 5.0-6.0, and the adsorption temperature is 20-35°C.
[0008] Preferably, in step (4), the organic solvent includes one or more of anhydrous ethanol, glacial acetic acid, and anhydrous ethyl acetate.
[0009] Preferably, in step (4), the pH of the phosphorus-containing solution is 4.5-5.5; and the molar ratio of the magnesium element in the deweighted solution to the phosphorus element in the phosphorus-containing solution is 1:(1-1.1).
[0010] Preferably, in step (4), the temperature for the reaction to produce precipitation is 20-35° C., and the reaction time is 40-60 min.
[0011] Preferably, the above process further comprises step (5): adjusting the pH of the magnesium precipitation liquid to 10.5-11.0 by using lime milk, reacting at 70-80°C for 2-4 hours to obtain ammonia gas and deammoniation slurry; absorbing the ammonia gas to obtain ammonia water; and performing solid-liquid separation on the deammoniation slurry to obtain gypsum and deammoniation liquid.
[0012] Preferably, the process further comprises step (6): sequentially concentrating and cooling the deammoniation liquid to obtain crude sodium sulfate crystals, and reversely dissolving and crystallizing the crude sodium sulfate crystals to obtain refined sodium sulfate crystals; and dehydrating the refined sodium sulfate crystals to obtain glauber salt.
[0013] The beneficial effects of the present invention are: The invention mixes cobalt raffinate and nickel raffinate in a certain proportion, performs oil removal and weight removal treatment on the mixture, removes magnesium in waste water, reduces waste residue accumulation and recovers ammonium and magnesium in the waste water, converts 70-80% of ammonium and 99% of magnesium into magnesium ammonium phosphate with economic value, and realizes resource utilization of magnesium and ammonium in waste water.
[0014] The present invention realizes the recovery of ammonia in wastewater by sequentially distilling ammonia on the liquid after magnesium precipitation, and can prepare ammonia water with a certain concentration for reuse in production. Meanwhile, the byproduct dihydrate gypsum can be sold as gypsum building materials, and the sodium sulfate after concentration and crystallization can be sold as glauber salt, thereby realizing the comprehensive utilization of cobalt and nickel raffinate. BRIEF DESCRIPTION OF THE DRAWINGS
[0015] In order to more clearly illustrate the technical solution of the embodiment of the present invention, the drawings of the embodiment are briefly introduced below.
[0016] Figure 1 The present invention is a schematic flow chart of a method for comprehensive utilization of cobalt-nickel raffinate. DETAILED DESCRIPTION
[0017] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0018] See also Figure 1 The embodiment of the present invention provides a method for comprehensive utilization of cobalt-nickel raffinate, comprising the following steps: (1) The cobalt raffinate and the nickel raffinate are respectively subjected to deoiling treatment to obtain a deoiled cobalt raffinate and a deoiled nickel raffinate; preferably, the deoiling treatment process comprises: allowing the cobalt raffinate to stand and then separating the liquids to obtain an oil phase and an aqueous phase; using activated carbon to adsorb the aqueous phase, and after solid-liquid separation, obtaining a deoiled cobalt raffinate; allowing the nickel raffinate to stand and then separating the liquids to obtain an oil phase and an aqueous phase; using activated carbon to adsorb the aqueous phase, and after solid-liquid separation, obtaining a deoiled nickel raffinate; wherein the activated carbon is preferably an activated carbon powder with a 200 mesh sieving rate greater than 95%, and the amount of activated carbon used is 20-100 g / L; the conditions for the adsorption treatment are: after mixing the activated carbon and the aqueous phase, stirring at 20-35° C. for 4-10 hours.
[0019] (2) The deoiled nickel raffinate and the deoiled cobalt raffinate are mixed at a molar ratio of ammonium to magnesium of (1-1.2):1 to obtain a mixed liquid.
[0020] (3) performing a weight removal treatment on the mixed liquid to obtain a weight-removed liquid and a weight-removed slag; preferably, the weight removal treatment process includes a rough weight removal and a fine weight removal; The rough de-heaving process comprises: mixing the mixed liquid with sulfide according to the amount of sulfide being 1.5 to 2.5 times the total mass of cobalt and nickel in the mixed liquid; the sulfide is one or more of sodium sulfide and ammonium sulfide; then, reacting at a temperature of 60 to 80°C for 2 to 4 hours, the initial pH of the reaction being greater than 5.0, and separating the solid and the liquid after the reaction to obtain rough de-heaving slag and rough de-heaving liquid; The fine de-weighting process includes: using D851 or D852 resin to adsorb the crude de-weighting liquid, and the adsorption conditions include: the flow rate of the crude de-weighting liquid is 2-4BV, the pH of the crude de-weighting liquid is 5.0-6.0, and the adsorption temperature is 20-35°C.
[0021] (4) Mixing the deweighted liquid with an organic solvent and a phosphorus-containing solution, and then adjusting the pH of the mixed solution to alkaline, preferably pH=8.5-9.5. After the pH stabilizes, continue the reaction for 40-60 minutes, control the temperature at 20-35°C, and separate the solid and liquid to obtain magnesium ammonium phosphate and magnesium precipitation liquid. The organic solvent includes but is not limited to one or more of anhydrous ethanol, glacial acetic acid, and anhydrous ethyl acetate. The organic solvent can accelerate the precipitation of the magnesium ammonium phosphate product. The molar ratio of the magnesium element in the deweighted liquid to the phosphorus element in the phosphorus-containing solution is 1: (1~1.1). Adjusting the pH of the mixed solution to alkaline can promote the precipitation of the magnesium ammonium phosphate generated by the reaction.
[0022] (5) The pH of the magnesium precipitation liquid is adjusted to 10.5-11.0 by using lime milk, and after reacting at 70-80°C for 2-4 hours, ammonia gas and deammoniation slurry are obtained; then, the ammonia gas is absorbed to obtain ammonia water, and the deammoniation slurry is subjected to solid-liquid separation to obtain gypsum and deammoniation liquid.
[0023] (6) The deammoniation liquid is concentrated and cooled to crystallize in turn to obtain crude sodium sulfate crystals, and the crude sodium sulfate crystals are reverse-dissolved and crystallized to obtain refined sodium sulfate crystals; the refined sodium sulfate crystals are dehydrated to obtain glauber salt.
[0024] In some preferred embodiments, the pH of the phosphorus-containing solution in step (4) is 4.5-5.5. By adding an acidic phosphorus-containing solution, it is possible to avoid the production of magnesium hydroxide in the liquid after weight removal in the early stage of the reaction due to excessive alkalinity, thereby affecting the purity of the final magnesium ammonium phosphate product.
[0025] In the present embodiment, the cobalt raffinate mainly contains Na + 15-20g / L, Co 2+ 0.2-0.5g / L, Ni 2+ 0.5-1.5g / L and Mg 2+ 10-15g / L, anion is SO4 2- , the nickel raffinate mainly contains Na + 10-15g / L, Ni 2+0.05-0.6g / L and NH4 + 5-10g / L, anion is SO4 2- .
[0026] In order to make the objectives, technical solutions and advantages of the present invention more clear, the embodiments of the present invention will be described in further detail below.
[0027] Example 1 The nickel raffinate obtained from a nickel finished product line contains: Na + 13.5g / L, Ni 2+ 0.55g / L and NH4 + 8.57g / L, SO4 2- 52.33g / L; The cobalt raffinate obtained from a cobalt finished product line contains: Na + 15.67g / L, Co 2+ 0.22g / L, Ni 2+ 1.35g / L and Mg 2+ 13.77g / L, SO4 2- 91.34g / L.
[0028] (1) Taking an appropriate amount of nickel raffinate and letting it stand for 24 hours, then separating the liquids to obtain an oil phase and an aqueous phase; adding 75 g / L activated carbon powder (200 mesh sieving rate is greater than 95%) to the aqueous phase, stirring at 25°C for 5 hours, and filtering to obtain a deoiled nickel raffinate; taking an appropriate amount of cobalt raffinate and letting it stand for 24 hours, then separating the liquids to obtain an oil phase and an aqueous phase; adding 75 g / L activated carbon powder (200 mesh sieving rate is greater than 95%) to the aqueous phase, stirring at 25°C for 5 hours, and filtering to obtain a deoiled cobalt raffinate.
[0029] (2) The deoiled nickel raffinate and the deoiled cobalt raffinate are mixed at a molar ratio of ammonium to magnesium of 1.2:1 to obtain a mixed liquid.
[0030] (3) Sodium sulfide is added to the mixed liquid at an amount of 2.0 times the total mass of cobalt and nickel in the mixed liquid, and the mixture is reacted at 75°C for 2 hours. After the reaction, the solid and liquid are separated to obtain coarse de-weighted slag and coarse de-weighted liquid. The coarse de-weighted slag is packed and stored, wherein the coarse de-weighted slag contains 1-2% cobalt, 7-15% nickel and 40-50% water, and the coarse de-weighted liquid contains 5 mg / L cobalt and 64 mg / L nickel. The coarse de-weighted liquid is passed through D851 resin at a flow rate of 4BV for adsorption, and the adsorption temperature is 30°C to obtain a refined de-weighted liquid, in which the cobalt and nickel contents of the refined de-weighted liquid are both less than 0.1 mg / L.
[0031] (4) Take an appropriate amount of the de-weighted liquid and add it to 25 mL of anhydrous ethanol and disperse it for 15 minutes. Then add a sodium phosphate solution with a pH of 5.0 to adjust the magnesium-phosphorus ratio in the mixed solution to 1:1.1, and disperse it again for 15 minutes. Then adjust the pH of the mixed solution to 9.0 with ammonia water. After the pH stabilizes, continue to react at 20°C for 50 minutes. After the reaction is completed, filter to obtain ammonium magnesium phosphate and magnesium precipitation liquid. The magnesium precipitation liquid contains 22.54 g / L ammonium, 0.1 mg / L magnesium, 478 mg / L phosphorus, and 72.73 g / L sodium.
[0032] (5) Add the magnesium precipitation liquid to the ammonia still, and add 50% lime milk to adjust the pH of the magnesium precipitation liquid to 10.5, raise the temperature to 75°C, and react for 3 hours. During the reaction, lime milk is added to control the pH of the solution to be maintained at 10.5-11.0 to obtain ammonia gas and deammoniation slurry. Use water to absorb the ammonia gas to obtain ammonia water, which is reused in step (4) to adjust the pH; pump the deammoniation slurry into a filter press for solid-liquid separation to obtain gypsum and deammoniation liquid. The gypsum can be sold as gypsum building materials.
[0033] (6) The deammoniation liquid is concentrated, cooled and crystallized in turn to obtain crude sodium sulfate crystals, and the crude sodium sulfate crystals are reverse-dissolved and crystallized to obtain refined sodium sulfate crystals. The refined sodium sulfate crystals are dehydrated to obtain sodium sulfate for sale. The mother liquor produced by concentration and crystallization is diluted and used to absorb ammonia.
[0034] Example 2 The nickel raffinate obtained from a nickel finished product line contains: Na + 10.05g / L, Ni 2+ 0.08g / L and NH4 + 5.5g / L, SO4 2- 36.1g / L; The cobalt raffinate obtained from a cobalt finished product line contains: Na + 15.5g / L, Co 2+ 0.25g / L, Ni 2+ 0.6g / L and Mg 2+ 10.5g / L, SO4 2- 76.0g / L.
[0035] (1) Taking an appropriate amount of nickel raffinate and letting it stand for 24 hours, then separating the liquids to obtain an oil phase and an aqueous phase; adding 85 g / L activated carbon powder (200 mesh sieving rate is greater than 95%) to the aqueous phase, stirring at 25°C for 5 hours, and filtering to obtain a deoiled nickel raffinate; taking an appropriate amount of cobalt raffinate and letting it stand for 24 hours, then separating the liquids to obtain an oil phase and an aqueous phase; adding 85 g / L activated carbon powder (200 mesh sieving rate is greater than 95%) to the aqueous phase, stirring at 25°C for 5 hours, and filtering to obtain a deoiled cobalt raffinate.
[0036] (2) The deoiled nickel raffinate and the deoiled cobalt raffinate were mixed at a molar ratio of ammonium to magnesium of 1.1:1 to obtain a mixed liquid.
[0037] (3) Sodium sulfide was added to the mixed liquid at an amount of 1.0 times the total mass of cobalt and nickel in the mixed liquid, and the mixture was reacted at 75°C for 2 hours. After the reaction, the solid and liquid were separated to obtain coarse de-weighted slag and coarse de-weighted liquid. The coarse de-weighted slag was packed and stored. The coarse de-weighted liquid was passed through D851 resin at a flow rate of 4BV for adsorption at an adsorption temperature of 30°C to obtain a fine de-weighted liquid.
[0038] (4) Take an appropriate amount of the de-weighted liquid and add it to 35 mL of anhydrous ethanol and disperse it for 15 minutes. Then add a sodium phosphate solution with a pH of 5.0 to adjust the magnesium-phosphorus ratio in the mixed solution to 1:1.05, and disperse it again for 15 minutes. Then adjust the pH of the mixed solution to 9.0 with ammonia water. After the pH stabilizes, continue to react at 25°C for 50 minutes. After the reaction is completed, filter to obtain magnesium ammonium phosphate and magnesium precipitation liquid.
[0039] (5) The magnesium precipitation liquid is added to the ammonia still, and 50% lime milk is added to adjust the pH of the magnesium precipitation liquid to 10.5, and the temperature is raised to 75°C. The reaction is carried out for 3 hours. During the reaction, lime milk is added to control the pH of the solution to be maintained at 10.5-11.0, and ammonia gas and deammoniation slurry are obtained. The ammonia gas is absorbed by concentrated water and diluted mother liquor to obtain ammonia water which is reused in step (4) for pH adjustment; the deammoniation slurry is pumped into a filter press for solid-liquid separation to obtain gypsum and deammoniation liquid. The gypsum can be sold as gypsum building materials.
[0040] (6) The deammoniation liquid is concentrated, cooled and crystallized in turn to obtain crude sodium sulfate crystals, and the crude sodium sulfate crystals are reverse-dissolved and crystallized to obtain refined sodium sulfate crystals. The refined sodium sulfate crystals are dehydrated to obtain sodium sulfate for sale. The mother liquor produced by concentration and crystallization is diluted and used to absorb ammonia.
[0041] Example 3 The nickel raffinate obtained from a nickel finished product line contains: Na + 14.5g / L, Ni 2+ 0.5g / L and NH4 + 8.9g / L, SO4 2- 55.1g / L; The cobalt raffinate obtained from a cobalt finished product line contains: Na + 18.5g / L, Co 2+ 0.3g / L, Ni 2+ 1.05g / L and Mg 2+ 13.9g / L, SO4 2- 97.1g / L.
[0042] (1) Taking an appropriate amount of nickel raffinate and letting it stand for 24 hours, then separating the liquids to obtain an oil phase and an aqueous phase; adding 50 g / L activated carbon powder (200 mesh sieving rate is greater than 95%) to the aqueous phase, stirring at 25°C for 5 hours, and filtering to obtain a deoiled nickel raffinate; taking an appropriate amount of cobalt raffinate and letting it stand for 24 hours, then separating the liquids to obtain an oil phase and an aqueous phase; adding 50 g / L activated carbon powder (200 mesh sieving rate is greater than 95%) to the aqueous phase, stirring at 25°C for 5 hours, and filtering to obtain a deoiled cobalt raffinate.
[0043] (2) The deoiled nickel raffinate and the deoiled cobalt raffinate were mixed at a molar ratio of ammonium to magnesium of 1.1:1 to obtain a mixed liquid.
[0044] (3) Sodium sulfide was added to the mixed liquid at an amount of 1.5 times the total mass of cobalt and nickel in the mixed liquid, and the mixture was reacted at 80°C for 2 hours. After the reaction, the solid and liquid were separated to obtain coarse de-weighted slag and coarse de-weighted liquid. The coarse de-weighted slag was packed and stored. The coarse de-weighted liquid was passed through D851 resin at a flow rate of 4BV for adsorption at an adsorption temperature of 25°C to obtain a fine de-weighted liquid.
[0045] (4) Take an appropriate amount of the de-weighted liquid and add it to 50 mL of anhydrous ethanol and disperse it for 15 minutes. Then add a sodium phosphate solution with a pH of 5.0 to adjust the magnesium-phosphorus ratio in the mixed solution to 1:1.08, and disperse it again for 15 minutes. Then adjust the pH of the mixed solution to 9.0 with ammonia water. After the pH stabilizes, continue to react at 25°C for 50 minutes. After the reaction is completed, filter to obtain magnesium ammonium phosphate and magnesium precipitation liquid.
[0046] (5) The magnesium precipitation liquid is added to the ammonia still, and 50% lime milk is added to adjust the pH of the magnesium precipitation liquid to 11, and the temperature is raised to 75°C, and the reaction is carried out for 3 hours. During the reaction, lime milk is added to control the pH of the solution to be maintained at 10.5-11.0, and ammonia gas and deammoniation slurry are obtained. The ammonia gas is absorbed by concentrated water and diluted mother liquor to obtain ammonia water which is reused in step (4) for pH adjustment; the deammoniation slurry is pumped into a filter press for solid-liquid separation to obtain gypsum and deammoniation liquid, and the gypsum can be sold as gypsum building materials.
[0047] (6) The deammoniation liquid is concentrated, cooled and crystallized in turn to obtain crude sodium sulfate crystals, and the crude sodium sulfate crystals are reverse-dissolved and crystallized to obtain refined sodium sulfate crystals. The refined sodium sulfate crystals are dehydrated to obtain sodium sulfate for sale. The mother liquor produced by concentration and crystallization is diluted and used to absorb ammonia.
[0048] The contents of magnesium, ammonium and phosphorus in the solution after magnesium precipitation and the content of recovered ammonia in Examples 1 to 3 were tested respectively, and the recovery rate of magnesium, the recovery rate of ammonium, the recovery rate of phosphorus and the recovery rate of ammonia after ammonia distillation were calculated. The results are shown in Table 1.
[0049] Table 1
[0050] It can be seen from the above table that the method for comprehensive utilization of cobalt-nickel raffinate provided by the present invention can open the way for magnesium, reduce the accumulation of waste residues, and recover ammonium and magnesium in wastewater at the same time. 70-80% of ammonium and more than 99% of magnesium are converted into economically valuable magnesium ammonium phosphate, and the recovered product magnesium ammonium phosphate meets the national standard requirements. At the same time, the ammonium in the liquid after magnesium precipitation is converted into ammonia gas for recovery, and sulfate is recovered in the form of gypsum and sodium sulfate, realizing the comprehensive utilization of wastewater and having certain economic value.
[0051] It should be noted that the above embodiments all belong to the same inventive concept, and the description of each embodiment has its own focus. For matters that are not described in detail in some embodiments, reference may be made to the description in other embodiments.
[0052] The above-mentioned embodiments only express the implementation methods of the present invention, and the descriptions thereof are relatively specific and detailed, but they cannot be understood as limiting the scope of the invention patent. It should be pointed out that, for ordinary technicians in this field, several variations and improvements can be made without departing from the concept of the present invention, which all belong to the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention shall be subject to the attached claims.
Claims
1. A method for comprehensive utilization of cobalt-nickel raffinate, characterized in that: The following steps are involved: (1) deoiling the cobalt raffinate and the nickel raffinate respectively to obtain a deoiled cobalt raffinate and a deoiled nickel raffinate; (2) mixing the deoiled nickel raffinate and the deoiled cobalt raffinate at a molar ratio of ammonium to magnesium of (1-1.2):1 to obtain a mixed liquid; (3) performing a weight-removing treatment on the mixed liquid to obtain a weight-removed liquid and a weight-removed residue; (4) The deweighted liquid is mixed with an organic solvent and a phosphorus-containing solution, and then the pH of the mixed liquid is adjusted to alkaline. After a precipitate is produced by reaction, solid-liquid separation is performed to obtain magnesium ammonium phosphate and a magnesium precipitate liquid.
2. The method for comprehensive utilization of cobalt-nickel raffinate according to claim 1, characterized in that: In step (1), the oil removal treatment process comprises: allowing the cobalt raffinate or the nickel raffinate to stand and then separating the liquids to obtain an oil phase and an aqueous phase; using activated carbon to adsorb the aqueous phase, and after solid-liquid separation, obtaining a deoiled cobalt raffinate or a deoiled nickel raffinate.
3. The method for comprehensive utilization of cobalt-nickel raffinate according to claim 1, characterized in that: In step (3), the weight removal process includes rough weight removal and fine weight removal; The rough de-weighting process comprises: mixing the mixed liquid with sulfide, reacting at a temperature of 60-80°C, and obtaining rough de-weighting slag and rough de-weighting liquid after solid-liquid separation; The fine de-weighting process comprises: using D851 or D852 resin to adsorb the coarse de-weighting liquid to obtain the fine de-weighting liquid.
4. The method for comprehensive utilization of cobalt-nickel raffinate according to claim 3, characterized in that: In the rough weight removal process, the amount of sulfide used is 1.5 to 2.5 times the total mass of cobalt and nickel in the mixed liquid; the sulfide is one or more of sodium sulfide and ammonium sulfide; In the fine de-weighting process, the adsorption conditions include: the flow rate of the crude de-weighting liquid is 2-4BV, the pH of the crude de-weighting liquid is 5.0-6.0, and the adsorption temperature is 20-35°C.
5. The method for comprehensive utilization of cobalt-nickel raffinate according to claim 1, characterized in that: In step (4), the organic solvent includes one or more of anhydrous ethanol, glacial acetic acid, and anhydrous ethyl acetate.
6. The method for comprehensive utilization of cobalt-nickel raffinate according to claim 1, characterized in that: In step (4), the molar ratio of the magnesium element in the deweighted solution to the phosphorus element in the phosphorus-containing solution is 1:(1-1.1).
7. The method for comprehensive utilization of cobalt-nickel raffinate according to claim 1, characterized in that: In step (4), the pH of the phosphorus-containing solution is 4.5-5.
5.
8. The method for comprehensive utilization of cobalt-nickel raffinate according to claim 1, characterized in that: In step (4), the temperature for producing precipitation in the reaction is 20-35°C, and the reaction time is 40-60 min.
9. The method for comprehensive utilization of cobalt-nickel raffinate according to claim 1, characterized in that: The method further comprises step (5): adjusting the pH of the magnesium precipitation liquid to 10.5-11.0 by using lime milk, reacting at 70-80° C. for 2-4 hours to obtain ammonia gas and deammoniation slurry; absorbing the ammonia gas to obtain ammonia water; and performing solid-liquid separation on the deammoniation slurry to obtain gypsum and deammoniation liquid.
10. The method for comprehensive utilization of cobalt-nickel raffinate according to claim 1, characterized in that: The method further comprises step (6): sequentially concentrating and cooling the deammoniation liquid to obtain crude sodium sulfate crystals, and reversely dissolving and crystallizing the crude sodium sulfate crystals to obtain refined sodium sulfate crystals; and dehydrating the refined sodium sulfate crystals to obtain glauber salt.
Citation Information
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