CN113816439A - Method and system for purifying nickel sulfate - Google Patents
Method and system for purifying nickel sulfate Download PDFInfo
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- CN113816439A CN113816439A CN202110961229.1A CN202110961229A CN113816439A CN 113816439 A CN113816439 A CN 113816439A CN 202110961229 A CN202110961229 A CN 202110961229A CN 113816439 A CN113816439 A CN 113816439A
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- C01G53/00—Compounds of nickel
- C01G53/10—Sulfates
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- Y—GENERAL 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
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Abstract
The invention discloses a method and a system for purifying nickel sulfate, which comprises the steps of firstly adding ammonia water into a nickel sulfate primary liquid to adjust the pH value, then aging, carrying out solid-liquid separation to obtain an impurity-removed liquid, carrying out deamination treatment on the impurity-removed liquid to obtain a deaminated liquid, adding an alcohol solution into the deaminated liquid, heating, adding a nickel sulfate seed crystal, aging for a certain time, and carrying out solid-liquid separation to obtain a high-purity nickel sulfate crystal. The system comprises a purification unit, a deamination unit and a dissolving-out unit, wherein the purification unit comprises a purification tank and an ammonia storage tank, the deamination unit comprises a deamination tank, a deamination liquid inlet pipe and a deamination liquid outlet pipe, and the dissolving-out unit comprises a dissolving-out tank and an alcohol storage tank. Compared with the traditional nickel sulfate purification process for removing different elements step by extraction, the method only uses ammonia water for impurity removal, and adds alcohol for precipitation and crystallization under heating, so that most of impurities can be removed in two steps, the impurity removal steps are shortened, the process is simplified, new impurities cannot be introduced, and nickel sulfate crystals with higher purity are generated.
Description
Technical Field
The invention belongs to the technical field of nickel sulfate, and particularly relates to a method and a system for purifying nickel sulfate.
Background
Nickel is an important resource for strategic development in China, is an important raw material for high-temperature, rust-proof, hard and magnetic alloys and nickel-containing compounds, and is widely applied to the fields of aerospace, motor and electrical appliances, chemical industry, ceramic and battery industry and the like. The nickel oxide ore accounts for more than 70 percent of the world nickel reserves, and is an important nickel resource, wherein the laterite nickel ore is the most common nickel oxide ore. The chemical composition of lateritic nickel ores and the mineral structure of ores are generally different due to the different ore development in different regions. Laterite ores often contain various impurities such as iron, zinc, magnesium, manganese, cobalt, calcium, aluminum and chromium in addition to the desired nickel, cobalt, etc. components.
At present, the main process for extracting nickel by smelting laterite nickel ore comprises the following steps: reducing and smelting to obtain nickel-containing metals such as nickel iron, nickel-containing pig iron, nickel-iron alloy and the like, and leaching by a wet method to obtain nickel salt. For example, nickel sulfate solution is obtained by dissolving nickel iron with sulfuric acid, but the nickel sulfate solution still contains low-content impurity metals in the nickel sulfate primary solution after primary impurity removal operation, in order to improve the quality of nickel sulfate products, impurities are usually removed by using methods such as an extractant method, a precipitation step-by-step impurity removal method and the like, considering that the impurities are more in variety, different impurities are large in content difference, various active metal impurities are contained, the concentration of a target product is lower, the impurity removal steps are more, the related equipment is various, the purification treatment difficulty is high, and the impurity process is complex. In view of the current situation, a method and a corresponding impurity removal system which can reduce the steps for impurity removal, have low energy consumption and can synchronously remove various impurities are urgently needed in the nickel sulfate impurity removal process.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art described above. Therefore, the invention provides a method and a system for purifying nickel sulfate.
According to one aspect of the present invention, there is provided a method of purifying nickel sulfate, comprising the steps of:
s1: adding ammonia water into the nickel sulfate primary liquid to adjust the pH, then aging, and carrying out solid-liquid separation to obtain a liquid after impurity removal; the pH adjustment condition is as follows: 1.2< pH <2.8 to obtain ferric hydroxide precipitate; 3.0< pH <4.8 to obtain aluminum hydroxide precipitate; the pH value is more than 5.0 and less than 6.5, so that chromium hydroxide and zinc hydroxide precipitate is obtained, and ammonia water is slowly added until the pH value is near 6.5, so that precipitates of iron, aluminum, chromium and zinc can be generated;
s2: carrying out deamination treatment on the solution after impurity removal to obtain a solution after deamination;
s3: adding an alcohol solution into the deamination solution, heating, adding nickel sulfate seed crystals, aging for a certain time, and performing solid-liquid separation to obtain high-purity nickel sulfate crystals.
In some embodiments of the invention, in step S1, the pH is 3.5 to 6.5. Preferably, the pH is 5.0 to 6.5.
In some embodiments of the present invention, in step S1, the aging time is 120-.
In some embodiments of the present invention, the temperature of aging is controlled to be 40-50 ℃ in step S1.
In some embodiments of the present invention, in step S1, stirring is performed while adjusting pH, the stirring speed is 120-300rmp, and after adjusting pH, the stirring is stopped and aging is started.
In some embodiments of the present invention, in step S1, the mass concentration of the ammonia water added is 0.01 to 5%. Preferably, the mass concentration of the ammonia water is 0.01-0.5%.
In some embodiments of the present invention, in step S2, the process parameters of the deamination treatment are: controlling the feeding amount of the liquid after impurity removal to be 0.15-0.65t/h, the steam feeding amount to be 1-5t/h and the pressure to be 1.0-1.5 Mpa.
In some embodiments of the invention, in step S3, the nickel sulfate seed crystal is added in an amount of 0.1-20g per 100L of the post-deamination solution.
In some embodiments of the invention, in step S3, the alcohol solution is one of methanol, ethanol, or propanol.
In some embodiments of the invention, the heating temperature is 50-90 ℃ in step S3. The heating temperature is adjusted according to the kind of the alcoholic solution, and is 50-60 deg.C when the alcoholic solution is methanol, 50-70 deg.C when the alcoholic solution is ethanol, and 50-90 deg.C when the alcoholic solution is propanol.
In some embodiments of the present invention, after the nickel sulfate seed crystal is added and before the aging, a second alcohol solution is further added in step S3, and the specific process of step S3 is to add the alcohol solution to the deaminated solution for the first time, heat the solution, add the nickel sulfate seed crystal, until nickel sulfate crystals are gradually formed, then add the alcohol solution for the second time, and age the solution for a certain time. The crystal growth can be controlled by adding the alcoholic solution in two portions.
In some embodiments of the invention, in step S3, the first alcohol solution is added in an amount of 10-20% of the volume of the solution after deamination, and the second alcohol solution is added in an amount of 30-60% of the volume of the solution after deamination.
In some embodiments of the present invention, in step S3, the aging time is 2-8 h.
In some embodiments of the present invention, in step S3, an alcohol-containing solution is also obtained after the solid-liquid separation, and the alcohol-containing solution is heated to recover the volatilized alcohol. Further, the temperature of the heated alcohol solution is adjusted according to the kind of the alcohol solution, when the alcohol solution is methanol, the heating temperature is 60-70 ℃, when the alcohol solution is ethanol, the heating temperature is 80-90 ℃, when the alcohol solution is propanol, the heating temperature is 90-98 ℃, and the heating time is 1-8 h.
The invention also provides a nickel sulfate purification system, which is used for realizing the method for purifying nickel sulfate; the system comprises a cleaning unit, a deamination unit and a dissolving unit;
the purification unit comprises a purification tank and an ammonia storage tank, wherein a stirrer and a pH meter are arranged in the purification tank, a slag outlet is formed in the bottom of the purification tank, and the purification tank is connected with the ammonia storage tank through a pipeline;
the deamination unit comprises a deamination tank, a deamination liquid inlet pipe and a deamination liquid outlet pipe, and the deamination tank is connected with the purification tank through the deamination liquid inlet pipe;
the elution unit comprises an elution tank and an alcohol storage tank, wherein a stirrer and a heater are arranged in the elution tank, a discharger is arranged at the bottom of the elution tank, the elution tank is connected with the alcohol storage tank through a pipeline, and the deamination tank is connected with the deamination liquid outlet pipe.
In some embodiments of the invention, the device further comprises a dealcoholization unit, wherein the dealcoholization unit comprises a dealcoholization tank, a condensation tank and a waste liquid tank, a stirrer and a heater are arranged in the dealcoholization tank, a liquid outlet is arranged at the bottom of the dealcoholization tank, the condensation tank is connected between the dealcoholization tank and the alcohol storage tank, and the dealcoholization tank is connected with the elution tank through a pipeline.
In some embodiments of the present invention, an alcohol solution inlet pipe is further disposed in the elution tank, one end of the alcohol solution inlet pipe is communicated with the alcohol storage tank, and the other end of the alcohol solution inlet pipe is disposed horizontally and has a plurality of liquid outlet holes along an axial direction. Is favorable for the dispersion of the alcoholic solution.
In some embodiments of the invention, the elution tank and/or the dealcoholation tank are provided with a temperature detector. The temperature sensor is used for detecting the temperature in the tank in real time.
In some embodiments of the present invention, the upper part of the ammonia removal tank is provided with a liquid inlet and an ammonia outlet, and the lower part is provided with a steam inlet and a liquid outlet. Steam lets in from the bottom, makes the upper portion drench the ammoniac liquid heating that comes, dissociates out the ammonia simultaneously, and the ammonia of dissociation out is taken away by steam source constantly, and the vapor of taking the ammonia is cooled by the condensation at the top, and ammonia in the middle of the while is dissolved in cold water to reach the mesh of deamination, the aqueous ammonia flows back to ammonia storage tank from the ammonia outlet, and the solution after the deamination is discharged from the liquid outlet of bottom.
In some embodiments of the invention, the bottom of the decontamination tank is provided with an inclined floor from which the slag can smoothly fall to the slag outlet.
In some embodiments of the present invention, the alcohol storage tank is provided with a liquid inlet and a liquid outlet, the liquid inlet of the alcohol storage tank is connected to the condensing tank, and the liquid outlet of the alcohol storage tank is connected to the elution tank. And the alcohol recovered from the dealcoholization tank is collected into an alcohol storage tank, and the alcohol storage tank supplies the alcohol solution to the elution tank, so that the recycling of the alcohol solution is realized.
In some embodiments of the invention, a feed pump is arranged on the deamination liquid outlet pipe and used for pumping the liquid in the deamination tank to the deamination tank.
In some embodiments of the present invention, a feeding pump is disposed on the connecting pipeline of the elution tank and the dealcoholization tank, and is used for pumping the liquid in the elution tank to the dealcoholization tank.
According to a preferred embodiment of the present invention, at least the following advantages are provided:
1. compared with the traditional nickel sulfate purification process for removing different elements step by extraction, the method only uses ammonia water for impurity removal, and adds alcohol for precipitation and crystallization under heating, so that most of impurities can be removed in two steps, the impurity removal steps are shortened, the process is simplified, new impurities cannot be introduced, and nickel sulfate crystals with higher purity are generated. In the impurity removal process, ammonia water is slowly added to gradually increase the pH value of the nickel sulfate solution, precipitates of iron, aluminum, chromium and zinc are respectively generated, and the impurity precipitate can be simply separated. In the dissolving-out process, by utilizing the principle that an alcohol solution is mutually soluble with water as a solvent in a nickel sulfate solution, but the alcohol solution is not mutually soluble with nickel sulfate, after deamination treatment, the alcohol solution dissolves more and more water along with the addition of the alcohol solution, the balance between solute nickel sulfate and water in the nickel sulfate solution is broken, the solubility of solute nickel sulfate is reduced, and because the concentration of nickel sulfate is high, the condition of crystal formation is preferentially achieved, so that nickel sulfate crystals are promoted to be formed, meanwhile, by utilizing the heating condition, various impurity ions still have high activity, the solid-liquid separation can separate the nickel sulfate crystals and impurities, and the further impurity removal effect is achieved.
2. The ammonia water and the alcohol solution can be recycled for multiple times, and the cost of impurity removal is saved. In the system, ammonia-containing nickel sulfate solution after impurity removal is pumped into a deamination unit, ammonia water discharged from a deamination tank flows back to an ammonia storage tank, and then is used for removing impurities in a purification unit; and pumping the alcohol solution after the dissolution in the dissolution unit into a dealcoholization unit, volatilizing the alcohol by heating, recovering the alcohol to an alcohol storage tank, and continuously using the alcohol to dissolve and purify the nickel sulfate crystals.
Drawings
The invention is further described with reference to the following figures and examples, in which:
FIG. 1 is a schematic diagram of the overall structure of a nickel sulfate purification system according to the present invention.
Reference numerals: the device comprises a cleaning tank 110, an ammonia storage tank 120, a cleaning tank stirrer 111, a pH meter 112, a bottom plate 113, a deamination tank 210, a deamination liquid inlet pipe 220, a deamination liquid outlet pipe 230, a feeding pump 240, a elution tank 310, a elution tank stirrer 311, a elution tank heater 312, a elution tank temperature detector 313, a discharger 314, an alcohol solution liquid inlet pipe 315, an alcohol storage tank 320, a dealcoholization tank 410, a dealcoholization tank stirrer 411, a dealcoholization tank heater 412, a dealcoholization tank temperature detector 413, a condensation tank 420 and a waste liquid tank 430.
Detailed Description
The concept and technical effects of the present invention will be clearly and completely described below in conjunction with the embodiments to fully understand the objects, features and effects of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and those skilled in the art can obtain other embodiments without inventive effort based on the embodiments of the present invention, and all embodiments are within the protection scope of the present invention.
Example 1
A nickel sulfate purification system comprises a purification unit, a deamination unit, a elution unit and a dealcoholization unit;
the cleaning unit comprises a cleaning tank 110 and an ammonia storage tank 120, a cleaning tank stirrer 111 and a pH meter 112 are arranged in the cleaning tank, a slag outlet and an inclined bottom plate 113 are arranged at the bottom of the cleaning tank, and the cleaning tank is connected with the ammonia storage tank through a pipeline;
the deamination unit comprises a deamination tank 210, a deamination liquid inlet pipe 220 and a deamination liquid outlet pipe 230, wherein the deamination tank 210 is connected with the purification tank 110 through the deamination liquid inlet pipe, the upper part of the deamination tank 210 is provided with a liquid inlet and an ammonia outlet, the lower part of the deamination tank is provided with a steam inlet and a liquid outlet, and the deamination liquid outlet pipe is provided with a feed pump 240;
the elution unit comprises an elution tank 310 and an alcohol storage tank 320, wherein an elution tank stirrer 311, an elution tank heater 312 and an elution tank temperature detector 313 are arranged in the elution tank 310, a discharger 314 is arranged at the bottom of the elution tank, the elution tank 310 is connected with the alcohol storage tank 320 through a pipeline, the deamination tank 210 is connected with the elution tank 310 through a deamination liquid outlet pipe 230, an alcohol solution liquid inlet pipe 315 is arranged in the elution tank, one end of the alcohol solution liquid inlet pipe 315 is communicated with the alcohol storage tank 320, and the other end of the alcohol solution liquid inlet pipe 315 is horizontally arranged and is provided with a plurality of liquid outlet holes at intervals along the axial direction;
the dealcoholization unit comprises a dealcoholization tank 410, a condensation tank 420 and a waste liquid tank 430, a dealcoholization tank stirrer 411, a dealcoholization tank heater 412 and a dealcoholization tank temperature detector 413 are arranged in the dealcoholization tank 410, a liquid discharge port is formed in the bottom of the dealcoholization tank, the condensation tank 420 is connected between the dealcoholization tank 410 and the alcohol storage tank 320, the dealcoholization tank 320 and the elution tank 310 are connected through pipelines, a feeding pump 240 is arranged on a connecting pipeline, the alcohol storage tank is provided with a liquid inlet and a liquid outlet, the liquid inlet of the alcohol storage tank is connected with the condensation tank, and the liquid outlet of the alcohol storage tank is connected with the elution tank.
A method for purifying nickel sulfate is carried out by adopting the system, and the specific process is as follows:
(1) removing: injecting 650L of nickel sulfate primary liquid into a purification tank, starting a stirrer and a pH meter of the purification tank, controlling the frequency of the stirrer to be 180rmp, opening a valve of an ammonia storage tank, slowly adding ammonia water with the mass concentration of 0.25%, gradually generating precipitate in the purification tank until the pH of the nickel sulfate primary liquid is adjusted to be 6.3, closing the valve of the ammonia storage tank, closing the stirrer of the purification tank, controlling the reaction temperature to be about 46 ℃, aging for 140min, starting a feeding pump of an ammonia removal tank, pumping out the nickel sulfate solution after impurity removal, opening a slag outlet valve of the purification tank, and discharging precipitate slag;
(2) and (3) deamination: pumping the nickel sulfate solution after impurity removal to a deamination tank for deamination treatment, controlling the feeding amount of the nickel sulfate solution at 0.25t/h, the feeding amount of steam at 1.3t/h and the feeding amount of steam at 1.09Mpa, and pumping the nickel sulfate solution after deamination to the next unit;
(3) high-temperature dissolution: starting a stirrer of a stripping tank and a temperature measurer of the stripping tank, wherein the frequency of the stirrer is 240rmp, pumping the deaminated nickel sulfate solution into the stripping tank, starting a heater of the stripping tank, injecting ethanol into the stripping tank for the first time through an alcohol solution inlet pipe, wherein the addition amount of the ethanol is 18.3% of the volume of the deaminated nickel sulfate solution, heating to 65 ℃ and keeping unchanged, then adding 15.2g of nickel sulfate seed crystals into the stripping tank, adding the ethanol for the second time when the nickel sulfate crystals are gradually generated, wherein the addition amount of the ethanol is 42.6% of the volume of the deaminated nickel sulfate solution, aging for 4.5 hours, gradually generating high-purity nickel sulfate crystals, then starting a feeding pump of a dealcoholization tank, pumping out the ethanol on the upper layer of the high-purity nickel sulfate crystals, and discharging the high-purity nickel sulfate crystals through a discharger of the stripping tank;
(4) dealcoholizing: pumping the ethanol after high-temperature elution into a dealcoholization tank, starting a dealcoholization tank heater and a dealcoholization tank stirrer, heating to 83 ℃ under the stirring of 120rmp, wherein the heating time is 3h, recovering volatilized alcohol into an alcohol storage tank, pumping the waste liquid into a waste liquid tank through a liquid outlet at the bottom, and pumping the ethanol into a elution tank by starting a discharge pump of the alcohol storage tank.
Example 2
A method for purifying nickel sulfate is carried out by adopting the system of the embodiment 1, and the specific process is as follows:
(1) removing: injecting 430L of nickel sulfate primary liquid into a purification tank, starting a stirrer and a pH meter of the purification tank, controlling the frequency of the stirrer to be 150rmp, opening a valve of an ammonia storage tank, slowly adding ammonia water with the mass concentration of 0.28%, gradually generating precipitate in the purification tank until the pH of the nickel sulfate primary liquid is adjusted to be 6.2, closing the valve of the ammonia storage tank, closing the stirrer of the purification tank, controlling the reaction temperature to be about 48 ℃, aging for 130min, then starting a feeding pump of an ammonia removal tank, pumping out the nickel sulfate solution after impurity removal, opening a slag outlet valve of the purification tank, and discharging precipitate slag;
(2) and (3) deamination: pumping the nickel sulfate solution after impurity removal to a deamination tank for deamination treatment, controlling the feeding amount of the nickel sulfate solution at 0.14t/h, the feeding amount of steam at 1.33t/h and the feeding amount of steam at 1.12Mpa, and pumping the nickel sulfate solution after deamination to the next unit;
(3) high-temperature dissolution: starting a stirrer of a stripping tank and a temperature measurer of the stripping tank, wherein the frequency of the stirrer is 240rmp, pumping the deaminated nickel sulfate solution into the stripping tank, starting a heater of the stripping tank, injecting ethanol into the stripping tank for the first time through an alcohol solution inlet pipe, heating the ethanol to 55 ℃ until the ethanol is 16.8% of the volume of the deaminated nickel sulfate solution, adding 22.8g of nickel sulfate seed crystal into the stripping tank, adding ethanol for the second time when the nickel sulfate crystal is gradually generated, aging the ethanol for 4.5 hours until the ethanol is 41.0% of the volume of the deaminated nickel sulfate solution, gradually generating high-purity nickel sulfate crystal, starting a feeding pump of a dealcoholization tank, pumping out ethanol on the upper layer of the high-purity nickel sulfate crystal, and discharging the high-purity nickel sulfate crystal through a discharger of the stripping tank;
(4) dealcoholizing: pumping the ethanol after high-temperature elution into a dealcoholization tank, starting a dealcoholization tank heater and a dealcoholization tank stirrer, heating to 85 ℃ under the stirring of 150rmp, wherein the heating time is 3h, recovering volatilized alcohol into an alcohol storage tank, pumping the waste liquid into a waste liquid tank through a liquid outlet at the bottom, and pumping the ethanol into a elution tank by starting a discharge pump of the alcohol storage tank.
Example 3
A method for purifying nickel sulfate is carried out by adopting the system of the embodiment 1, and the specific process is as follows:
(1) removing: injecting 560L of nickel sulfate primary liquid into a purification tank, starting a stirrer and a pH meter of the purification tank, controlling the frequency of the stirrer to be 120rmp, opening a valve of an ammonia storage tank, slowly adding ammonia water with the mass concentration of 0.35%, gradually generating precipitate in the purification tank until the pH of the nickel sulfate primary liquid is adjusted to 6.5, closing the valve of the ammonia storage tank, closing the stirrer of the purification tank, controlling the reaction temperature to be about 44 ℃, aging for 165min, starting a feeding pump of an ammonia removal tank, pumping out the nickel sulfate solution after impurity removal, opening a slag outlet valve of the purification tank, and discharging precipitate slag;
(2) and (3) deamination: pumping the nickel sulfate solution after impurity removal to a deamination tank for deamination treatment, controlling the feeding amount of the nickel sulfate solution at 0.135t/h, the feeding amount of steam at 2.3t/h and the feeding amount of steam at 1.23Mpa, and pumping the nickel sulfate solution after deamination to the next unit;
(3) high-temperature dissolution: starting a stirrer of a stripping tank and a temperature measurer of the stripping tank, wherein the frequency of the stirrer is 180rmp, pumping the deaminated nickel sulfate solution into the stripping tank, starting a heater of the stripping tank, injecting ethanol into the stripping tank for the first time through an alcohol solution inlet pipe, heating the ethanol to 50 ℃ until the ethanol is 18.7% of the volume of the deaminated nickel sulfate solution, adding 19.4g of nickel sulfate seed crystal into the stripping tank, gradually generating nickel sulfate crystals, adding ethanol for the second time, wherein the ethanol is 56.2% of the volume of the deaminated nickel sulfate solution, aging the nickel sulfate crystals for 5 hours, gradually generating high-purity nickel sulfate crystals, starting a feed pump of the dealcoholization tank, pumping out ethanol on the upper layer of the high-purity nickel sulfate crystals, and discharging the high-purity nickel sulfate crystals through a discharger of the stripping tank;
(4) dealcoholizing: pumping the ethanol after high-temperature elution into a dealcoholization tank, starting a dealcoholization tank heater and a dealcoholization tank stirrer, heating to 80 ℃ under the stirring of 150rmp, wherein the heating time is 6h, recovering volatilized alcohol into an alcohol storage tank, pumping the waste liquid into a waste liquid tank through a liquid outlet at the bottom, and pumping the ethanol into a elution tank by starting a discharge pump of the alcohol storage tank.
Test examples
The nickel sulfate solutions of the different stages of examples 1-3 were acidified with 17.4% nitric acid, nickel sulfate solution: the volume ratio of the nitric acid is 10: 1, mixing, and adding deionized water for dilution to obtain a sample to be detected; nickel sulfate crystal: the solid-to-liquid ratio of the nitric acid is 25: 1(g/mL), and adding deionized water for dilution to obtain a sample to be detected. The sample to be measured was measured by Atomic Absorption Spectroscopy (AAS), and the results are shown in table 1.
TABLE 1 concentration of each element in nickel sulfate of different forms in examples 1-3
After the nickel sulfate primary liquid of examples 1-3 in table 1 is subjected to impurity removal by a removing unit, the concentrations of Al, Fe, Zn and Cr in the removed nickel sulfate solution are all significantly reduced, the reduction amount is greater than 81%, only the reduction amount of the concentration of magnesium is small (the concentrations of magnesium in examples 1-3 are respectively reduced by 15.00%, 23.13% and 13.43%), while the reduction amounts of the concentration of nickel in the removed nickel sulfate solution are respectively 1.97%, 1.94% and 3.84%, and the loss of nickel is small. The nickel content in the prepared nickel sulfate crystal is more than 22.27 percent, and Al, Fe, Mg, Zn and Cr in the nickel sulfate crystal are respectively less than or equal to 0.00058 percent, less than or equal to 0.00019 percent, less than or equal to 0.00212 percent, less than or equal to 0.00021 percent and less than 0.00001 percent, so that the purity of the nickel sulfate crystal is high, and the effect of purifying the primary nickel sulfate solution is good.
The embodiments of the present invention have been described in detail with reference to the accompanying drawings, but the present invention is not limited to the above embodiments, and various changes can be made within the knowledge of those skilled in the art without departing from the gist of the present invention. Furthermore, the embodiments of the present invention and the features of the embodiments may be combined with each other without conflict.
Claims (10)
1. A method for purifying nickel sulfate, comprising the steps of:
s1: adding ammonia water into the nickel sulfate primary liquid to adjust the pH, then aging, and carrying out solid-liquid separation to obtain a liquid after impurity removal;
s2: carrying out deamination treatment on the solution after impurity removal to obtain a solution after deamination;
s3: adding an alcohol solution into the deamination solution, heating, adding nickel sulfate seed crystals, aging for a certain time, and performing solid-liquid separation to obtain high-purity nickel sulfate crystals.
2. The method according to claim 1, wherein the pH is 3.5-6.5 in step S1.
3. The method as claimed in claim 1, wherein the aging time in step S1 is 180min and 120 min.
4. The method of claim 1, wherein in step S3, the amount of the nickel sulfate seed crystals added is 0.1-20g per 100L of the deaminated solution.
5. The method of claim 1, wherein step S3 further comprises adding an alcohol solution for a second time after adding the nickel sulfate seed crystal and before aging, and step S3 is performed by adding the alcohol solution for the first time to the deaminated solution, heating, adding the nickel sulfate seed crystal until nickel sulfate crystals are gradually formed, adding the alcohol solution for a second time, and aging for a certain time.
6. The method of claim 5, wherein in step S3, the first alcohol solution is added in an amount of 10-20% by volume of the deaminated solution and the second alcohol solution is added in an amount of 30-60% by volume of the deaminated solution.
7. The method according to claim 1 or 5, wherein in step S3, the aging time is 2-8 h.
8. The method according to claim 1, wherein in step S3, an alcohol-containing solution is obtained after solid-liquid separation, and the alcohol-containing solution is heated to recover the volatilized alcohol.
9. A nickel sulfate purification system for carrying out the method of purifying nickel sulfate of claim 1; the system comprises a cleaning unit, a deamination unit and a dissolving unit;
the purification unit comprises a purification tank and an ammonia storage tank, wherein a stirrer and a pH meter are arranged in the purification tank, a slag outlet is formed in the bottom of the purification tank, and the purification tank is connected with the ammonia storage tank through a pipeline;
the deamination unit comprises a deamination tank, a deamination liquid inlet pipe and a deamination liquid outlet pipe, and the deamination tank is connected with the purification tank through the deamination liquid inlet pipe;
the elution unit comprises an elution tank and an alcohol storage tank, wherein a stirrer and a heater are arranged in the elution tank, a discharger is arranged at the bottom of the elution tank, the elution tank is connected with the alcohol storage tank through a pipeline, and the deamination tank is connected with the deamination liquid outlet pipe.
10. The system for purifying nickel sulfate according to claim 9, further comprising a dealcoholization unit, wherein the dealcoholization unit comprises a dealcoholization tank, a condensation tank and a waste liquid tank, a stirrer and a heater are arranged in the dealcoholization tank, a liquid outlet is formed in the bottom of the dealcoholization tank, the condensation tank is connected between the dealcoholization tank and the alcohol storage tank, and the dealcoholization tank and the elution tank are connected through a pipeline.
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| CN114959301A (en) * | 2022-05-30 | 2022-08-30 | 安徽格派锂电循环科技有限公司 | Method for preparing coarse-particle nickel sulfate from cobalt raffinate |
| WO2023020041A1 (en) * | 2021-08-20 | 2023-02-23 | 广东邦普循环科技有限公司 | Method and system for purifying nickel sulfate |
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| JP4259165B2 (en) * | 2003-04-08 | 2009-04-30 | 住友金属鉱山株式会社 | Purification method of aqueous nickel sulfate solution containing cobalt and calcium |
| CN102115816B (en) * | 2011-01-07 | 2013-01-09 | 东北大学 | Comprehensive utilization method for laterite-nickel ore |
| CN103922428B (en) * | 2014-04-30 | 2015-09-16 | 辽宁石化职业技术学院 | A kind of method utilizing inactivated nickel catalyst preparing high-purity sulfuric acid nickel |
| CN104630465A (en) * | 2014-12-31 | 2015-05-20 | 金川集团股份有限公司 | Method for extracting nickel and cobalt from leaching solution obtained by normal-pressure acid leaching of laterite-nickel ore |
| CN109234526B (en) * | 2018-11-26 | 2020-11-03 | 中国恩菲工程技术有限公司 | Treatment method of laterite-nickel ore |
| CN211619954U (en) * | 2019-07-05 | 2020-10-02 | 河海大学 | System for retrieve nickel sulfate in follow metallic nickel waste material |
| CN110655121B (en) * | 2019-09-25 | 2021-08-10 | 中南大学 | Refining method of crude nickel sulfate |
| CN113816439A (en) * | 2021-08-20 | 2021-12-21 | 广东邦普循环科技有限公司 | Method and system for purifying nickel sulfate |
| CN215886393U (en) * | 2021-08-20 | 2022-02-22 | 广东邦普循环科技有限公司 | Nickel sulfate purification system |
-
2021
- 2021-08-20 CN CN202110961229.1A patent/CN113816439A/en active Pending
-
2022
- 2022-05-12 WO PCT/CN2022/092460 patent/WO2023020041A1/en unknown
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023020041A1 (en) * | 2021-08-20 | 2023-02-23 | 广东邦普循环科技有限公司 | Method and system for purifying nickel sulfate |
| CN114959301A (en) * | 2022-05-30 | 2022-08-30 | 安徽格派锂电循环科技有限公司 | Method for preparing coarse-particle nickel sulfate from cobalt raffinate |
| CN114959301B (en) * | 2022-05-30 | 2024-01-19 | 安徽格派锂电循环科技有限公司 | Method for preparing coarse-particle nickel sulfate from cobalt raffinate |
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| WO2023020041A1 (en) | 2023-02-23 |
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