CN112062171A - Method for separating nickel and magnesium from crude nickel carbonate - Google Patents
Method for separating nickel and magnesium from crude nickel carbonate Download PDFInfo
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- CN112062171A CN112062171A CN201910495709.6A CN201910495709A CN112062171A CN 112062171 A CN112062171 A CN 112062171A CN 201910495709 A CN201910495709 A CN 201910495709A CN 112062171 A CN112062171 A CN 112062171A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/06—Carbonates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention provides a method for separating nickel and magnesium from crude nickel carbonate, which comprises the following steps of dissolving crude nickel carbonate by using sulfuric acid with the concentration of 3.50mol/L, and slowly adding saturated sodium carbonate solution into the nickel sulfate solution obtained in the step (1). the method for separating nickel and magnesium from crude nickel carbonate adopts refined nickel carbonate products produced by using crude nickel carbonate as a raw material, and directly uses sulfuric acid to dissolve crude nickel carbonate without additionally adding a catalyst, so that impurities are prevented from being introduced; the process is simple and the flow is short; the invention provides a method for controlling the pH of a solution to achieve accurate precipitation.
Description
Technical Field
The invention relates to the technical field of separation by a precipitation method, in particular to a method for separating nickel and magnesium from crude nickel carbonate.
Background
Coarse nickel carbonate is used as a raw material, refined nickel carbonate with a chemical formula NiCO3 is recovered to the maximum extent, is an oblique light green crystal, and is mainly used in the industries of catalysts, electroplating, ceramics and the like. Magnesium-containing oil-containing nickel carbonate can be generated in the workshop process, unnecessary waste can be caused if the magnesium-containing oil-containing nickel carbonate is discarded, and in order to save the company cost, a research and development center tries to determine whether impurities such as magnesium, oil and the like in the crude nickel carbonate can be separated, so that the aim of changing waste into valuable is fulfilled.
Disclosure of Invention
The invention provides a method for separating nickel and magnesium from crude nickel carbonate, which has simple process flow and controllable technical conditions.
The method for separating nickel and magnesium from crude nickel carbonate comprises the following specific operation methods:
(1) dissolving crude nickel carbonate by using sulfuric acid with the concentration of 3.50mol/L, selecting sulfuric acid with the hydrogen ion concentration of 7mol/L and crude nickel carbonate as raw materials during operation, wherein the liquid-solid ratio of the sulfuric acid to the crude nickel carbonate is 1: 1.5, selecting, namely firstly putting sulfuric acid into a reaction tank, then adding crude nickel carbonate into the reaction tank, wherein a solution system is easy to overflow from the tank due to residual organic matters in raw materials, slowly adding the sulfuric acid while stirring, controlling the pH to be below 3 as far as possible when the solution is saturated, and then performing oil removal and filtration operation to obtain a saturated nickel sulfate magnesium sulfate-containing solution;
(2) and (2) slowly adding a saturated sodium carbonate solution into the nickel sulfate solution obtained in the step (1), controlling the flow rate of the saturated sodium carbonate solution to be 3-4ml/min, and when the pH value of the solution reaches 5.6, starting to generate nickel carbonate crystals in the system, namely, the purity is higher, so that the purpose of nickel-magnesium separation is realized.
The method comprises the following steps that in the step (1), waste oily crude nickel carbonate containing magnesium after workshop production is adopted, and the content of nickel in the crude nickel carbonate is 22.86% by mass.
The reaction temperature of the solution in the step (1) is 60-80 ℃.
The consumption of the activated carbon required by the oil removal in the step (2) is 60 g/1.5L.
The reaction temperature of the solution in the step (2) is 60-80 ℃.
The flow rate of the saturated sodium carbonate solution in the step (2) is controlled to be 3-4ml/min (V solution is 1.5L).
The method for separating nickel and magnesium from crude nickel carbonate has the advantages that the crude nickel carbonate is used as a raw material to produce a refined nickel carbonate product, sulfuric acid is directly used for dissolving the crude nickel carbonate, a catalyst is not required to be additionally added, and impurities are prevented from being introduced; the process is simple and the flow is short; the invention provides a method for controlling the pH of a solution to achieve accurate precipitation.
Drawings
FIG. 1 is a schematic view of the process of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
Example 1
As shown in figure 1, the method for separating nickel and magnesium from crude nickel carbonate comprises the following steps:
(1) dissolving crude nickel carbonate by using sulfuric acid with the concentration of 3.50mol/L, wherein the sulfuric acid with the hydrogen ion concentration of 7mol/L and the crude nickel carbonate are mixed according to the liquid-solid ratio of 1: 1.5, when the reaction temperature of the solution is between 60 and 80 ℃, and the pH value of the solution reaches 1, because organic matters are remained in the raw materials, a solution system is easy to be poured into a tank, the raw materials are added frequently and slowly, the concentration of nickel sulfate reaches 80 to 85g/L, namely, the nickel sulfate is saturated, the pH value is controlled below 3, and the impurities are removed by filtering; adding activated carbon into an oil-containing magnesium-containing nickel sulfate solution for deoiling, wherein the consumption of the activated carbon for deoiling is 60g/1.5L, the solution is stirred for 1h at the temperature of 60-80 ℃, and filtering and deoiling are carried out;
(2) slowly adding a saturated sodium carbonate solution into the nickel sulfate solution obtained in the step (1), controlling the flow rate of the saturated sodium carbonate solution at 3-4ml/min, controlling the temperature of the solution at 60-80 ℃, and starting to generate nickel carbonate crystals (with higher purity) in the system when the pH of the solution reaches 5.6, thereby realizing the purpose of nickel-magnesium separation; when the pH value of the solution is 5.6-6.2, nickel carbonate precipitate can be collected, and the nickel carbonate is slurried for 0.5h or washed with hot water for three times to obtain the refined nickel carbonate with higher purity.
The reaction principle of the invention is as follows:
adding crude nickel carbonate to the acidic aqueous solution to dissolve:
MCO3+H2SO4＝＝MSO4+CO2↑+H2O
the nickel sulfate and the magnesium sulfate coexist in the solution, saturated liquid sodium carbonate solution is slowly added into the solution, and the saturated sodium carbonate solution preferentially precipitates Ni, so that the purpose of separating nickel and magnesium is achieved:
NiSO4+Na2CO3＝＝Na2SO4+NiCO3↓
the composition of the crude nickel carbonate (N-7490) used in the following examples is shown in Table 1.
TABLE 1 crude Nickel carbonate composition
Example 2
a. Preparation of nickel sulfate solution
Dissolving crude nickel carbonate by using sulfuric acid with the hydrogen ion concentration of 7mol/L, wherein the reaction temperature is 60-80 ℃, the volume of the sulfuric acid with the hydrogen ion concentration of 7mol/L is 1.5L, and the weight of the crude nickel carbonate is 777.14g, when the pH value reaches about 1, the crude nickel carbonate contains organic matters, so that a solution system is easy to tank, less material adding duty is needed for observation, and when the pH value reaches about 3, filtering and removing impurities; adding activated carbon into the filtered oil-containing magnesium-containing nickel sulfate solution to remove oil, wherein the consumption of the activated carbon required for oil removal is 60g/1.5L, the reaction temperature is 60-80 ℃, stirring for 1h, and filtering to obtain the magnesium-containing nickel sulfate solution.
b. Magnesium removal
Slowly adding saturated sodium carbonate solution into magnesium-containing nickel sulfate solution by using peristaltic pump, wherein the flow rate of the saturated sodium carbonate solution is controlled to be 3-4ml/min (V)Solutions of1.5L), the reaction temperature is 60-80 ℃, when the pH value reaches 5.4, the pH value of the solution does not rise for a long time, when the pH value reaches 5.6, precipitation (nickel carbonate with high purity) begins to appear in the solution, when the pH value of the solution is 5.6-6.2, nickel carbonate with high purity can be collected and precipitated, and the solution is filtered; slurrying the refined nickel carbonate for 0.5h or flushing the refined nickel carbonate with hot water for three times.
The refined nickel carbonate product contains 49.21% of nickel and 0.54% of magnesium.
Example 3
a. Preparation of nickel sulfate solution
Dissolving crude nickel carbonate by using sulfuric acid with the hydrogen ion concentration of 7.5mol/L, wherein the reaction temperature is 60-80 ℃, the volume of the sulfuric acid with the hydrogen ion concentration of 7.5mol/L is 1.5L, and the weight of the crude nickel carbonate is 827.26g, when the pH value reaches about 1, the crude nickel carbonate contains organic matters, a solution system is easy to be poured into a tank, less material adding duty is needed for observation, and when the pH value reaches about 3.3, filtering and removing impurities; adding activated carbon into the filtered oil-containing magnesium-containing nickel sulfate solution to remove oil, wherein the consumption of the activated carbon required for oil removal is 65g/1.5L, the reaction temperature is 60-80 ℃, stirring for 1.2h, and filtering to obtain the magnesium-containing nickel sulfate solution.
b. Magnesium removal
Slowly adding saturated sodium carbonate solution into magnesium-containing nickel sulfate solution by using peristaltic pump, wherein the flow rate of the saturated sodium carbonate solution is controlled to be 4-5ml/min (V)Solutions of1.5L), the reaction temperature is 60-80 ℃, and when the pH reaches 5.4, the pH of the solution is higherThe solution does not rise for a long time, when the pH value reaches 5.6, precipitation (nickel carbonate with higher purity) begins to appear in the solution, and when the pH value of the solution is 5.6-6.2, the nickel carbonate precipitation with higher purity can be collected and filtered; slurrying the refined nickel carbonate for 0.5h or flushing the refined nickel carbonate with hot water for three times.
The refined nickel carbonate product contains 48.64 percent of nickel and 0.41 percent of magnesium.
Example 4
a. Preparation of nickel sulfate solution
Dissolving crude nickel carbonate by using sulfuric acid with hydrogen ion concentration of 6.7mol/L, wherein the reaction temperature is 60-80 ℃, the volume of the sulfuric acid with the hydrogen ion concentration of 6.7mol/L is 1.5L, and the weight of the crude nickel carbonate is 742.41g, when the pH value reaches about 1, the crude nickel carbonate contains organic matters, a solution system is easy to be poured into a tank, less material adding duty is needed for observation, and when the pH value reaches about 3, filtering and removing impurities; adding activated carbon into the filtered oil-containing magnesium-containing nickel sulfate solution to remove oil, wherein the consumption of the activated carbon for oil removal is 60g/1.5L, the reaction temperature is 60-80 ℃, stirring for 1h, and filtering to obtain the magnesium-containing nickel sulfate solution.
b. Magnesium removal
Slowly adding saturated sodium carbonate solution into magnesium-containing nickel sulfate solution by using peristaltic pump, wherein the flow rate of the saturated sodium carbonate solution is controlled to be 3-4ml/min (V)Solutions of1.5L), the reaction temperature is 60-80 ℃, when the pH value reaches 5.4, the pH value of the solution does not rise for a long time, when the pH value reaches 5.6, precipitation (nickel carbonate with high purity) begins to appear in the solution, when the pH value of the solution is 5.6-6.2, nickel carbonate with high purity can be collected and precipitated, and the solution is filtered; slurrying the refined nickel carbonate for 0.5h or flushing the refined nickel carbonate with hot water for three times.
The refined nickel carbonate product contains 48.84% of nickel and 0.34% of magnesium.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. The method for separating nickel and magnesium from crude nickel carbonate comprises the following specific operation methods:
(1) dissolving crude nickel carbonate by using sulfuric acid with the concentration of 3.50mol/L, selecting sulfuric acid with the hydrogen ion concentration of 7mol/L and crude nickel carbonate as raw materials during operation, wherein the liquid-solid ratio of the sulfuric acid to the crude nickel carbonate is 1: 1.5, selecting, namely firstly putting sulfuric acid into a reaction tank, then adding crude nickel carbonate into the reaction tank, wherein a solution system is easy to overflow from the tank due to residual organic matters in raw materials, slowly adding the crude nickel carbonate while stirring, controlling the pH to be below 3 as much as possible when the solution is saturated, and then performing oil removal and filtration operation to obtain a saturated nickel sulfate magnesium sulfate-containing solution;
(2) and (2) slowly adding a saturated sodium carbonate solution into the nickel sulfate solution obtained in the step (1), controlling the flow rate of the saturated sodium carbonate solution to be 3-4ml/min, and when the pH value of the solution reaches 5.6, beginning to generate nickel carbonate crystals in the system, namely, the purity is higher, so that the purpose of nickel-magnesium separation is realized.
2. The method for separating nickel and magnesium from crude nickel carbonate according to the claim, characterized in that the step (1) adopts the oil-containing crude magnesium-containing nickel carbonate which is discarded after workshop production, and the nickel content in the crude nickel carbonate is 22.86 percent by mass.
3. The method for separating nickel and magnesium from crude nickel carbonate, which is recited in the claim, characterized in that the reaction temperature of the solution in the step (1) is 60-80 ℃.
4. The method for separating nickel and magnesium from crude nickel carbonate according to the claim, characterized in that the amount of activated carbon required for removing oil in the step (2) is 60 g/1.5L.
5. The method for separating nickel and magnesium from crude nickel carbonate, which is recited in the claim, wherein the reaction temperature of the solution in the step (2) is 60-80 ℃.
6. The method for separating nickel and magnesium from crude nickel carbonate according to the claim, characterized in that the flow rate of the saturated sodium carbonate solution in the step (2) is controlled to be 3-4ml/min (V solution is 1.5L).
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150078972A1 (en) * | 2012-03-29 | 2015-03-19 | Sumitomo Metal Mining Co., Ltd. | Method for producing high-purity nickel sulfate |
| CN104591304A (en) * | 2015-01-13 | 2015-05-06 | 江西赣锋锂业股份有限公司 | Method for treating waste material containing nickel sulfate |
| CN107935063A (en) * | 2017-11-20 | 2018-04-20 | 中国科学院兰州化学物理研究所 | Utilize the nickel oxide method that directly leaching prepares nickel salt under normal pressure |
| CN108456787A (en) * | 2017-12-22 | 2018-08-28 | 东营方圆有色金属有限公司 | A kind of method that crude nickle sulphate refines valuable element synthetical recovery |
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- 2019-06-10 CN CN201910495709.6A patent/CN112062171A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150078972A1 (en) * | 2012-03-29 | 2015-03-19 | Sumitomo Metal Mining Co., Ltd. | Method for producing high-purity nickel sulfate |
| CN104591304A (en) * | 2015-01-13 | 2015-05-06 | 江西赣锋锂业股份有限公司 | Method for treating waste material containing nickel sulfate |
| CN107935063A (en) * | 2017-11-20 | 2018-04-20 | 中国科学院兰州化学物理研究所 | Utilize the nickel oxide method that directly leaching prepares nickel salt under normal pressure |
| CN108456787A (en) * | 2017-12-22 | 2018-08-28 | 东营方圆有色金属有限公司 | A kind of method that crude nickle sulphate refines valuable element synthetical recovery |
Non-Patent Citations (1)
| Title |
|---|
| 侯嫔，张春晖，何绪文: "《水处理过程化学》", 31 May 2015 * |
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