CN115353128A - Method for removing iron in lithium carbonate production process - Google Patents
Method for removing iron in lithium carbonate production process Download PDFInfo
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- CN115353128A CN115353128A CN202211036041.7A CN202211036041A CN115353128A CN 115353128 A CN115353128 A CN 115353128A CN 202211036041 A CN202211036041 A CN 202211036041A CN 115353128 A CN115353128 A CN 115353128A
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- iron
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- lithium carbonate
- filter cake
- production process
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
Abstract
The invention provides a method for removing iron in the production process of lithium carbonate, slurry prepared during the production of lithium carbonate is introduced into a demagnetization mechanism for filtration to obtain filtered slurry, limestone powder slurry is added into the filtered slurry, and the pH value is adjusted to 6~7 to obtain leachate and a filter cake; purifying the leachate by adopting an alkalization decalcification method, alkalizing the leachate by using lime milk, increasing the pH value to 11-12, and hydrolyzing the iron into hydroxide precipitate to obtain a purified liquid; adding deionized water into the filter cake obtained in the step S2, introducing high-purity carbon dioxide, and stirring and mixing; pumping the slurry prepared in the step S4 into a demagnetizing mechanism for secondary filtration; and (5) continuously repeating the step (S2) on the filtered slurry in the step (S5) to obtain a filter cake, wherein the filter cake is the lithium carbonate mixture subjected to iron removal. The beneficial effects are that: the method adopts different modes to remove the impurity iron in the slurry and the filter cake, adopts two removal modes of physics and chemistry, has high removal efficiency and more thorough removal.
Description
Technical Field
The invention relates to the technical field of lithium carbonate production, in particular to a method for removing iron in a lithium carbonate production process.
Background
Lithium carbonate is an inorganic compound with the chemical formula of Li2CO3, the molecular weight of 73.89, colorless monoclinic crystal, slightly soluble in water and dilute acid, and insoluble in ethanol and acetone. The thermal stability is lower than that of carbonates of other elements in the same group in the periodic table, and the carbonate does not deliquesce in air.
Lithium carbonate is the main raw material of lithium ion battery positive electrode materials (nickel cobalt lithium manganate, lithium cobaltate, lithium iron phosphate, etc.), the new energy field is the main increment source for pulling the lithium carbonate requirement in the future, especially the rising of the power electric automobile industry, the power battery can rapidly grow in the fields of automobiles, energy storage, etc., the requirement of the power battery on the materials can be higher and higher, the existence of magnetic foreign matters brings great hidden dangers to the safety performance of the lithium battery, especially the existence of iron has greater potential safety hazards, and the product quality of the lithium ion battery materials, especially the control of the magnetic foreign matters, is the key for solving the safety problem of the lithium ion battery.
At present, the iron removal mode in the lithium carbonate production process is to introduce lithium carbonate slurry into a magnetic removal or iron removal mechanism for iron removal, but in some production processes, iron-containing compounds exist in the lithium carbonate slurry, and the magnetic foreign matters cannot be completely removed only by removing the iron-containing compounds singly.
Disclosure of Invention
Based on the technical problem, the invention provides a method for removing iron in the lithium carbonate production process.
A method for removing iron in the production process of lithium carbonate comprises the following steps:
s1, introducing slurry prepared during lithium carbonate production into a demagnetizing mechanism for filtering to obtain filtered slurry;
s2, adding limestone powder slurry into the filtered slurry, and adjusting the pH value to 6~7 to obtain leachate and a filter cake;
s3, purifying the leachate by adopting an alkalization decalcification method, alkalizing the leachate by using lime milk, increasing the pH value to 11-12, and hydrolyzing the iron into hydroxide precipitate to obtain a purified liquid;
s4, adding deionized water into the filter cake obtained in the step S2, introducing high-purity carbon dioxide, and stirring and mixing;
s5, pumping the slurry prepared in the step S4 into a demagnetizing mechanism for secondary filtration;
and S6, continuously repeating the step S2 on the filtered slurry in the step S5 to obtain a filter cake, wherein the filter cake is the lithium carbonate mixture subjected to iron removal.
Further, in step S1, the slurry is pumped into a vessel equipped with a deironing device at a low speed by a magnetic pump to remove iron impurities.
Further, in step S2, the content of calcium hydroxide in the limestone powder slurry is 50 to 150g/L.
Further, in step S3, the CaO content in the lime milk is 100-150 g/L.
Further, in the step S2, S4, S5 of removing iron from the cake, iron removal may be repeated a plurality of times.
Has the advantages that: the method adopts different modes to remove the impurity iron in the slurry and the filter cake, adopts two removal modes of physics and chemistry, has high removal efficiency and more thorough removal.
Detailed Description
In order that the above objects, features and advantages of the present invention can be more clearly understood, the present invention will be described in further detail with reference to specific embodiments. It should be noted that the embodiments and features of the embodiments of the present application may be combined with each other without conflict.
A method for removing iron in the production process of lithium carbonate comprises the following steps:
firstly, slurry prepared during lithium carbonate production is introduced into a demagnetizing mechanism for filtering to obtain filtered slurry, the slurry is pumped into a container provided with an iron remover by a magnetic pump at a low speed to remove iron impurities, the iron impurities are impurities in the raw materials during slurry preparation of the raw materials or iron fragments falling into the slurry in a mixing device, and the iron remover adsorbs the iron impurities and removes part of the iron impurities in advance;
and adding limestone powder slurry into the filtered slurry, wherein the main component of the limestone powder slurry is sodium hydroxide, the content of calcium hydroxide in the limestone powder slurry is 50-150g/L, the PH value is adjusted to 6~7, most of impurities such as iron, aluminum and the like can be removed, and the solid ratio of the leaching solution is about 1:2, obtaining a leaching solution and a filter cake, wherein the filter cake contains water with the water content of about 35%, the leaching residue attachment solution contains lithium sulfate, and in order to reduce lithium loss, the leaching residue is reversely stirred and washed, and the washing solution is returned to be subjected to size mixing and leaching;
the leachate is purified by an alkalization calcium removal method, lime milk is used for alkalizing the leachate, the CaO content in the lime milk is 100-150 g/L, the pH value is increased to 11-12, the iron is hydrolyzed into hydroxide precipitate to obtain purified liquid, and the purified liquid is reacted with sodium carbonate solution and calcium sulfate to produce calcium carbonate precipitate, so that calcium in the leachate and calcium brought by the alkalization agent lime milk are removed. Carrying out liquid-solid separation on the alkalized calcium-removing slurry to obtain a solution, namely a purified solution, wherein the calcium-lithium ratio is less than x 10 < -4 >, a filter cake is calcium slag, and returning to size mixing and leaching;
adding deionized water into the filter cake obtained in the step S2, introducing high-purity carbon dioxide, stirring and mixing, and filtering after the impurities are easily dissolved in the deionized water in order to increase the solubility of soluble impurities in the subsequent stirring and washing, wherein the temperature of the introduced deionized water can be set to 70-75 ℃;
pumping the slurry prepared in the step S4 into a demagnetizing mechanism for secondary filtration;
and (5) continuously repeating the step (S2) on the filtered slurry in the step (S5) to obtain a filter cake, wherein the filter cake is the lithium carbonate mixture subjected to iron removal.
In the filter cake iron removing steps S2, S4 and S5, iron can be removed repeatedly for multiple times.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A method for removing iron in the production process of lithium carbonate is characterized by comprising the following steps:
s1, introducing slurry prepared during lithium carbonate production into a demagnetizing mechanism for filtering to obtain filtered slurry;
s2, adding limestone powder slurry into the filtered slurry, and adjusting the pH value to 6~7 to obtain leachate and a filter cake;
s3, purifying the leachate by adopting an alkalization decalcification method, alkalizing the leachate by using lime milk, increasing the pH value to 11-12, and hydrolyzing the iron into hydroxide precipitate to obtain a purified liquid;
s4, adding deionized water into the filter cake obtained in the step S2, introducing high-purity carbon dioxide, and stirring and mixing;
s5, pumping the slurry prepared in the step S4 into a demagnetization mechanism for secondary filtration;
and S6, continuously repeating the step S2 on the filtered slurry in the step S5 to obtain a filter cake, wherein the filter cake is the lithium carbonate mixture subjected to iron removal.
2. The method for removing iron in the lithium carbonate production process according to claim 1, wherein in the step S1, the slurry is pumped into a container provided with an iron remover by a magnetic pump at a low speed to remove iron impurities.
3. The method for removing iron in the lithium carbonate production process according to claim 1, wherein in the step S2, the content of calcium hydroxide in the limestone powder slurry is 50 to 150g/L.
4. The method for removing iron in the lithium carbonate production process according to claim 1, wherein in the step S3, the CaO content in the lime milk is 100-150 g/L.
5. The method for removing iron in the lithium carbonate production process according to claim 1, wherein the iron removal step S2, S4 and S5 is repeated for a plurality of times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202211036041.7A CN115353128A (en) | 2022-08-27 | 2022-08-27 | Method for removing iron in lithium carbonate production process |
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| CN202211036041.7A CN115353128A (en) | 2022-08-27 | 2022-08-27 | Method for removing iron in lithium carbonate production process |
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| CN202211036041.7A Pending CN115353128A (en) | 2022-08-27 | 2022-08-27 | Method for removing iron in lithium carbonate production process |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106505225A (en) * | 2016-12-12 | 2017-03-15 | 江西赣锋锂业股份有限公司 | The method that lithium prepares battery-level lithium carbonate is reclaimed in a kind of old and useless battery from lithium |
| CN110407236A (en) * | 2018-04-26 | 2019-11-05 | 天齐锂业股份有限公司 | The preparation method of electric car level lithium carbonate |
| CN112758964A (en) * | 2021-01-21 | 2021-05-07 | 广西天源新能源材料有限公司 | Process for producing lithium carbonate by mixing spodumene and salt lake ore |
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- 2022-08-27 CN CN202211036041.7A patent/CN115353128A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106505225A (en) * | 2016-12-12 | 2017-03-15 | 江西赣锋锂业股份有限公司 | The method that lithium prepares battery-level lithium carbonate is reclaimed in a kind of old and useless battery from lithium |
| CN110407236A (en) * | 2018-04-26 | 2019-11-05 | 天齐锂业股份有限公司 | The preparation method of electric car level lithium carbonate |
| CN112758964A (en) * | 2021-01-21 | 2021-05-07 | 广西天源新能源材料有限公司 | Process for producing lithium carbonate by mixing spodumene and salt lake ore |
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