CN115304085A - Method for recovering waste medical lithium carbonate - Google Patents
Method for recovering waste medical lithium carbonate Download PDFInfo
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- CN115304085A CN115304085A CN202210738899.1A CN202210738899A CN115304085A CN 115304085 A CN115304085 A CN 115304085A CN 202210738899 A CN202210738899 A CN 202210738899A CN 115304085 A CN115304085 A CN 115304085A
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- lithium carbonate
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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
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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
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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
- C01P2006/82—Compositional purity water content
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
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Abstract
The invention provides a method for recovering waste medical lithium carbonate, which comprises the following steps: (1) roasting: burning clinker; (2) crushing: crushing the materials; (3) leaching: leaching liquor; (4) removing impurities: purifying the liquid; (5) precipitating lithium: lithium carbonate. According to the method for recovering the waste medical lithium carbonate, the solid waste medical lithium carbonate raw material is added with sulfuric acid through the leaching step to form liquid lithium sulfate, magnesium sulfate, manganese sulfate, aluminum sulfate and potassium sulfate, namely leachate, and first fixed slag is separated out.
Description
Technical Field
The invention relates to the technical field of lithium extraction processes, and particularly relates to a method for recovering waste medical lithium carbonate.
Background
Medical lithium carbonate (lithium carbonate tablets) is a prescription drug and belongs to a national basic drug. The traditional Chinese medicine composition is mainly used for treating mania, has good treatment and recurrence prevention effects on bipolar affective disorder with alternating attack of mania and depression, has a prevention attack effect on recurrent depression, and is also used for treating schizoaffective disorder.
With the increasing medical demand, the generated waste medical lithium carbonate is increased, and the waste medical lithium carbonate contains a large amount of valuable metals. Therefore, the recovery of the waste lithium ion battery is very important. The waste lithium ion battery is recycled, so that a large amount of metals can be recycled, the production cost is reduced, the pollution of the waste lithium ion battery to the environment can be reduced, and meanwhile, the efficient recycling of the waste medical lithium carbonate is of great importance to the sustainable development of the lithium carbonate industry.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for recovering waste medical lithium carbonate so as to solve the defects in the related technology.
The invention provides a method for recovering waste medical lithium carbonate, which comprises the following steps:
(1) Roasting: roasting the waste medical lithium carbonate to obtain a roasted clinker;
(2) Crushing: crushing the clinker to obtain a crushed material;
(3) Leaching: leaching and dissolving the crushed materials to separate solid from liquid, so as to obtain a leaching solution and first solid slag;
(4) Removing impurities: adding alkali into the leachate to remove impurities, and carrying out solid-liquid separation to obtain a purified solution and second solid slag;
(5) And (3) lithium deposition: adding the purified liquid into a sodium carbonate saturated solution prepared in advance to perform solid-liquid separation on the purified liquid to obtain wet lithium carbonate and filtrate;
(6) Drying and crushing: and drying and crushing the wet lithium carbonate in sequence to obtain the lithium carbonate meeting the purity requirement.
According to one aspect of the technical scheme, in the step (1), lepidolite roasting rotary kiln is adopted for synergistic combustion in roasting, the roasting temperature is 450-550 ℃, and the roasting time is 1-2 hours.
According to one aspect of the above technical solution, in the step (2), the crushed material has a crushed particle size of 100 mesh or larger.
According to an aspect of the foregoing technical solution, in the step (3), the leaching and dissolving specifically includes:
and adding water into the crushed materials, stirring for 1h, and then dropwise adding sulfuric acid with the concentration of 98% and the pH value of 1.5 into the dissolving tank, wherein the reaction time is 1h.
According to one aspect of the technical scheme, in the step (4), the alkali is flake sodium hydroxide and solid sodium carbonate to adjust the pH value of the leachate to 7-9, the reaction time of the impurity removal step is 1-1.5 h, and the reaction temperature is controlled to be 60-80 ℃.
According to one aspect of the above technical scheme, in the step (5), the reaction temperature is controlled to be 85-100 ℃, and the reaction time is 1-3 h.
According to one aspect of the above technical solution, in the step (6), the drying temperature is 85 to 100 ℃.
According to an aspect of the above technical solution, in the step (6), a particle diameter D50 of the lithium carbonate is 5 to 8 μm.
Compared with the prior art, the invention has the beneficial effects that: the method comprises the steps of roasting medical lithium carbonate serving as a raw material, crushing, leaching, removing impurities, depositing lithium, recycling the waste lithium carbonate again, adding sulfuric acid with the concentration of 98% into a solid waste medical lithium carbonate raw material to form liquid lithium sulfate, magnesium sulfate, manganese sulfate, aluminum sulfate and potassium sulfate, namely leachate, leaching liquid, separating other insoluble substances to form first fixed slag, further removing impurities, adding sodium hydroxide and sodium carbonate to form magnesium hydroxide, manganese hydroxide, aluminum hydroxide and calcium carbonate precipitates, removing magnesium, manganese, aluminum and calcium in the leachate, and depositing lithium sulfate in the leachate to form high-purity lithium carbonate.
Detailed Description
In order to facilitate an understanding of the invention, the invention will now be described more fully and in detail with reference to the preferred embodiments, but the scope of the invention is not limited to the specific embodiments described below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the invention.
Unless otherwise specifically indicated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
The invention will be further illustrated with reference to specific embodiments:
first embodiment
A method for recovering waste medical lithium carbonate comprises the following steps:
(1) Roasting: and roasting the waste medical lithium carbonate to obtain a roasted clinker. Specifically, in the step, the calcination mainly utilizes a lepidolite calcination rotary kiln to carry out synergistic combustion, wherein the calcination temperature is 500 ℃, and the calcination time is 1h.
(2) Crushing: and crushing the clinker to obtain a crushed material. Specifically, in this step, the particle size of the crushed material is 100 mesh or larger.
(3) Leaching: and leaching and dissolving the crushed materials to separate solid from liquid, thereby obtaining a leaching solution and first solid slag. Specifically, in this step, the leaching and dissolving step specifically includes:
and (3) placing the crushed material in a dissolving tank, adding water, stirring, and dropwise adding 98% sulfuric acid into the dissolving tank after stirring for 1h, wherein the pH value is 1.5, and the reaction time is 1h. Further, in the step, the main reaction formula is as follows:
Li 2 CO 3 +H 2 SO 4 ＝Li 2 SO 4 +H 2 O+CO 2 . The crushed material mainly comprises solid lithium carbonate, wherein lithium exists in a solid state, and since the conversion rate of lithium in an acidic environment is higher, sulfuric acid is added to react to form liquid lithium sulfate, and the leachate comprises liquid lithium sulfate, magnesium sulfate, manganese sulfate, aluminum sulfate and potassium sulfate. In addition, as the waste medical lithium carbonate raw material needs to be roasted in the kiln, scrap iron and other impurities brought in the kiln are stored in the kiln, the lithium carbonate and the sulfuric acid which are mainly needed can be dissolved, and other partial impurities are insoluble, namely the first fixed slag.
(4) Removing impurities: and adding alkali into the leachate to remove impurities, and carrying out solid-liquid separation to obtain a purified solution and second solid slag. Specifically, in the step, the alkali is flake sodium hydroxide and solid sodium carbonate, the sodium hydroxide and the sodium carbonate are mainly used for removing impurities (calcium, magnesium, aluminum and manganese) in the leachate, the pH value of the leachate is adjusted to 7, the reaction time is 1h, and the reaction temperature is controlled at 60 ℃. Further, in this step, the relevant main chemical formula is:
MgSO 4 +2NaOH＝Mg(OH) 2 ↓+Na 2 SO 4 ；
MnSO 4 +2NaOH＝Mn(OH) 2 ↓+Na 2 SO 4 ；
Al 2 (SO4) 3 +6NaOH＝2Al(OH) 3 ↓+3Na 2 SO 4 ；
Ca(OH) 2 +Na 2 CO 3 ＝CaCO 3 ↓ +2NaOH. Adding sodium hydroxide to react with magnesium sulfate in the leachate to generate magnesium hydroxide precipitate so as to remove magnesium in the leachate; sodium hydroxide is added to react with manganese sulfate in the leachate to generate manganese hydroxide precipitate so as to remove manganese hydroxide in the leachateMagnesium; adding sodium hydroxide to react with aluminum sulfate in the leachate to generate an aluminum hydroxide precipitate so as to remove aluminum in the leachate; the calcium carbonate precipitate is generated by adding sodium carbonate to react with calcium hydroxide in the leaching solution so as to remove calcium in the leaching solution. And filtering the calcium carbonate, the magnesium hydroxide, the aluminum hydroxide and the manganese hydroxide, namely the second fixed slag, to form a leachate, wherein the leachate after the impurity removal step mainly comprises liquid lithium sulfate, liquid potassium sulfate and liquid sodium sulfate.
(5) And (3) lithium deposition: and adding the purified liquid into a sodium carbonate saturated solution prepared in advance to perform solid-liquid separation on the purified liquid, so as to obtain wet lithium carbonate and filtrate. Specifically, in the present step, the reaction temperature is 90 ℃, the reaction time is 2h, and the related reaction chemical formula is:
Na 2 CO 3 +Li 2 SO4＝Li 2 CO 3 ↓+Na 2 SO 4 . The purification liquid, namely liquid lithium sulfate and potassium sulfate, is added into the saturated solution of sodium carbonate, and the liquid lithium sulfate reacts with the sodium carbonate to generate solid lithium carbonate and liquid sodium sulfate. The filtrate, namely the liquid sodium sulfate and the potassium sulfate, is equivalent to the separation of sodium, potassium and lithium in the leachate. Specifically, the above saturated solution of sodium carbonate is used in an amount of 20% excess in terms of complete reaction of lithium with sodium carbonate.
(6) Drying and crushing: and drying and crushing the wet lithium carbonate in sequence to obtain the lithium carbonate meeting the purity requirement. Specifically, in this step, the drying temperature was 95 ℃.
The waste medical lithium carbonate comprises the following components:
| composition (I) | Li 2 CO 3 | H 2 O | SO 4 2- | Al | Ca | Fe | K | Na | Mg | Mn | Zn |
| Content (%) | 85.58 | 22.89 | 0.15 | 0.01 | 0.13 | 0.03 | 0.05 | 9.80 | 0.03 | 0.02 | 0.03 |
Watch 1
In this embodiment, the liquid phase detection data of the leaching solution and the purifying solution are shown in the following table two:
watch 2
In this embodiment, the detection data of the high-purity lithium carbonate product is shown in the following table three:
watch III
Second embodiment
A method for recovering waste medical lithium carbonate comprises the following steps:
(1) Roasting: and roasting the waste medical lithium carbonate to obtain a roasted clinker.
(2) Crushing: and crushing the clinker to obtain a crushed material.
(3) Leaching: and leaching and dissolving the crushed materials to separate solid from liquid, thereby obtaining a leaching solution and first solid slag.
(4) Removing impurities: and adding alkali to the leachate to remove impurities, and performing solid-liquid separation to obtain a purified solution and second solid slag.
(5) And (3) precipitating lithium: adding the purification liquid into a sodium carbonate saturated solution prepared in advance to perform solid-liquid separation on the purification liquid to obtain wet lithium carbonate and filtrate
(6) Drying and crushing: and drying and crushing the wet lithium carbonate in sequence to obtain the lithium carbonate meeting the purity requirement.
In this example, in step (4), the pH of the leachate was 9, the reaction time was 1.5h, and the reaction temperature was controlled at 80 ℃.
In this embodiment, the liquid phase detection data of the leachate and the purified solution are shown in the following table four:
watch four
In this embodiment, the detection data of the high-purity lithium carbonate product is shown in the following table five:
watch five
Third embodiment
A method for recovering waste medical lithium carbonate comprises the following steps:
(1) Roasting: and roasting the waste medical lithium carbonate to obtain a roasted clinker.
(2) Crushing: and crushing the clinker to obtain a crushed material.
(3) Leaching: and leaching and dissolving the crushed materials, and carrying out solid-liquid separation to obtain a leaching solution and first solid slag.
(4) Removing impurities: and adding alkali into the leachate to remove impurities, and carrying out solid-liquid separation to obtain a purified solution and second solid slag.
(5) And (3) precipitating lithium: adding the purification liquid into a sodium carbonate saturated solution prepared in advance to perform solid-liquid separation on the purification liquid to obtain wet lithium carbonate and filtrate
(6) Drying and crushing: and drying and crushing the wet lithium carbonate in sequence to obtain the lithium carbonate meeting the purity requirement.
In this example, in step (4), the pH of the leachate was 8, the reaction time was 1.5h, and the reaction temperature was controlled at 80 ℃.
In this embodiment, the liquid phase detection data of the leaching solution and the purifying solution are shown in the following table six:
watch six
In this embodiment, the detection data of the high-purity lithium carbonate product is shown in table seven below:
watch seven
Fourth embodiment
A method for recovering waste medical lithium carbonate comprises the following steps:
(1) Roasting: and roasting the waste medical lithium carbonate to obtain a roasted clinker.
(2) Crushing: and crushing the clinker to obtain a crushed material.
(3) Leaching: and leaching and dissolving the crushed materials, and carrying out solid-liquid separation to obtain a leaching solution and first solid slag.
(4) Removing impurities: and adding alkali into the leachate to remove impurities, and carrying out solid-liquid separation to obtain a purified solution and second solid slag.
(5) And (3) lithium deposition: adding the purified liquid into a sodium carbonate saturated solution prepared in advance to perform solid-liquid separation on the purified liquid to obtain wet lithium carbonate and filtrate
(6) Drying and crushing: and drying and crushing the wet lithium carbonate in sequence to obtain the lithium carbonate meeting the purity requirement.
In this example, in step (5), the reaction temperature is 100 ℃ and the reaction time is 3h;
in the step (6), the drying temperature is 100 ℃.
In this embodiment, the detection data of the high-purity lithium carbonate product is shown in table eight below:
table eight
Fifth embodiment
A method for recovering waste medical lithium carbonate comprises the following steps:
(1) Roasting: and roasting the waste medical lithium carbonate to obtain a roasted clinker.
(2) Crushing: and crushing the clinker to obtain a crushed material.
(3) Leaching: and leaching and dissolving the crushed materials to separate solid from liquid, thereby obtaining a leaching solution and first solid slag.
(4) Removing impurities: and adding alkali into the leachate to remove impurities, and carrying out solid-liquid separation to obtain a purified solution and second solid slag.
(5) And (3) precipitating lithium: adding the purified liquid into a sodium carbonate saturated solution prepared in advance to perform solid-liquid separation on the purified liquid to obtain wet lithium carbonate and filtrate
(6) Drying and crushing: and drying and crushing the wet lithium carbonate in sequence to obtain the lithium carbonate meeting the purity requirement.
In this example, in step (5), the reaction temperature is 85 ℃ and the reaction time is 1h;
in the step (6), the drying temperature is 85 ℃.
In this embodiment, the detection data of the high purity lithium carbonate product is shown in table nine below:
watch nine
In summary, in the method for recovering waste medical lithium carbonate in the embodiments of the present invention, waste medical lithium carbonate is used as a raw material, medical lithium carbonate is firstly roasted, and then crushing, leaching, impurity removal and lithium precipitation are performed, so as to recover the waste lithium carbonate again, specifically, through the leaching step, a solid waste medical lithium carbonate raw material is added with sulfuric acid with a concentration of 98% to form liquid lithium sulfate, magnesium sulfate, manganese sulfate, aluminum sulfate and potassium sulfate, i.e., leachate, and other insoluble substances are separated to form first fixed slag, and further through the impurity removal step, sodium hydroxide and sodium carbonate are added to form magnesium hydroxide, manganese hydroxide, aluminum hydroxide and calcium carbonate precipitates, magnesium, manganese, aluminum and calcium in the leachate are removed, and through the lithium precipitation step, the lithium sulfate in the leachate is precipitated to form high-purity lithium carbonate.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The above examples are merely illustrative of several embodiments of the present invention, and the description thereof is more specific and detailed, but not to be construed as limiting the scope of the invention. It should be noted that various changes and modifications can be made by those skilled in the art without departing from the spirit of the invention, and these changes and modifications are all within the scope of the invention. Therefore, the protection scope of the present invention should be subject to the appended claims.
Claims (8)
1. A method for recovering waste medical lithium carbonate is characterized by comprising the following steps:
(1) Roasting: roasting the waste medical lithium carbonate to obtain a roasted clinker;
(2) Crushing: crushing the clinker to obtain a crushed material;
(3) Leaching: leaching and dissolving the crushed materials to separate solid from liquid to obtain leachate and first solid residue;
(4) Removing impurities: adding alkali to the leachate to remove impurities, and performing solid-liquid separation to obtain a purified solution and second solid slag;
(5) And (3) lithium deposition: adding the purified liquid into a sodium carbonate saturated solution prepared in advance to perform solid-liquid separation on the purified liquid to obtain wet lithium carbonate and filtrate;
(6) Drying and crushing: and drying and crushing the wet lithium carbonate in sequence to obtain the lithium carbonate meeting the purity requirement.
2. The method for recycling the waste medical lithium carbonate as claimed in claim 1, wherein in the step (1), the calcination adopts a lepidolite calcination rotary kiln to cooperatively combust, the calcination temperature is 450-550 ℃, and the calcination time is 1-2 h.
3. The method for recycling the waste medical lithium carbonate as claimed in claim 1, wherein in the step (2), the crushed material has a crushing size of 100 meshes or more.
4. The method for recovering waste medical lithium carbonate according to claim 1, wherein in the step (3), the leaching and dissolving step specifically comprises:
and adding water into the crushed materials, stirring for 1h, and then dropwise adding sulfuric acid with the concentration of 98% and the pH value of 1.5 into the dissolving tank, wherein the reaction time is 1h.
5. The method for recovering waste medical lithium carbonate according to claim 1, wherein in the step (4), the alkali is flake sodium hydroxide and solid sodium carbonate so as to adjust the pH value of the leachate to 7-9, and the reaction time of the impurity removal step is 1-1.5 hours, and the reaction temperature is controlled to be 60-80 ℃.
6. The method for recycling the waste medical lithium carbonate as claimed in claim 1, wherein in the step (5), the reaction temperature is controlled to be 85-100 ℃, and the reaction time is 1-3 h.
7. The method for recycling the waste medical lithium carbonate as claimed in claim 1, wherein in the step (6), the drying temperature is 85-100 ℃.
8. The method for recycling the waste medical lithium carbonate as claimed in claim 1, wherein in the step (6), the particle size D50 of the lithium carbonate is 5-8 μm.
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| CN202210738899.1A CN115304085A (en) | 2022-06-27 | 2022-06-27 | Method for recovering waste medical lithium carbonate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2623593A (en) * | 2022-10-21 | 2024-04-24 | Res By British Lithium Limited | Impurity removal and leaching of lithium material |
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| CN110760686A (en) * | 2019-12-13 | 2020-02-07 | 九江天赐高新材料有限公司 | Method for recovering lithium from waste lithium ion battery |
| CN113258158A (en) * | 2021-04-27 | 2021-08-13 | 湖北金泉新材料有限公司 | Treatment method for recycling waste lithium ion batteries |
| CN113930619A (en) * | 2021-11-03 | 2022-01-14 | 金川集团股份有限公司 | Method for preferentially extracting lithium from waste ternary lithium ion battery anode material and recovering valuable metal |
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Patent Citations (5)
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| CN107742760A (en) * | 2017-09-26 | 2018-02-27 | 北京矿冶研究总院 | Method for extracting lithium from waste lithium ion battery |
| CN110616331A (en) * | 2019-10-16 | 2019-12-27 | 衢州华友资源再生科技有限公司 | Method for recycling all metals of power lithium ion battery |
| CN110760686A (en) * | 2019-12-13 | 2020-02-07 | 九江天赐高新材料有限公司 | Method for recovering lithium from waste lithium ion battery |
| CN113258158A (en) * | 2021-04-27 | 2021-08-13 | 湖北金泉新材料有限公司 | Treatment method for recycling waste lithium ion batteries |
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| GB2623593A (en) * | 2022-10-21 | 2024-04-24 | Res By British Lithium Limited | Impurity removal and leaching of lithium material |
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