CN110923452A - Process for recovering potassium and sodium salts from lithium-precipitated liquid of lepidolite by using ethanol - Google Patents
Process for recovering potassium and sodium salts from lithium-precipitated liquid of lepidolite by using ethanol Download PDFInfo
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- CN110923452A CN110923452A CN201911096033.XA CN201911096033A CN110923452A CN 110923452 A CN110923452 A CN 110923452A CN 201911096033 A CN201911096033 A CN 201911096033A CN 110923452 A CN110923452 A CN 110923452A
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
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Abstract
The invention relates to a process for recovering potassium sodium salt from a liquid obtained after lithium precipitation of lepidolite by using ethanol, belonging to the technical field of industrial water treatment. The invention comprises the process steps of ore roasting, water leaching, purification, lithium carbonate precipitation, lithium precipitation mother liquor and ethanol mixing and sedimentation, induced crystallization, crystal slurry centrifugal separation, MVR evaporation separation of alcohol-water mixed liquor and the like.
Description
Technical Field
The invention relates to a process for recovering potassium sodium salt from a liquid obtained after lithium precipitation of lepidolite by using ethanol, belonging to the technical field of industrial water treatment.
Background
With the increasingly prominent energy problem, research and development and industrialization of new energy materials such as lithium ion batteries and the like are vigorously developed. China has a large amount of lepidolite mineral resources, and the extraction of metals such as lithium, rubidium, cesium and the like from lepidolite raw materials has a good development prospect. However, the content of lithium in the lepidolite raw material is about 1.7%, and the content of potassium and sodium is as high as 6.5% and 1.25%, and because potassium sodium salt has extremely high solubility in water, the impurities can reduce the quality of the lithium carbonate product on one hand, and can reduce the production efficiency on the other hand, and even can not successfully carry out the production. The existing potassium-sodium salt recovery process comprises a freezing crystallization method and an evaporation concentration method, wherein the freezing crystallization method can only primarily remove potassium ions in a solution, and the removal effect on sodium ions is not ideal; the evaporation concentration method inevitably generates potassium-sodium-lithium double salt, which causes great loss of lithium, and has low production efficiency and high energy consumption.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provide a process for recovering potassium sodium salt from the liquid after lithium precipitation of lepidolite by using ethanol, so that the common recovery of the potassium sodium salt and the ethanol can be realized, and the energy consumption is low.
In order to solve the technical problems, the process for recovering potassium and sodium salts from the liquid obtained after lithium precipitation of lepidolite by using ethanol comprises the following specific steps of:
the method comprises the following steps: mixing lepidolite ore with sodium sulfate, potassium sulfate and calcium carbonate, roasting, soaking in water, purifying to obtain a solution before lithium precipitation, adding carbon dioxide or sodium carbonate to precipitate lithium carbonate to obtain a solution after lithium precipitation;
step two: introducing the liquid after lithium precipitation into a settling tank, adding ethanol accounting for 14-16% of the liquid after lithium precipitation and potassium sulfate crystals accounting for 0.05-0.1% of the liquid after lithium precipitation at the temperature below 20 ℃, standing for 28-35min, and filtering to obtain crystal mush I and filtrate A;
step three: adding ethanol with the volume of 18-20% of that of the filtrate A into the filtrate A, uniformly stirring, standing for at least 30min, and filtering to obtain a crystal mush II and alcohol-water mixed solution;
step four: introducing the alcohol-water mixed solution into a Mechanical Vapor Recompression (MVR) evaporation system, evaporating ethanol at the temperature of 78-80 ℃, storing the ethanol in a storage tank for the next use, and returning the finished solution to the water leaching and purifying process in the first step through a water tank;
step five: the crystal mush I and the crystal mush II respectively enter a centrifugal machine for separation to obtain crude potassium sulfate and crude sodium potassium sulfate, and supernate discharged by the centrifugal machine returns to the step II;
step six: and fifthly, drying, inspecting and packaging the crude potassium sulfate obtained in the step five, and selling the crude potassium sulfate, and returning the crude potassium sulfate sodium to the mixed roasting process in the step one after drying.
The invention relates to a process for recovering potassium and sodium salts from a lithium-precipitated liquid of lepidolite by using ethanol, wherein the lithium-precipitated liquid in the first step contains 60-90 g/L of sodium, 30-40 g/L of potassium and 2-4 g/L of lithium.
The invention relates to a process for recovering potassium and sodium salts from a lithium-precipitated liquid of lepidolite by using ethanol, wherein the lithium-precipitated liquid in the first step contains 75-80 g/L of sodium, 30-35 g/L of potassium and 3-3.5 g/L of lithium.
The invention relates to a process for recovering potassium sodium salt from a lithium-precipitated liquid of lepidolite by using ethanol, wherein in the second step, the lithium-precipitated liquid and the ethanol are uniformly mixed, and the temperature is controlled to be 15-20 ℃.
As a further scheme of the invention, the stirring speed in the third step is more than 800 revolutions per minute, preferably 1000 revolutions per minute and 1200 revolutions per minute, and the stirring rapid mixing is enhanced to reduce the crystallization of the lithium sulfate.
As a further scheme of the invention, in the fourth step, the boiling point of the MVR evaporation system is increased by 1-2 ℃, and the temperature of the compressor is increased by 8-10 ℃.
The invention relates to a process for recovering potassium sodium salt from a liquid obtained after lithium precipitation of lepidolite by using ethanol, wherein in crude potassium sulfate, the content of sodium sulfate is 14.5 wt%, and the content of lithium sulfate is 2.0 wt%; in the crude sodium potassium sulfate, the mass ratio of potassium sulfate to sodium sulfate is as follows: 26-27.5:68-70, and the content of lithium sulfate in the crude sodium potassium sulfate is less than or equal to 4.5%.
Preferably, the invention relates to a process for recovering potassium sodium salt from a liquid obtained after lithium precipitation of lepidolite by using ethanol, wherein in crude potassium sulfate, the content of potassium sulfate is 85.4 wt%, the content of sodium sulfate is 12.8 wt%, lithium sulfate is 1.8 wt%, the content of potassium sulfate in potassium sodium salt is 26.0 wt%, sodium sulfate is 69.8 wt%, and lithium sulfate is 4.2 wt%.
Compared with the prior art, the invention has the beneficial effects that: the invention comprises the process steps of ore roasting, water leaching, purification, lithium carbonate precipitation, lithium precipitation mother liquor and ethanol mixing and sedimentation, induced crystallization, crystal slurry centrifugal separation, MVR evaporation separation of alcohol-water mixed liquor and the like.
Drawings
FIG. 1 is a flow chart of a process for recovering potassium sodium salt from a liquid obtained after lithium precipitation from lepidolite by using ethanol.
Detailed Description
The present invention will be described in detail with reference to examples. The examples were carried out using the same lepidolite mineral, the composition of which is shown in table 1.
Table 1 lepidolite mineral composition, wt. -%)
Example 1
The method comprises the following steps:
after the lepidolite ore is roasted, soaked in water, purified and precipitated with lithium carbonate, a solution obtained after lithium precipitation contains 80.7g/L of sodium, 28.9g/L of potassium and 3.6g/L of lithium;
introducing 10L of the lithium-precipitated solution into a settling tank, pumping 1.5L of ethanol from an ethanol storage tank, mixing uniformly, naturally cooling to 18 ℃, adding 10g of ground potassium sulfate crystals, standing for 30min, and filtering to obtain crystal slurry I; pumping 1.8L of ethanol into the filtrate, rapidly stirring and uniformly mixing, standing for 30min, and filtering to obtain a crystal mush II and alcohol-water mixed solution;
respectively pumping the crystal slurry I and the crystal slurry II into a centrifuge for separation, wherein the rotating speed of the centrifuge is 1000r/min, discharging crude potassium sulfate and sodium potassium sulfate from a solid phase outlet after centrifuging for 20min, and merging supernatant into the solution after precipitating lithium;
pumping the alcohol-water mixed solution into a Mechanical Vapor Recompression (MVR) evaporation system, wherein the evaporation temperature is 78 ℃, the boiling point of the evaporation system is increased by 1 ℃, the temperature of a compressor is increased by 8 ℃, evaporating ethanol returns to a settling tank through an ethanol storage tank, the finished solution returns to water leaching and purifying processes through a water tank, and one-time material circulation is finished.
Through detection, the recovery rates of water and ethanol in the circulation are respectively 98% and 97%, the recovery rates of potassium sulfate, sodium sulfate and lithium sulfate in the coarse potassium sulfate are respectively 85.4%, 12.8%, 1.8%, 26.0%, 69.8% and 4.2%, and the precipitation rates of potassium, sodium and lithium are respectively 86.1%, 39.8% and 22.0%, so that better recovery and separation effects are achieved.
Example 2
The method comprises the following steps:
after the lepidolite ore is roasted, soaked in water, purified and precipitated with lithium carbonate, a solution obtained after lithium precipitation contains 78.6g/L of sodium, 27.9g/L of potassium and 3.4g/L of lithium;
introducing 10L of the lithium-precipitated solution into a settling tank, pumping 1.5L of ethanol from an ethanol storage tank, mixing uniformly, naturally cooling to 18 ℃, adding 8g of ground potassium sulfate crystals, standing for 30min, and filtering to obtain crystal slurry I; pumping 2.0L of ethanol into the filtrate, rapidly stirring and uniformly mixing, standing for 30min, and filtering to obtain a crystal mush II and alcohol-water mixed solution;
respectively pumping the crystal slurry I and the crystal slurry II into a centrifuge for separation, wherein the rotating speed of the centrifuge is 1000r/min, discharging crude potassium sulfate and sodium potassium sulfate from a solid phase outlet after centrifuging for 25min, and merging supernatant into the solution after precipitating lithium;
pumping the alcohol-water mixed solution into a Mechanical Vapor Recompression (MVR) evaporation system, wherein the evaporation temperature is 78 ℃, the boiling point of the evaporation system is increased by 1 ℃, the temperature of a compressor is increased by 8 ℃, evaporating ethanol returns to a settling tank through an ethanol storage tank, the finished solution returns to water leaching and purifying processes through a water tank, and one-time material circulation is finished.
Through detection, the recovery rates of water and ethanol in the circulation are respectively 95% and 96%, the recovery rates of potassium sulfate, sodium sulfate and lithium sulfate in the coarse potassium sulfate are respectively 84.2%, 14.2%, 1.6%, 27.2%, 68.3% and 4.5%, and the precipitation rates of potassium, sodium and lithium are respectively 88.2%, 40.6% and 24.8%, so that better recovery and separation effects are achieved.
Comparative example 1
The operating conditions were identical to those of example 2, the only difference being that no potassium sulfate seed crystals were added in comparative example 1. Through detection, the recovery rates of water and ethanol in the circulation are respectively 96% and 96%, the recovery rates of potassium sulfate, sodium sulfate and lithium in the coarse potassium sulfate are respectively 56.3%, 35.2%, 8.5%, 27.6%, 67.7% and 4.7%, and the precipitation rates of potassium, sodium and lithium are respectively 74.8%, 39.4% and 29.0%. In this example, the precipitation rate of potassium and sodium was lower than that in example 2, and the loss rate of lithium was higher than that in example 2, which was not good.
Comparative example 2
The operating conditions were the same as in example 2, the only difference being that the temperature of the crystallization process after seeding in comparative example 2 was maintained at 30 ℃. Through detection, the recovery rates of water and ethanol in the circulation are respectively 95% and 96%, the recovery rates of potassium sulfate, sodium sulfate and lithium sulfate in the coarse potassium sulfate are respectively 68.5%, 25.3%, 6.2%, 26.2%, 69.6% and 4.2%, and the precipitation rates of potassium, sodium and lithium are respectively 65.0%, 33.3% and 21.2%. In this example, the precipitation rates of potassium, sodium and lithium were all significantly lower than those in example 2, and the effect was not good.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (8)
1. A process for recovering potassium sodium salt from a liquid obtained after lithium precipitation of lepidolite by using ethanol is characterized by comprising the following specific steps of:
the method comprises the following steps: mixing lepidolite ore with sodium sulfate, potassium sulfate and calcium carbonate, roasting, soaking in water, purifying to obtain a solution before lithium precipitation, adding carbon dioxide or sodium carbonate to precipitate lithium carbonate to obtain a solution after lithium precipitation;
step two: introducing the liquid after lithium precipitation into a settling tank, adding ethanol accounting for 14-16% of the liquid after lithium precipitation and potassium sulfate crystals accounting for 0.05-0.1% of the liquid after lithium precipitation at the temperature below 20 ℃, standing for 28-35min, and filtering to obtain crystal mush I and filtrate A;
step three: adding ethanol with the volume of 18-20% of that of the filtrate A into the filtrate A, uniformly stirring, standing for at least 30min, and filtering to obtain a crystal mush II and alcohol-water mixed solution;
step four: introducing the alcohol-water mixed solution into a Mechanical Vapor Recompression (MVR) evaporation system, evaporating ethanol at the temperature of 78-80 ℃, storing the ethanol in a storage tank for the next use, and returning the finished solution to the water leaching and purifying process in the first step through a water tank;
step five: the crystal mush I and the crystal mush II respectively enter a centrifugal machine for separation to obtain crude potassium sulfate and crude sodium potassium sulfate, and supernate discharged by the centrifugal machine returns to the step II;
step six: and fifthly, drying, inspecting and packaging the crude potassium sulfate obtained in the step five, and selling the crude potassium sulfate, and returning the crude potassium sulfate sodium to the mixed roasting process in the step one after drying.
2. The process for recovering the potassium sodium salt from the lithium precipitated liquid of the lepidolite by using the ethanol according to claim 1, wherein the lithium precipitated liquid in the step one contains 60 to 90g/L of sodium, 30 to 40g/L of potassium and 2 to 4g/L of lithium.
3. The process for recovering the potassium sodium salt from the lithium precipitated liquid of lepidolite by using ethanol according to claim 2, wherein the lithium precipitated liquid in the step one contains 75-80 g/L of sodium, 30-35 g/L of potassium and 3-3.5 g/L of lithium.
4. The process for recovering the potassium sodium salt from the lithium precipitated liquid of the lepidolite by using the ethanol as claimed in claim 1, wherein the temperature of the lithium precipitated liquid in the second step is controlled to be 15-20 ℃ after the lithium precipitated liquid and the ethanol are uniformly mixed.
5. The process for recovering potassium sodium salt from the liquid after lithium precipitation of lepidolite by using ethanol as claimed in claim 1, wherein the stirring speed in the third step is more than 800 revolutions per minute.
6. The process for recovering the potassium sodium salt from the lithium precipitated liquid of the lepidolite by using the ethanol according to claim 1, wherein the boiling point of the MVR evaporation system in the fourth step is increased by 1-2 ℃ and the temperature of the compressor is increased by 8-10 ℃.
7. The process for recovering potassium sodium salt from the liquid after lithium precipitation of lepidolite by using ethanol according to claim 1, wherein the process comprises the following steps: in the crude potassium sulfate, the content of sodium sulfate was 14.5 wt%, and the content of lithium sulfate was 2.0 wt%; in the crude sodium potassium sulfate, the mass ratio of potassium sulfate to sodium sulfate is as follows: 26-27.5:68-70, and the content of lithium sulfate in the crude sodium potassium sulfate is less than or equal to 4.5%.
8. The process of claim 7, wherein the potassium sodium salt is recovered from the lithium precipitation solution of lepidolite by using ethanol, and the process comprises the following steps: in the crude potassium sulfate, the content of potassium sulfate was 85.4 wt%, the content of sodium sulfate was 12.8 wt%, and the content of lithium sulfate was 1.8 wt%, and the content of potassium sulfate-sodium salt contained 26.0 wt%, sodium sulfate was 69.8 wt%, and lithium sulfate was 4.2 wt%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113387374A (en) * | 2021-06-28 | 2021-09-14 | 四川能投鼎盛锂业有限公司 | Potassium removing process of ore lithium extraction production system |
| CN113620321A (en) * | 2021-09-10 | 2021-11-09 | 宜春银锂新能源有限责任公司 | Method for preparing industrial special-grade lithium carbonate from low-concentration lithium liquid after primary lithium precipitation |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113387374A (en) * | 2021-06-28 | 2021-09-14 | 四川能投鼎盛锂业有限公司 | Potassium removing process of ore lithium extraction production system |
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