CN113912090A - Method for recovering high-purity lithium carbonate by causticizing, freezing and removing mirabilite from lithium precipitation mother liquor - Google Patents
Method for recovering high-purity lithium carbonate by causticizing, freezing and removing mirabilite from lithium precipitation mother liquor Download PDFInfo
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- CN113912090A CN113912090A CN202111345751.3A CN202111345751A CN113912090A CN 113912090 A CN113912090 A CN 113912090A CN 202111345751 A CN202111345751 A CN 202111345751A CN 113912090 A CN113912090 A CN 113912090A
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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
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/004—Preparation in the form of granules, pieces or other shaped products
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/16—Purification
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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 discloses a method for recovering high-purity lithium carbonate by causticizing, freezing and removing mirabilite in lithium precipitation mother liquor, which comprises the following steps: 1. lime causticization, 2, evaporation concentration, 3, freezing crystallization and 4, lithium precipitation by carbonization. The invention has the beneficial effects that: and adding calcium oxide to remove the influence of the sulfate ions in the lithium precipitation mother liquor, concentrating, removing the sulfate ions and sodium ions by using sodium sulfate decahydrate formed by sodium sulfate at a low temperature, and absorbing carbon dioxide for carbonization to obtain the high-purity lithium carbonate. According to the method, the carbonate ions are removed through causticization of the cheap quicklime, so that a complex route that the carbonate ions are removed through acidification of sulfuric acid in the traditional route and the sodium carbonate is continuously supplemented for lithium precipitation after subsequent concentration is avoided, the added raw materials are few and cheap, the cost is low, and the high-purity lithium carbonate is finally recycled and prepared.
Description
Technical Field
The invention relates to the field of recovery and preparation of high-purity lithium carbonate from lithium precipitation mother liquor, and particularly relates to a method for recovering high-purity lithium carbonate by causticizing, freezing and removing mirabilite from lithium precipitation mother liquor.
Background
In industrial production, the mother liquor obtained after lithium sulfate is added with sodium carbonate to precipitate lithium also contains a certain amount of lithium ions which can be recycled, the existing process for preparing lithium carbonate by recovering the lithium precipitation mother liquor is complex, the cost is high, and the recovered lithium carbonate generally can only reach an industrial grade (the concentration of lithium carbonate is more than or equal to 99.2%) and a battery grade (the concentration of lithium carbonate is more than or equal to 99.5%), so that the significance of how to efficiently utilize the lithium precipitation mother liquor to recover and prepare high-purity lithium carbonate is important.
Lithium carbonate is a basic material for lithium salt industry and has various industrial uses, wherein battery grade lithium carbonate is most widely used, and the preparation method of battery grade lithium carbonate generally adopts Li2SO4Adding sodium carbonate into the solution to carry out lithium precipitation operation, wherein a small amount of Li ions still exist in the solution after the lithium precipitation is finished, the solution is called lithium precipitation mother liquor, and the preparation of lithium carbonate by utilizing the lithium precipitation mother liquor is a key problem for improving the recovery rate of lithium. The existing recovery process route generally comprises the steps of firstly adding acid to destroy carbonate, then concentrating to remove sodium sulfate, and then adding sodium carbonate to precipitate lithium, so that the consumption of sulfuric acid and sodium carbonate in the whole process flow is large, the cost is high, and the recovery rate of lithium is low.
The invention patent (ZL 201110122564.9) discloses a processing method of a battery-grade lithium carbonate lithium precipitation mother solution, which comprises the steps of firstly utilizing sulfuric acid to acidify the lithium precipitation mother solution, evaporating and concentrating, then recovering the battery-grade lithium carbonate mother solution by adopting the steps of sodium precipitation, lithium precipitation, mother solution circulation and the like to prepare battery-grade lithium carbonate.
The invention patent (ZL 201711171953.4) discloses a process for recycling lithium precipitation mother liquor by using battery-grade lithium carbonate to prepare high-purity lithium carbonate, firstly, impurities in the mother liquor are precipitated in a precipitation mode by using a precipitator, the lithium precipitation mother liquor is acidified by using sulfuric acid, then, lime powder causticization conversion is added, the mother liquor containing lithium hydroxide is obtained after impurity removal operations such as evaporation concentration, freezing crystallization and the like, and then, the lithium precipitation operation is finally carried out by evaporation and extraction technologies to obtain a high-purity lithium carbonate product. Although the process flow is green and clean, the technology has the problems of high consumption of chemical agents, high energy consumption of evaporation and concentration, toxic liquid of an extractant carbon tetrachloride and the like.
The invention patent (ZL 201110190405.2) discloses a method for preparing battery-grade lithium dihydrogen phosphate by utilizing high-purity lithium carbonate lithium precipitation mother liquor, which comprises the steps of firstly utilizing phosphoric acid to primarily precipitate lithium from lithium carbonate lithium precipitation mother liquor, then utilizing phosphate to deeply extract lithium from the lithium carbonate lithium precipitation mother liquor to obtain a mixture of lithium phosphate and lithium dihydrogen phosphate, and then carrying out evaporation concentration, cooling crystallization, centrifugal separation, saturated washing, drying, airflow crushing and packaging to obtain the battery-grade lithium dihydrogen phosphate. The process technology is complex, the lithium recovery rate is not high, and the treatment cost is also high.
Disclosure of Invention
The invention provides a method for preparing high-purity lithium carbonate by causticizing, freezing and removing mirabilite from lithium precipitation mother liquor containing lithium sulfate.
The technical scheme of the invention is realized as follows:
a method for preparing high-purity lithium carbonate by causticizing, freezing and removing mirabilite from lithium precipitation mother liquor containing lithium sulfate comprises the following steps:
s1 causticizing and removing impurities: adding calcium oxide into the lithium precipitation mother liquor, adjusting the pH =12-14, reacting for 2.0-8.5h at 30-60 ℃, and then carrying out centrifugal filtration to separate calcium carbonate precipitation and causticization liquor.
The purpose of adding calcium oxide into the lithium precipitation mother liquor is to precipitate carbonate ions in the lithium precipitation mother liquor in the form of calcium carbonate precipitation. Too low pH can cause insufficient precipitation of calcium carbonate generated by carbonate ions, and too high pH can waste more calcium oxide and also can cause too high concentration of calcium ions in the lithium precipitation mother liquor. The reaction equation is as follows:
Ca++CO3 2-=CaCO3↓
s2 evaporation concentration: and (4) evaporating and concentrating the causticized liquid obtained in the step (S1) until the specific gravity of the solution is 1.2-1.3. Then solid-liquid separation is carried out to obtain concentrated solution and sodium sulfate crystals.
The purpose of evaporation concentration is to remove part of water in the lithium precipitation mother liquor, so that sodium sulfate is supersaturated, and sodium sulfate crystals are separated out. The concentration of lithium ions in the solution is increased after evaporation and concentration, so that the subsequent lithium carbonization and precipitation operation is facilitated.
S3 freeze crystallization: and (4) cooling the concentrated solution obtained in the step (S2) by a heat exchanger to a temperature of-15-0 ℃, then carrying out solid-liquid separation, and filtering out mirabilite crystals to obtain a frozen mother solution.
The purpose of freezing crystallization is to separate out sulfate ions and sodium ions in the concentrated solution in the form of sodium sulfate decahydrate, after the sodium sulfate decahydrate is separated out, the loss of lithium ions can be effectively reduced due to small entrainment because the crystal particles of the sodium sulfate decahydrate are large, the concentration of the lithium ions in the final filtrate is more than or equal to 10g/L, and the concentration of the sulfate ions is less than or equal to 20 g/L. The chemical reaction equation is as follows:
2Na++SO42-+10H2O→Na2SO4 .10H2O
s4 carbonization lithium precipitation: introducing carbon dioxide into the frozen mother liquor in the step S3 in a vacuum spraying mode at normal temperature to enable the frozen mother liquor to fully react with the solution, wherein the chemical reaction equation is as follows:
2LiOH+CO2=Li2CO3↓+H2O
and carbon dioxide is introduced in the carbonization step in a spraying mode, so that the contact area of the carbon dioxide and the solution is increased as much as possible, the pH value at the end point of the reaction is 8.5-9.5, the content of impurity ions in the lithium carbonate prepared by the lithium deposition operation is low, and the content of lithium carbonate is more than or equal to 99.9 percent and reaches the standard of high-purity lithium carbonate.
Compared with the prior art, the invention has the advantages that:
and adding calcium oxide to remove the influence of the sulfate ions in the lithium precipitation mother liquor, concentrating, removing the sulfate ions and sodium ions by using sodium sulfate decahydrate formed by sodium sulfate at a low temperature, and absorbing carbon dioxide for carbonization to obtain the high-purity lithium carbonate. According to the method, the carbonate ions are removed through causticization of the cheap quicklime, so that a complex route that the carbonate ions are removed through acidification of sulfuric acid in the traditional route and the sodium carbonate is continuously supplemented for lithium precipitation after subsequent concentration is avoided, the added raw materials are few and cheap, the cost is low, and the high-purity lithium carbonate is finally recycled and prepared.
Drawings
Fig. 1 is a process flow diagram of a method for removing mirabilite from a lithium precipitation mother solution and recovering high-purity lithium carbonate.
Detailed Description
In order to facilitate understanding of the present invention, the present invention will be described in more detail with reference to the following examples, but the scope of the present invention is not limited to the following specific examples.
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 herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1
A method for recovering high-purity lithium carbonate by causticizing, freezing and removing mirabilite from lithium precipitation mother liquor comprises the following steps: s1, causticizing and removing impurities: the lithium precipitation mother liquor is the mother liquor obtained after lithium sulfate solution is added with sodium carbonate for lithium precipitation and separation, wherein the lithium ion content is 2.3g/L, the carbonate ion content is 13g/L, the sodium ion content is 70g/L, and the sulfate ion content is 150 g/L. Adding calcium oxide with the molar weight 1.1-1.3 times of that of carbonate ions, wherein the specific amount of the lithium precipitation mother liquor is 5L, the addition amount of the calcium oxide is 73g, the pH of the solution after the calcium oxide is added is =12.2, carrying out causticization stirring reaction for 2.5h, and filtering at 50 ℃ to obtain calcium carbonate precipitation and causticized liquid. S2, evaporation and concentration: the causticized solution obtained in the step S1 is evaporated and concentrated until the specific gravity of the solution is 1.2, and then solid-liquid separation is carried out to obtain a concentrated solution (the concentration of lithium ions is 6.5 g/L) and sodium sulfate crystals. S3, freezing and crystallizing: and (4) freezing the concentrated solution obtained in the step (S2) to-15 ℃ to separate out mirabilite, and separating to obtain mirabilite and frozen mother liquor, wherein the concentration of lithium ions in the frozen mother liquor is 10.2g/L, and the concentration of sulfate ions in the frozen mother liquor is 8.5 g/L. S4, carbonizing and precipitating lithium: and introducing 40L of carbon dioxide into the frozen mother liquor obtained in the step S3 in a vacuum injection mode, wherein the reaction temperature is 70 ℃, the pH value of the reaction end point is 8.5, and high-purity grade lithium carbonate 48.5g with the purity of 99.92% of lithium carbonate is obtained through separation. The lithium ion recovery rate of the process is 82%.
Example 2
A method for recovering high-purity lithium carbonate by causticizing, freezing and removing mirabilite from lithium precipitation mother liquor comprises the following steps: s1, causticizing and removing impurities: the lithium precipitation mother liquor is the mother liquor obtained after lithium sulfate solution is added with sodium carbonate for lithium precipitation and separation, wherein the lithium ion content is 2.5g/L, the carbonate ion content is 15g/L, the sodium ion content is 75g/L, and the sulfate ion content is 160 g/L. Adding calcium oxide with the molar weight 1.1-1.3 times of that of carbonate ions, wherein the specific amount of the lithium precipitation mother liquor is 5L, the addition amount of the calcium oxide is 91g, the pH =12.5 of the solution after the calcium oxide is added, carrying out causticization, stirring and reaction for 3h at the temperature of 60 ℃, and filtering to obtain calcium carbonate precipitation and causticized solution. S2, evaporation and concentration: the causticized solution obtained in the step S1 is evaporated and concentrated until the specific gravity of the solution is 1.23, and then solid-liquid separation is carried out to obtain a concentrated solution (the concentration of lithium ions is 6.6 g/L) and sodium sulfate crystals. S3, freezing and crystallizing: and (4) freezing the concentrated solution obtained in the step (S2) to-10 ℃ to separate out mirabilite, and separating to obtain mirabilite and frozen mother liquor, wherein the concentration of lithium ions in the frozen mother liquor is 10.5g/L, and the concentration of sulfate ions in the frozen mother liquor is 9 g/L. S4, carbonizing and precipitating lithium: and introducing 42L of carbon dioxide into the frozen mother liquor obtained in the step S3 in a vacuum injection mode, wherein the reaction temperature is 75 ℃, the pH value of the reaction end point is 8.7, and 55g of high-purity grade lithium carbonate with the purity of 99.93 percent is obtained by separation. The lithium ion recovery rate of the process is 83%.
Example 3
A method for recovering high-purity lithium carbonate by causticizing, freezing and removing mirabilite from lithium precipitation mother liquor comprises the following steps: s1, causticizing and removing impurities: the lithium precipitation mother liquor is the mother liquor obtained after lithium sulfate solution is added with sodium carbonate for lithium precipitation and separation, wherein the lithium ion content is 2.7g/L, the carbonate ion content is 20g/L, the sodium ion content is 80g/L, and the sulfate ion content is 170 g/L. Adding calcium oxide with the molar weight 1.1-1.3 times of that of carbonate ions, wherein the specific amount of the lithium precipitation mother liquor is 5L, the addition amount of the calcium oxide is 116g, the pH of the solution after the calcium oxide is added is =12.7, carrying out causticization stirring reaction for 3h at the temperature of 70 ℃, and filtering to obtain calcium carbonate precipitation and causticized solution. S2, evaporation and concentration: the causticized solution obtained in the step S1 is evaporated and concentrated until the specific gravity of the solution is 1.25, and then solid-liquid separation is carried out to obtain a concentrated solution (the concentration of lithium ions is 6.8 g/L) and sodium sulfate crystals. S3, freezing and crystallizing: and (4) freezing the concentrated solution obtained in the step (S2) to-5 ℃ to separate out mirabilite, and separating to obtain mirabilite and frozen mother liquor, wherein the concentration of lithium ions in the frozen mother liquor is 10.7g/L, and the concentration of sulfate ions in the frozen mother liquor is 9.1 g/L. S4, carbonizing and precipitating lithium: 43L of carbon dioxide was introduced into the frozen mother liquor obtained in the step S3 in the form of vacuum injection, the reaction temperature was 80 ℃, the reaction end point pH was 8.9, and 59g of high-purity-grade lithium carbonate with a lithium carbonate purity of 99.95% was isolated. The lithium ion recovery rate of the process is 85%.
Example 4
A method for recovering high-purity lithium carbonate by causticizing, freezing and removing mirabilite from lithium precipitation mother liquor comprises the following steps: s1, causticizing and removing impurities: the lithium precipitation mother liquor is the mother liquor obtained after lithium sulfate solution is added with sodium carbonate for lithium precipitation and separation, wherein the lithium ion content is 2.9g/L, the carbonate ion content is 25g/L, the sodium ion content is 85g/L, and the sulfate radical content is 190 g/L. Adding calcium oxide with the molar weight 1.1-1.3 times of carbonate, wherein the specific amount of the lithium precipitation mother liquor is 5L, the addition amount of the calcium oxide is 140g, the pH =12.8 of the solution after the calcium oxide is added, carrying out causticization, stirring and reacting for 3.5h at the temperature of 80 ℃, and filtering to obtain calcium carbonate precipitation and causticization liquid. S2, evaporation and concentration: the causticized solution obtained in the step S1 is evaporated and concentrated until the specific gravity of the solution is 1.27, and then solid-liquid separation is carried out to obtain a concentrated solution (the concentration of lithium ions is 7 g/L) and sodium sulfate crystals. S3, freezing and crystallizing: and (4) freezing the concentrated solution obtained in the step (S2) to-3 ℃ to separate out mirabilite, and separating to obtain mirabilite and frozen mother liquor, wherein the concentration of lithium ions in the frozen mother liquor is 10.9g/L, and the concentration of sulfate ions in the frozen mother liquor is 9.2 g/L. S4, carbonizing and precipitating lithium: and introducing 46L of carbon dioxide into the frozen mother liquor obtained in the step S3 in a vacuum injection mode, wherein the reaction temperature is 85 ℃, the pH value of the reaction end point is 9.1, and high-purity grade lithium carbonate 64g with the purity of 99.96% of lithium carbonate is obtained through separation. The lithium ion recovery rate of the process was 84%.
Example 5
A method for recovering high-purity lithium carbonate by causticizing, freezing and removing mirabilite from lithium precipitation mother liquor comprises the following steps: s1, causticizing and removing impurities: the lithium precipitation mother liquor is the mother liquor obtained after lithium sulfate solution is added with sodium carbonate for lithium precipitation and separation, wherein the lithium ion content is 3.0g/L, the carbonate ion content is 30g/L, the sodium ion content is 90g/L, and the sulfate ion content is 190 g/L. Adding calcium oxide with the molar weight of carbonate ions being 1.1-1.3 times, wherein the specific amount of the lithium precipitation mother liquor is 5L, the addition amount of the calcium oxide is 175g, the pH =12.9 of the solution is subjected to causticization, stirring and reaction for 3.5h, the temperature is 80 ℃, and filtering to obtain calcium carbonate precipitation and causticization liquid. S2, evaporation and concentration: the causticized solution obtained in the step S1 is evaporated and concentrated until the specific gravity of the solution is 1.29, and then solid-liquid separation is carried out to obtain a concentrated solution (the concentration of lithium ions is 7.2 g/L) and sodium sulfate crystals. S3, freezing and crystallizing: and (4) freezing the concentrated solution obtained in the step (S2) to 0 ℃ to separate out mirabilite, and separating to obtain mirabilite and frozen mother liquor, wherein the concentration of lithium ions in the frozen mother liquor is 11.2g/L, and the concentration of sulfate ions in the frozen mother liquor is 9.3 g/L. S4, carbonizing and precipitating lithium: 48L of carbon dioxide is introduced into the frozen mother liquor obtained in the step S3 in a vacuum injection mode, the reaction temperature is 90 ℃, the pH value of the reaction end point is 9.3, and 67g of high-purity-grade lithium carbonate with the purity of 99.97 percent of lithium carbonate is obtained through separation. The lithium ion recovery rate of the process is 85%.
The above description is only intended to illustrate the embodiments of the present invention, but not to limit the scope of the present invention, and any person skilled in the art should be able to make equivalent changes or simple modifications based on the technical solution and concept of the present invention to be included in the scope of the present invention.
Claims (7)
1. A method for recovering high-purity lithium carbonate by causticizing, freezing and removing mirabilite from lithium precipitation mother liquor is characterized by comprising the following steps: the method comprises the following steps:
s1 lime causticization: adding a certain amount of calcium oxide into the lithium precipitation mother liquor, causticizing and stirring, adjusting the pH =12-14, reacting for 2.0-8.5h at 30-60 ℃, and filtering to obtain calcium carbonate precipitation and causticized liquor;
s2 evaporation concentration: evaporating and concentrating the causticized liquid obtained in the step S1, and then carrying out solid-liquid separation to obtain a concentrated liquid and sodium sulfate crystals;
s3 freeze crystallization: freezing the concentrated solution obtained in the step S2 to separate out mirabilite, and separating to obtain mirabilite and a frozen mother solution;
s4 carbonization lithium precipitation: and (4) introducing carbon dioxide into the frozen mother liquor obtained in the step S3 in a vacuum injection mode at normal temperature, and separating to obtain high-purity lithium carbonate.
2. The method for recovering high-purity lithium carbonate by causticizing, freezing and removing mirabilite from lithium precipitation mother liquor according to claim 1, which is characterized by comprising the following steps: the lithium precipitation mother liquor in the step S1 is the mother liquor obtained after lithium sulfate solution is added with sodium carbonate for lithium precipitation and separation, wherein the lithium ion content is 2-3g/L, the carbonate ion content is 10-30g/L, the sodium ion content is 50-100g/L, and the sulfate ion content is 100-250 g/L.
3. The method for recovering high-purity lithium carbonate by causticizing, freezing and removing mirabilite from lithium precipitation mother liquor according to claim 1, which is characterized by comprising the following steps: the addition amount of the calcium oxide in the step S1 is 1.1-1.3 times of the molar amount of the carbonate ions contained in the lithium precipitation mother liquor.
4. The method for recovering high-purity lithium carbonate by causticizing, freezing and removing mirabilite from lithium precipitation mother liquor according to claim 1, which is characterized by comprising the following steps: and (4) evaporating and concentrating the causticized liquid in the step S2 until the specific gravity of the solution is 1.2-1.3 and the concentration of lithium ions is more than or equal to 6 g/L.
5. The method for recovering high-purity lithium carbonate by causticizing, freezing and removing mirabilite from lithium precipitation mother liquor according to claim 1, which is characterized by comprising the following steps: the cooling operation in step S3 specifically includes: cooling the filtrate to-15-0 ℃; the concentration of lithium ions in the frozen mother liquor is more than or equal to 10g/L, and the concentration of sulfate ions is less than or equal to 10 g/L.
6. The method for recovering high-purity lithium carbonate by causticizing, freezing and removing mirabilite from lithium precipitation mother liquor according to claim 1, which is characterized by comprising the following steps: and the pH of the carbonization reaction end solution introduced with carbon dioxide in the step S4 is =8.5-9.5, and the reaction temperature is 50-90 ℃.
7. The method for recovering high-purity lithium carbonate by causticizing, freezing and removing mirabilite from lithium precipitation mother liquor according to claim 1, which is characterized by comprising the following steps: the content of lithium carbonate in the obtained high-purity lithium carbonate is more than or equal to 99.9 percent.
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