CN110759364A - Method for preparing high-purity lithium carbonate by using crude lithium phosphate - Google Patents
Method for preparing high-purity lithium carbonate by using crude lithium phosphate Download PDFInfo
- Publication number
- CN110759364A CN110759364A CN201911108142.9A CN201911108142A CN110759364A CN 110759364 A CN110759364 A CN 110759364A CN 201911108142 A CN201911108142 A CN 201911108142A CN 110759364 A CN110759364 A CN 110759364A
- Authority
- CN
- China
- Prior art keywords
- lithium
- phosphate
- crude
- lithium carbonate
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Secondary Cells (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a method for preparing high-purity lithium carbonate by utilizing lithium phosphate, which takes crude lithium phosphate as a raw material and comprises the following steps of 1) preparing, stirring and mixing the crude lithium phosphate and pure water to obtain crude lithium phosphate slurry; 2) charging hot water or hot water vapor into the crude lithium phosphate slurry to prepare a crude lithium phosphate solution, 3) adding a phosphate radical ion remover into the soluble clear lithium phosphate solution, and filtering to obtain a phosphate mixed solution; 4) filter pressing, namely putting the phosphate mixed solution into a filter device, and filtering under a pressure filtering state to obtain a lithium-containing solution; 5) adding an impurity removing agent into the lithium-containing solution, and performing impurity removing treatment to obtain a pure lithium solution; 6) preparing coarse lithium carbonate, adding a lithium carbonate preparation auxiliary agent into the pure lithium solution in the previous step in a heating state, and performing a coarse lithium carbonate preparation reaction to obtain coarse lithium carbonate; 7) preparing high-purity lithium carbonate, adding hot purified water into the crude lithium carbonate, stirring for 1-2h, and purifying for several times to obtain the high-purity lithium carbonate.
Description
The technical field is as follows:
the invention relates to the technical field of preparation of lithium carbonate by using non-mineral raw materials, in particular to a method for preparing high-purity lithium carbonate by using crude lithium phosphate.
Background art:
lithium carbonate is an important chemical raw material, and with the rapid development of low-carbon economy and green new energy industry, especially with the breakthrough and popularization and application of large-capacity power battery technology, the novel lithium electric vehicle industry rises rapidly, and the rapid development of the lithium electric industry becomes a common consensus of people. With the emergence of the national new energy development planning, the lithium battery new energy becomes one of the energy industries which are key in national support development; lithium carbonate is used as an important basic raw material for the development of new energy of lithium batteries, and the demand of lithium carbonate is increasing.
According to the difference of raw materials, the industrial preparation method of lithium carbonate is mainly divided into two types: one is that from the brine containing lithium, through carrying on the comprehensive extraction and utilization to other valuable metallic minerals in the brine, make lithium in the brine enrich, and then extract lithium and get lithium carbonate through further processing, however, because the salt lake brine of China has the characteristic of low magnesium-lithium ratio mostly, the development difficulty is great, the industrial implementation of extracting lithium from brine is difficult;
the other method is to destroy the original gangue structure of the main lithium-containing ores, namely spodumene and lepidolite, by dry or wet treatment, so that lithium oxide in the gangue structure is dissolved out in the form of soluble lithium salt, and then lithium is precipitated by carbonization or soda ash to obtain a lithium carbonate product. The preparation method for extracting lithium carbonate by taking lepidolite ore as a raw material mainly comprises a calcination method and an acid leaching method, and the production yield of lithium carbonate is not ideal, so that the production benefit of enterprises is influenced.
However, in the existing production process for preparing lithium carbonate, there are many methods for preparing lithium carbonate by using lithium-containing ores such as lepidolite and the like as raw materials, and technical schemes for preparing lithium carbonate by using other lithium salts as raw materials are not common, for example, a method for preparing high-purity lithium carbonate by using crude lithium phosphate salt as a raw material is a technical scheme for preparing high-purity lithium carbonate with a high cost performance and an excellent control on environment and production process.
The invention content is as follows:
the invention aims to provide a method for preparing high-purity lithium carbonate by using lithium phosphate, which takes crude lithium phosphate as a raw material to solve the problems in the background technology.
The invention discloses a method for preparing high-purity lithium carbonate by using lithium phosphate, which takes rough lithium phosphate as a raw material and is characterized by comprising the following steps:
1) mixing and stirring the crude lithium phosphate and pure water to obtain crude lithium phosphate slurry;
2) filling hot water or hot water vapor into the crude lithium phosphate slurry to prepare a crude lithium phosphate solution, and then adding an acid clarifying agent to dissolve the crude lithium phosphate solution to prepare a soluble clarified lithium phosphate liquid;
3) adding a phosphate radical ion remover into a soluble clear lithium phosphate liquid, adjusting the pH of the solution to be under an acidic condition, controlling the removal reaction time to be 0.5-2h, and after the reaction is finished, performing heat preservation treatment to obtain a phosphate mixed solution;
4) filtering, namely placing the phosphate mixed solution into a filtering device, and filtering under a pressure filtering state to obtain a lithium-containing solution;
5) adding an impurity removing agent into the lithium-containing solution, and performing impurity removing treatment to obtain a pure lithium solution;
6) preparing coarse lithium carbonate, adding a lithium carbonate preparation auxiliary agent into the pure lithium solution in the previous step in a heating state, and performing a coarse lithium carbonate preparation reaction to obtain coarse lithium carbonate;
7) preparing high-purity lithium carbonate, adding hot purified water with the mass 2-3 times of that of the crude lithium carbonate into the crude lithium carbonate, stirring the crude lithium carbonate at the temperature of 65-90 ℃ for 1-2 hours, and purifying the crude lithium carbonate for a plurality of times to obtain the high-purity lithium carbonate.
In the step 2), the temperature of hot water or hot water steam filled into the crude lithium phosphate slurry is controlled to be more than or equal to 80 ℃, so that the crude lithium phosphate slurry is fully dissolved to prepare the crude lithium phosphate solution.
The method for preparing the high-purity lithium carbonate by using the lithium phosphate is further characterized in that in the step 2), an acid clarifying agent is added to remove calcium, magnesium and aluminum impurity ions in the crude lithium phosphate solution, so as to prepare a soluble clarified lithium phosphate liquid.
Preferably, the step 3) is to add the phosphate ion remover under the pressurized state; controlling the heat preservation treatment time to be 25-40min and controlling the pH value to be 2-5.
In the method for preparing the high-purity lithium carbonate by using the lithium phosphate, the filtration in the step 4) is separation and filtration by adopting a plate frame.
The method for preparing the high-purity lithium carbonate by using the lithium phosphate comprises the step 5) of using the sodium carbonate or the flake caustic soda as the impurity removing agent, and controlling the adding amount of the sodium carbonate or the flake caustic soda to enable the impurity content in the pure lithium solution obtained after impurity removing treatment to meet the requirement of battery-grade lithium carbonate.
In the method for preparing high-purity lithium carbonate by using lithium phosphate, the lithium deposition in the step 6) adopts a lithium carbide deposition method to prepare crude lithium carbonate; and the lithium carbonate preparation is to add a sodium carbonate solution into the pure lithium solution or fill carbon dioxide gas into the pure lithium solution, and to control the reaction of preparing the crude lithium carbonate to be more than 30min under the heating and heat preservation state.
Furthermore, the adding amount of the phosphate ion remover is controlled to be equal to the amount of phosphate ion substances in the solution.
Preferably, the phosphate ion remover is a mixture of the following components in percentage by mass: 25-28% of potassium permanganate, 28-35% of ferric trichloride, 0.5-1.5% of polyacrylamide, 8-25% of polyaluminum chloride, 8-15% of potassium hypochlorite, 3-6% of potassium silicate and 7-15% of active aluminum oxide.
Preferably, the acid clarifying agent is sulfuric acid or organic acid acetic acid; the amount of the added acid clarifying agent is controlled to be equivalent to the amount of calcium, magnesium and aluminum impurity ionic substances in the crude lithium phosphate solution.
The invention discloses a method for preparing high-purity lithium carbonate by using lithium phosphate, which mainly comprises the following preparation and production processes: adding water into raw material crude lithium phosphate to prepare lithium phosphate slurry → adding organic acid and the like for stirring → clarifying liquid → adding metal ions → adjusting pH, filtering, squeezing → adding alkali → lithium-containing solution → removing impurities → adding sodium carbonate solution → heating → lithium solution → heating → crude lithium carbonate → stirring and cleaning → high-purity lithium carbonate.
Compared with the prior art, the invention has the beneficial effects that:
firstly, the method for preparing the high-purity lithium carbonate does not take the lepidolite ore as the raw material, but takes the coarse lithium phosphate which is a byproduct in industrial production as the raw material to extract the high-purity lepidolite, so that the yield of the high-purity lithium carbonate is high, and the waste of the raw material is avoided.
The method is based on the extraction process for extracting the high-purity lithium carbonate by taking the crude lithium phosphate as the raw material, and has the advantages of simple process, low production cost, less environmental pollution and important market value and social value.
Detailed Description
The technical solution of the present invention will be described in further detail with reference to specific embodiments.
Example 1
The invention discloses a method for preparing high-purity lithium carbonate by using lithium phosphate, which takes rough lithium phosphate as a raw material and adopts the following method steps:
1) mixing and stirring crude lithium phosphate and pure water, wherein the pure water can be deionized water, namely water without other impurity ions, and mixing and continuously stirring the crude lithium phosphate and the water to prepare crude lithium phosphate slurry;
2) charging hot water with the temperature of 80-90 ℃ into the crude lithium phosphate slurry, continuously and fully stirring to prepare a crude lithium phosphate solution, and then adding an acidic clarifying agent sulfuric acid solution, wherein concentrated sulfuric acid is added in the embodiment, and the adding amount of the concentrated sulfuric acid is controlled to be equivalent to the amount of calcium, magnesium and aluminum impurity ionic substances in the crude lithium phosphate solution, so that the calcium, magnesium and aluminum impurity ionic substances in the crude lithium phosphate solution can be substantially removed and dissolved to prepare a soluble clarified lithium phosphate liquid;
3) adding a phosphate radical ion remover into a soluble clarified lithium phosphate liquid, wherein the added phosphate radical ion remover comprises 25% of potassium permanganate, 29% of ferric trichloride, 1.0% of polyacrylamide, 25% of polyaluminum chloride, 10% of potassium hypochlorite, 3% of potassium silicate and 7% of active aluminum oxide by mass, controlling the removal reaction time to be 0.5h under the acidic condition of adjusting the pH of the soluble clarified lithium phosphate liquid solution to be 2.5, and after the reaction is finished, performing heat preservation treatment for 0.5h at the temperature of about 80 ℃ to obtain a phosphate mixed solution;
4) filtering, namely placing the phosphate mixed solution into a filtering device, filtering in a pressure filtering state, and performing plate and frame type squeezing filtration to obtain a lithium-containing solution;
5) adding an impurity removing agent into the lithium-containing solution, namely adding sodium carbonate serving as the impurity removing agent, and controlling the adding amount of the sodium carbonate so that the impurity content in the pure lithium solution obtained after impurity removing treatment meets the requirement of battery-grade lithium carbonate to obtain the pure lithium solution; namely, ensuring that the removal of impurity ions in the lithium-containing solution meets the quality requirement of preparing high-purity lithium carbonate;
6) preparing crude lithium carbonate, namely adding a lithium-containing solution prepared in the step 5) into a lithium carbonate preparation auxiliary agent in a heating state, wherein the lithium carbonate preparation auxiliary agent is a sodium carbonate solution, the adding amount of the sodium carbonate solution is controlled to ensure that lithium ions in the lithium-containing solution are fully converted to generate lithium carbonate, and the lithium carbonate is subjected to heat preservation treatment for 0.7h at the temperature of about 80 ℃ to obtain crude lithium carbonate;
7) preparing high-purity lithium carbonate, adding hot purified water 2-3 times of the total mass of the crude lithium carbonate prepared in the step 6), stirring at 65-90 ℃ for 1-2h, purifying for 3 times, and drying to obtain the high-purity lithium carbonate.
The high purity lithium carbonate prepared by the method of the above embodiment of the present invention is detected by relevant departments, and the main components of the high purity lithium carbonate or battery grade lithium carbonate are as follows (except the main content, the rest is ppm) through detection and analysis, and is shown in table 1.
TABLE 1
Description of the drawings: the high purity lithium carbonate product prepared by the method of the invention has a height of more than 99.5 percent and low content of other impurities.
Example 2
The parts not described in this example are the same as those in example 1.
The invention discloses a method for preparing high-purity lithium carbonate by using lithium phosphate, which takes rough lithium phosphate as a raw material and adopts the following method steps:
1) mixing and stirring crude lithium phosphate and pure water, wherein the pure water can be deionized water, namely water without other impurity ions, and mixing and continuously stirring the crude lithium phosphate and the water to prepare crude lithium phosphate slurry;
2) charging hot water with the temperature of 60-75 ℃ into the crude lithium phosphate slurry, continuously and fully stirring to prepare a crude lithium phosphate solution, then adding an acidic clarifier acetic acid solution, controlling the addition amount of the acetic acid to be equivalent to the amount of calcium, magnesium and aluminum impurity ionic substances in the crude lithium phosphate solution, and roughly removing the calcium, magnesium and aluminum impurity ionic substances in the crude lithium phosphate solution to prepare a soluble clarified lithium phosphate liquid by dissolution;
3) adding a phosphate radical ion remover into a soluble clarified lithium phosphate liquid, wherein the added phosphate radical ion remover comprises 25% of potassium permanganate, 29.5% of ferric trichloride, 0.5% of polyacrylamide, 20% of polyaluminium chloride, 13% of potassium hypochlorite, 3% of potassium silicate and 9% of active aluminum oxide by mass, controlling the removal reaction time to be 1.5h under the acidic condition of adjusting the pH of the soluble clarified lithium phosphate liquid solution to be 3.5, heating the solution at the temperature of about 80 ℃ after the reaction is finished, and performing heat preservation treatment for 1h to obtain a phosphate mixed solution;
4) filtering, namely placing the phosphate mixed solution into a filtering device, filtering in a pressure filtering state, and performing plate and frame type squeezing filtration to obtain a lithium-containing solution;
5) adding an impurity removing agent into the lithium-containing solution, namely adding impurity removing agent flake caustic soda, namely solid sodium hydroxide, and controlling the addition amount of the flake caustic soda to ensure that the impurity content in the pure lithium solution obtained after impurity removal treatment meets the requirement of battery-grade lithium carbonate to obtain the pure lithium solution; namely, ensuring that the removal of impurity ions in the lithium-containing solution meets the quality requirement of preparing high-purity lithium carbonate or battery-grade lithium carbonate;
6) preparing crude lithium carbonate, namely adding a lithium carbonate preparation auxiliary agent into the lithium-containing solution prepared in the step 5) in a heating state, wherein the lithium carbonate preparation auxiliary agent is carbon dioxide gas, the amount of the carbon dioxide gas is controlled to ensure that lithium ions in the lithium-containing solution are fully converted to generate lithium carbonate, and the lithium carbonate is subjected to heat preservation treatment for 1.5 hours at the temperature of about 65 ℃ to obtain crude lithium carbonate;
7) preparing high-purity lithium carbonate, adding hot purified water 2-3 times of the total mass of the crude lithium carbonate prepared in the step 6), stirring at 80-90 ℃ for 1-2h, purifying for 4 times, and drying to obtain the high-purity lithium carbonate.
The high purity lithium carbonate prepared by the method of the above embodiment of the present invention is detected by relevant departments, and the main components of the high purity lithium carbonate or battery grade lithium carbonate are as follows (except the main content, the rest is ppm) through detection and analysis, and is shown in table 2.
TABLE 2
Description of the drawings: the high purity lithium carbonate product prepared by the method of the invention has a height of more than 99.8 percent and low content of other impurities.
Example 3
The invention discloses a method for preparing high-purity lithium carbonate by using lithium phosphate, which takes rough lithium phosphate as a raw material and adopts the following method steps:
1) mixing and stirring crude lithium phosphate and pure water, wherein the pure water can be deionized water, namely water without other impurity ions, and mixing and continuously stirring the crude lithium phosphate and the water to prepare crude lithium phosphate slurry;
2) charging hot water with the temperature of 80-90 ℃ into the crude lithium phosphate slurry, continuously and fully stirring to prepare a crude lithium phosphate solution, and then adding an acidic clarifying agent sulfuric acid solution, wherein concentrated sulfuric acid is added in the embodiment, and the adding amount of the concentrated sulfuric acid is controlled to be equivalent to the amount of calcium, magnesium and aluminum impurity ionic substances in the crude lithium phosphate solution, so that the calcium, magnesium and aluminum impurity ionic substances in the crude lithium phosphate solution can be substantially removed and dissolved to prepare a soluble clarified lithium phosphate liquid;
3) adding a phosphate radical ion remover into a soluble clarified lithium phosphate liquid, wherein the added phosphate radical ion remover comprises 26% of potassium permanganate, 28% of ferric trichloride, 1.5% of polyacrylamide, 24.5% of polyaluminum chloride, 9% of potassium hypochlorite, 3% of potassium silicate and 8% of active aluminum oxide by mass, controlling the removal reaction time to be 0.5h under the acidic condition of adjusting the pH of the soluble clarified lithium phosphate liquid solution to be 4.5, and after the reaction is finished, performing heat preservation treatment for 0.5h at the temperature of about 80 ℃ to obtain a phosphate mixed solution;
4) filtering, namely placing the phosphate mixed solution into a filtering device, filtering in a pressure filtering state, and performing plate and frame type squeezing filtration to obtain a lithium-containing solution;
5) adding an impurity removing agent into the lithium-containing solution, namely adding sodium carbonate serving as the impurity removing agent, and controlling the adding amount of the sodium carbonate so that the impurity content in the pure lithium solution obtained after impurity removing treatment meets the requirement of battery-grade lithium carbonate to obtain the pure lithium solution; namely, ensuring that the removal of impurity ions in the lithium-containing solution meets the quality requirement of preparing high-purity lithium carbonate;
6) preparing crude lithium carbonate, namely adding a lithium-containing solution prepared in the step 5) into a lithium carbonate preparation auxiliary agent in a heating state, wherein the lithium carbonate preparation auxiliary agent is a sodium carbonate solution, the adding amount of the sodium carbonate solution is controlled to ensure that lithium ions in the lithium-containing solution are fully converted to generate lithium carbonate, and the lithium carbonate is subjected to heat preservation treatment for 0.6h at the temperature of about 80 ℃ to obtain crude lithium carbonate;
7) preparing high-purity lithium carbonate, adding hot purified water 2-3 times of the total mass of the crude lithium carbonate prepared in the step 6), stirring at 75-90 ℃ for 1-2h, purifying for 2 times, and drying to obtain the high-purity lithium carbonate.
The high purity lithium carbonate prepared by the method of the above embodiment of the present invention is detected by relevant departments, and the main components of the high purity lithium carbonate or battery grade lithium carbonate are as follows (except the main content, the rest is ppm) through detection and analysis, and is shown in table 3.
TABLE 3
Description of the drawings: the high purity lithium carbonate product prepared by the method of the invention has a height of more than 99.8 percent and low content of other impurities.
Example 4
The parts not described in this example are the same as those in example 1.
The invention discloses a method for preparing high-purity lithium carbonate by using lithium phosphate, which takes rough lithium phosphate as a raw material and adopts the following method steps:
1) mixing and stirring crude lithium phosphate and pure water, wherein the pure water can be deionized water, namely water without other impurity ions, and mixing and continuously stirring the crude lithium phosphate and the water to prepare crude lithium phosphate slurry;
2) charging hot water with the temperature of 60-75 ℃ into the crude lithium phosphate slurry, continuously and fully stirring to prepare a crude lithium phosphate solution, then adding an acidic clarifier acetic acid solution, controlling the addition amount of the acetic acid to be equivalent to the amount of calcium, magnesium and aluminum impurity ionic substances in the crude lithium phosphate solution, and roughly removing the calcium, magnesium and aluminum impurity ionic substances in the crude lithium phosphate solution to prepare a soluble clarified lithium phosphate liquid by dissolution;
3) adding a phosphate radical ion remover into a soluble clarified lithium phosphate liquid, wherein the added phosphate radical ion remover comprises 26% of potassium permanganate, 28% of ferric trichloride, 1.0% of polyacrylamide, 15% of polyaluminum chloride, 13% of potassium hypochlorite, 5% of potassium silicate and 12% of active aluminum oxide by mass, controlling the removal reaction time to be 1.0h under the acidic condition of adjusting the pH of the soluble clarified lithium phosphate liquid solution to be 2.5, heating the solution at the temperature of about 80 ℃ after the reaction is finished, and performing heat preservation treatment for 1h to obtain a phosphate mixed solution;
4) filtering, namely placing the phosphate mixed solution into a filtering device, filtering in a pressure filtering state, and performing plate and frame type squeezing filtration to obtain a lithium-containing solution;
5) adding an impurity removing agent into the lithium-containing solution, namely adding impurity removing agent flake caustic soda, namely solid sodium hydroxide, and controlling the addition amount of the flake caustic soda to ensure that the impurity content in the pure lithium solution obtained after impurity removal treatment meets the requirement of battery-grade lithium carbonate to obtain the pure lithium solution; namely, ensuring that the removal of impurity ions in the lithium-containing solution meets the quality requirement of preparing high-purity lithium carbonate or battery-grade lithium carbonate;
6) preparing crude lithium carbonate, namely adding a lithium carbonate preparation auxiliary agent into the lithium-containing solution prepared in the step 5) in a heating state, wherein the lithium carbonate preparation auxiliary agent is carbon dioxide gas, the amount of the carbon dioxide gas is controlled to ensure that lithium ions in the lithium-containing solution are fully converted to generate lithium carbonate, and the lithium carbonate is subjected to heat preservation treatment for 1.5 hours at the temperature of about 65 ℃ to obtain crude lithium carbonate;
7) preparing high-purity lithium carbonate, adding hot purified water 2-3 times of the total mass of the crude lithium carbonate prepared in the step 6), stirring at 80-90 ℃ for 1-2h, purifying for 4 times, and drying to obtain the high-purity lithium carbonate.
The high purity lithium carbonate prepared by the method of the above embodiment of the present invention is detected by relevant departments, and the main components of the high purity lithium carbonate or battery grade lithium carbonate are as follows (except the main content, the rest units are ppm) through detection and analysis, and is shown in table 4.
TABLE 4
Description of the drawings: the high purity lithium carbonate product prepared by the method of the invention has a height of more than 99.5 percent and low content of other impurities.
By adopting the lithium carbonate extraction process provided by the embodiment of the invention, the prepared battery-grade lithium carbonate has high purity, and the waste of raw materials is avoided. The lithium carbonate extraction process based on crude lithium phosphate as the raw material has the advantages of simple process, less environmental pollution and important market value and social value.
Technical features not described in the present invention may be implemented by or using the prior art, and are not described herein again. Of course, what should be noted is: the above technical solutions disclosed in the present invention are not limited thereto; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention, and they should be construed as being included in the following claims and description.
Claims (10)
1. A method for preparing high-purity lithium carbonate by using crude lithium phosphate takes the crude lithium phosphate as a raw material, and is characterized by comprising the following steps:
1) mixing and stirring the crude lithium phosphate and pure water to obtain crude lithium phosphate slurry;
2) filling hot water or hot water vapor into the crude lithium phosphate slurry to prepare a crude lithium phosphate solution, and then adding an acid clarifying agent to dissolve the crude lithium phosphate solution to prepare a soluble clarified lithium phosphate liquid;
3) adding a phosphate radical ion remover into a soluble clear lithium phosphate liquid, adjusting the pH of the solution to be under an acidic condition, controlling the removal reaction time to be 0.5-2h, and after the reaction is finished, performing heat preservation treatment and filtering to obtain a phosphate mixed solution;
4) filter pressing, namely putting the phosphate mixed solution into a filter device, and filtering under a pressure filtering state to obtain a lithium-containing solution;
5) adding an impurity removing agent into the lithium-containing solution, and performing impurity removing treatment to obtain a pure lithium solution;
6) preparing coarse lithium carbonate, adding a lithium carbonate preparation auxiliary agent into the pure lithium solution in the previous step in a heating state, and performing a coarse lithium carbonate preparation reaction to obtain coarse lithium carbonate;
7) preparing high-purity lithium carbonate, adding hot purified water with the mass 2-3 times of that of the crude lithium carbonate into the crude lithium carbonate, stirring the crude lithium carbonate at the temperature of 65-90 ℃ for 1-2 hours, and purifying the crude lithium carbonate for a plurality of times to obtain the high-purity lithium carbonate.
2. The method for preparing high-purity lithium carbonate by using crude lithium phosphate as claimed in claim 1, wherein in the step 2), the temperature of hot water or hot water vapor filled in the crude lithium phosphate slurry is controlled to be not less than 80 ℃, so that the crude lithium phosphate slurry is fully dissolved to prepare the crude lithium phosphate solution.
3. The method for preparing high-purity lithium carbonate by using crude lithium phosphate as claimed in claim 1, wherein in the step 2), an acid clarifying agent is added to remove calcium, magnesium and aluminum impurity ions in the crude lithium phosphate solution, so as to prepare a soluble clarified lithium phosphate liquid.
4. The method for preparing high-purity lithium carbonate by using crude lithium phosphate as claimed in claim 1, wherein the step 3) is to add a phosphate ion remover under a pressurized state; controlling the heat preservation treatment time to be 25-40min and controlling the pH value to be 2-5.
5. The method for preparing high-purity lithium carbonate by using lithium phosphate as claimed in claim 1, wherein the method is characterized in that the lithium phosphate obtained in the step 4) is used
The filtration is plate-frame separation filtration.
6. The method for preparing high-purity lithium carbonate by using crude lithium phosphate according to claim 1, wherein the impurity removing agent in the step 5) is soda ash or flake caustic soda, and the addition amount of the soda ash or flake caustic soda is controlled so that the impurity content in the pure lithium solution obtained after impurity removal treatment meets the requirement of battery-grade lithium carbonate.
7. The method for preparing high-purity lithium carbonate by using crude lithium phosphate according to claim 1, wherein the lithium precipitation in the step 6) is performed by a lithium carbide precipitation method to prepare crude lithium carbonate; and the lithium carbonate preparation is to add a sodium carbonate solution into the pure lithium solution or fill carbon dioxide gas into the pure lithium solution, and to control the reaction of preparing the crude lithium carbonate to be more than 30min under the heating and heat preservation state.
8. The method for preparing high-purity lithium carbonate from crude lithium phosphate as claimed in claim 1 or 4, wherein the amount of the phosphate ion removing agent added is controlled to be equivalent to the amount of the phosphate ion material in the solution.
9. The method for preparing high-purity lithium carbonate by using crude lithium phosphate as claimed in claim 1 or 4, wherein the phosphate ion remover is a mixture of the following components in percentage by mass: 25-28% of potassium permanganate, 28-35% of ferric trichloride, 0.5-1.5% of polyacrylamide, 8-25% of polyaluminum chloride, 8-15% of potassium hypochlorite, 3-6% of potassium silicate and 7-15% of active aluminum oxide.
10. The method for preparing high-purity lithium carbonate by using crude lithium phosphate according to claim 1 or 4, wherein the acid clarifying agent is sulfuric acid or organic acid acetic acid; the amount of the added acid clarifying agent is controlled to be equivalent to the amount of calcium, magnesium and aluminum impurity ionic substances in the crude lithium phosphate solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911108142.9A CN110759364A (en) | 2019-11-13 | 2019-11-13 | Method for preparing high-purity lithium carbonate by using crude lithium phosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911108142.9A CN110759364A (en) | 2019-11-13 | 2019-11-13 | Method for preparing high-purity lithium carbonate by using crude lithium phosphate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110759364A true CN110759364A (en) | 2020-02-07 |
Family
ID=69337633
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911108142.9A Pending CN110759364A (en) | 2019-11-13 | 2019-11-13 | Method for preparing high-purity lithium carbonate by using crude lithium phosphate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110759364A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112357938A (en) * | 2020-11-12 | 2021-02-12 | 萍乡市拓源实业有限公司 | Method for preparing battery-grade lithium carbonate by using lithium phosphate |
| CN114318937A (en) * | 2020-09-27 | 2022-04-12 | 牡丹江市海洋新材料科技有限责任公司 | Novel method for combined use of soluble silicate, polyaluminium chloride and flocculant in multiple fields |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1843961A (en) * | 2006-05-19 | 2006-10-11 | 北京工业大学 | Composite dephosphorizing coagulant dedicated for drinking water |
| CN105018814A (en) * | 2014-08-21 | 2015-11-04 | 太仓钧浩自行车科技有限公司 | Tungsten-molybdenum alloy and preparation method thereof |
| CN106745099A (en) * | 2016-12-05 | 2017-05-31 | 天津二八科技股份有限公司 | A kind of method that utilization lithium phosphate prepares lithium carbonate |
| KR20180074177A (en) * | 2016-12-23 | 2018-07-03 | 주식회사 포스코 | Method for manufacturing lithium hydroxide and lithium carbonate |
| CN108285156A (en) * | 2017-11-24 | 2018-07-17 | 中南大学 | A method of extracting pure Lithium Carbonate or lithium hydroxide from phosphoric acid lithium waste residue |
| CN108675323A (en) * | 2018-05-23 | 2018-10-19 | 赣州有色冶金研究所 | A kind of method that low-grade lithium phosphate acidic conversion method prepares battery carbon acid lithium |
| CN108862335A (en) * | 2018-07-20 | 2018-11-23 | 上海中锂实业有限公司 | A method of lithium carbonate is prepared with lithium phosphate |
| CN110127731A (en) * | 2019-05-15 | 2019-08-16 | 上海中锂实业有限公司 | A method of battery-level lithium carbonate is directly prepared by lithium phosphate |
-
2019
- 2019-11-13 CN CN201911108142.9A patent/CN110759364A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1843961A (en) * | 2006-05-19 | 2006-10-11 | 北京工业大学 | Composite dephosphorizing coagulant dedicated for drinking water |
| CN105018814A (en) * | 2014-08-21 | 2015-11-04 | 太仓钧浩自行车科技有限公司 | Tungsten-molybdenum alloy and preparation method thereof |
| CN106745099A (en) * | 2016-12-05 | 2017-05-31 | 天津二八科技股份有限公司 | A kind of method that utilization lithium phosphate prepares lithium carbonate |
| KR20180074177A (en) * | 2016-12-23 | 2018-07-03 | 주식회사 포스코 | Method for manufacturing lithium hydroxide and lithium carbonate |
| CN108285156A (en) * | 2017-11-24 | 2018-07-17 | 中南大学 | A method of extracting pure Lithium Carbonate or lithium hydroxide from phosphoric acid lithium waste residue |
| CN108675323A (en) * | 2018-05-23 | 2018-10-19 | 赣州有色冶金研究所 | A kind of method that low-grade lithium phosphate acidic conversion method prepares battery carbon acid lithium |
| CN108862335A (en) * | 2018-07-20 | 2018-11-23 | 上海中锂实业有限公司 | A method of lithium carbonate is prepared with lithium phosphate |
| CN110127731A (en) * | 2019-05-15 | 2019-08-16 | 上海中锂实业有限公司 | A method of battery-level lithium carbonate is directly prepared by lithium phosphate |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114318937A (en) * | 2020-09-27 | 2022-04-12 | 牡丹江市海洋新材料科技有限责任公司 | Novel method for combined use of soluble silicate, polyaluminium chloride and flocculant in multiple fields |
| CN112357938A (en) * | 2020-11-12 | 2021-02-12 | 萍乡市拓源实业有限公司 | Method for preparing battery-grade lithium carbonate by using lithium phosphate |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN113737018A (en) | Method for recovering anode raw material of waste battery | |
| CN109650415B (en) | Method for extracting lithium carbonate from scrapped lithium iron phosphate battery positive electrode powder | |
| CN108075202A (en) | A kind of comprehensive recovering process of lithium iron phosphate positive material | |
| CN110885090A (en) | Method for preparing battery-grade lithium carbonate by using lepidolite as raw material through one-step method | |
| CN107098365B (en) | A method of extracting lithium carbonate from lepidolite ore | |
| CN115216645B (en) | Method for extracting lithium from electrolytic aluminum waste residue by mixed salt calcination | |
| CN101899576A (en) | Method for recycling lead from lead-acid battery paste | |
| CN109167118B (en) | Comprehensive utilization method of lithium iron phosphate battery electrode material | |
| CN105036159A (en) | Method for preparing lithium carbonate with high-lithium salt lake bittern | |
| CN115287469B (en) | Method for selectively extracting lithium from clay-type lithium ore | |
| CN108946772A (en) | A method of pure Lithium Carbonate is prepared by lithium ore | |
| CN113511663A (en) | Process for preparing lithium carbonate by extracting lithium from oil field underground brine | |
| CN110759364A (en) | Method for preparing high-purity lithium carbonate by using crude lithium phosphate | |
| CN113955775B (en) | Method for extracting lithium carbonate from lithium-rich clay by acid-base combined method | |
| CN110592383A (en) | Method for extracting lithium from fly ash by adsorption method | |
| CN116814957A (en) | Method for synchronously decyanating overhaul slag and extracting lithium | |
| CN115246651B (en) | Method for preparing lithium carbonate by recovering fluorine-containing lithium tailings | |
| CN111592017A (en) | Method for preparing battery-grade lithium chloride by pressing and soaking spodumene | |
| CN110407236B (en) | Preparation method of electric automobile-grade lithium carbonate | |
| CN103103351A (en) | Method for preparing high-purity calcium carbonate for saponifying rare earth extraction agent | |
| WO2018072547A1 (en) | Method of recovering indium from liquid crystal-containing indium concentrate | |
| CN117327923B (en) | Method for jointly extracting lithium from waste aluminum electrolyte and overhaul slag | |
| CN113044866B (en) | Method for preparing aluminum sulfate from aluminum-containing acid treatment liquid | |
| CN111498872B (en) | Lithium phosphate recycling process | |
| CN114231741B (en) | Method for selectively separating lithium from potassium |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200207 |
|
| RJ01 | Rejection of invention patent application after publication |