CN114590825A - Purification method and purification equipment for sodium-containing lithium chloride - Google Patents
Purification method and purification equipment for sodium-containing lithium chloride Download PDFInfo
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- CN114590825A CN114590825A CN202210192269.9A CN202210192269A CN114590825A CN 114590825 A CN114590825 A CN 114590825A CN 202210192269 A CN202210192269 A CN 202210192269A CN 114590825 A CN114590825 A CN 114590825A
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- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 title claims abstract description 240
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 title claims abstract description 54
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 54
- 239000011734 sodium Substances 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 44
- 238000000746 purification Methods 0.000 title abstract description 27
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims abstract description 67
- 238000001816 cooling Methods 0.000 claims abstract description 44
- 239000000463 material Substances 0.000 claims abstract description 28
- 238000001035 drying Methods 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 17
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 239000012452 mother liquor Substances 0.000 claims description 32
- 238000000926 separation method Methods 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 13
- 238000011084 recovery Methods 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 8
- 238000004064 recycling Methods 0.000 claims description 5
- 230000008569 process Effects 0.000 abstract description 9
- 239000003960 organic solvent Substances 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 44
- 239000011780 sodium chloride Substances 0.000 description 22
- 230000032683 aging Effects 0.000 description 7
- 238000002425 crystallisation Methods 0.000 description 7
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 6
- 230000001376 precipitating effect Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
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
- C01D15/04—Halides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0004—Crystallisation cooling by heat exchange
- B01D9/0013—Crystallisation cooling by heat exchange by indirect heat exchange
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention belongs to the technical field of lithium chloride purification, and mainly discloses lake purification equipment for a sodium-containing lithium chloride purification method, wherein the sodium-containing lithium chloride purification method comprises the following steps: s1: adding a certain amount of sodium-containing lithium chloride into N-methylpyrrolidone, heating to 90-200 ℃, stirring for dissolving, and filtering while hot to obtain a first purified solution; s2: and cooling the first purified solution to-15-30 ℃, crystallizing, separating out, separating to obtain a lithium chloride wet material, and drying to obtain a lithium chloride product. The method provided by the invention has the advantages of simple operation, few process steps, lower temperature and lower energy consumption, the organic solvent NMP is recycled in the process, the environment is not polluted, no auxiliary material is added in the purification process, the production cost is low, and the product is not polluted.
Description
Technical Field
The invention relates to the technical field of lithium chloride purification, in particular to a method and equipment for purifying lithium chloride containing sodium.
Background
The lithium chloride in salt lake and the lithium chloride recovered from waste materials often contain high-content sodium chloride impurities. The general purification methods include a thermal concentration crystallization method, a cooling crystallization method, an extraction method, and the like, and these methods have respective drawbacks.
Wherein, the thermal concentration crystallization method comprises the following steps: and (3) concentrating the lithium chloride solution containing sodium chloride until the solution is supersaturated, separating out the sodium chloride before the lithium chloride is crystallized by utilizing the same ion effect, and separating to remove the sodium chloride. The method is extremely difficult to control the concentration of precipitated sodium chloride, and sodium chloride and lithium chloride are precipitated simultaneously when the concentration is higher, the final removal effect of sodium chloride is very poor, and the obtained product cannot meet the standard requirement of industrial-grade lithium chloride; cooling crystallization method: adding lithium hydroxide into the supersaturated solution after concentration, precipitating sodium chloride under a freezing condition, and separating and removing the sodium chloride. The method has the advantages of thorough precipitation of sodium chloride and capability of obtaining industrial-grade lithium chloride. But also has the problems of higher energy consumption and high cost of adding lithium hydroxide; extraction-back extraction method: dissolving and extracting the lithium chloride by using an alcohol extractant, evaporating and separating to obtain a lithium chloride product. The method has good effect, can obtain purer lithium chloride products, and can also be used for producing battery-grade lithium chloride products. However, when the alcohol extractant is evaporated to dryness, a large amount of energy is consumed, a large amount of flammable and explosive organic gas is generated, the safety risk is great, and the risk of environmental pollution also exists.
In conclusion, the research personnel in the field need to provide a method for purifying lithium chloride with high efficiency, low cost and little pollution.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention mainly aims to provide a method for purifying sodium-containing lithium chloride, which has the advantages of simple operation, low process temperature, safe process, no environmental pollution, high lithium chloride yield and the like.
It is still another object of the present invention to provide a purification apparatus suitable for the above purification method.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for purifying sodium-containing lithium chloride comprises the following steps:
s1: adding a certain amount of sodium-containing lithium chloride into N-methylpyrrolidone (NMP), heating to 90-200 ℃, stirring for dissolving, and filtering while hot to obtain a first purified solution;
s2: and cooling the first purified solution to-15-30 ℃, crystallizing, separating out, separating to obtain a wet lithium chloride material, and drying to obtain a lithium chloride product.
Further, in the step S1, the solid-liquid mass ratio of the sodium-containing lithium chloride to the NMP is (15-30) to 100.
Further, the stirring and dissolving in the step S1 is stirring for 1-6 hours at the temperature of 90-200 ℃.
Further, in the step S2, the first purified solution is cooled at a cooling rate of 0.5-5 ℃/min.
Further, aging for 0.5-3 h after crystallization in the step S2.
Further, the separation in the step S2 may be performed by centrifugation.
Further, the lithium chloride wet material in the step S2 is dried at the temperature of 200-300 ℃.
Further, the NMP mother liquor separated and dried in the step S2 can be recycled after being collected in the step S1
Further, the difference between the heating temperature in the step S1 and the cooling temperature in the step S2 should be greater than or equal to 100 ℃.
The invention also provides a sodium-containing lithium chloride purification device, which comprises: the device comprises a dissolving separation component, a cooling separation component and a drying recovery component;
the dissolving and separating component comprises a powder bin, a dissolving kettle, a first conveying pump and a filter, wherein the powder bin, the dissolving kettle, the first conveying pump and the filter are communicated in sequence;
the cooling separation assembly comprises a cooling kettle and a centrifugal separation device, the cooling kettle is communicated with the filter, and the centrifugal separation device is communicated with the cooling kettle;
the dry subassembly of retrieving includes desiccator, cooler, NMP mother liquor jar and second delivery pump, the desiccator with the centrifuge intercommunication is followed the centrifuge receives solid-state separation thing, NMP mother liquor jar with the centrifuge intercommunication is followed the centrifuge receives liquid separation thing, the desiccator passes through the cooler with NMP mother liquor jar intercommunication, NMP mother liquor jar passes through the second delivery pump with dissolve the cauldron intercommunication.
Compared with the prior art, the invention has the following advantages:
1. the purification method of the sodium-containing lithium chloride has the advantages of simple operation, few process steps, lower temperature and lower energy consumption.
2. The organic solvent NMP adopted by the invention is in a liquid state in the process, the explosion risk is low, and the organic solvent NMP is recycled in the process, so that the environment is not polluted.
3. The invention does not need to add any auxiliary materials in the purification process, has low production cost and no pollution to products.
4. The method provided by the invention can be used for treating lithium chloride containing any amount of sodium chloride, and the sodium content in the finally obtained lithium chloride product is less than 200ppm and far lower than the requirement that the sodium content in national standard level 1 of industrial-grade lithium chloride is less than 2500 ppm.
Drawings
FIG. 1 is a process flow diagram of the purification method of lithium chloride containing sodium provided by the present invention.
Fig. 2 is a schematic structural diagram of a sodium-containing lithium chloride purification apparatus provided by the present invention.
Detailed Description
The present invention will be described in further detail below with reference to specific embodiments and examples in conjunction with the accompanying drawings, but the embodiments of the present invention are not limited thereto. All the raw materials and reagents used in the present invention are commercially available raw materials and reagents, unless otherwise specified. In the examples, the components are used in g and mL in parts by mass.
A method for purifying sodium-containing lithium chloride comprises the following steps:
s1: adding a certain amount of sodium-containing lithium chloride into N-methylpyrrolidone (NMP), heating to 90-200 ℃, stirring for dissolving, and filtering while hot to obtain a first purified solution;
s2: and cooling the first purified solution to-15-30 ℃, crystallizing, separating out, separating to obtain a lithium chloride wet material, and drying to obtain a lithium chloride product.
Referring to FIG. 1, a process flow diagram of a method for purifying lithium chloride containing sodium according to the present invention is shown.
In the method, sodium chloride is separated and removed by a method of high-temperature dissolution and low-temperature crystallization, utilizing the property that lithium chloride has a much higher solubility in NMP than sodium chloride and has a greatly variable solubility with temperature. For example, lithium chloride has a solubility in NMP (N-methylpyrrolidone) of 8g and sodium chloride has a solubility of 0.016g at 25 ℃; at 95 ℃, the solubility of lithium chloride in NMP is 15g, and the solubility of sodium chloride is 0.017 g; at 200 ℃, the solubility of lithium chloride in NMP is 30g, the solubility of sodium chloride still has no obvious change, and NMP is a relatively stable organic solvent with the boiling point of 202 ℃ under normal pressure. Therefore, the lithium chloride and the sodium chloride are separated by the solubility difference of the lithium chloride and the sodium chloride in the NMP, and the NMP can be recycled, so that the method has the advantages of no environmental pollution, high lithium chloride yield, low cost and the like.
S1: adding a certain amount of sodium-containing lithium chloride into N-methylpyrrolidone (NMP), heating to 90-200 ℃, stirring for dissolving, and filtering while hot to obtain a first purified solution.
The solid-liquid mass ratio of the sodium-containing lithium chloride to the NMP is (15-30) to 100, so that the sodium-containing lithium chloride can be in a supersaturated state in the NMP to improve the purification efficiency, and the sodium-containing lithium chloride is dry sodium-containing lithium chloride, so that the NMP mother liquor is not polluted by water, and the solubility of the sodium chloride in a solution system can be further reduced, so that the purity of a final lithium chloride product is improved. The stirring and dissolving process includes stirring at 90-200 ℃ for 1-6 hours, and filtering while hot to obtain the first purification solution, so that lithium chloride in the sodium-containing lithium chloride is fully dissolved in the NMP mother liquor, most of sodium chloride is not dissolved at the temperature, and the first purification of the sodium-containing lithium chloride is realized.
S2: and cooling the first purified solution to-15-30 ℃, crystallizing, separating out, separating to obtain a lithium chloride wet material, and drying to obtain a lithium chloride product.
When the first purified solution is cooled to-15 to 30 ℃, the solubility of sodium chloride in the solution does not change greatly at the temperature, and the sodium chloride is not precipitated, but the solubility of lithium chloride is sharply reduced, so that crystallization is precipitated, and thus the second purification of lithium chloride containing sodium is completed, and after cooling to-15 to 30 ℃, lithium chloride is crystallized at the temperature, and aging is performed for 0.5 to 3 hours, so that the purity of precipitated lithium chloride crystals can be further improved.
Further, the first purification solution is cooled at a cooling rate of 0.5-5 ℃/min, and the constant cooling rate is kept, so that the growth and the purity improvement of lithium chloride crystals are facilitated, for example, the cooling rate can be 1 ℃/min, 2 ℃/min, 3 ℃/min and 4 ℃/min.
Further, the separation can be performed by centrifugal separation, and after the centrifugal separation, the lithium chloride wet material and the NMP mother liquor are obtained respectively, wherein the NMP mother liquor can be returned to the step S1 for recycling after being collected.
Further, the lithium chloride wet material is dried at the temperature of 200-300 ℃, and NMP generated by drying is evaporated into a cooler and condensed into NMP liquid, and then the NMP liquid can be returned to the step S1 for recycling. Wherein, the wet lithium chloride material can be dried by adopting a disc drier or an electrothermal kiln. In this way, the NMP solvent remaining on the lithium chloride can be removed, and the NMP solvent can be recycled.
Further, the difference between the heating temperature in the step S1 and the cooling temperature in the step S2 should be greater than or equal to 100 ℃, and the applicant found that ensuring a certain temperature difference can improve the purity and recovery rate of lithium chloride.
Referring to fig. 2, the present invention further provides a sodium-containing lithium chloride purifying apparatus 10, where the sodium-containing lithium chloride purifying apparatus 10 includes: a dissolution separation module 100, a cooling separation module 200, and a drying recovery module 300;
the dissolving and separating assembly 100 comprises a powder bin 110, a dissolving kettle 120, a first conveying pump 130 and a filter 140, wherein the powder bin 110, the dissolving kettle 120, the first conveying pump 130 and the filter 140 are communicated in sequence;
the cooling and separating assembly 200 comprises a cooling kettle 210 and a centrifugal separator 220, wherein the cooling kettle 210 is communicated with the filter 140, and the centrifugal separator 220 is communicated with the cooling kettle 210;
the drying and recovering module 300 includes a dryer 310, a cooler 320, an NMP mother liquor tank 330, and a second transfer pump 340, wherein the dryer 310 communicates with the centrifuge 220 to receive the solid separated material from the centrifuge 220, the NMP mother liquor tank 330 communicates with the centrifuge 220 to receive the liquid separated material from the centrifuge 220, the dryer 310 communicates with the NMP mother liquor tank 330 through the cooler 320, and the NMP mother liquor tank 330 communicates with the dissolving tank 120 through the second transfer pump 340.
The operation steps of the sodium-containing lithium chloride purifying device 10 are as follows:
s100: conveying the dried sodium-containing lithium chloride material into a powder bin 110;
s200: adding the sodium-containing lithium chloride material in the powder bin 110 into a dissolving kettle 120 containing an NMP solution according to the solid-liquid mass ratio of (15-30) to 100, starting stirring and heating, and stirring for 1-6 h at the temperature of 90-200 ℃. Obtaining NMP mother liquor;
s300: starting a first transfer pump to transfer the NMP mother liquor in the dissolving kettle 120 to a filter 140 for filtering to obtain a first purified solution;
s400: conveying the first purified solution into a cooling kettle 210, starting cooling, cooling to-15-30 ℃, and crystallizing to obtain a solid-liquid mixture;
s500: the solid-liquid mixture is conveyed to a centrifugal separator 220 for separation, the liquid is conveyed to an NMP mother liquor tank 330, and the lithium chloride wet material is conveyed to a dryer 310;
s600: starting the drying function of the dryer 310 to dry the lithium chloride wet material, and recycling the steam generated by drying into the NMP mother liquor tank 330 through the cooler 320;
s700, according to the use condition, a second transmission pump is started, and the NMP mother liquor collected in the NMP mother liquor tank 330 is conveyed back to the dissolving kettle 120 for recycling.
The following is a detailed description.
Example 1
S1: adding 15 parts by mass of sodium-containing lithium chloride into 100 parts by mass of NMP solution, stirring for 2 hours at 95 ℃, and filtering while the solution is hot to obtain a first purified solution;
s2: and cooling the first purified solution to-15 ℃ at a cooling speed of 1 ℃/min, crystallizing, precipitating, aging for 2 hours, separating to obtain a lithium chloride wet material, and drying the lithium chloride wet material at 250 ℃ to obtain a lithium chloride product.
S3: the NMP mother liquor separated and dried in the S2 step was collected, and the NMP mother liquor was reused in the S1 step.
Example 2
S1: adding 30 parts by mass of sodium-containing lithium chloride into 100 parts by mass of NMP solution, stirring for 1h at 200 ℃, and filtering while hot to obtain a first purified solution;
s2: and cooling the first purified solution to 30 ℃ at a cooling speed of 3 ℃/min, crystallizing, precipitating, aging for 1h, separating to obtain a wet lithium chloride material, and drying the wet lithium chloride material at 250 ℃ to obtain a lithium chloride product.
S3: the NMP mother liquor separated and dried in the S2 step was collected and reused in the S1 step.
Example 3
S1: adding 20 parts by mass of sodium-containing lithium chloride into 100 parts by mass of NMP solution, stirring for 6 hours at 150 ℃, and filtering while hot to obtain a first purified solution;
s2: and cooling the first purified solution to 0 ℃ at the cooling speed of 2 ℃/min, crystallizing, aging for 3 hours, separating to obtain a wet lithium chloride material, and drying to obtain a lithium chloride product.
S3: the NMP mother liquor separated and dried in the S2 step was collected and reused in the S1 step.
Example 4
S1: adding 15 parts by mass of sodium-containing lithium chloride into 100 parts by mass of NMP solution, stirring for 2 hours at 95 ℃, and filtering while the solution is hot to obtain a first purified solution;
s2: cooling the first purified solution to 30 ℃, crystallizing, precipitating, aging for 2 hours, separating to obtain a lithium chloride wet material, and drying the lithium chloride wet material at 250 ℃ to obtain a lithium chloride product;
s3: the NMP mother liquor separated and dried in the S2 step was collected, and the NMP mother liquor was reused in the S1 step.
Comparative example 1
S1: adding 15 parts by mass of sodium-containing lithium chloride into 100 parts by mass of NMP solution, stirring for 2 hours at 80 ℃, and filtering while the solution is hot to obtain a first purified solution;
s2: and cooling the first purified solution to 30 ℃, crystallizing, precipitating, aging for 2 hours, separating to obtain a lithium chloride wet material, and drying the lithium chloride wet material at 250 ℃ to obtain a lithium chloride product.
The sodium content of the lithium chloride products prepared in the examples 1-4 and the comparative example 1 is detected according to a GB/T11064.4-2013 test method, and the recovery rate is calculated, wherein the specific results are shown in Table 1.
TABLE 1 test results of lithium chloride of each example
| Item | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 |
| Sodium content | 64ppm | 49ppm | 52ppm | 196ppm | 688ppm |
| Lithium chloride recovery rate | 99.5％ | 99.7％ | 99.7％ | 92.5％ | 76.3％ |
The test results in table 1 show that the sodium content of lithium chloride obtained by purifying lithium chloride by the purification method of the present invention can be less than 200ppm, which is far lower than the requirement that the sodium content in national standard level 1 of industrial lithium chloride is less than 2500ppm, wherein examples 1 to 3 are preferred examples of the present invention, the sodium content of the lithium chloride can be controlled below 65ppm, and meanwhile, the recovery rate of lithium chloride reaches more than 99.5%, which indicates that in the purification process, the temperature difference between the heating temperature and the cooling rate can be ensured, and the purity and the recovery rate of lithium chloride can be positively influenced; as can be seen from comparative example 1, when the heating temperature does not reach the temperature range of the present invention, the sodium content and recovery rate of the lithium chloride product finally prepared are significantly different from those of the present invention.
In conclusion, the purification method of lithium chloride containing sodium provided by the invention has the characteristics of simple process steps, no addition of any auxiliary material in the purification process, and the used NMP solvent can be recycled, so that the process cost is low and the environment is not polluted.
The above embodiments are the best mode for carrying out the present invention, but the embodiments of the present invention are not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be regarded as equivalent substitutions and are included in the scope of the present invention.
Claims (8)
1. A method for purifying sodium-containing lithium chloride is characterized by comprising the following steps:
s1: adding a certain amount of sodium-containing lithium chloride into N-methylpyrrolidone, heating to 90-200 ℃, stirring for dissolving, and filtering while hot to obtain a first purified solution;
s2: and cooling the first purified solution to-15-30 ℃, crystallizing, separating out, separating to obtain a lithium chloride wet material, and drying to obtain a lithium chloride product.
2. The method of purifying lithium chloride containing sodium according to claim 1, wherein: and in the step S1, the solid-liquid mass ratio of the sodium-containing lithium chloride to the N-methyl pyrrolidone is (15-30) to 100.
3. The method of purifying lithium chloride containing sodium according to claim 1, wherein: and in the step S1, stirring and dissolving are carried out for 1-6 hours at the temperature of 90-200 ℃.
4. The method of purifying lithium chloride containing sodium according to claim 1, wherein: and cooling the first purified solution in the step S2 at a cooling rate of 0.5-5 ℃/min.
5. The method of purifying lithium chloride containing sodium according to claim 1, wherein: and S2, drying the lithium chloride wet material at 200-300 ℃.
6. The method of purifying lithium chloride containing sodium according to claim 1, wherein: and (4) separating and drying in the step S2 to obtain N-methyl pyrrolidone mother liquor, collecting the N-methyl pyrrolidone mother liquor, and returning the N-methyl pyrrolidone mother liquor to the step S1 for recycling.
7. The method of purifying lithium chloride containing sodium according to claim 1, wherein: the difference between the heating temperature in the step S1 and the cooling temperature in the step S2 is 100 ℃.
8. A sodium-containing lithium chloride purifying device is characterized by comprising: the device comprises a dissolving separation component, a cooling separation component and a drying recovery component;
the dissolving and separating component comprises a powder bin, a dissolving kettle, a first conveying pump and a filter, wherein the powder bin, the dissolving kettle, the first conveying pump and the filter are communicated in sequence;
the cooling separation assembly comprises a cooling kettle and a centrifugal separation device, the cooling kettle is communicated with the filter, and the centrifugal separation device is communicated with the cooling kettle;
the dry subassembly of retrieving includes desiccator, cooler, NMP mother liquor jar and second delivery pump, the desiccator with the centrifuge intercommunication is followed the centrifuge receives solid-state separation thing, NMP mother liquor jar with the centrifuge intercommunication is followed the centrifuge receives liquid separation thing, the desiccator passes through the cooler with NMP mother liquor jar intercommunication, NMP mother liquor jar passes through the second delivery pump with dissolve the cauldron intercommunication.
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