CN113800541A - Processing technology for refining lithium chloride by lithium carbonate precipitation and conversion - Google Patents
Processing technology for refining lithium chloride by lithium carbonate precipitation and conversion Download PDFInfo
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- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 title claims abstract description 152
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 title claims abstract description 78
- 229910052808 lithium carbonate Inorganic materials 0.000 title claims abstract description 78
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 65
- 238000001556 precipitation Methods 0.000 title claims abstract description 36
- 238000005516 engineering process Methods 0.000 title claims abstract description 26
- 238000007670 refining Methods 0.000 title claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 61
- 150000003839 salts Chemical class 0.000 claims abstract description 37
- 238000005406 washing Methods 0.000 claims abstract description 25
- 230000000694 effects Effects 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000012535 impurity Substances 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 238000010521 absorption reaction Methods 0.000 claims abstract description 9
- 238000000909 electrodialysis Methods 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 7
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 52
- 238000001704 evaporation Methods 0.000 claims description 48
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 45
- 230000008020 evaporation Effects 0.000 claims description 36
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 34
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 28
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 26
- 239000000047 product Substances 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000011780 sodium chloride Substances 0.000 claims description 17
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 14
- 239000001569 carbon dioxide Substances 0.000 claims description 14
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 14
- 239000012043 crude product Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 239000013505 freshwater Substances 0.000 claims description 7
- 239000001103 potassium chloride Substances 0.000 claims description 7
- 235000011164 potassium chloride Nutrition 0.000 claims description 7
- 239000000498 cooling water Substances 0.000 claims description 6
- 230000018044 dehydration Effects 0.000 claims description 6
- 238000006297 dehydration reaction Methods 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 6
- 238000000605 extraction Methods 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 238000000638 solvent extraction Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims 12
- 239000011259 mixed solution Substances 0.000 claims 1
- 238000002203 pretreatment Methods 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 12
- 229910052799 carbon Inorganic materials 0.000 abstract description 12
- 238000006386 neutralization reaction Methods 0.000 abstract description 7
- 229910052744 lithium Inorganic materials 0.000 description 4
- 238000002156 mixing Methods 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- UTBYQPSPFXHANA-UHFFFAOYSA-N [K].[Na].[Li] Chemical class [K].[Na].[Li] UTBYQPSPFXHANA-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000005323 carbonate salts Chemical class 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 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
Abstract
The invention relates to the technical field of lithium chloride recovery, in particular to a processing technology for refining lithium chloride by lithium carbonate precipitation and conversion, and solves the problems that in the prior art, the processing conversion efficiency and the carbon recovery effect of the processing technology for converting lithium carbonate precipitation into refined lithium chloride need to be improved. A processing technology for refining lithium chloride by lithium carbonate precipitation and conversion comprises the following steps: a pretreatment working section: the concentration of inlet water is increased and reduced through ultrafiltration UF and electrodialysis ED, and solid impurities in feed liquid are removed; precipitation and washing section: a reduction and solution preparation section. According to the invention, the effect that the total yield of lithium chloride exceeds 95% is realized by arranging the pretreatment working section, the reaction and absorption working section and the lithium chloride reduction and solution preparation working section, and the effect of carbon recovery and carbon neutralization in the process of preparing lithium chloride by lithium carbonate precipitation conversion is realized by arranging the mixed salt recovery unit, so that the processing technology of converting lithium carbonate into lithium chloride with high lithium chloride recovery rate and capable of realizing carbon neutralization is realized.
Description
Technical Field
The invention relates to the technical field of lithium chloride recovery, in particular to a processing technology for refining lithium chloride by lithium carbonate precipitation and conversion.
Background
Lithium metal is widely used in the fields of rechargeable batteries, glass, ceramics, alloys, lubricants, medicines, etc., and particularly, rechargeable lithium batteries have recently received much attention as a main power source of hybrid vehicles and electric vehicles. In addition, there is a huge market for lithium used for existing small batteries such as mobile phones and notebook computers. Therefore, the demand for lithium metal is large both domestically and abroad in the entire industrial field. Lithium chloride is one of the lithium salts. Lithium chloride is an important and expensive alkali metal, and the unique electronic structure and the special physicochemical properties brought by the atomic radius of the lithium chloride play an important role in the production and living activities of the lithium chloride nowadays.
Lithium carbonate is one of the main raw materials of the current lithium ion battery, and plays a significant role in the whole new energy industrial chain under the background that the new energy technology is rapidly developed and becomes a main power source. The rational recovery of the cells is of great importance for the corresponding carbon neutralization.
The processing of converting lithium carbonate precipitation into refined lithium chloride is a method for preparing the existing lithium chloride, but the existing lithium carbonate precipitation is used for processing lithium chloride for recovery, and the lithium chloride is recovered in an evaporation, concentration, cooling and crystallization mode, so that the energy consumption and serious high-temperature corrosion in the evaporation process of the recovery process are caused because the boiling point of the lithium chloride is raised too high;
the lithium chloride with a certain concentration is converted into lithium carbonate precipitate, and the lithium carbonate precipitate, sodium chloride and potassium chloride are separated from water, so that purification is realized, hydrochloric acid is added into the lithium carbonate to convert the lithium carbonate into lithium chloride and carbon dioxide, and the carbon dioxide adopts a circulating design, so that the carbon-neutralization-type efficient processing technology for refining lithium chloride from lithium carbonate is realized.
Disclosure of Invention
The invention aims to provide a processing technology for converting lithium carbonate precipitation into refined lithium chloride, which solves the problem that the processing conversion efficiency and the carbon recovery effect of the processing technology for converting lithium carbonate precipitation into refined lithium chloride in the prior art need to be improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
a processing technology for refining lithium chloride by lithium carbonate precipitation and conversion comprises the following steps:
a pretreatment working section: the concentration of inlet water is increased and reduced through ultrafiltration UF and electrodialysis ED, and solid impurities in feed liquid are removed;
precipitation and washing section:
(5) carrying out precipitation reaction on the mixed material liquid, the recovered sodium carbonate solution and a part of supplemented sodium carbonate solution in a reaction kettle to generate a crude lithium carbonate product;
(6) concentrating by a triple effect evaporation process, and further evaporating to obtain a crude lithium carbonate product;
(7) the lithium carbonate crude product obtained in the two steps of reaction and evaporation concentration is continuously or intermittently washed by two-stage to three-stage countercurrent water washing so as to further remove soluble sodium chloride and potassium chloride impurities in the crude product;
(8) evaporating the condensate liquid, and performing filter pressing and dehydration on the washing liquid through a plate frame to form a lithium carbonate product;
a reduction and solution preparation section:
(3) reacting the lithium carbonate product with 10% dilute hydrochloric acid to generate a lithium chloride solution, and preparing the lithium chloride solution with the required concentration suitable for workshop production through correcting the conductivity or the density by temperature;
(4) the lithium chloride solution and hydrochloric acid react intermittently in the reaction kettle, the generated carbon dioxide is absorbed by sodium hydroxide, and the absorption liquid returns to the reaction kettle of the reaction and washing unit to continuously produce lithium carbonate, so that the internal circulation of the carbon dioxide is realized;
a mixed salt treatment unit: the concentrated feed liquid for removing the lithium carbonate by evaporation and concentration of a mixed salt evaporation and drying system mainly contains sodium chloride and sodium carbonate;
public subsidiary unit: low-pressure steam, circulating cooling water, dilute hydrochloric acid and sodium carbonate solution are provided for the whole process.
Preferably, in the pretreatment section, the dilute liquid with low salt content is concentrated after UF and ED treatment.
Preferably, in the pretreatment section, the dilute liquid after UF and ED treatment and the concentrated liquid after UF filtration are mixed to form mixed liquid.
Preferably, in the pretreatment working section, fresh water generated by the ED system is reused as reclaimed water for other production working sections.
Preferably, in the reduction and solution preparation working section, the lithium chloride solution and the hydrochloric acid are operated in a batch kettle manner in the reaction kettle, and the pH needs to be accurately controlled.
Preferably, in the mixed salt treatment unit, the crude dilute liquid neutralized by hydrochloric acid is mixed and enters a mixed salt evaporation drying system, and after the concentration of the triple effect evaporation system, the concentrated liquid is treated by a roller dryer.
Preferably, in the mixed salt treatment unit, lithium chloride in the mixed salt is recovered by organic solvent extraction or complex extraction.
The invention has at least the following beneficial effects:
the effect that the total yield of lithium chloride exceeds 95% is realized by setting a pretreatment working section, a reaction and absorption working section and a lithium chloride reduction and solution preparation working section, and the effect of carbon recovery and carbon neutralization in the process of preparing lithium chloride by lithium carbonate precipitation conversion is realized by setting a mixed salt recovery unit, so that the processing technology of converting lithium carbonate into lithium chloride with high lithium chloride recovery rate and capable of realizing carbon neutralization is realized.
The invention also has the following beneficial effects:
1. fresh water generated by the ED system is used as reclaimed water for other production sections, so that the effect of low material consumption in the cycle of the whole conversion processing technology of lithium chloride is improved; through the arrangement of the mixed salt treatment unit, the zero emission of the concentrated solution is realized, so that sodium chloride and sodium carbonate in the concentrated solution are removed.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a block diagram of a process flow;
FIG. 2 is a graph of the solubility of the alkali, hydrochloride and carbonate salts of lithium sodium potassium;
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example one
Referring to fig. 1 and 2, a processing technology for refining lithium chloride by lithium carbonate precipitation and conversion comprises the following steps:
a pretreatment working section: the concentration of inlet water is increased and reduced through ultrafiltration UF and electrodialysis ED, and solid impurities in feed liquid are removed;
precipitation and washing section:
(1) carrying out precipitation reaction on the mixed material liquid, the recovered sodium carbonate solution and a part of supplemented sodium carbonate solution in a reaction kettle to generate a crude lithium carbonate product;
(2) concentrating by a triple effect evaporation process, and further evaporating to obtain a crude lithium carbonate product;
(3) the lithium carbonate crude product obtained in the two steps of reaction and evaporation concentration is continuously or intermittently washed by two-stage to three-stage countercurrent water washing so as to further remove soluble sodium chloride and potassium chloride impurities in the crude product;
(4) evaporating the condensate liquid, and performing filter pressing and dehydration on the washing liquid through a plate frame to form a lithium carbonate product; specifically, by adopting a triple effect evaporation process, sodium chloride in the solution is controlled not to reach a saturated concentration, crude lithium carbonate can be obtained as much as possible through evaporation, and meanwhile, lithium carbonate can be further recovered by combining a technology for preventing lithium carbonate from scaling by a seed crystal method, so that the total yield of lithium carbonate can be improved to more than 95%;
a reduction and solution preparation section:
(1) reacting the lithium carbonate product with 10% dilute hydrochloric acid to generate a lithium chloride solution, and preparing the lithium chloride solution with the required concentration suitable for workshop production through correcting the conductivity or the density by temperature;
(2) the lithium chloride solution and hydrochloric acid react intermittently in the reaction kettle, the generated carbon dioxide is absorbed by sodium hydroxide, and the absorption liquid returns to the reaction kettle of the reaction and washing unit to continuously produce lithium carbonate, so that the internal circulation of the carbon dioxide is realized;
a mixed salt treatment unit: the concentrated feed liquid for removing the lithium carbonate by evaporation and concentration of a mixed salt evaporation and drying system mainly contains sodium chloride and sodium carbonate;
public subsidiary unit: providing low-pressure steam, circulating cooling water, dilute hydrochloric acid and sodium carbonate solution for the whole process;
in this embodiment: the effect that the total yield of lithium chloride exceeds 95% is realized by setting a pretreatment working section, a reaction and absorption working section and a lithium chloride reduction and solution preparation working section, and the effect of carbon recovery and carbon neutralization in the process of preparing lithium chloride by lithium carbonate precipitation conversion is realized by setting a mixed salt recovery unit, so that the processing technology of converting lithium carbonate into lithium chloride with high lithium chloride recovery rate and capable of realizing carbon neutralization is realized.
Example two
Referring to fig. 1 and 2, a processing technology for refining lithium chloride by lithium carbonate precipitation and conversion comprises the following steps:
a pretreatment working section: the concentration of inlet water is increased and reduced through ultrafiltration UF and electrodialysis ED, and solid impurities in feed liquid are removed; treating dilute feed liquid with low salt content by UF and ED, and concentrating; mixing the dilute feed liquid treated by UF and ED with the concentrated feed liquid filtered by UF to form mixed feed liquid; in the pretreatment working section, fresh water generated by an ED system is used as reclaimed water for other production working sections;
precipitation and washing section:
(1) carrying out precipitation reaction on the mixed material liquid, the recovered sodium carbonate solution and a part of supplemented sodium carbonate solution in a reaction kettle to generate a crude lithium carbonate product;
(2) concentrating by a triple effect evaporation process, and further evaporating to obtain a crude lithium carbonate product;
(3) the lithium carbonate crude product obtained in the two steps of reaction and evaporation concentration is continuously or intermittently washed by two-stage to three-stage countercurrent water washing so as to further remove soluble sodium chloride and potassium chloride impurities in the crude product;
(4) evaporating the condensate liquid, and performing filter pressing and dehydration on the washing liquid through a plate frame to form a lithium carbonate product;
a reduction and solution preparation section:
(1) reacting the lithium carbonate product with 10% dilute hydrochloric acid to generate a lithium chloride solution, and preparing the lithium chloride solution with the required concentration suitable for workshop production through correcting the conductivity or the density by temperature;
(2) the lithium chloride solution and hydrochloric acid react intermittently in the reaction kettle, the generated carbon dioxide is absorbed by sodium hydroxide, and the absorption liquid returns to the reaction kettle of the reaction and washing unit to continuously produce lithium carbonate, so that the internal circulation of the carbon dioxide is realized;
a mixed salt treatment unit: the concentrated feed liquid for removing the lithium carbonate by evaporation and concentration of a mixed salt evaporation and drying system mainly contains sodium chloride and sodium carbonate;
public subsidiary unit: providing low-pressure steam, circulating cooling water, dilute hydrochloric acid and sodium carbonate solution for the whole process;
in this embodiment: fresh water generated by the ED system is used as reclaimed water for other production sections, so that the effect of low material consumption in the cycle of the whole conversion processing technology of lithium chloride is improved.
EXAMPLE III
Referring to fig. 1 and 2, a processing technology for refining lithium chloride by lithium carbonate precipitation and conversion comprises the following steps:
a pretreatment working section: the concentration of inlet water is increased and reduced through ultrafiltration UF and electrodialysis ED, and solid impurities in feed liquid are removed; treating dilute feed liquid with low salt content by UF and ED, and concentrating; mixing the dilute feed liquid treated by UF and ED with the concentrated feed liquid filtered by UF to form mixed feed liquid; in the pretreatment working section, fresh water generated by an ED system is used as reclaimed water for other production working sections;
precipitation and washing section:
(1) carrying out precipitation reaction on the mixed material liquid, the recovered sodium carbonate solution and a part of supplemented sodium carbonate solution in a reaction kettle to generate a crude lithium carbonate product;
(2) concentrating by a triple effect evaporation process, and further evaporating to obtain a crude lithium carbonate product;
(3) the lithium carbonate crude product obtained in the two steps of reaction and evaporation concentration is continuously or intermittently washed by two-stage to three-stage countercurrent water washing so as to further remove soluble sodium chloride and potassium chloride impurities in the crude product;
(4) evaporating the condensate liquid, and performing filter pressing and dehydration on the washing liquid through a plate frame to form a lithium carbonate product;
a reduction and solution preparation section:
(1) reacting the lithium carbonate product with 10% dilute hydrochloric acid to generate a lithium chloride solution, and preparing the lithium chloride solution with the required concentration suitable for workshop production through correcting the conductivity or the density by temperature;
(2) the lithium chloride solution and hydrochloric acid react intermittently in the reaction kettle, the generated carbon dioxide is absorbed by sodium hydroxide, and the absorption liquid returns to the reaction kettle of the reaction and washing unit to continuously produce lithium carbonate, so that the internal circulation of the carbon dioxide is realized; the lithium chloride solution and the hydrochloric acid are operated in a batch kettle manner in the reaction kettle, and the pH needs to be accurately controlled;
a mixed salt treatment unit: the concentrated feed liquid for removing the lithium carbonate by evaporation and concentration of a mixed salt evaporation and drying system mainly contains sodium chloride and sodium carbonate; in the mixed salt treatment unit, the crude dilute feed liquid neutralized by hydrochloric acid is mixed and enters a mixed salt evaporation drying system, and after the concentration of the triple effect evaporation system, the concentrated feed liquid is treated by a roller dryer;
public subsidiary unit: providing low-pressure steam, circulating cooling water, dilute hydrochloric acid and sodium carbonate solution for the whole process;
in this embodiment: through the arrangement of the mixed salt treatment unit, the zero emission of the concentrated solution is realized, so that sodium chloride and sodium carbonate in the concentrated solution are removed.
Example four
Referring to fig. 1 and 2, a processing technology for refining lithium chloride by lithium carbonate precipitation and conversion comprises the following steps:
a pretreatment working section: the concentration of inlet water is increased and reduced through ultrafiltration UF and electrodialysis ED, and solid impurities in feed liquid are removed; treating dilute feed liquid with low salt content by UF and ED, and concentrating; mixing the dilute feed liquid treated by UF and ED with the concentrated feed liquid filtered by UF to form mixed feed liquid; in the pretreatment working section, fresh water generated by an ED system is used as reclaimed water for other production working sections;
precipitation and washing section:
(1) carrying out precipitation reaction on the mixed material liquid, the recovered sodium carbonate solution and a part of supplemented sodium carbonate solution in a reaction kettle to generate a crude lithium carbonate product;
(2) concentrating by a triple effect evaporation process, and further evaporating to obtain a crude lithium carbonate product;
(3) the lithium carbonate crude product obtained in the two steps of reaction and evaporation concentration is continuously or intermittently washed by two-stage to three-stage countercurrent water washing so as to further remove soluble sodium chloride and potassium chloride impurities in the crude product;
(4) evaporating the condensate liquid, and performing filter pressing and dehydration on the washing liquid through a plate frame to form a lithium carbonate product;
a reduction and solution preparation section:
(1) reacting the lithium carbonate product with 10% dilute hydrochloric acid to generate a lithium chloride solution, and preparing the lithium chloride solution with the required concentration suitable for workshop production through correcting the conductivity or the density by temperature;
(2) the lithium chloride solution and hydrochloric acid react intermittently in the reaction kettle, the generated carbon dioxide is absorbed by sodium hydroxide, and the absorption liquid returns to the reaction kettle of the reaction and washing unit to continuously produce lithium carbonate, so that the internal circulation of the carbon dioxide is realized; the lithium chloride solution and the hydrochloric acid are operated in a batch kettle manner in the reaction kettle, and the pH needs to be accurately controlled;
a mixed salt treatment unit: the concentrated feed liquid for removing the lithium carbonate by evaporation and concentration of a mixed salt evaporation and drying system mainly contains sodium chloride and sodium carbonate; in the mixed salt treatment unit, the crude dilute feed liquid neutralized by hydrochloric acid is mixed and enters a mixed salt evaporation drying system, and after the concentration of the triple effect evaporation system, the concentrated feed liquid is treated by a roller dryer; in the mixed salt treatment unit, lithium chloride in the mixed salt is extracted and recovered by an organic solvent or complexing extraction;
public subsidiary unit: providing low-pressure steam, circulating cooling water, dilute hydrochloric acid and sodium carbonate solution for the whole process;
in this embodiment: in the mixed salt treatment unit, after being regulated by hydrochloric acid, the main components in the concentrated solution are only sodium chloride and a small amount of lithium chloride, and the recovery of the small amount of lithium chloride can be realized through organic solvent extraction or complex extraction.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (7)
1. A processing technology for refining lithium chloride by lithium carbonate precipitation and conversion is characterized by comprising the following steps:
a pretreatment working section: the concentration of inlet water is increased and reduced through ultrafiltration UF and electrodialysis ED, and solid impurities in feed liquid are removed;
precipitation and washing section:
(1) carrying out precipitation reaction on the mixed material liquid, the recovered sodium carbonate solution and a part of supplemented sodium carbonate solution in a reaction kettle to generate a crude lithium carbonate product;
(2) concentrating by a triple effect evaporation process, and further evaporating to obtain a crude lithium carbonate product;
(3) the lithium carbonate crude product obtained in the two steps of reaction and evaporation concentration is continuously or intermittently washed by two-stage to three-stage countercurrent water washing so as to further remove soluble sodium chloride and potassium chloride impurities in the crude product;
(4) evaporating the condensate liquid, and performing filter pressing and dehydration on the washing liquid through a plate frame to form a lithium carbonate product;
a reduction and solution preparation section:
(1) reacting the lithium carbonate product with 10% dilute hydrochloric acid to generate a lithium chloride solution, and preparing the lithium chloride solution with the required concentration suitable for workshop production through correcting the conductivity or the density by temperature;
(2) the lithium chloride solution and hydrochloric acid react intermittently in the reaction kettle, the generated carbon dioxide is absorbed by sodium hydroxide, and the absorption liquid returns to the reaction kettle of the reaction and washing unit to continuously produce lithium carbonate, so that the internal circulation of the carbon dioxide is realized;
a mixed salt treatment unit: the concentrated feed liquid for removing the lithium carbonate by evaporation and concentration of a mixed salt evaporation and drying system mainly contains sodium chloride and sodium carbonate;
public subsidiary unit: low-pressure steam, circulating cooling water, dilute hydrochloric acid and sodium carbonate solution are provided for the whole process.
2. The process of claim 1, wherein in the pretreatment stage, the dilute solution with low salt content is treated with UF and ED and then concentrated.
3. The process of claim 1, wherein in the pre-treatment stage, the dilute solution after UF and ED treatment is mixed with the concentrated solution after UF filtration to form a mixed solution.
4. The processing technology for refining lithium chloride through lithium carbonate precipitation and conversion according to claim 1, wherein in the pretreatment section, fresh water generated by an ED system is used as reclaimed water for other production sections.
5. The processing technology for refining the lithium chloride by the precipitation and conversion of the lithium carbonate as claimed in claim 1, wherein in the reduction and solution section, the lithium chloride solution and the hydrochloric acid are operated in a batch kettle manner in the reaction kettle, and the pH needs to be accurately controlled.
6. The processing technology for refining lithium chloride through precipitation and conversion of lithium carbonate as claimed in claim 1, wherein in the mixed salt processing unit, the crude diluted material liquid neutralized by hydrochloric acid is mixed and enters the mixed salt evaporation drying system, and after the concentration in the triple effect evaporation system, the concentrated material liquid is processed by the roller dryer.
7. The processing technology for refining the lithium chloride through the precipitation and conversion of the lithium carbonate as claimed in claim 1, wherein the lithium chloride in the mixed salt is recovered through organic solvent extraction or complex extraction in the mixed salt processing unit.
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| CN114669257A (en) * | 2022-02-22 | 2022-06-28 | 乌鲁木齐市亚欧稀有金属有限责任公司 | Be used for lithium carbonate strength batching conveyor system |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4271131A (en) * | 1979-04-11 | 1981-06-02 | Foote Mineral Company | Production of highly pure lithium chloride from impure brines |
| JPH10182147A (en) * | 1996-12-26 | 1998-07-07 | Tosoh Corp | Recovery of lithium |
| CN101481125A (en) * | 2009-02-13 | 2009-07-15 | 海门容汇通用锂业有限公司 | Method for cyclically using lithium deposition for preparing sodium carbonate solution to produce lithium carbonate |
| CN102099296A (en) * | 2008-07-18 | 2011-06-15 | 里肯锂有限公司 | A process for recovering lithium from a brine |
| CN105347364A (en) * | 2015-10-30 | 2016-02-24 | 华陆工程科技有限责任公司 | Method for closed-loop recycling of lithium precipitation mother liquor in lithium carbonate production |
| CN106882822A (en) * | 2017-03-15 | 2017-06-23 | 江苏容汇通用锂业股份有限公司 | A kind of method that lithium is recycled into battery-level lithium carbonate in sinker mother liquor |
| CN110451536A (en) * | 2019-08-26 | 2019-11-15 | 新中天环保股份有限公司 | A method of recycling lithium from battery-level lithium carbonate mother liquor |
| CN111252788A (en) * | 2020-04-03 | 2020-06-09 | 启迪清源（北京）科技有限公司 | Method for preparing high-purity lithium carbonate by using fractional crystallization technology |
| KR20210105140A (en) * | 2020-02-18 | 2021-08-26 | 한국원자력연구원 | Method and apparatus for recovery of refined salt in salt wastes |
-
2021
- 2021-11-08 CN CN202111314650.XA patent/CN113800541A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4271131A (en) * | 1979-04-11 | 1981-06-02 | Foote Mineral Company | Production of highly pure lithium chloride from impure brines |
| JPH10182147A (en) * | 1996-12-26 | 1998-07-07 | Tosoh Corp | Recovery of lithium |
| CN102099296A (en) * | 2008-07-18 | 2011-06-15 | 里肯锂有限公司 | A process for recovering lithium from a brine |
| CN101481125A (en) * | 2009-02-13 | 2009-07-15 | 海门容汇通用锂业有限公司 | Method for cyclically using lithium deposition for preparing sodium carbonate solution to produce lithium carbonate |
| CN105347364A (en) * | 2015-10-30 | 2016-02-24 | 华陆工程科技有限责任公司 | Method for closed-loop recycling of lithium precipitation mother liquor in lithium carbonate production |
| CN106882822A (en) * | 2017-03-15 | 2017-06-23 | 江苏容汇通用锂业股份有限公司 | A kind of method that lithium is recycled into battery-level lithium carbonate in sinker mother liquor |
| CN110451536A (en) * | 2019-08-26 | 2019-11-15 | 新中天环保股份有限公司 | A method of recycling lithium from battery-level lithium carbonate mother liquor |
| KR20210105140A (en) * | 2020-02-18 | 2021-08-26 | 한국원자력연구원 | Method and apparatus for recovery of refined salt in salt wastes |
| CN111252788A (en) * | 2020-04-03 | 2020-06-09 | 启迪清源（北京）科技有限公司 | Method for preparing high-purity lithium carbonate by using fractional crystallization technology |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114669257A (en) * | 2022-02-22 | 2022-06-28 | 乌鲁木齐市亚欧稀有金属有限责任公司 | Be used for lithium carbonate strength batching conveyor system |
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Application publication date: 20211217 |