CN104338441A - Treatment process of lithium precipitation mother solution - Google Patents
Treatment process of lithium precipitation mother solution Download PDFInfo
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- CN104338441A CN104338441A CN201410551826.7A CN201410551826A CN104338441A CN 104338441 A CN104338441 A CN 104338441A CN 201410551826 A CN201410551826 A CN 201410551826A CN 104338441 A CN104338441 A CN 104338441A
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Abstract
The invention relates to the production of industrial lithium salt, in particular relates to an after-treatment process of lithium salt, and more in particular relates to a treatment process of a lithium precipitation mother solution. Aiming at the problem that a large amount of a lithium-containing lithium precipitation mother solution generated in industrial lithium salt production currently, in particular an evaporative crystallization production method, cannot be effectively used, a membrane concentration process method applied to the lithium precipitation mother solution is provided creatively, and therefore, a high-concentration lithium ion solution enriched with lithium ions is obtained; in addition, the basis is provided for taking lithium precipitation mother solution as a lithium salt production raw material.
Description
Technical field
The present invention relates to industrial lithium salts to produce, particularly relate to lithium salts aftertreatment technology, more specifically relate to sinker mother liquor treatment process.
Background technology
Lithium carbonate is the basic compound of lithium, is widely used in space flight, military project, pottery, glass, lithium battery, medicine and other fields.Lithium carbonate, as a kind of basic material of lithium, can change into other multiple lithium compound, as lithium phosphate, lithium fluoride etc.
Although China is also at active development saline lake lithium resource in recent years.But because the content of magnesium in China's salt lake bittern is higher, magnesium and lithium this two kinds of elements are more difficult is separated, also do not have large-scale industrialization to produce up till now, so China extracts lithium salts from lithium ore always.At present, the method extracting lithium salts from lithium ore mainly contains, Production By Sulfuric Acid Process technique, spodumene and sulfate mixed sintering production technology and chloridising roasting production technology, and these methods are liquid phase method, and by evaporative crystallization, obtain lithium carbonate, yield is generally 85%.Evaporative crystallization produces the not high reason of lithium carbonate yield mainly: still containing a large amount of lithiums in lithium carbonate evaporative crystallization mother liquor, but lithium carbonate evaporative crystallization mother liquor is difficult to recycle, current lithium carbonate evaporative crystallization mother liquor can only as row outer after wastewater treatment, cause the wasting of resources, lithium carbonate yield is on the low side.
Those skilled in the art is in order to improve the utilization of lithium carbonate sinker mother liquor, tentative using its mother liquor as raw material, prepare the industrial lithium salts such as lithium phosphate, lithium fluoride, but cannot improve due to the content of lithium ion in unit lithium carbonate sinker mother liquor always, cause that to recycle cost high.
Summary of the invention
The present invention is directed in current industrial lithium salts production, particularly in evaporative crystallization production method, the a large amount of problems that cannot effectively utilize containing lithium sinker mother liquor produced, creatively propose film and concentrate this enrichment method, thus obtain the high concentration lithium ion solution being rich in lithium ion, for sinker mother liquor provides the foundation as lithium salts raw materials for production.
The invention discloses a kind of sinker mother liquor treatment process, comprise the following steps: successively
(1) dilute sulfuric acid adding mass fraction 98% in sinker mother liquor 3 ~ 7 to mixed solution pH, is then constantly monitored pH value of solution and maintains mixed solution pH 3 ~ 7 by controlling sulphuric acid;
(2) mixed liquor after step (1) being processed is successively by NF film, RO film, and collection membrane front end retains lower solution respectively, and will retain solution and be again mixed into step (1) sinker mother liquor;
(3) repeat step (1), (2), and obtain high concentration lithium ion solution at NF film and the collection of RO film front end.
NF film mentioned here refers to NF membrane, and RO film refers to reverse osmosis membrane.
In order to protect NF film, RO film, according to existing operating guidance; we need the sinker mother liquor after to step (1) process successively by multi-medium filtering, activated carbon filtration, secondary filter and ultrafiltration; thus the precipitation in removal mother liquor, suspension and larger molecular organics.Meet after upper film requires through the solution of a whole set of filtering process, then carried out film process according to step (2).
Wherein preferably pH is 4.5.
As the preferred mode of one, we disclose the carbon dioxide of discharging in time in described step (1) and generating further.
Carbon dioxide is discharged in time the reaction efficiency that reaction unit can improve step (1) further, reduce the reaction time, discharge method can with reference in prior art about gas discharge technology.In the present invention, preferably adopting the technological means passing into air, by passing into air by the carbon dioxide blowout in mother liquor, accelerating the conversion of lithium carbonate to high-dissolvability lithium salt compound.
Meanwhile, we emphasize that the processing mode of above sinker mother liquor is particularly preferably applicable to lithium carbonate sinker mother liquor, or lithium phosphate sinker mother liquor.
We also disclosed another sinker mother liquor treatment process in the present invention, comprise the following steps successively:
(1) add alkalescence in sinker mother liquor and regulate solution, regulate pH value of solution to 6 ~ 11;
(2) in the solution after step (1) process, add excessive calcium ions solution, cross and filter calcium fluoride precipitate, collect filtered fluid;
(3) step (2) gained filtered fluid is passed through ion exchange resin, remove excessive calcium ion, collect flow liquid;
(4) will remove the flow liquid of calcium ion through RO film, collection membrane front end retains lower solution, and is again mixed into retaining solution in the flow liquid of this step;
(5) repeatedly repeat step (4), and collection obtains high concentration lithium ion solution in RO film front end;
Described sinker mother liquor is lithium fluoride sinker mother liquor.
In order to protect RO film, according to existing operating guidance, we need the sinker mother liquor after to step (3) process successively by multi-medium filtering, activated carbon filtration, secondary filter and ultrafiltration, thus remove precipitation, suspension and the larger molecular organics in mother liquor.Meet after upper film requires through the solution of a whole set of filtering process, then carried out film process according to step (4).
In order to remove fluorine ion further, suitably can increase the access times of step (2), producing one-level except fluorine, secondary are except fluorine ... etc. process.
Further, we are preferred described step (4) middle employing two-stage RO film also, remove the flow liquid of calcium ion successively by one-level RO film, secondary RO film, and that collects one-level RO film and secondary RO film front end respectively retains solution, and solution will be retained again be mixed in flow liquid, again by one-level RO film, secondary RO film.
As preferably, we also disclose adjustment pH in described step (1) is further 4.5.
Simultaneously we also disclose described alkalescence adjustment solution is any one in sodium hydroxide solution, calcium oxide or aqua calcis, is particularly preferably calcium oxide herein.
Preferred as one, the invention also discloses in step (1) and regulate pH value of solution to 10.5.
Further, the present invention also openly the industrial lithium salts of application of aforementioned sinker mother liquor treatment process prepare method for treating waste liquid.
Further, we are also disclosed in industrial lithium salts and prepare in method for treating waste liquid the pure water preferably meeting environmental protection standard in RO film backend collection.
The present invention overcomes the technical barrier that membrane concentration method cannot be suitable in the application of sinker mother liquor, specifically when adopting membrane concentration method, because film surface ion concentration is generally 50 times into water solution concentration, therefore the lithium salts on film surface because of supersaturation crystallization, cause film to be blocked, limit the application of embrane method in lithium salts reclaims.
The elemental lithium in lithium salts evaporative crystallization mother liquor is effectively reclaimed by film concentration technology, more than 99% is reached to the rejection of elemental lithium, achieves the resource recycling of lithium salts sinker mother liquor, improve yield prepared by lithium salts, decrease resource loss, for enterprise increases the benefit.
The present invention by preconditioning technique solve lithium salts sinker mother liquor because of solubility not high, membrane concentration method is adopted easily to cause the problem of stifled film, achieve the application of membrane concentration method in lithium salts concentrated mother liquor reclaims, elemental lithium content in lithium salts sinker mother liquor can be promoted 5 times, can direct reuse to production technology, solve the low difficult problem being difficult to reuse of lithium salts sinker mother liquor elemental lithium content.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention will be described further and explain.
Embodiment 1 adopts the treatment process of lithium carbonate sinker solution of the present invention
Lithium carbonate sinker mother liquor: certain factory's lithium carbonate sinker mother liquor, pH value is 10.04, and lithium concentration is 0.98g/L, and electrical conductivity is 11.89ms/cm, water yield 100L.
(1) in lithium carbonate sinker mother liquor, add the concentrated sulfuric acid that mass fraction is 98%, adjust ph to 6.5, (2) pass into air in the lithium carbonate sinker mother liquor after step (1) process, ventilation 0.5h.
(3) the lithium carbonate sinker mother liquor after step (2) process is successively by multi-medium filtering, and activated carbon filtration, secondary filter and ultrafiltration, remove precipitation, suspension and the larger molecular organics in mother liquor.The trapped fluid of ultrafiltration is back to ultrafiltration water inlet end.
(4) permeate after step (3) hyperfiltration treatment carries out nanofiltration, trapped fluid water outlet water yield 21L, lithium concentration 4.51g/L, pH value is 7.22, and electrical conductivity is 31.3ms/cm, permeate water outlet water yield 75L, lithium concentration is 0.015g/L, and pH value is 5.66, and electrical conductivity is 0.248ms/cm.
(5) the permeate reuse after step (4) nanofiltration process is to production technology, and trapped fluid is back to step (4) nanofiltration water inlet end.The permeate water outlet water yield is 61L, pH is 5.61, and electrical conductivity is 0.017ms/cm, and lithium concentration is 0.0039g/L.
The elemental lithium rate of recovery reaches 96.6%, and elemental lithium rejection reaches 99.7%, and elemental lithium cycles of concentration is 4.6 times.
Embodiment 2 adopts the treatment process of lithium phosphate sinker solution of the present invention
Lithium phosphate crystalline mother solution: certain factory's lithium phosphate crystalline mother solution, pH value is 8.71, and lithium concentration is 0.29g/L, and electrical conductivity is 10.62ms/cm, water yield 100L.
(1) in lithium phosphate sinker mother liquor, the concentrated sulfuric acid that mass fraction is 98% is added, adjust ph to 4.5, (2) the lithium phosphate sinker mother liquor after step (1) process passes through multi-medium filtering successively, activated carbon filtration, secondary filter and ultrafiltration, remove precipitation, suspension and the larger molecular organics in mother liquor.The trapped fluid of ultrafiltration is back to ultrafiltration water inlet end.
(3) permeate after step (2) hyperfiltration treatment carries out nanofiltration, trapped fluid water outlet water yield 23L, lithium concentration 1.18g/L, pH value is 4.14, and electrical conductivity is 28.9ms/cm, permeate water outlet water yield 71L, lithium concentration is 0.0016g/L, and pH value is 5.18, and electrical conductivity is 0.112ms/L.
(4) the permeate reuse after step (3) nanofiltration process is to production technology, and trapped fluid is back to step (3) nanofiltration water inlet end.The permeate water outlet water yield is 58L, pH is 5.33, and electrical conductivity is 0.0028ms/cm, and lithium concentration is 0.0012g/L.
The elemental lithium rate of recovery reaches 93.6%, and elemental lithium rejection reaches 99.76%, and elemental lithium cycles of concentration is 4.07 times.
Embodiment 3 adopts the treatment process of lithium fluoride sinker solution of the present invention
Lithium fluoride sinker mother liquor: certain factory's lithium fluoride sinker mother liquor, pH value is 3.69, and lithium concentration is 0.8205g/L, and electrical conductivity is 4.05ms/cm, water yield 100L.
(1) in lithium fluoride sinker mother liquor, calcium oxide is added, adjust ph to 10.5;
(2) the lithium fluoride sinker mother liquor after step (1) process adds calcium chloride and removes fluorine ion;
(3) the lithium fluoride sinker mother liquor after step (2) process carries out ion exchange resin, removes the foreign ions such as this magnesium;
(4) the lithium fluoride sinker mother liquor after step (3) process is successively by multi-medium filtering, and activated carbon filtration, secondary filter and ultrafiltration, remove precipitation, suspension and the larger molecular organics in mother liquor.The trapped fluid of ultrafiltration is back to ultrafiltration water inlet end;
(5) permeate after step (4) hyperfiltration treatment enters the process of first-stage reverse osmosis film, first-stage reverse osmosis trapped fluid water outlet water yield 30L, lithium concentration 2.51g/L, pH value is 8.15, electrical conductivity is 11.06ms/cm, first-stage reverse osmosis permeate water outlet water yield 67L, and lithium concentration is 0.0083g/L, pH value is 6.72, and electrical conductivity is 0.257ms/cm.
(6) step (5) first-stage reverse osmosis permeate carries out two-pass reverse osmosis, and the reuse of two-pass reverse osmosis permeate is to production technology, and two-pass reverse osmosis trapped fluid is back to first-stage reverse osmosis water inlet end.Two-pass reverse osmosis permeate water yield 51L, lithium concentration 0.0019g/L, pH value is 6.93, and electrical conductivity is 0.0099ms/cm.
The elemental lithium rate of recovery reaches 91.7%, and elemental lithium rejection reaches 99.8%, and elemental lithium cycles of concentration is 3.06 times.
Embodiment 4 by sinker mother liquor directly by experimental result that film is concentrated
4-1 lithium carbonate sinker mother liquor
Lithium carbonate sinker mother liquor directly carries out nanofiltration process, after running a period of time, permeate flow reduces, and trapped fluid flow increases, and intake pressure increases, after running 1h, intake pressure exceedes the upper limit, cannot continue to run, and now lithium concentration is still at reduced levels, and due to cannot continued operation, therefore do not meet industrialization demand.
4-2 lithium phosphate sinker mother liquor
Lithium phosphate sinker mother liquor directly carries out nanofiltration process, after running a period of time, permeate flow reduces, and trapped fluid flow increases, and intake pressure increases, after running 1h, intake pressure exceedes the upper limit, cannot continue to run, and now lithium concentration is still at reduced levels, and due to cannot continued operation, therefore do not meet industrialization demand.
4-3 lithium fluoride sinker mother liquor
Adopt lithium fluoride sinker mother liquor directly to carry out reverse-osmosis treated, after running a period of time, because lithium fluoride itself has very strong corrosivity to film, therefore in the short time, RO film is damaged, and film concentrated effect cannot realize.
Claims (10)
1. sinker mother liquor treatment process, is characterized in that, comprises the following steps: successively
(1) dilute sulfuric acid adding mass fraction 98% in sinker mother liquor about 3 ~ 7 to mixed solution pH, is then constantly monitored pH value of solution and maintains mixed solution pH 3 ~ 7 by controlling sulphuric acid;
(2) mixed liquor after step (1) being processed is successively by NF film, RO film, and collection membrane front end retains lower solution respectively, and will retain solution and be again mixed into step (1) sinker mother liquor;
(3) repeat step (1), (2), and obtain high concentration lithium ion solution at NF film and the collection of RO film front end.
2. sinker mother liquor treatment process according to claim 1, is characterized in that, discharges the carbon dioxide generated in described step (1) in time.
3. sinker mother liquor treatment process according to claim 1, is characterized in that, described sinker mother liquor is lithium carbonate sinker mother liquor, or lithium phosphate sinker mother liquor.
4. sinker mother liquor treatment process according to claim 1, is characterized in that, in described step (1), pH is 4.5.
5. sinker mother liquor treatment process, is characterized in that, comprises the following steps successively:
(1) add alkalescence in sinker mother liquor and regulate solution, regulate pH value of solution to 6 ~ 11;
(2) in the solution after step (1) process, add excessive calcium ions solution, cross and filter calcium fluoride precipitate, collect filtered fluid;
(3) step (2) gained filtered fluid is passed through ion exchange resin, remove excessive calcium ion, collect flow liquid;
(4) will remove the flow liquid of calcium ion through RO film, collection membrane front end retains lower solution, and is again mixed into retaining solution in the flow liquid of this step;
(5) repeatedly repeat step (4), and collection obtains high concentration lithium ion solution in RO film front end;
Described sinker mother liquor is lithium fluoride sinker mother liquor.
6. sinker mother liquor treatment process according to claim 5, it is characterized in that, two-stage RO film is adopted in described step (4), remove the flow liquid of calcium ion successively by one-level RO film, secondary RO film, and that collects one-level RO film and secondary RO film front end respectively retains solution, and solution will be retained again be mixed in flow liquid, again by one-level RO film, secondary RO film.
7. sinker mother liquor treatment process according to claim 5, is characterized in that, described alkalescence regulates solution to be any one in sodium hydroxide solution, calcium oxide solution or aqua calcis.
8. sinker mother liquor treatment process according to claim 5, is characterized in that, regulates pH value of solution to 10.5 in step (1).
9. an application rights requires that method for treating waste liquid prepared by the industrial lithium salts of the sinker mother liquor treatment process in 1 ~ 8 described in any one.
10. application according to claim 9, is characterized in that, meets the pure water of environmental protection standard in RO film backend collection.
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| CN104787784A (en) * | 2015-03-18 | 2015-07-22 | 江西赣锋锂业股份有限公司 | Method for preparing lithium salt through recycling lithium fluoride-containing waste material material |
| CN105925799A (en) * | 2016-05-26 | 2016-09-07 | 四川思达能环保科技有限公司 | Wet metallurgy film concentration process |
| CN106315629A (en) * | 2016-08-30 | 2017-01-11 | 山东瑞福锂业有限公司 | Technology for preparing high-purity lithium carbonate through recovering of battery-grade lithium carbonate lithium precipitation mother liquor |
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