CN104030322B - A kind ofly recycle salt lake lithium liquor and the method for by-product magnesium basic carbonate - Google Patents
A kind ofly recycle salt lake lithium liquor and the method for by-product magnesium basic carbonate Download PDFInfo
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Abstract
The invention provides and a kind ofly recycle salt lake lithium liquor and the method for by-product magnesium basic carbonate.First Quilonum Retard mother liquor one and Quilonum Retard mother liquor two are mixed according to a certain percentage in the method, after reaction, filtration, washing, drying, namely obtain industrial hydrated basic magnesium carbonate.After reaction, remaining carbanion 31% technical hydrochloric acid is removed in mother liquor, and the mother liquor after removing carbonate is mixed in proportion with the raw brine of production Quilonum Retard, and the spontaneous nucleation through 10 ~ 20 days analyses Li after sodium
+content reaches 5 ~ 6g/L, Na
+content is less than 2.5g/L, reaches the condition that workshop uses, and makes Quilonum Retard lithium liquor become the raw brine producing Quilonum Retard in this way.The method technique is simple, and cost is low, effectively raises the comprehensive utilization ratio of lithium resource.
Description
Technical field
the invention belongs to technical field of inorganic chemical industry, specifically relate to the recoverying and utilizing method of a kind of salt lake lithium liquor.
Background technology
quilonum Retard is as the basic lithium salts of lithium, and maximum consumption market is for the additive in glass manufacture and Production of Ceramics process and fusing assistant.In recent years the demand of lithium salts product every year with 6% ~ 8% speed steady-state growth, particularly along with the develop rapidly of the industries such as building materials, electronics, automobile, information, energy-storage battery, Quilonum Retard has become most important product in lithium compound.
the production of Quilonum Retard is because of the difference of its raw material, and production technique is also different, generally can be divided into ore be raw material ore method and take bittern as the bittern method of raw material.Because of the technique of to be bittern the be raw material that Qinghai Li Ye company limited adopts, so introduce the bittern Quilonum Retard situation of producing both at home and abroad.
the enterprise being engaged in Quilonum Retard production abroad mainly contains the FMC of the U.S., the SQM of Chile and the Chemtall of Germany, the Quilonum Retard output of three companies was once accounting for about 80% of worldwide production, and the Quilonum Retard more than 70% of three companies is raw material production with bittern, the salt lake resources that three enterprises have has a common feature to be exactly low Mg/Li ratio, because Mg/Li ratio is lower, the separation realizing magnesium lithium that can be very economical, Quilonum Retard production technique is fairly simple.
the saline lake lithium resource of China mainly contains two classes, and a kind of is sulfuric acid hypotype, and another kind is carbonate type.The salt lake brine of carbonate type is after the solarization of beach, salt pan is concentrated, and the lithium in bittern deposits to salt Tanaka with the form of Quilonum Retard and becomes Crude lithium Carbonate, and it is exactly in fact purifying again to Crude lithium Carbonate Gu Kuang that the Quilonum Retard in such salt lake is produced.The saline lake lithium resource of the sulfuric acid hypotype of China, there is the feature of Mg/Li ratio, generally Mg/Li ratio all reaches more than 20:1, because magnesium lithium has individual oblique line principle in the periodic table of elements, their ionic radius closely, is a global difficult problem to the feasible separation of their economy all the time.
though Qinghai Province is the large province of reserves of saline lake lithium resource, owing to being separated the puzzlement of a difficult problem by high Mg/Li ratio, the exploitation of lithium resource is more late.The enterprise that current Qinghai Province is engaged in saline lake lithium resource exploitation mainly contains four, Qinghai Li Ye company limited (being called for short Qinghai lithium industry), Qinghai Landtek Li Ye company limited (being called for short Landtek lithium industry) and Li Ye Science and Technology Ltd. of Qinghai CITIC Guoan (being called for short Guoan's lithium industry), also have just at the salt lake Minmetals Group of construction period.The technique of four enterprises is different, Qinghai lithium industry carries out the separation of magnesium lithium by embrane method, Landtek lithium industry adopts absorption method to carry out the separation of magnesium lithium, Guoan's lithium industry adopts calcination method to carry out the separation of magnesium lithium, due to the difference of three kinds of techniques, the Quilonum Retard tail washings that each enterprise produces is different, in tail washings recycling San Jia enterprise nothing can experience for reference mutually, the raw materials for production of external salt lake brine Quilonum Retard enterprise are the bittern of low Mg/Li ratio, the physico-chemical property of tail washings also has larger difference compared with my company, therefore to Quilonum Retard tail washings recycling aspect also few of reference of my company.
the technical process of Qinghai Li Ye company limited is as follows: first pass through by quartz sand, the more medium filter removing silt of manganese sand and activated carbon composition and iron, then according to magnesium, the difference of lithium ion valency and ionic radius, utilizes ion selectivity tripping device, makes the magnesium in raw brine under electrical forces effect, lithium ion is moved, when raw brine by have optionally separatory membrane time, lithium, the monovalent ions such as sodium pass through, magnesium, the divalent ions such as calcium are isolated, thus achieve magnesium, the object that lithium ion is separated, obtains the rich lithium bittern of low Mg/Li ratio after separation, carry out the degree of depth except Ca2+ to the rich lithium bittern of low Mg/Li ratio, K+, SO42-, the impurity such as Mg2+, and the purification carrying out auxiliary material soda ash solution, in the rich lithium bittern acid adjustment after deep impurity-removing and after carry out three-effect evaporation and condensation, the rich lithium bittern after concentrated carries out adding alkali sinker at a certain temperature, then carries out press filtration, wash and starch, centrifugation is washed, and finally carry out drying and cool and obtain battery-level lithium carbonate finished product, this product reaches the requirement of Qinghai Province provincial standard DB63/T1113-2012 (bittern battery Quilonum Retard).
the magnesium lithium achieving salt lake brine with high magnesium-lithium ratio of this technics comparing economy of Qinghai lithium industry is separated, few containing mixing with the product of this explained hereafter, good product quality, but also there is the low shortcoming of yield.This technique creates two class Quilonum Retard mother liquors, and one is that high Mg/Li ratio separation circuit creates mother liquor one, and in this mother liquor, lithium content is about 0.6 ~ 0.8 grams per liter, and two is transform sinker operation to create mother liquor two, and in this mother liquor, lithium content is 1.8 ~ 2.2 grams per liters.When Quilonum Retard first phase 3000 tons of projects, two kinds of mother liquors are emitted on a discarded salt Tanaka respectively, do not carry out any recycling.Quilonum Retard in May, 2012,7000 tons of projects second phase are gone into operation, following process has been carried out to two kinds of mother liquors, first by after two kinds of mother liquor mixings a to Buffer Pool, the mother liquor of mixing has imported the salt Tanaka that deposits tail washings specially, after two kinds of mother liquor mixing, tail washings system becomes very complicated, adds difficulty to recycling.
Summary of the invention
the object of this invention is to provide a kind of method recycling salt lake lithium liquor, become by successful conversion the raw brine producing Quilonum Retard by the method salt lake lithium liquor two, it is a kind of method indirectly improving saline lake lithium resource utilization ratio, and by-product industry hydrated basic magnesium carbonate, this product reaches the requirement of premium grads in HG/T2959-2010.
method of the present invention, has following steps:
(1) lithium liquor one is the tail washings that high Mg/Li ratio raw brine magnesium lithium separation circuit produces, in this tail washings, the content of lithium and magnesium is respectively: Li+ content is 0.6 ~ 0.8g/L, Mg2+ content is 38 ~ 48g/L, mother liquor two is the tail washings transforming the generation of sinker operation, in this tail washings except containing the Li+ ion of 1.8 ~ 2.2g/L, also containing the CO32-ion of 15 ~ 20g/L and the NaCl of 80 ~ 100g/L, the temperature of mother liquor one is between 25 DEG C ~ 35 DEG C, the temperature of mother liquor two is between 85 DEG C ~ 95 DEG C, mother liquor two is mixed by 6:1 ~ 4:1 with mother liquor one, after mixing, the temperature of solution is between 50 DEG C ~ 60 DEG C, stirring reaction 20 ~ 30 minutes after mixed, Mg2+ in mother liquor one in CO32-ion and mother liquor two defines magnesium basic carbonate, thick magnesium basic carbonate is obtained after carrying out press filtration separation, after press filtration, mother liquor needs process further.
the thick magnesium basic carbonate of step (1) gained is washed and starched, washing and starching solid-to-liquid ratio controls 30% ~ 40%, centrifugation is carried out after washing and starching, wet magnesium basic carbonate after separation carries out drying at 130 ~ 140 DEG C, must reach the product of HG/T2959-2010 (industrial hydrated basic magnesium carbonate) premium grads.
2 ~ 4g/LCO32-ion is had not to be completely removed in mother liquor in step (1) after press filtration separation, the technical hydrochloric acid that need add 31% is removed, the add-on of hydrochloric acid is that the pH value controlling reaction end is less than or equal to 4.6, and now in this mother liquor, CO32-ion just can be completely removed.
after being mixed in the ratio of 4:1 ~ 2:1 with the raw brine producing Quilonum Retard by the mother liquor of the CO32-ion removed completely in step (3), in halogen storage pool, under physical environment, crystallization analysed sodium after 10 ~ 20 days, Na+ content is less than 2.5g/L, reach the condition that workshop uses, by above-mentioned a series for the treatment of processess, Quilonum Retard lithium liquor has been finally converted into the raw brine producing Quilonum Retard, thus achieves the recycling of Quilonum Retard lithium liquor.
the present invention has the following advantages:
1, whole recyclings of Quilonum Retard mother liquor two that the inventive method is real, have also recycled part Quilonum Retard mother liquor one in the process utilizing Quilonum Retard mother liquor two.
, utilize the CO32-ion in the Mg2+ in Quilonum Retard mother liquor one and Quilonum Retard mother liquor two to synthesize byproduct hydrated basic magnesium carbonate when increasing cost hardly in the present invention, the quality of this byproduct reaches the requirement of HG/T2959-2010 (industrial hydrated basic magnesium carbonate) premium grads, and this byproduct added value can reduce the production cost of Quilonum Retard.
, present invention process cost is low, pollution-free, meets the theory of environmental protection Sustainable development.
, the present invention meets the requirement of salt lake resources to " become more meticulous, high-valued, seriation " future development, improve the recovery utilization rate that lithium resource is carried in salt lake, the salt lake resources advantage in Qinghai is made to be transformed to economic advantages, method of the present invention is successful obtains application in Qinghai Li Ye company limited, achieves good Social benefit and economic benefit.
Accompanying drawing explanation
the present invention is a kind of recycles salt lake lithium liquor and the method for by-product magnesium basic carbonate has following accompanying drawing:
to be that the present invention is a kind of recycle salt lake lithium liquor and primary chemical composition schematic diagram (unit: g ∕ L) of the mother liquor that high magnesium lithium separation circuit produces in lithium technique is carried in the method salt lake of by-product magnesium basic carbonate to Fig. 1.
fig. 2 be the present invention a kind of recycle salt lake lithium liquor and the method salt lake of by-product magnesium basic carbonate carry in lithium technique transform sinker operation produce mother liquor two primary chemical composition.
fig. 3 be the present invention a kind of recycle salt lake lithium liquor and the method for by-product magnesium basic carbonate industry hydrated basic magnesium carbonate (HG/T2959-2010) industry standard in physical and chemical index.
to be that the present invention is a kind of recycle salt lake lithium liquor and the method for by-product magnesium basic carbonate utilizes the typical physical and chemical index of the byproduct hydrated basic magnesium carbonate of the inventive method gained to Fig. 4.
fig. 5 is the process flow sheet of the inventive method.
concrete embodiment
embodiment one
(1) lithium liquor one is the tail washings that high Mg/Li ratio raw brine magnesium lithium separation circuit produces, in this tail washings, the content of lithium and magnesium is respectively: Li+ content is 0.6g/L, Mg2+ content is 38g/L, mother liquor two is the tail washings transforming the generation of sinker operation, in this tail washings except the Li+ ion containing 2.2g/L, also containing the CO32-ion of 15g/L and the NaCl of 80g/L, the temperature of mother liquor one is between 25 DEG C, the temperature of mother liquor two is between 85 DEG C, mother liquor two is mixed by 6:1 with mother liquor one, after mixing, the temperature of solution is between 50 DEG C, stirring reaction 25 minutes after mixed, Mg2+ in mother liquor one in CO32-ion and mother liquor two defines magnesium basic carbonate, thick magnesium basic carbonate is obtained after carrying out press filtration separation, after press filtration, mother liquor needs process further.
the thick magnesium basic carbonate of step (1) gained is washed and starched, washing and starching solid-to-liquid ratio controls 35%, carry out centrifugation after washing and starching, the wet magnesium basic carbonate after separation carries out drying at 135 DEG C, must reach the product of HG/T2959-2010 (industrial hydrated basic magnesium carbonate) premium grads.
in mother liquor in step (1) after press filtration separation, CO32-ion is not completely removed, the content of CO32-ion is 4g/L, the technical hydrochloric acid that need add 31% is removed, and the add-on of hydrochloric acid is the pH value controlling reaction end is 4.6, and now in this mother liquor, CO32-ion is completely removed.
after being mixed in the ratio of 4:1 with the raw brine producing Quilonum Retard by the mother liquor removing CO32-ion in step (3) completely, in halogen storage pool, under physical environment, crystallization analysed sodium after 10 days, Na+ content is less than 2.5g/L, reach the condition that workshop uses, by above-mentioned a series for the treatment of processess, Quilonum Retard lithium liquor has been finally converted into the raw brine producing Quilonum Retard, thus achieves the recycling of Quilonum Retard lithium liquor.
embodiment two
(1) lithium liquor one is the tail washings that high Mg/Li ratio raw brine magnesium lithium separation circuit produces, in this tail washings, the content of lithium and magnesium is respectively: Li+ content is 0.7g/L, Mg2+ content is 43g/L, mother liquor two is the tail washings transforming the generation of sinker operation, in this tail washings except the Li+ ion containing 2.0g/L, also containing the CO32-ion of 17g/L and the NaCl of 90g/L, the temperature of mother liquor one is 30 DEG C, the temperature of mother liquor two is 90 DEG C, mother liquor two is mixed by 5:1 with mother liquor one, after mixing, the temperature of solution is 55 DEG C, stirring reaction 25 minutes after mixed, Mg2+ in mother liquor one in CO32-ion and mother liquor two defines magnesium basic carbonate, thick magnesium basic carbonate is obtained after carrying out press filtration separation, after press filtration, mother liquor needs process further.
the thick magnesium basic carbonate of step (1) gained is washed and starched, washing and starching solid-to-liquid ratio controls 35%, carry out centrifugation after washing and starching, the wet magnesium basic carbonate after separation carries out drying at 135 DEG C, must reach the product of HG/T2959-2010 (industrial hydrated basic magnesium carbonate) premium grads.
in mother liquor in step (1) after press filtration separation, CO32-ion is not completely removed, the content of CO32-ion is 3g/L, the technical hydrochloric acid that need add 31% is removed, and the add-on of hydrochloric acid is the pH value controlling reaction end is 4.6, and now in this mother liquor, CO32-ion is completely removed.
after being mixed in the ratio of 3:1 with the raw brine producing Quilonum Retard by the mother liquor removing CO32-ion in step (3) completely, in halogen storage pool, under physical environment, crystallization analysed sodium after 15 days, Na+ content is less than 2.5g/L, reach the condition that workshop uses, by above-mentioned a series for the treatment of processess, Quilonum Retard lithium liquor has been finally converted into the raw brine producing Quilonum Retard, thus achieves the recycling of Quilonum Retard lithium liquor.
embodiment three
(1) lithium liquor one is the tail washings that high Mg/Li ratio raw brine magnesium lithium separation circuit produces, in this tail washings, the content of lithium and magnesium is respectively: Li+ content is 0.8g/L, Mg2+ content is 48g/L, mother liquor two is the tail washings transforming the generation of sinker operation, in this tail washings except the Li+ ion containing 1.8g/L, also containing the CO32-ion of 20g/L and the NaCl of 100g/L, the temperature of mother liquor one is 35 DEG C, the temperature of mother liquor two is 95 DEG C, mother liquor two is mixed by 4:1 with mother liquor one, after mixing, the temperature of solution is 60 DEG C, stirring reaction 25 minutes after mixed, Mg2+ in mother liquor one in CO32-ion and mother liquor two defines magnesium basic carbonate, thick magnesium basic carbonate is obtained after carrying out press filtration separation, after press filtration, mother liquor needs process further.
the thick magnesium basic carbonate of step (1) gained is washed and starched, washing and starching solid-to-liquid ratio controls 35%, carry out centrifugation after washing and starching, the wet magnesium basic carbonate after separation carries out drying at 135 DEG C, must reach the product of HG/T2959-2010 (industrial hydrated basic magnesium carbonate) premium grads.
in mother liquor in step (1) after press filtration separation, CO32-ion is not completely removed, the content of CO32-ion is 2g/L, the technical hydrochloric acid that need add 31% is removed, the add-on of hydrochloric acid is the pH value controlling reaction end is 4.6, and now in this mother liquor, CO32-ion just can be completely removed.
after being mixed in the ratio of 2:1 with the raw brine producing Quilonum Retard by the mother liquor of the CO32-ion removed completely in step (3), in halogen storage pool, under physical environment, crystallization analysed sodium after 20 days, Na+ content is less than 2.5g/L, reach the condition that workshop uses, by above-mentioned a series for the treatment of processess, Quilonum Retard lithium liquor has been finally converted into the raw brine producing Quilonum Retard, thus achieves the recycling of Quilonum Retard lithium liquor.
Claims (5)
1. recycle salt lake lithium liquor and a method for by-product magnesium basic carbonate, comprise following processing step:
(1) lithium liquor one and lithium liquor two are mixed in proportion, stir 20 ~ 30 minutes after mixing, the CO in mother liquor one
3 2-mg in ion and mother liquor two
2+generate magnesium basic carbonate, obtain thick magnesium basic carbonate after carrying out press filtration separation, after press filtration, mother liquor needs process further;
Lithium liquor one in step (1) is the tail washings that high Mg/Li ratio raw brine magnesium lithium separation circuit produces, and in this tail washings, the content of lithium and magnesium is respectively: Li
+content is 0.6 ~ 0.8g/L, Mg
2+content is 38 ~ 48g/L, and lithium liquor two is the tail washings transforming the generation of sinker operation, except the Li containing 1.8 ~ 2.2g/L in this tail washings
+outside ion, the CO also containing 15 ~ 20g/L
3 2-the NaCl of ion and 80 ~ 100g/L, the temperature of mother liquor one is between 25 DEG C ~ 35 DEG C, the temperature of mother liquor two is between 85 DEG C ~ 95 DEG C, mother liquor two is mixed by 6:1 ~ 4:1 with mother liquor one, after mixing, the temperature of solution is between 50 DEG C ~ 60 DEG C, and after mixed, stirring reaction carries out press filtration separation in 20 ~ 30 minutes;
(2) the thick magnesium basic carbonate after step (1) being separated is washed and starched, and carry out centrifugation washing after washing and starching, the solid phase after centrifugation is carried out dry packing and namely obtained industrial hydrated basic magnesium carbonate;
(3) 2 ~ 4g/LCO in the mother liquor in step (1) after press filtration separation
3 2-ion is not completely removed, and the technical hydrochloric acid that need add 31% is removed;
(4) step (3) is removed CO completely
3 2-the mother liquor of ion is mixed in proportion with the raw brine producing Quilonum Retard, carries out spontaneous nucleation, the Na in bittern to be mixed after mixing at halogen storage pool
+ion reaches requirement, and this mixing bittern just becomes the raw brine producing Quilonum Retard, is transported to the production that Quilonum Retard is carried out in workshop.
2. a kind ofly as claimed in claim 1 recycle salt lake lithium liquor and the method for by-product magnesium basic carbonate, it is characterized in that: the thick magnesium basic carbonate after the step (1) described in step (2) is separated is washed and starched, solid-to-liquid ratio controls 30% ~ 40%, centrifugation is carried out after washing and starching, wet solid phase after separation carries out drying at 130 ~ 140 DEG C, must reach the product of HG/T2959-2010 (industrial hydrated basic magnesium carbonate) premium grads;
3. a kind ofly as claimed in claim 1 recycle salt lake lithium liquor and the method for by-product magnesium basic carbonate, it is characterized in that: in the step (1) described in step (3) press filtration be separated after mother liquor further except CO
3 2-need the technical hydrochloric acid adding 31% in the process of ion, the add-on of hydrochloric acid is that the pH value controlling reaction end is less than or equal to 4.6.
4. a kind ofly as claimed in claim 1 recycle salt lake lithium liquor and the method for by-product magnesium basic carbonate, it is characterized in that: the raw brine of the production Quilonum Retard described in step (4) is the bischofite saturated bittern of rich lithium, this bittern is also saturated to sodium-chlor.
5. a kind ofly as claimed in claim 1 recycle salt lake lithium liquor and the method for by-product magnesium basic carbonate, it is characterized in that: described in step (4), step (3) is removed CO completely
3 2-after the mother liquor of ion mixes by 4:1 ~ 2:1 with the raw brine producing Quilonum Retard, in halogen storage pool, under physical environment, crystallization analyses sodium after 10 ~ 20 days, Na
+content reaches the condition that workshop uses when being less than 2.5g/L, by above-mentioned a series for the treatment of processess, Quilonum Retard lithium liquor has changed into the raw brine producing Quilonum Retard.
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- 2014-02-11 CN CN201410047103.3A patent/CN104030322B/en active Active
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