CN105776257A - Method for separating magnesium and lithium in salt lake brine and producing magnesium hydroxide and high-purity magnesium oxide - Google Patents
Method for separating magnesium and lithium in salt lake brine and producing magnesium hydroxide and high-purity magnesium oxide Download PDFInfo
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- CN105776257A CN105776257A CN201610070611.2A CN201610070611A CN105776257A CN 105776257 A CN105776257 A CN 105776257A CN 201610070611 A CN201610070611 A CN 201610070611A CN 105776257 A CN105776257 A CN 105776257A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/02—Magnesia
- C01F5/06—Magnesia by thermal decomposition of magnesium compounds
- C01F5/08—Magnesia by thermal decomposition of magnesium compounds by calcining magnesium hydroxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
- C01F5/22—Magnesium hydroxide from magnesium compounds with alkali hydroxides or alkaline- earth oxides or hydroxides
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- 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
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Abstract
The invention provides a method for separating magnesium and lithium in salt lake brine and producing magnesium hydroxide and high-purity magnesium oxide.According to the method, the salt lake brine is subjected to solar evaporation and filtration to remove insoluble impurities, and then an old brine solution is obtained; an alkaline solution and the old brine solution are mixed for a precipitation reaction or fully back-mixed in a colloid mill for quick precipitation and then transferred into a reactor to be crystallized at proper temperature; filtration and drying are carried out to obtain Mg(OH)2 with the purity higher than 99%; roasting is carried out to obtain a solid magnesium oxide product with the purity higher than 99%.Filtrate is evaporated and concentrated to obtain a lithium-rich solution which can be directly used for preparing a lithium carbonate product.By the adoption of the reaction-separation coupling technology, nanoscale magnesium hydroxide and the high-purity magnesium oxide product are produced while magnesium and lithium in the salt lake brine are separated.The loss rate of lithium is small (smaller than 10%), the yield is high (larger than 90%), the separation process is simple, and prepared magnesium hydroxide is high in purity.
Description
Technical field
The present invention relates to one utilizes reaction-separation coupling technology separating magnesium, lithium from salt lake bittern to produce magnesium hydroxide and height simultaneously
The method of pure zirconia magnesium.
Background technology
Lithium and compound thereof are the key metal materials of 21 century development in Hi-Tech, have in energy storage material and Clear nuclear energy are developed
Important strategic position, is described as " promoting the energy metal of world's progress ".Saline lake lithium resource accounts for world's lithium resource commercial reserves
More than 69%, China's lithium resource reserves occupy the whole world the 5th, and wherein saline lake lithium resource accounts for 71%, and extracting lithium from salt lake bittern becomes
The most important thing on China's contention energy strategy highland, is great strategy demand towards the country.
Salt lake is contained and has many valuable sources, such as: potassium, sodium, magnesium, lithium, boron etc., be to produce multiple industry, agricultural products
Important source material.China's salt lake resources is enriched, and is mainly distributed on west area (Qinghai, Tibet etc.).Compare other parts of the world
Salt lake, China's Qinghai Salt Lake compositing characteristic is that content of magnesium is high, magnesium/lithium ratio is high, is very suitable for development and utilization magnesium resource, such as:
The magnesium of the Cha Er Han Salt Lake bittern in the Caidamu Basin/lithium ratio up to 1836, big bavin denier salt lake is 114, east, West Taijinar Salt Lake
Bittern magnesium/lithium, than for 40-60, is the most tens of or even thousand times.Owing to the chemical property of magnesium, lithium is sufficiently close to, a large amount of magnesium exist
Cause the difficulty separating, extracting lithium to increase, be the bittern bottleneck that carries lithium.
The method extracting at present lithium from salt lake bittern mainly has: the precipitation method, calcination method, extraction, ion exchange adsorption,
Selectively semi-transparent embrane method.The precipitation method, owing to technique is simple, cost is relatively low, are to be applied to salt lake the earliest to put forward the technology of lithium, the method
Workable, utilize Exposure to Sunlight to concentrate, it is possible to decrease energy consumption, to facilitate implementation industrialization, but shortcoming be earlier stage treatment process flow process
Longer, lithium yield is the highest, lithium resource utilization rate low [Zhang Baoquan. Salt Lake Brines In Qaidam Basin carries lithium research overview [J]. sea lake salt and chemical industry,
2000(04):9–13].The consumption of raw materials amount of calcination method is few, the overall recovery of lithium reach about 80% [Liu Yuanhui, Deng Tianlong. both at home and abroad from salt
Lake bittern water carries lithium technology progress [J]. world technology research and development, 2006,28 (5): 69-75].But the utilization to magnesium resource
Difficulty, foreign ion difficulty removes, affect the quality of lithium product, and to the seriously corroded of equipment, evaporated quantity of water greatly, power disappears
Consumption is big.Extraction is high to the requirement of extraction equipment and extractant, single recovery of extraction relatively low [Zhou Yuan, Li Lijuan, Wu Zhijian, Lee
Xiang. Qinghai Salt Lake development of resources and comprehensive utilization [J]. chemical progress, 2013,25 (10): 1613-1624].The method flow process is complicated, equipment
Seriously corroded, relatively costly.Ion exchange adsorption is higher to the requirement of high-selectivity adsorption agent, current adsorbent preparation side
Method is complicated, exchange rate is low, be not suitable for large-scale operation uses [Zhang Yan, Zhong Hui, Yan Ming. the research of Separating Materials on Extracting Lithium from Salt Lake Brine
Progress [J]. Guangdong trace element science, 2006,13 (2): 7-11].Selectively semi-transparent embrane method mainly utilizes monovalence selective ion exchange membrane pair
Lithium is circulated concentration and obtains rich lithium, low magnesium bittern, adds soda ash precipitation and produces lithium carbonate product, the extraction rate reached 80% of lithium
Above [Ma Peihua, Deng little Chuan, Wen Xianmin. separating magnesium and the method [P] of concentration lithium from salt lake bittern. China: CN1626443,2005].
But the method is very strong for the dependence of membrane material, and related film material is monopolized by external producer.Above method is all from bittern
Middle extraction lithium, and the magnesium stayed after carrying lithium is not fully used, a large amount of valuable magnesium resource abandoneds, causes resource the most unrestrained
Take.
Magnesium hydroxide is a kind of chemical materials important, large, is widely used in fire retardant, and particularly nanometric magnesium hydroxide is as poly-
Compound (plastics) additive, has excellent flame retardant effect.And high purity magnesium hydroxide is prepare magnesia (magnesia) former
Material.By the magnesium preparing magnesium hydroxide in salt lake bittern, preparing magnesia further is the important channel that magnesium resource utilizes on a large scale.
Summary of the invention
It is an object of the invention to provide magnesium in salt lake bittern, lithium separates and utilizes reaction-separation coupling technology to produce nanoscale hydrogen-oxygen simultaneously
Change magnesium and the method for high-purity magnesium oxide.
A kind of utilize magnesium, lithium in reaction-separation coupling technology separation salt lake bittern to produce the side of magnesium hydroxide and high-purity magnesium oxide simultaneously
Method, concretely comprises the following steps:
A. salt lake bittern is separated out a large amount of NaCl, KCl by solar evaporation, refilter removal insoluble impurities, obtain old halogen
Solution；The most each cation concn is: [Li+]=0.3～10g/L, [Mg2+]=30～100g/L, [K+]=0.5～12g/L, [Na+]=1～20
g/L；
Described salt lake bittern is Salt Lake Brines In Qaidam Basin, and the most each cation concn is: [Li+]=0.3～10g/L, [Mg2+]
=10～100g/L, [K+]=1～30g/L, [Na+]=10～90g/L；
B. preparing aqueous slkali B according to the magnesium ion content in halogen old in step A, its volume is identical with solution A volume, and alkali
Molal quantity be 1.6-2.5 times of magnesium ion；Described aqueous slkali is the aqueous solution of NaOH or potassium hydroxide；
C. precipitation reaction: by the aqueous slkali B of preparation, join in old halogen A by 1～5mL/min rate of addition, to solution
PH=11～12；Carry out precipitation reaction, be then transferred in reactor, stirring reaction 6～48 hours at 40 DEG C～100 DEG C；Reaction
After end, solution temperature is down to 20～60 DEG C, is filtrated to get Mg (OH)2Filter cake, is dried 6～24 hours at 60～100 DEG C,
To solid hydrogen magnesium oxide product, molecular formula is: Mg (OH)2, purity is more than 99%.
D. magnesium hydroxide solid step C obtained, under air or oxygen atmosphere, rises to 1-10 DEG C/min heating rate
500 DEG C～1000 DEG C of temperature, roasting 3-12 hour, obtain high purity solid magnesium oxide product, and molecular formula is: MgO, and purity is more than
99%.
E. being concentrated by evaporation the filtrate of the filtration of step C to lithium concentration is 5～20g/L, obtains rich lithium solution, can be direct
For preparing lithium carbonate product.
Precipitation reaction described in step C, more preferable technique is to pour the old halogen of step A into colloid mill with aqueous slkali B simultaneously, with
1000-5000 turns/and the rotating speed of min rotates 1-10 minute, forms Mg (OH)2Nucleus solution；According still further to the side described in step C
Method crystallization, filter, be dried.Obtaining solid hydrogen magnesium oxide product, molecular formula is: Mg (OH)2, purity is more than 99%.
Beneficial effects of the present invention:
(1) while salt lake bittern magnesium, lithium separate, produce nanometric magnesium hydroxide and high-purity magnesium oxide product, be a kind of anti-
Should-separation coupling technology.Not only achieve efficiently separating of salt lake separation and Extraction resource important, difficult, obtain again important magnesium products.
(2) magnesium in bittern is separated by forming magnesium hydroxide solid, overcomes traditional dividing solution from high magnesium/lithium ratio
From magnesium, the difficulty of lithium method, the loss late of lithium is little (less than 10%), and yield is high (more than 90%), and separation process is simple.
(3) the magnesium hydroxide purity prepared is high, it is ensured that the magnesia obtained after roasting has high-purity (> 99%), meet each
Plant the requirement to magnesium oxide product purity under application.
Detailed description of the invention
Solution used by example below is Bittern from East Taijinaier Salt Lake, and its composition see table
Embodiment 1
A. in salt lake bittern solution A: [Mg2+]=80g/L, [Li+]=5g/L, takes 250mL solution.
B. weigh NaOH 66.7g, be dissolved in 250mL deionized water, obtain aqueous slkali B.
C. pour old halogen solution A into colloid mill with aqueous slkali B simultaneously, rotate 2 minutes with the rotating speed of 1000r/min, formed
Mg(OH)2Nucleus, transfers to reactor by nucleus solution, stirs crystallization 10 hours at 40 DEG C, reacts solution temperature after terminating
Degree is down to 20 DEG C, is filtrated to get Mg (OH)2Filter cake, is dried 8 hours at 60 DEG C, obtains solid Mg (OH)2Product, molecule
Formula is: Mg (OH)2, purity 99.0%
D. the Mg (OH) step C obtained2Solid is under air atmosphere, with 5 DEG C/min of heating rate, rises to 600 DEG C, protects
Temperature 6 hours, roasting obtains solid oxidation magnesium, and molecular formula is: MgO, purity 99.0%
E. the filtrate of step C being concentrated by evaporation at 40 DEG C to lithium concentration is 5g/L, and now the sodium ion in filtrate is with NaCl
Crystallization.Lithium sodium ion in liquor content < 10%.In filtrate, the loss late of lithium is 6.5%.
Embodiment 2
A. in salt lake bittern solution A: [Mg2+]=60g/L, [Li+]=1g/L, takes 250mL solution.
B. weigh NaOH 50g, be dissolved in 250mL deionized water, obtain aqueous slkali B.
C. pour old halogen solution A into colloid mill with aqueous slkali B simultaneously, rotate 2 minutes with the rotating speed of 1000r/min, formed
Mg(OH)2Nucleus, transfers to reactor by nucleus solution, stirs crystallization 10 hours at 40 DEG C, reacts solution temperature after terminating
Degree is down to 20 DEG C, is filtrated to get Mg (OH)2Filter cake, is dried 8 hours at 60 DEG C, obtains solid Mg (OH)2Product, molecule
Formula is: Mg (OH)2, purity 99.2%.
D. the Mg (OH) step C obtained2Solid roasting under air atmosphere, 2 DEG C/min of heating rate, rise to 500 DEG C, protect
Temperature 5 hours, obtains solid oxidation magnesium, and molecular formula is: MgO, purity 99.2%.
E. the filtrate of step C being concentrated by evaporation at 60 DEG C to lithium concentration is 6g/L, and now the sodium ion in filtrate is with NaCl
Crystallization.Lithium sodium ion in liquor content < 10%.In filtrate, the loss late of lithium is 4.5%.
Embodiment 3
A. in salt lake bittern solution A: [Mg2+]=70g/L, [Li+]=3g/L, takes 250mL solution.
B. weigh NaOH 58.3g, be dissolved in 250mL deionized water, obtain aqueous slkali B.
C. pour old halogen solution A into colloid mill with aqueous slkali B simultaneously, rotate 3 minutes with the rotating speed of 3000r/min, formed
Mg(OH)2Nucleus, transfers to reactor by nucleus solution, stirs crystallization 12 hours at 50 DEG C, reacts solution temperature after terminating
Degree is down to 30 DEG C, is filtrated to get Mg (OH)2Filter cake, is dried 10 hours at 70 DEG C, obtains solid Mg (OH)2Product, molecule
Formula is: Mg (OH)2, purity 99.0%.
D. the Mg (OH) step C obtained2Solid roasting under air atmosphere, 7 DEG C/min of heating rate, rise to 700 DEG C, protect
Temperature 8 hours, obtains solid oxidation magnesium, and molecular formula is: MgO, purity 99.0%.
E. the filtrate of step C being concentrated by evaporation at 50 DEG C to lithium concentration is 8g/L, and now the sodium ion in filtrate is with NaCl
Crystallization.Lithium sodium ion in liquor content < 10%.In filtrate, the loss late of lithium is 5.2%.
Embodiment 4
A. in salt lake bittern solution A: [Mg2+]=90g/L, [Li+]=10g/L, takes 250mL solution.
B. weigh NaOH 75g, be dissolved in 250mL deionized water, obtain aqueous slkali B.
C. pour old halogen solution A into colloid mill with aqueous slkali B simultaneously, rotate 5 minutes with the rotating speed of 4000r/min, formed
Mg(OH)2Nucleus, transfers to reactor by nucleus solution, stirs crystallization 24 hours at 80 DEG C, reacts solution temperature after terminating
Degree is down to 50 DEG C, is filtrated to get Mg (OH)2Filter cake, is dried 12 hours at 90 DEG C, obtains solid Mg (OH)2Product, molecule
Formula is: Mg (OH)2, purity 99.3%.
D. the Mg (OH) step C obtained2Solid roasting under air atmosphere, 8 DEG C/min of heating rate, rise to 800 DEG C, protect
Temperature 10 hours, obtains solid oxidation magnesium, and molecular formula is: MgO, purity 99.3%.
E. the filtrate of step C being concentrated by evaporation at 80 DEG C to lithium concentration is 9g/L, and now the sodium ion in filtrate is with NaCl
Crystallization.Lithium sodium ion in liquor content < 10%.In filtrate, the loss late of lithium is 6.8%.
Claims (2)
1. the method that salt lake bittern magnesium, lithium separated and produced magnesium hydroxide and high-purity magnesium oxide, concretely comprises the following steps:
A. salt lake bittern is separated out a large amount of NaCl, KCl by solar evaporation, refilter removal insoluble impurities, obtain old halogen
Solution；The most each cation concn is: [Li+]=0.3～10g/L, [Mg2+]=30～100g/L, [K+]=0.5～12g/L, [Na+]=1～20
g/L；
Described salt lake bittern is Salt Lake Brines In Qaidam Basin, and the most each cation concn is: [Li+]=0.3～10g/L, [Mg2+]
=10～100g/L, [K+]=1～30g/L, [Na+]=10～90g/L；
B. preparing aqueous slkali B according to the magnesium ion content in halogen old in step A, its volume is identical with solution A volume, and alkali
Molal quantity be 1.6-2.5 times of magnesium ion；Described aqueous slkali is the aqueous solution of NaOH or potassium hydroxide；
C. precipitation reaction: by the aqueous slkali B of preparation, join in old halogen A by 1～5mL/min rate of addition, to solution
PH=11～12；Carry out precipitation reaction, be then transferred in reactor, stirring reaction 6～48 hours at 40 DEG C～100 DEG C；Reaction
After end, solution temperature is down to 20～60 DEG C, is filtrated to get Mg (OH)2Filter cake, is dried 6～24 hours at 60～100 DEG C,
To solid hydrogen magnesium oxide product, molecular formula is: Mg (OH)2, purity is more than 99%；
D. magnesium hydroxide solid step C obtained, under air or oxygen atmosphere, rises to 1-10 DEG C/min heating rate
500 DEG C～1000 DEG C of temperature, roasting 3-12 hour, obtain high purity solid magnesium oxide product, and molecular formula is: MgO, and purity is more than
99%；
E. being concentrated by evaporation the filtrate of the filtration of step C to lithium concentration is 5～20g/L, obtains rich lithium solution, can be direct
For preparing lithium carbonate product.
The method that salt lake bittern magnesium the most according to claim 1, lithium separated and produced magnesium hydroxide and high-purity magnesium oxide, its feature
It is the precipitation reaction described in step C, is to pour the old halogen of step A into colloid mill with aqueous slkali B simultaneously, turns with 1000-5000
The rotating speed of/min rotates 1-10 minute, forms Mg (OH)2Nucleus solution；According still further to the method crystallization described in step C, filtration,
It is dried, obtains solid Mg (OH)2, purity is more than 99%.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107043116A (en) * | 2017-04-24 | 2017-08-15 | 北京化工大学 | Lithium and the method for preparing battery-level lithium carbonate are extracted from demagging bittern |
| CN107805715A (en) * | 2017-09-21 | 2018-03-16 | 中国科学院青海盐湖研究所 | Salt lake puies forward the method for comprehensive utilization of lithium by-product magnesium hydroxide |
| CN110817909A (en) * | 2019-11-19 | 2020-02-21 | 中国科学院过程工程研究所 | Lithium-magnesium separation method |
| CN112624162A (en) * | 2021-01-13 | 2021-04-09 | 中国科学院上海应用物理研究所 | Method for preparing industrial-grade magnesium oxide by taking bischofite as raw material |
| CN113371740A (en) * | 2020-02-25 | 2021-09-10 | 中国科学院青海盐湖研究所 | Device for refining lithium-containing feed liquid to remove magnesium and coproduce magnesium hydroxide and use method |
| CN113371739A (en) * | 2020-02-25 | 2021-09-10 | 中国科学院青海盐湖研究所 | Preparation method of hexagonal flaky magnesium hydroxide nanosheet |
| CN114797171A (en) * | 2022-06-24 | 2022-07-29 | 北京化工大学 | Production device and production process for extracting lithium from brine by efficient adsorption method |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107043116A (en) * | 2017-04-24 | 2017-08-15 | 北京化工大学 | Lithium and the method for preparing battery-level lithium carbonate are extracted from demagging bittern |
| CN107805715A (en) * | 2017-09-21 | 2018-03-16 | 中国科学院青海盐湖研究所 | Salt lake puies forward the method for comprehensive utilization of lithium by-product magnesium hydroxide |
| CN110817909A (en) * | 2019-11-19 | 2020-02-21 | 中国科学院过程工程研究所 | Lithium-magnesium separation method |
| CN113371740A (en) * | 2020-02-25 | 2021-09-10 | 中国科学院青海盐湖研究所 | Device for refining lithium-containing feed liquid to remove magnesium and coproduce magnesium hydroxide and use method |
| CN113371739A (en) * | 2020-02-25 | 2021-09-10 | 中国科学院青海盐湖研究所 | Preparation method of hexagonal flaky magnesium hydroxide nanosheet |
| CN112624162A (en) * | 2021-01-13 | 2021-04-09 | 中国科学院上海应用物理研究所 | Method for preparing industrial-grade magnesium oxide by taking bischofite as raw material |
| CN114797171A (en) * | 2022-06-24 | 2022-07-29 | 北京化工大学 | Production device and production process for extracting lithium from brine by efficient adsorption method |
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