CN105776257B - Salt lake bittern separating magnesium and lithium and the method for producing magnesium hydroxide and high-purity magnesium oxide - Google Patents
Salt lake bittern separating magnesium and lithium and the method for producing magnesium hydroxide and high-purity magnesium oxide Download PDFInfo
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- CN105776257B CN105776257B CN201610070611.2A CN201610070611A CN105776257B CN 105776257 B CN105776257 B CN 105776257B CN 201610070611 A CN201610070611 A CN 201610070611A CN 105776257 B CN105776257 B CN 105776257B
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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 magnesium, lithium and the method for producing magnesium hydroxide and high-purity magnesium oxide in a kind of separation salt lake bittern, be by salt lake bittern by solar evaporation, filter off except obtaining old halogen solution after insoluble impurities, aqueous slkali is mixed with old halogen solution and carries out precipitation reaction, or the full back-mixing rapid precipitation in colloid mill, crystallization at moderate temperatures is then transferred in reactor, it is filtered, dry, obtain the Mg (OH) that purity is more than 99%2, then by roasting obtain purity be more than 99% solid oxidation magnesium products.Filtrate is concentrated by evaporation to obtain rich lithium solution, can be directly used for preparing lithium carbonate product.The present invention while salt lake bittern magnesium, lithium is separated, produces nanometric magnesium hydroxide and high-purity magnesium oxide product using reaction separation coupling technology.The loss late of lithium is small (being less than 10%), and high income (is more than 90%), and separation process is simple, and the magnesium hydroxide purity of preparation is high.
Description
Technical field
The present invention relates to one kind, using reaction-separation coupling technology, separating magnesium, lithium from salt lake bittern produce hydrogen-oxygen simultaneously
Change the method for magnesium and high-purity magnesium oxide.
Background technology
Lithium and its compound are the key metal materials of 21 century development in Hi-Tech, are developed in energy storage material and Clear nuclear energy
In there is important strategic position, be described as the energy metal of world's progress " promote ".Saline lake lithium resource accounts for world's lithium resource work
More than the 69% of industry reserves, China's lithium resource reserves occupy the whole world the 5th, and wherein saline lake lithium resource accounts for 71%, is carried from salt lake bittern
Take lithium to turn into the most important thing on China contention energy strategy highland, be great strategy demand towards the country.
Containing in salt lake has many valuable sources, such as：Potassium, sodium, magnesium, lithium, boron etc., it is a variety of industry of production, agricultural products
Important source material.China's salt lake resources are enriched, and are mainly distributed on west area (Qinghai, Tibet etc.).Compared to other parts of the world
Salt lake, China's Qinghai Salt Lake compositing characteristic be content of magnesium is high, magnesium/lithium than high, be very suitable for developing and utilizing magnesium resource, example
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 are 114, east, West Taijinar
Salt lake bittern magnesium/lithium ratio is 40-60, is external tens of or even thousand times.Because the chemical property of magnesium, lithium is sufficiently close to, a large amount of magnesium
It is the bottleneck that bittern carries lithium in the presence of causing the difficulty for separating, extracting lithium to increase.
The method for extracting lithium from salt lake bittern at present mainly has：The precipitation method, calcination method, extraction, ion exchange absorption
Method, the semi-transparent embrane method of selectivity.The precipitation method are to be applied to the technology that salt lake carries lithium, the party earliest because technique is simple, cost is relatively low
Method it is workable, concentrated using Exposure to Sunlight, energy consumption can be reduced, be easy to implement industrialization, but shortcoming is earlier stage treatment process stream
Journey is longer, lithium yield is not high, and lithium resource utilization rate is low, and [Zhang Baoquan Salt Lake Brines In Qaidam Basins carry lithium research overview [J] seas
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 up to 80% or so [Liu Yuanhui,
Deng Tianlong are both at home and abroad from extracting lithium from salt lake brine technology progress [J] world technology research and developments, and 2006,28
(5):69-75].But to magnesium resource using difficult, the difficult quality for removing, influenceing lithium product of foreign ion, and to equipment
Seriously corroded, evaporated quantity of water is big, power consumption is big.Requirement of the extraction to extraction equipment and extractant is high, and single extracts back
Yield it is relatively low [Zhou Yuan, Li Lijuan, Wu Zhijian, Li Xiang Qinghai Salt Lakes development of resources and comprehensive utilization [J] chemical progress, 2013,
25(10):1613-1624].This method flow is complicated, equipment corrosion is serious, cost is higher.Ion exchange adsorption is to high selection
Property adsorbent requirement it is higher, current sorbent preparation method is complicated, exchange rate is low, is not suitable for large-scale operation use
[progress [J] the Guangdong trace element science of Zhang Yan, Zhong Hui, Yan Ming Separating Materials on Extracting Lithium from Salt Lake Brine, 2006,13
(2):7-11].The semi-transparent embrane method of selectivity mainly lithium is carried out using monovalence selective ion exchange membrane circulation concentration obtain rich lithium,
Low magnesium bittern, add soda ash precipitation and produce lithium carbonate product, [Ma Peihua, Deng little Chuan, temperature are existing for the extraction rate reached more than 80% of lithium
People method [P] China of separating magnesium and concentration lithium from salt lake bittern:CN1626443,2005].But this method is for membrane material
The dependence of material is very strong, and related membrane material is monopolized by external producer.Method above all simply extracts lithium from bittern, and carries lithium
The magnesium left afterwards is not fully used, and a large amount of valuable magnesium resource abandoneds, causes resource serious waste.
Magnesium hydroxide is a kind of important, large chemical materials, is widely used in fire retardant, particularly nanometric magnesium hydroxide and makees
For polymer (plastics) additive, there is excellent flame retardant effect.And high purity magnesium hydroxide prepares magnesia (magnesia)
Raw material.By the magnesium preparing magnesium hydroxide in salt lake bittern, it is the important way that magnesium resource utilizes on a large scale further to prepare magnesia
Footpath.
The content of the invention
It is an object of the invention to provide magnesium, lithium separation in salt lake bittern to be received using the production of reaction-separation coupling technology simultaneously
The method of meter level magnesium hydroxide and high-purity magnesium oxide.
One kind produces magnesium hydroxide and high pure oxygen simultaneously using magnesium, lithium in reaction-separation coupling technology separation salt lake bittern
Change the method for magnesium, concretely comprise the following steps：
A. salt lake bittern is separated out into a large amount of NaCl, KCl by solar evaporation, refilters removal insoluble impurities, obtained old
Halogen solution；Wherein each cation concn is：[Li+]=0.3~10g/L, [Mg2+]=30~100g/L, [K+]=0.5~12g/
L, [Na+]=1~20g/L；
Described salt lake bittern is Salt Lake Brines In Qaidam Basin, wherein each cation concn is：[Li+]=0.3~
10g/L, [Mg2+]=10~100g/L, [K+]=1~30g/L, [Na+]=10~90g/L；
B. the magnesium ion content in old halogen in step A prepares aqueous slkali B, and its volume is identical with solution A volume, and alkali
Molal quantity be 1.6-2.5 times of magnesium ion；The aqueous slkali is the aqueous solution of sodium hydroxide or potassium hydroxide；
C. precipitation reaction：It is added in old halogen A, the aqueous slkali B of preparation to solution by 1~5mL/min rate of addition
PH=11~12；Precipitation reaction is carried out, is then transferred in reactor, the stirring reaction 6~48 hours at 40 DEG C~100 DEG C；Instead
Solution temperature is down to 20~60 DEG C after should terminating, is filtrated to get Mg (OH)2Filter cake, dried 6~24 hours at 60~100 DEG C,
Solid magnesium hydroxide products are obtained, molecular formula is：Mg(OH)2, purity is more than 99%.
D. magnesium hydroxide solid step C obtained, under air or oxygen atmosphere, with 1-10 DEG C/min heating rate liters
To 500 DEG C~1000 DEG C temperature, 3-12 hours are calcined, obtain high purity solid magnesium oxide product, molecular formula is：MgO, purity are more than
99%.
E. it is 5~20g/L the filtrate of step C filtering to be concentrated by evaporation to lithium concentration, obtains rich lithium solution, can be straight
Connect for preparing lithium carbonate product.
Precipitation reaction described in step C, more preferable technique is by step A old halogen and aqueous slkali B while pours into colloid mill,
1-10 minutes are rotated with 1000-5000 turns/min rotating speed, form Mg (OH)2Nucleus solution；According still further to the method described in step C
Crystallization, filtering, drying.Solid magnesium hydroxide products are obtained, molecular formula is：Mg(OH)2, purity is more than 99%.
Beneficial effects of the present invention：
(1) while salt lake bittern magnesium, lithium separation, nanometric magnesium hydroxide and high-purity magnesium oxide product is produced, is one
Kind reaction-separation coupling technology.Not only realize salt lake it is important, it is difficult separation and Extraction resource efficiently separate, again obtain it is important
Magnesium products.
(2) magnesium in bittern is separated by forming magnesium hydroxide solid, overcome it is traditional from high magnesium/lithium than molten
Separating magnesium, the difficulty of lithium method in liquid, the loss late of lithium is small (being less than 10%), and high income (is more than 90%), and separation process is simple.
(3) the magnesium hydroxide purity prepared is high, ensure that the magnesia obtained after roasting have high-purity (>99%) it is, full
Requirement under the various applications of foot to magnesium oxide product purity.
Embodiment
Solution used in example below is Bittern from East Taijinaier Salt Lake, and its composition see the table below
Embodiment 1
A. in salt lake bittern solution A：[Mg2+]=80g/L, [Li+]=5g/L, take 250mL solution.
B. NaOH 66.7g are weighed, are dissolved in 250mL deionized waters, obtain aqueous slkali B.
C. old halogen solution A and aqueous slkali B are poured into colloid mill simultaneously, rotated 2 minutes with 1000r/min rotating speed, formed
Mg(OH)2Nucleus, nucleus solution is transferred to reactor, crystallization is stirred 10 hours at 40 DEG C, reacted solution temperature after terminating
20 DEG C are down to, is filtrated to get Mg (OH)2Filter cake, dried 8 hours at 60 DEG C, obtain solid Mg (OH)2Product, molecular formula are：Mg
(OH)2, purity 99.0%
D. the Mg (OH) step C obtained2Solid, with 5 DEG C/min of heating rate, rises to 600 DEG C, insulation under air atmosphere
6 hours, roasting obtained solid oxidation magnesium, and molecular formula is：MgO, purity 99.0%
E. it is 5g/L step C filtrate to be concentrated by evaporation at 40 DEG C to lithium concentration, now the sodium ion in filtrate
Crystallized and separated out with NaCl.Lithium sodium ion in liquor content<10%.The loss late of lithium is 6.5% in filtrate.
Embodiment 2
A. in salt lake bittern solution A：[Mg2+]=60g/L, [Li+]=1g/L, take 250mL solution.
B. NaOH 50g are weighed, are dissolved in 250mL deionized waters, obtain aqueous slkali B.
C. old halogen solution A and aqueous slkali B are poured into colloid mill simultaneously, rotated 2 minutes with 1000r/min rotating speed, formed
Mg(OH)2Nucleus, nucleus solution is transferred to reactor, crystallization is stirred 10 hours at 40 DEG C, reacted solution temperature after terminating
20 DEG C are down to, is filtrated to get Mg (OH)2Filter cake, dried 8 hours at 60 DEG C, obtain solid Mg (OH)2Product, molecular formula are：Mg
(OH)2, purity 99.2%.
D. the Mg (OH) step C obtained2Solid is calcined under air atmosphere, 2 DEG C/min of heating rate, rises to 500 DEG C, is protected
Temperature 5 hours, obtains solid oxidation magnesium, molecular formula is：MgO, purity 99.2%.
E. it is 6g/L step C filtrate to be concentrated by evaporation at 60 DEG C to lithium concentration, now the sodium ion in filtrate
Crystallized and separated out with NaCl.Lithium sodium ion in liquor content<10%.The loss late of lithium is 4.5% in filtrate.
Embodiment 3
A. in salt lake bittern solution A：[Mg2+]=70g/L, [Li+]=3g/L, take 250mL solution.
B. NaOH 58.3g are weighed, are dissolved in 250mL deionized waters, obtain aqueous slkali B.
C. old halogen solution A and aqueous slkali B are poured into colloid mill simultaneously, rotated 3 minutes with 3000r/min rotating speed, formed
Mg(OH)2Nucleus, nucleus solution is transferred to reactor, crystallization is stirred 12 hours at 50 DEG C, reacted solution temperature after terminating
30 DEG C are down to, is filtrated to get Mg (OH)2Filter cake, dried 10 hours at 70 DEG C, obtain solid Mg (OH)2Product, molecular formula are：Mg
(OH)2, purity 99.0%.
D. the Mg (OH) step C obtained2Solid is calcined under air atmosphere, 7 DEG C/min of heating rate, rises to 700 DEG C, is protected
Temperature 8 hours, obtains solid oxidation magnesium, molecular formula is：MgO, purity 99.0%.
E. it is 8g/L step C filtrate to be concentrated by evaporation at 50 DEG C to lithium concentration, now the sodium ion in filtrate
Crystallized and separated out with NaCl.Lithium sodium ion in liquor content<10%.The loss late of lithium is 5.2% in filtrate.
Embodiment 4
A. in salt lake bittern solution A：[Mg2+]=90g/L, [Li+]=10g/L, take 250mL solution.
B. NaOH 75g are weighed, are dissolved in 250mL deionized waters, obtain aqueous slkali B.
C. old halogen solution A and aqueous slkali B are poured into colloid mill simultaneously, rotated 5 minutes with 4000r/min rotating speed, formed
Mg(OH)2Nucleus, nucleus solution is transferred to reactor, crystallization is stirred 24 hours at 80 DEG C, reacted solution temperature after terminating
50 DEG C are down to, is filtrated to get Mg (OH)2Filter cake, dried 12 hours at 90 DEG C, obtain solid Mg (OH)2Product, molecular formula are：Mg
(OH)2, purity 99.3%.
D. the Mg (OH) step C obtained2Solid is calcined under air atmosphere, 8 DEG C/min of heating rate, rises to 800 DEG C, is protected
Temperature 10 hours, obtains solid oxidation magnesium, molecular formula is：MgO, purity 99.3%.
E. it is 9g/L step C filtrate to be concentrated by evaporation at 80 DEG C to lithium concentration, now the sodium ion in filtrate
Crystallized and separated out with NaCl.Lithium sodium ion in liquor content<10%.The loss late of lithium is 6.8% in filtrate.
Claims (1)
1. a kind of salt lake bittern magnesium, lithium separate and produce magnesium hydroxide and the method for high-purity magnesium oxide, concretely comprise the following steps：
A. salt lake bittern is separated out into a large amount of NaCl, KCl by solar evaporation, refilters removal insoluble impurities, it is molten to obtain old halogen
Liquid；Wherein each cation concn is：[Li+]=0.3~10g/L, [Mg2+]=30~100g/L, [K+]=0.5~12g/L,
[Na+]=1~20g/L；
Described salt lake bittern is Salt Lake Brines In Qaidam Basin, wherein each cation concn is：[Li+]=0.3~10g/L,
[Mg2+]=10~100g/L, [K+]=1~30g/L, [Na+]=10~90g/L；
B. magnesium ion content in old halogen in step A prepares aqueous slkali B, its volume is identical with solution A volume, and alkali rubs
Your number is 1.6-2.5 times of magnesium ion；The aqueous slkali is the aqueous solution of sodium hydroxide or potassium hydroxide；
C. step A old halogen and aqueous slkali B are poured into colloid mill simultaneously, with 1000-5000 turns/min 1-10 points of rotating speed rotation
Clock, form Mg (OH)2Nucleus solution；It is then transferred in reactor, the stirring reaction 6~48 hours at 40 DEG C~100 DEG C；Reaction
Solution temperature is down to 20~60 DEG C after end, is filtrated to get Mg (OH)2Filter cake, dry 6~24 hours, obtain at 60~100 DEG C
To solid magnesium hydroxide products, molecular formula is：Mg(OH)2, purity is more than 99%；
D. magnesium hydroxide solid step C obtained, under air or oxygen atmosphere, risen to 1-10 DEG C/min heating rates
500 DEG C~1000 DEG C temperature, 3-12 hours are calcined, obtain high purity solid magnesium oxide product, molecular formula is：MgO, purity are more than
99%；
E. it is 5~20g/L the filtrate of step C filtering to be concentrated by evaporation to lithium concentration, obtains rich lithium solution, can directly use
In preparing lithium carbonate product.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107043116B (en) * | 2017-04-24 | 2018-10-23 | 北京化工大学 | The method extracted lithium from demagging brine and prepare battery-level lithium carbonate |
| 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 |
| CN110817909B (en) * | 2019-11-19 | 2022-07-12 | 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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| CN105060320A (en) * | 2015-07-23 | 2015-11-18 | 韦海棉 | Method for preparing magnesium hydroxide by high magnesium-lithium ratio salt lake brine |
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| CN105060320A (en) * | 2015-07-23 | 2015-11-18 | 韦海棉 | Method for preparing magnesium hydroxide by high magnesium-lithium ratio salt lake brine |
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