CN110482576A - A kind of method that lepidolite hydro-thermal prepares lithium salts - Google Patents
A kind of method that lepidolite hydro-thermal prepares lithium salts Download PDFInfo
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- CN110482576A CN110482576A CN201910914545.6A CN201910914545A CN110482576A CN 110482576 A CN110482576 A CN 110482576A CN 201910914545 A CN201910914545 A CN 201910914545A CN 110482576 A CN110482576 A CN 110482576A
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- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/02—Oxides; Hydroxides
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Abstract
The invention belongs to ore extractive technique fields, and in particular to a kind of method that lepidolite hydro-thermal prepares lithium salts, the essence of method be roast defluorinate lepidolite occurs in hydro-thermal reaction replace mention lithium and along with the reconstruct of mine phase.The sial ratio during defluorinate lepidolite reconstructs zeolite is adjusted as additive using sodium aluminate in the present invention, lepidolite powder, alkali and the additive and water that roast defluorinate are sized mixing in proportion and sent into normal-pressure reaction kettle, low-temperature hydrothermal reaction leaching mentions lithium and reconstructs generation zeolite, it is separated by filtration zeolite filter residue and obtains filtrate, final lithium salts product can be obtained through removal of impurities concentration, Crystallization Separation, washing drying.This method process is short, safety and environmental protection, recovery rate are high, and reaction temperature is low, and reaction slag can comprehensively utilize again；Remarkable in economical benefits has good industrial prospect.
Description
Technical field
The invention belongs to ore extractive technique fields, particularly relate to a kind of method that lepidolite hydro-thermal prepares lithium salts.
Background technique
Lepidolite is one of the essential mineral resource for extracting lithium salts, and " lithium " is referred to as " energy gold of 21 century
Belong to ", it is applied in many ways in each industrial circle, especially in the lithium electricity New Energy Industry field quickly grown.In world energy sources shape
Under the situation of gesture growing tension, the development and utilization of new energy have become the joint demand of countries in the world.Lepidolite is as a kind of
Important lithium resource, Li2O content is generally in 1.2-5.9wt%.
Lepidolite category laminar silicic acid salt system, common is trioctahedron type structure.Active oxygen is opposite in structural unit layer
Two layers of [SiO4] one layer of [AlO of tetrahedron sandwich6] octahedra, unit interlayer deposits K+、Na+、Ca2+Etc. large radius cation it is flat
Weigh interlayer charge, and structural formula is K (Li, Al)3[(Si, Al)4O10](F, OH)2, wherein isomorph substitution is relatively broad,
Al-Li series is restricted isomorphism, and Fe-Li series is then perfect isomorphism, can occur mutually to replace between F and OH
Generation.Existing research shows that all micas containing Li, contain a certain number of F, and Li content is higher, F content is also got over
It is high.In lepidolite ore the height of fluorine content largely influence it is subsequent mention lithium yield, and fine and close layered silicate structure
And in octahedron charge ion constraint but also Li therein is difficult to be leached under normal pressure state.
It reports both at home and abroad at present and the lepidolite extracted lithium technique of exploitation is largely divided into wet process and pyrogenic process two major classes, by preparatory
Original mineral phase structure is destroyed, Li therein is made to be transformed into solvable lithium salts, obtains corresponding lithium salts product through subsequent carbonization sinker.Wherein
Wet process is divided into sulfuric acid process, fluorine chemistry method, pressure leaching method etc. again.
Patent of invention CN108163874A discloses a kind of method of High-temperature water heat treatment lepidolite production lithium hydroxide.It should
Method passes through first by lepidolite wet ball grinding, is then sent through 4 ~ 8h of preheating, preheating temperature in still preheater after mixing with calcium oxide
100℃.It is transferred to spray tower after completing, 90S or so is kept at 350 ~ 450 DEG C, slurry leaches concentration later, at desalination
Reason obtains lithium hydroxide.The method complex process is easily corroded under hot conditions since the fluorine element in mineral system does not remove
Production equipment and cause environmental pollution；Furthermore for a long time preheating and high temperature hydro-thermal can all cause a large amount of Si, Al, Ca,
Mg ion leaches therewith, so that impurity removal process is complicated, equipment investment increases.
A kind of technique of lepidolite sulfuric acid autoclaving extraction lithium salts is disclosed in patent CN104140117A, lepidolite exists in advance
800 DEG C or more high-temperature roasting transition, cooling levigate 1 ~ 3h of low-temperature bake together with the concentrated sulfuric acid roast slurry at 100 ~ 270 DEG C
1 ~ 3.5h of autoclaving obtains lithium sulfate solution, by separation, impurity removal, the sinker that is carbonized and etc. obtain lithium carbonate product.This method realizes
Lepidolite extracted lithium prepares the purpose of lithium salts, but since the method using double roasting handles lepidolite, heating energy consumption is high, consumption
The amount of sulfuric acid is also very big, complex process.Secondly 100 ~ 270 DEG C are heated to slurry using 0.8 ~ 6 MPa high steam to be pressed
Boil reaction, it is necessary to use pressure-resistant equipment, the requirement to technique and safety greatly improves.
A kind of method that the dissolution of defluorinate lepidolite pipeline mentions lithium is proposed in patent CN107739039A, is by defluorinate lithium
Mica miberal powder and alkali or alkaline earth metal sulfate, additive and water are in 1:(0.5 ~ 2): (0.01 ~ 1): the ratio of (4 ~ 20)
Mixing, which is transported to again in pipeline reactor, carries out high temperature and pressure dissolution reaction, and it is molten that the lithium progress ion exchange in mineral becomes salt
Out.It is to be easy to pressurize using pipeline reactor compared with other propose lithium technology, without stirring for reaching by feed liquid itself turbulent flow
The state mixed is contacted, but bonding phenomenon is easily occurred using pipeline reactor, influences mass transfer effect.And reaction product ingredient is multiple
Miscellaneous, separation process also needs to increase accordingly, and equipment throughput is big, and energy consumption is high.
Summary of the invention
It is an object of that present invention to provide a kind of simple process, low energy consumption, yield is high, environmentally protective lepidolite hydro-thermal system
The method of standby lithium salts.
In order to achieve the above object, the present invention takes following technical scheme:
A kind of method that lepidolite hydro-thermal prepares lithium salts, concrete technology flow process comprise the steps of:
(1) lepidolite ore by mechanical lapping to partial size less than 0.14mm is passed through steam at 800 ~ 900 DEG C and roasts 10 ~ 120min
Defluorinate transition is carried out, room temperature cooling is levigate to powder particle size < 0.074mm；
(2) the roasting clinker of above-mentioned milled is mixed with a certain amount of alkali and additive, the water that corresponding amount is added is sized mixing, and control is solid
Liquid mass ratio is (0.12 ~ 0.4): 1, then it is transferred to 1 ~ 6h of reaction in atmospheric agitation kettle
(3) by the leached mud countercurrent washing after above-mentioned reaction, isolated filter residue and filtrate, filter residue is absorption property good eight
Face zeolite can be used for the industries such as water process after separating-purifying.Filtrate cleans and carries out evaporation and concentration and freezing and crystallizing, centrifuge separation
After removal of impurities, then condensing crystallizing, centrifugal drying obtains monohydrate lithium hydroxide product, in lithium hydroxide crystalline mother solution and filter operation
The blending process of cleaning solution return step (2).
Further, when lepidolite described in step (1) roasts the steam flow that is passed through be per kilogram lepidolite 0.05 ~
0.5L/h, Li in lepidolite2O content is in 1.5 ~ 4.5wt%, fluorine content detection < 0.35wt% in the lepidolite ore after roasting.
Further, alkali described in step (2) is sodium hydroxide or potassium hydroxide；With lepidolite in mass ratio (0.05 ~
0.25): 1 mixing is sized mixing.
Further, additive is any one of sodium aluminate or sodium aluminate and sodium sulphate, sodium chloride composition, mass ratio
For lepidolite: sodium sulphate or sodium chloride: sodium aluminate=1:(0.01 ~ 3): (0.01 ~ 0.5).
Further, the reaction temperature of atmospheric agitation kettle is controlled at 60 ~ 100 DEG C in step (2).
Further, filtrate freezing and crystallizing impurity removing is saltcake or sodium chloride in step (3), back in step (2)
As additive again ingredient.
Wherein, the mass ratio of step (3) the leached mud countercurrent washing, wash water and filtrate is 2 ~ 6, washing lotion and lithium hydroxide
Crystalline mother solution is recycled to the allotment of step (2) for slurry together.
Remarkable advantage of the invention is:
The present invention is based on lepidolites to occur mineral phase structure recombination in roasting process, repeated arrangement in alumino-silicate main body
[SiO4] tetrahedron-[AlO6] octahedron-[SiO4] tetrahedral structural unit layer is changed by [SiO4] the leading rack-like of tetrahedron
Structure lithium aluminosilicate mineral realize that constant pressure hydro-thermal reaction mentions lithium and makes mine mutually reconstruct transformation again by improved formulations condition
For zeolite phase.The sial ratio in lepidolite restructuring procedure, the hydro-thermal of optimization are adjusted using addition sodium aluminate etc. in the present invention
Reaction temperature and quantity of alkali consumption is greatly reduced with reconstruction condition in leaching.Traditional high-pressure leaching process is changed into normal pressure behaviour
Make, realizes that production equipment requirement condition sexually revises at all, invests reduction, production security improves, and save the cost is suitble to scale
Production.
Detailed description of the invention
Fig. 1 is the flow diagram that the corresponding lepidolite hydro-thermal of embodiment 1 prepares lithium salts method.
Specific embodiment
The technical solution in the present invention is described further below with reference to embodiment, following embodiment is intended to elaborate
The present invention rather than invention is further limited.The percentage occurred in the present invention is mass percent.
Embodiment 1
Mechanical lapping to 300 mesh lepidolite ores (Li 1.58wt%, F 3.47wt%) is passed through to steam roasting defluorinate at 840 DEG C
50min, steam flow set are 0.4L/ (hkg), and room temperature cooling is levigate to account for 60wt% to powder particle size < 0.074mm, and fluorine contains
Amount is detected as 0.30wt%.The roasting clinker of defluorinate is mixed with sodium hydroxide, sodium aluminate 1:0.15:0.05 in mass ratio, simultaneously
The water that three parts of lepidolite quality are added is sized mixing, and is moved into temperature control and is stirred 5h in 80 DEG C of reaction kettle, lithium recovery rate is
91.38%.Twice with 50 DEG C of wash water countercurrent washing, each wash water quality is suitable with filtrate quality, washes simultaneously for filter residue after reaction
Water is returned directly to constant pressure hydro-thermal step and is used for slurry, the evaporation energy consumption of reduction subsequent concentration process；The filter residue being obtained by filtration point
It applies after choosing purification in fields such as water process, resource is fully used.The simple removal filtration of filtrate, gained filtrate and washing lotion are closed
And be concentrated by evaporation to the 1/4 of former filtrate volume, 30 DEG C of crystallizations, the separation of centrifugal drying water are cooled to, dries and obtains at 80 DEG C
Monohydrate lithium hydroxide product.Be centrifuged obtain lithium hydroxide crystalline mother solution with react wash heat water mix reach required wet end furnish after
It is recycled to lepidolite normal pressure leaching process.
Embodiment 2
Mechanical lapping to 400 mesh lepidolite ores (Li 1.10wt%, F 2.54wt%) is passed through to steam roasting defluorinate at 870 DEG C
20min, steam flow set are 0.1L/ (hkg), and room temperature cooling is levigate to account for 90wt% to powder particle size < 0.074mm, and fluorine contains
Amount is detected as 0.21wt%.It is mixed with 1:0.12:0.32:0.08 mass ratio that defluorinate roasts clinker and caustic potash, sodium sulphate and sodium aluminate
It closes, while the water that six parts of lepidolite quality are added is sized mixing, is moved into temperature control and stirs 2h, lithium in 100 DEG C of reaction kettle
Recovery rate is 94.45%.Filter residue after reaction is with wash water countercurrent washing four times of 30 DEG C, each wash water quality and filtrate quality phase
When, while wash water is returned directly to constant pressure hydro-thermal step and is used for slurry, the evaporation energy consumption of reduction subsequent concentration process；It is obtained by filtration
Filter residue sorting purification after apply in fields such as water process, resource is comprehensively utilized.The simple removal filtration of filtrate, gained filtrate
It is concentrated by evaporation with washing lotion merging to the 1/3 of former filtrate volume, freezing separating mirabilite crystallization；The crystallization of residual filtrate room temperature, from
Heart water dumping separation, drying obtains monohydrate lithium hydroxide product at 100 DEG C.Be centrifuged obtain lithium hydroxide crystalline mother solution with react
The mixing of wash heat water is recycled to lepidolite normal pressure leaching process after reaching required wet end furnish.
Embodiment 3
Mechanical lapping ~ 500 mesh lepidolite ores (Li 1.83wt%, F 4.01wt%) are passed through to steam roasting defluorinate at 860 DEG C
30min, steam flow set are 0.2L/ (hkg), and room temperature cooling is levigate to account for 80wt% to powder particle size < 0.074mm, and fluorine contains
Amount is detected as 0.34wt%.Roasting clinker is mixed with sodium hydroxide, sodium chloride and sodium aluminate with 1:0.1:0.15:0.2 mass ratio,
The water that five parts of lepidolite quality are added simultaneously is sized mixing, and is moved into 95 DEG C of temperature control of reaction kettle and is stirred 6h, lithium recovery rate is
92.96%.Three times with 20 DEG C of wash water countercurrent washing, each wash water quality is suitable with filtrate quality, washes simultaneously for filter residue after reaction
Water is returned directly to constant pressure hydro-thermal step and is used for slurry, the evaporation energy consumption of reduction subsequent concentration process；The filter residue being obtained by filtration is excellent
It is applied after choosing in fields such as soil remediations, resource is comprehensively utilized.The simple removal filtration of filtrate, gained filtrate and washing lotion merge
It is evaporated and is concentrated into the 1/4 of former filtrate volume, crystallisation by cooling, filtration washing, last centrifugal drying water separation dries at 90 DEG C
Obtain monohydrate lithium hydroxide product.It is centrifuged the lithium hydroxide crystalline mother solution obtained and reaches required slurry and match with reacting wash heat water and mix
Lepidolite normal pressure leaching process is recycled to than after.
The above is a part of the embodiments of the present invention, instead of all the embodiments.It should be pointed out that for this field
For technical staff, the several modifications and improvements done without making creative work also belong to guarantor of the present invention
The range of shield, these all will not influence the effect and patent practicability that the present invention is implemented.
Claims (6)
1. a kind of method that lepidolite hydro-thermal prepares lithium salts, it is characterised in that: the following steps are included:
(1) lepidolite ore by mechanical lapping to partial size less than 0.14mm is passed through steam at 800 ~ 900 DEG C and roasts 1 ~ 120min
Defluorinate is carried out, cooling is levigate to powder particle size < 0.074mm；
(2) the roasting clinker of above-mentioned milled is mixed with a certain amount of alkali and additive, the water that corresponding amount is added is sized mixing, control
Solid-liquid mass ratio is (0.12 ~ 0.4): 1,1 ~ 6h of reaction under certain temperature is then transferred in atmospheric agitation kettle；
(3) by the slurry filtration after above-mentioned reaction, leached mud countercurrent washing, isolated filter residue and filtrate, filter residue is industry boiling
Stone；Filtrate cleans and carries out evaporation and concentration and freezing and crystallizing, after centrifuge separation removal of impurities, then condensing crystallizing, it is dried to obtain single water hydrogen
Lithia product, the cleaning solution in lithium hydroxide crystalline mother solution and filter operation are back to the blending process of step (2).
2. the method that a kind of lepidolite hydro-thermal according to claim 1 prepares lithium salts, it is characterised in that: lithium in step (1)
The steam flow that mica is passed through when roasting is 0.05 ~ 0.5L/h of per kilogram lepidolite, Li in lepidolite2O content 1.5 ~
4.5wt%, fluorine content detection < 0.35wt% in the lepidolite ore after roasting.
3. the method that a kind of lepidolite hydro-thermal according to claim 1 prepares lithium salts, it is characterised in that: institute in step (2)
The alkali stated is potassium hydroxide or sodium hydroxide, and lepidolite (0.05 ~ 0.25) in mass ratio: 1 mixes and sizes mixing.
4. the method that a kind of lepidolite hydro-thermal according to claim 1 prepares lithium salts, it is characterised in that: institute in step (2)
Stating additive is that sodium aluminate or any one of sodium aluminate and sodium sulphate, sodium chloride form, and mass ratio is lepidolite: sodium sulphate
Or sodium chloride: sodium aluminate=1:(0.01 ~ 3): (0.01 ~ 0.5).
5. the method that a kind of lepidolite hydro-thermal according to claim 1 prepares lithium salts, it is characterised in that: institute in step (2)
The reaction temperature for stating atmospheric agitation kettle is controlled at 60 ~ 100 DEG C.
6. the method that a kind of lepidolite hydro-thermal according to claim 1 prepares lithium salts, it is characterised in that: filter in step (3)
Liquid freezing and crystallizing impurity removing is saltcake or sodium chloride, is used as additive ingredient again back to step (2) are middle.
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| CN111302365A (en) * | 2020-02-13 | 2020-06-19 | 雅化锂业(雅安)有限公司 | Production process of battery-grade lithium hydroxide |
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Effective date of registration: 20230802 Address after: 336699 North of Qingyi Road, Chengxi Industrial Park, Fenyi County, Xinyu City, Jiangxi Province Patentee after: Xinyu Guoxing Lithium Industry Co.,Ltd. Address before: School of petroleum and chemical engineering, Fuzhou University (Quangang campus), No.1 Xueyuan Road, Qianhuang Town, Quangang District, Quanzhou City, Fujian Province, 362801 Patentee before: FUZHOU University |
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