CN110482576B - Method for preparing lithium salt from lepidolite through hydrothermal method - Google Patents
Method for preparing lithium salt from lepidolite through hydrothermal method Download PDFInfo
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- CN110482576B CN110482576B CN201910914545.6A CN201910914545A CN110482576B CN 110482576 B CN110482576 B CN 110482576B CN 201910914545 A CN201910914545 A CN 201910914545A CN 110482576 B CN110482576 B CN 110482576B
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- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/02—Oxides; Hydroxides
Abstract
The invention belongs to the technical field of ore extraction, and particularly relates to a method for preparing lithium salt from lepidolite through hydrothermal reaction. In the invention, sodium aluminate is used as an additive to adjust the proportion of silicon and aluminum in the process of reconstructing zeolite by using the defluorinated lepidolite, calcined and defluorinated lepidolite powder, alkali, the additive and water are proportionally mixed and conveyed into a normal-pressure reaction kettle, low-temperature hydrothermal reaction is carried out to leach and extract lithium and reconstruct to generate zeolite, the zeolite filter residue is filtered and separated to obtain filtrate, and the final lithium salt product can be obtained through impurity removal, concentration, crystallization, separation, washing and drying. The method has the advantages of short flow, safety, environmental protection, high extraction rate, low reaction temperature and comprehensive utilization of reaction slag; has obvious economic benefit and good industrialization prospect.
Description
Technical Field
The invention belongs to the technical field of ore extraction, and particularly relates to a method for preparing lithium salt from lepidolite by hydrothermal method.
Background
Lepidolite is one of the main mineral resources for extracting lithium salt, and lithium is also called energy metal in the 21 st century, and is applied to various industrial fields, particularly the field of the lithium battery new energy industry which develops rapidly. Under the increasingly tense situation of world energy situation, the development and utilization of new energy has become a common demand of all countries in the world. Lepidolite as an important lithium resource, Li2The O content is generally from 1.2 to 5.9% by weight.
Lepidolite belongs to a layered silicate system and is usually of a trioctahedral structure. Two layers of active oxygen opposite in structural unit layer [ SiO ]4]A layer of AlO is clamped between the tetrahedron6]Octahedron, K being present between unit layers+、Na+、Ca2+The cations with the same radius balance interlayer charges, and the structural formula is K (Li, Al)3[(Si, Al)4O10](F, OH)2WhereinThe substitution of the isomorphism is wide, Al-Li series are incomplete isomorphism, Fe-Li series are complete isomorphism, and F and OH can be substituted mutually. It has been shown in previous studies that mica, where it contains Li, contains a certain amount of F, and the higher the Li content, the higher the F content. The fluorine content in the lepidolite ore greatly influences the subsequent lithium extraction yield, and the Li in the lepidolite ore is difficult to leach under the normal pressure state due to the compact layered silicate structure and the constraint of charge ions in octahedrons.
The lithium extracting process from lepidolite reported and developed at home and abroad at present mainly comprises a wet method and a fire method, wherein the original mineral phase structure is destroyed in advance to convert Li in the lepidolite into soluble lithium salt, and the lithium is subjected to subsequent carbonization and lithium precipitation to obtain a corresponding lithium salt product. The wet method is classified into a sulfuric acid method, a fluorine chemical method, a pressure leaching method, and the like.
The invention patent CN108163874A discloses a method for producing lithium hydroxide by high-temperature hydrothermal treatment of lepidolite. According to the method, lepidolite is subjected to ball milling by a wet method, is uniformly mixed with calcium oxide, and is sent to a preheating kettle to be preheated for 4-8 hours at the preheating temperature of 100 ℃. And transferring the mixture into a spray tower after the reaction is finished, keeping the temperature at 350-450 ℃ for about 90 seconds, leaching and concentrating the slurry, and desalting to obtain the lithium hydroxide. The method has complex process, and because the fluorine element in the mineral system is not removed, the method is very easy to corrode production equipment and cause environmental pollution under the high-temperature condition; in addition, a large amount of Si, Al, Ca and Mg ions are leached along with the long-time preheating and the high-temperature hydrothermal treatment, so that the impurity removal process is complex, and the equipment investment is increased.
The patent CN104140117A discloses a process for extracting lithium salt from lepidolite through sulfuric acid autoclaving, wherein lepidolite is roasted and transformed at a high temperature of more than 800 ℃ in advance, cooled and ground, roasted at a low temperature for 1-3 h together with concentrated sulfuric acid, roasting slurry is subjected to autoclaving at a temperature of 100-270 ℃ for 1-3.5 h to obtain a lithium sulfate solution, and a lithium carbonate product is obtained through steps of separation, impurity removal, carbonization, lithium precipitation and the like. The method realizes the purpose of extracting lithium from the lepidolite to prepare the lithium salt, but because the lepidolite is treated by adopting a twice roasting method, the heating energy consumption is high, the amount of consumed sulfuric acid is large, and the process is complex. And secondly, heating the slurry to 100-270 ℃ by using high-pressure steam of 0.8-6 MPa for autoclaving reaction, wherein pressure-resistant equipment is required, and the requirements on the process and the safety are greatly improved.
In patent CN107739039A, a method for tube stripping lithium extraction from defluorinated lepidolite is provided, which comprises the steps of mixing defluorinated lepidolite mineral powder with alkali metal or alkaline earth metal sulfate, additive and water according to the proportion of 1 (0.5-2): (0.01-1): (4-20), then conveying the mixture into a tube reactor for high-temperature and high-pressure stripping reaction, and carrying out ion exchange on lithium in minerals to convert the lithium into salt for stripping. Compared with other lithium extraction technologies, the method has the advantages that the pipeline reactor is easy to pressurize, stirring is not needed, the contact and uniform mixing state is achieved by the turbulence of the material liquid, but the pipeline reactor is easy to generate the bonding phenomenon, and the mass transfer effect is influenced. And the components of the reaction products are complex, the separation process is correspondingly increased, the material flux of the equipment is large, and the energy consumption is high.
Disclosure of Invention
The invention aims to provide a method for preparing lithium salt from lepidolite by a hydrothermal method, which is simple in process, low in energy consumption, high in yield and environment-friendly.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing lithium salt from lepidolite by hydrothermal method comprises the following steps:
(1) introducing water vapor into lepidolite ore which is mechanically ground to the particle size of less than 0.14mm at 800-900 ℃, roasting for 10-120 min, defluorinating and transforming, cooling at room temperature, and grinding until the particle size of the ore powder is less than 0.074 mm;
(2) mixing the ground roasting clinker with a certain amount of alkali and additives, adding a corresponding amount of water for size mixing, controlling the solid-liquid mass ratio to be (0.12-0.4): 1, and then transferring the mixture to a normal-pressure stirring kettle for reaction for 1-6 hours
(3) And (3) washing the leached residues after the reaction in a counter-current manner, separating to obtain filter residues and filtrate, wherein the filter residues are faujasite with good adsorption performance, and can be used in industries such as water treatment and the like after separation and purification. Removing impurities from the filtrate, evaporating, concentrating, freezing, crystallizing, centrifuging, drying to obtain lithium hydroxide monohydrate, and returning the lithium hydroxide crystallization mother liquor and the washing liquor in the filtering operation to the burdening process in the step (2).
Further, the flow rate of water vapor introduced during the calcination of the lepidolite in the step (1) is 0.05-0.5L/h per kilogram of the lepidolite, and Li in the lepidolite2The O content is 1.5-4.5 wt%, and the fluorine content in the calcined lepidolite ore is detected<0.35wt%。
Further, the alkali in the step (2) is sodium hydroxide or potassium hydroxide; mixing the mica powder and the lepidolite according to the mass ratio of (0.05-0.25) to 1, and mixing and pulping.
Further, the additive is sodium aluminate, or sodium aluminate and any one of sodium sulfate and sodium chloride, and the mass ratio is lepidolite: sodium sulfate or sodium chloride: sodium aluminate =1 (0.01-3) and (0.01-0.5).
Further, the reaction temperature of the normal-pressure stirring kettle in the step (2) is controlled to be 60-100 ℃.
Further, freezing and crystallizing the filtrate in the step (3) to remove impurities, namely mirabilite or sodium chloride, and returning to the step (2) to be used as an additive for re-compounding.
And (3) washing the leached residues in the step (3) in a counter-current manner, wherein the mass ratio of washing water to filtrate is 2-6, and the washing liquid and the lithium hydroxide crystallization mother liquor are circulated to the step (2) for preparing slurry.
The invention has the following remarkable advantages:
the invention is based on mineral phase structure recombination of lepidolite in roasting process, and repeated arrangement of [ SiO ] in aluminosilicate main body4]Tetrahedron- [ AlO6]Octahedron- [ SiO4]Conversion of tetrahedral structure unit layer from [ SiO ]4]The tetrahedron-dominated framework-structure lithium aluminosilicate mineral realizes normal-pressure hydrothermal reaction lithium extraction and enables the mineral phase to be reconstructed again and converted into a zeolite phase by improving the formula conditions. In the invention, sodium aluminate and the like are added to adjust the silicon-aluminum ratio in the process of reconstructing the lepidolite, and the reaction temperature and the alkali consumption are greatly reduced by the optimized hydrothermal leaching and reconstructing conditions. The traditional high-pressure leaching process is changed into normal-pressure operation, the method realizes the fundamental change of the required conditions of production equipment, reduces the investment, improves the production safety, saves the cost and is suitable for large-scale production.
Drawings
FIG. 1 is a schematic flow diagram of a hydrothermal lithium salt preparation method using lepidolite according to example 1.
Detailed Description
The technical solutions of the present invention are further illustrated below with reference to examples, which are intended to illustrate the invention in detail without further limiting the invention. The percentages presented in the present invention are mass percentages.
Example 1
The lepidolite ore (Li 1.58wt% and F3.47 wt%) mechanically ground to 300 meshes is put into water vapor at 840 ℃ for roasting and defluorination for 50min, the water vapor flow is set to be 0.4L/(h.kg), the lepidolite is cooled and ground at room temperature until the granularity of the mineral powder is less than 60wt% of 0.074mm, and the fluorine content is detected to be 0.30 wt%. Mixing the defluorinated roasted clinker with sodium hydroxide and sodium aluminate according to the mass ratio of 1:0.15:0.05, simultaneously adding three parts of water with the mass of lepidolite to mix, transferring the mixture into a reaction kettle with the temperature controlled at 80 ℃ and stirring for 5 hours, wherein the lithium extraction rate is 91.38%. Washing the reacted filter residue twice by washing water with the temperature of 50 ℃ in a countercurrent manner, wherein the quality of the washing water is equivalent to that of the filtrate every time, and meanwhile, the washing water directly returns to the normal-pressure hydrothermal step for pulp preparation, so that the evaporation energy consumption in the subsequent concentration process is reduced; the filter residue obtained by filtering is applied to the fields of water treatment and the like after separation and purification, and resources are fully utilized. And (3) simply removing impurities from the filtrate, filtering, combining the obtained filtrate and washing liquor, evaporating and concentrating to 1/4 of the volume of the original filtrate, cooling to 30 ℃ for crystallization, centrifuging, throwing water for separation, and drying at 80 ℃ to obtain a lithium hydroxide monohydrate product. And mixing the lithium hydroxide crystallization mother liquor obtained by centrifugation with reaction slag washing water to reach the required slurry proportion, and circulating to the lepidolite normal pressure leaching process.
Example 2
The lepidolite ore (Li 1.10wt% and F2.54 wt%) mechanically ground to 400 meshes is put into water vapor at 870 ℃ for roasting and defluorination for 20min, the water vapor flow is set to be 0.1L/(h.kg), the lepidolite is cooled and ground at room temperature until the granularity of the mineral powder is less than 90wt% of 0.074mm, and the fluorine content is detected to be 0.21 wt%. Mixing the defluorinated roasted clinker with caustic potash, sodium sulfate and sodium aluminate in the mass ratio of 1 to 0.12 to 0.32 to 0.08, adding six parts of lepidolite water for mixing, transferring the mixture into a reaction kettle with the temperature controlled at 100 ℃ and stirring for 2 hours, wherein the lithium extraction rate is 94.45 percent. Filter residues after reaction are washed by washing water at 30 ℃ in a countercurrent mode for four times, the quality of the washing water is equivalent to that of filtrate every time, and meanwhile the washing water directly returns to the normal-pressure hydrothermal step for pulp mixing, so that the evaporation energy consumption in the subsequent concentration process is reduced; the filter residue obtained by filtering is applied to the fields of water treatment and the like after separation and purification, and resources are comprehensively utilized. Removing impurities from the filtrate, filtering, mixing the filtrate and the washing solution, evaporating and concentrating to 1/3 of the volume of the original filtrate, and freeze-separating mirabilite crystal; crystallizing the residual filtrate at normal temperature, centrifuging, dewatering, and drying at 100 deg.C to obtain lithium hydroxide monohydrate. And mixing the lithium hydroxide crystallization mother liquor obtained by centrifugation with reaction slag washing water to reach the required slurry proportion, and circulating to the lepidolite normal pressure leaching process.
Example 3
And (2) introducing water vapor into the lepidolite ore (Li 1.83wt% and F4.01 wt%) mechanically ground to 500 meshes at 860 ℃ for roasting and defluorination for 30min, setting the water vapor flow at 0.2L/(h.kg), cooling and grinding at room temperature until the granularity of the ore powder is less than 80wt% of that of 0.074mm, and detecting the fluorine content at 0.34 wt%. Mixing the roasted clinker with sodium hydroxide, sodium chloride and sodium aluminate according to the mass ratio of 1:0.1:0.15:0.2, adding five parts of water with the mass of lepidolite to mix slurry, transferring the mixture into a reaction kettle with the temperature controlled at 95 ℃ and stirring the mixture for 6 hours, wherein the lithium extraction rate is 92.96%. Washing the reacted filter residue with washing water at 20 ℃ in a countercurrent manner for three times, wherein the quality of the washing water is equivalent to that of the filtrate every time, and meanwhile, the washing water is directly returned to the normal-pressure hydrothermal step for pulp preparation, so that the evaporation energy consumption in the subsequent concentration process is reduced; the filter residue obtained by filtering is preferably applied to the fields of soil remediation and the like, and resources are comprehensively utilized. And (3) simply removing impurities from the filtrate, filtering, combining the obtained filtrate and washing liquor, evaporating and concentrating to 1/4 of the volume of the original filtrate, cooling, crystallizing, filtering, washing, centrifuging, performing water-throwing separation, and drying at 90 ℃ to obtain a lithium hydroxide monohydrate product. And mixing the lithium hydroxide crystallization mother liquor obtained by centrifugation with reaction slag washing water to reach the required slurry proportion, and circulating to the lepidolite normal pressure leaching process.
The foregoing is directed to embodiments of the present invention, and not all embodiments of the present invention. It should be noted that, for those skilled in the art, changes and modifications can be made without inventive work within the scope of the present invention, which will not affect the effect of the present invention and the applicability of the patent.
Claims (3)
1. A method for preparing lithium salt from lepidolite by hydrothermal method is characterized by comprising the following steps: the method comprises the following steps:
(1) introducing water vapor into lepidolite ore which is mechanically ground to the particle size of less than 0.14mm at 800-900 ℃, roasting for 1-120 min for defluorination, cooling and grinding to the particle size of the ore powder of less than 0.074 mm;
(2) mixing the ground roasting clinker with a certain amount of alkali and an additive, adding a corresponding amount of water for size mixing, controlling the solid-liquid mass ratio to be (0.12-0.4): 1, and then transferring to a normal-pressure stirring kettle for reaction for 1-6 hours at a certain temperature;
(3) filtering the ore pulp after the reaction, washing leached residues in a counter-current manner, and separating to obtain filter residues and filtrate, wherein the filter residues are industrial zeolite; removing impurities from the filtrate, evaporating, concentrating, freezing, crystallizing, centrifugally separating, removing impurities, concentrating, crystallizing, drying to obtain a lithium hydroxide monohydrate product, and returning a lithium hydroxide crystallization mother liquor and a washing solution in the filtering operation to the burdening process in the step (2);
in the step (2), the additive is sodium aluminate or the additive is composed of sodium aluminate and any one of sodium sulfate and sodium chloride, and the mass ratio is lepidolite: sodium sulfate or sodium chloride: sodium aluminate =1 (0.01-3) and (0.01-0.5);
the alkali in the step (2) is potassium hydroxide or sodium hydroxide, and is mixed with lepidolite according to the mass ratio of (0.05-0.25) to 1 for size mixing;
and (3) controlling the reaction temperature of the normal-pressure stirring kettle in the step (2) to be 60-100 ℃.
2. The method for hydrothermally preparing lithium salt from lepidolite according to claim 1, wherein: in the step (1), the flow rate of introduced water vapor during the calcination of the lepidolite is 0.05-0.5L/h per kilogram of the lepidolite, and Li in the lepidolite2The O content is 1.5-4.5 wt%, and the fluorine content in the calcined lepidolite ore is detected<0.35wt%。
3. The method for hydrothermally preparing lithium salt from lepidolite according to claim 1, wherein: and (4) freezing and crystallizing the filtrate in the step (3) to remove impurities, namely mirabilite or sodium chloride, and returning to the step (2) to be used as an additive for re-compounding.
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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 |