CN109321748A - A method of extracting lithium, rubidium and by-product zeolite or kaliophilite from lepidolite ore - Google Patents
A method of extracting lithium, rubidium and by-product zeolite or kaliophilite from lepidolite ore Download PDFInfo
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- CN109321748A CN109321748A CN201811340951.8A CN201811340951A CN109321748A CN 109321748 A CN109321748 A CN 109321748A CN 201811340951 A CN201811340951 A CN 201811340951A CN 109321748 A CN109321748 A CN 109321748A
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- rubidium
- lithium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/12—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/26—Aluminium-containing silicates, i.e. silico-aluminates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/262—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds using alcohols or phenols
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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Abstract
The present invention provides a kind of method that lithium, rubidium and by-product zeolite or kaliophilite are extracted from lepidolite ore, belongs to technical field of wet metallurgy.Lepidolite ore is added in reactor with sodium hydroxide or potassium hydroxide solution and is stirred by this method, controls temperature appropriate in atmospheric conditions and carries out mine phase transition.By mine phase transition, lepidolite is changed into zeolite or kaliophilite, and the lithium, rubidium in lepidolite are then transferred into solution, obtains the solution containing lithium, rubidium, and lithium product can be obtained from solution by chemical precipitation, and rubidium can be recycled from solution by extraction.This method uses Whote-wet method technical treatment lepidolite ore, had both realized the extraction of valuable metal lithium, rubidium in the type lithium mine, and had obtained zeolite, the kaliophilite product of high added value further through mine phase transition, finally realized the comprehensive utilization of resource.Furthermore the present invention has the characteristics that process is short, process is few, energy consumption cost is low, and meets the environmental requirement of clean manufacturing.
Description
Technical field
The present invention relates to technical field of wet metallurgy, particularly relate to one kind and extract lithium, rubidium and by-product boiling from lepidolite ore
The method of stone or kaliophilite.
Background technique
Currently, the method for extracting lithium from lepidolite mainly has sulfuric acid process, lime-roasting method, autoclaving method, chlorinating roasting
Deng.Chinese patent CN201210512662.8 discloses a kind of method for extracting lithium from lepidolite raw material using sulfuric acid process, will
It is reacted under pressurised conditions with sulfuric acid solution after lepidolite calcining, acidleach temperature is 85~95 DEG C.Chinese patent
CN201210080657.4 discloses a kind of method using autoclaving method processing lepidolite ore, the calcining warp after lepidolite is roasted
Autoclaving leaches after mixing again with lime and alkali metal sulfates or alkali metal chloride after mechanical activation processing.Chinese patent
CN201711443400.X discloses a kind of method that two sections of chloridising roasting-water seaonings extract lithium from lepidolite, by lepidolite
It is added to mixing pelletizing in ammonium chloride solution after mine and calcium chloride are levigate and obtains green-ball, green-ball is carried out one at 150~300 DEG C
Section roasting, then carry out two-stage calcination at 500~800 DEG C and obtain clinker, clinker water logging is gone out, leachate is obtained, in water logging
Precipitating reagent sinker is added in liquid.Sulfuric acid process can generate a series of neutralization slags, and lime-roasting method has the utilization of leached mud difficulty,
For autoclaving method due to using pressure vessel, the high requirements on the equipment, chlorinating roasting be easy to cause equipment to corrode.It is mentioned from lepidolite
Lithium is a complicated chemical process, how to accomplish comprehensive utilization of resources during the extraction process, reduces pollutant emission, simplifies work
Skill process is to need constantly to solve the problems, such as.
The method of artificial synthetic zeolite mainly has hydrothermal synthesis method at present, using flyash or kaolin as raw material, 100~
It is synthesized in 200 DEG C of Hydro-thermal pressure reaction kettle.
Summary of the invention
The technical problem to be solved in the present invention is to provide one kind to extract lithium, rubidium and by-product zeolite or potassium rosy clouds from lepidolite ore
The method of stone.
Present invention process object is lepidolite ore, specifically includes that steps are as follows:
(1) lepidolite ore is added in reactor with sodium hydroxide solution or potassium hydroxide solution and is stirred, in normal pressure
Under the conditions of control temperature appropriate and carry out the reaction of mine phase transition；
(2) ore pulp of step (1) after the reaction was completed is diluted with water, by solid-liquor separation obtain containing lithium, rubidium solution and
Zeolite or kaliophilite product；
(3) sodium carbonate or sodium phosphate is added by precipitation reaction in the solution containing lithium, rubidium for obtaining step (2), is sunk
Liquid and lithium carbonate or lithium phosphate product after lithium；
(4) t-BAMBP extraction and recovery rubidium is added in liquid after the sinker for obtaining step (3).
Wherein, in step (1) lepidolite ore contain Li 0.1~3%, Rb 0.05~1%, feed size be 100 mesh hereinafter,
Reaction temperature is 260~350 DEG C, and reactor is normal pressure operation, and naoh concentration or concentration of potassium hydroxide are 50~90%, hydrogen
The weight ratio of sodium oxide molybdena or potassium hydroxide and lepidolite ore is 1:1~10:1, and the reaction time is 0.5~3h.
The weight that water used is diluted in step (2) is 2~10 times of lepidolite weight.
The present invention using high concentration alkaline media reactivity it is strong, good fluidity, boiling point are high, steam forces down the characteristics of,
It under condition of normal pressure, is reacted by the sodium hydroxide or potassium hydroxide of high concentration with lepidolite, makes its mine phase transition zeolite or potassium
Nepheline, while realizing the extraction of lithium, rubidium.
Above-mentioned technical proposal has the beneficial effect that:
It is reacted in atmospheric conditions by the sodium hydroxide or potassium hydroxide of high concentration with lepidolite, makes its mine phase transition
Zeolite or kaliophilite, while realizing the extraction of lithium, rubidium, realize the comprehensive utilization of resource.In addition synthesis under normal pressure is used, equipment is wanted
Ask simple.Technique has the advantageous feature for meeting clean manufacturing environmental requirement.
Detailed description of the invention
Fig. 1 is the method and process flow chart of the invention that lithium, rubidium and by-product zeolite or kaliophilite are extracted from lepidolite ore.
Specific embodiment
To keep the technical problem to be solved in the present invention, technical solution and advantage clearer, below in conjunction with attached drawing and tool
Body embodiment is described in detail.
The present invention provides a kind of method that lithium, rubidium and by-product zeolite or kaliophilite are extracted from lepidolite ore.Such as Fig. 1 institute
Show, is the process flow chart of this method.This method be specially mine phase transition react, be diluted with water, solid-liquor separation, below
It is explained in conjunction with specific embodiments.
Embodiment 1
(1) 80g lepidolite ore (containing Li 2.2%, Rb 0.6%, -100 mesh of granularity) is mixed with 60% sodium hydroxide solution
It closes, wherein the weight ratio of sodium hydroxide and lepidolite ore is 4.8:1, is 270 DEG C of reaction 2h in temperature.
(2) ore pulp of step (1) end of reaction being diluted with water, the weight for diluting water used is 3 times of lepidolite weight,
It is obtained by filtration lithium-containing solution and zeolite product, lithium recovery rate is up to 94.2%, and rubidium recovery rate is up to 96.4%.
(3) sodium carbonate is added by precipitation reaction in the solution containing lithium, rubidium for obtaining step (2), obtain after sinker liquid and
Lithium carbonate product.
(4) t-BAMBP extraction and recovery rubidium is added in liquid after the sinker for obtaining step (3).
Embodiment 2
(1) 80g lepidolite ore (containing Li 0.6%, Rb 0.09%, -100 mesh of granularity) is mixed with 70% sodium hydroxide solution
It closes, wherein the weight ratio of sodium hydroxide and lepidolite ore is 8:1, is 330 DEG C of reaction 0.5h in temperature.
(2) ore pulp of step (1) end of reaction being diluted with water, the weight for diluting water used is 5 times of lepidolite weight,
Solution and zeolite product containing lithium, rubidium is obtained by filtration, wherein lithium recovery rate is up to 99.1%, and rubidium recovery rate is up to 99.3%.
(3) sodium phosphate is added by precipitation reaction in the solution containing lithium, rubidium for obtaining step (2), obtain after sinker liquid and
Lithium phosphate product.
(4) t-BAMBP extraction and recovery rubidium is added in liquid after the sinker for obtaining step (3).
Embodiment 3
(1) 80g lepidolite ore (containing Li 1.8%, Rb 0.3%, -200 mesh of granularity) is mixed with 85% sodium hydroxide solution
It closes, wherein the weight ratio of sodium hydroxide and lepidolite ore is 2.8:1, is 270 DEG C of reaction 3h in temperature.
(2) ore pulp of step (1) end of reaction being diluted with water, the weight for diluting water used is 5 times of lepidolite weight,
Solution and zeolite product containing lithium, rubidium is obtained by filtration, wherein lithium recovery rate is up to 92.8%, and rubidium recovery rate is up to 94.6%.
(3) sodium phosphate is added by precipitation reaction in the solution containing lithium, rubidium for obtaining step (2), obtain after sinker liquid and
Lithium phosphate product.
(4) t-BAMBP extraction and recovery rubidium is added in liquid after the sinker for obtaining step (3).
Embodiment 4
(1) 80g lepidolite ore (containing Li 0.8%, Rb 0.09%, -100 mesh of granularity) is mixed with 60% potassium hydroxide solution
It closes, wherein the weight ratio of potassium hydroxide and lepidolite ore is 6:1, is 270 DEG C of reaction 1h in temperature.
(2) ore pulp of step (1) end of reaction being diluted with water, the weight for diluting water used is 3 times of lepidolite weight,
It is obtained by filtration containing lithium, the solution of rubidium and kaliophilite product, wherein lithium recovery rate is up to 94.4%, and rubidium recovery rate is up to 95.6%.
(3) sodium carbonate is added by precipitation reaction in the solution containing lithium, rubidium for obtaining step (2), obtain after sinker liquid and
Lithium carbonate product.
(4) t-BAMBP extraction and recovery rubidium is added in liquid after the sinker for obtaining step (3).
Embodiment 5
(1) 80g lepidolite ore (containing Li 1.6%, Rb 0.3%, -100 mesh of granularity) is mixed with 70% potassium hydroxide solution
It closes, wherein the weight ratio of potassium hydroxide and lepidolite ore is 7:1, is 260 DEG C of reaction 1h in temperature.
(2) ore pulp of step (1) end of reaction is diluted with water, the weight for diluting water used is the 3.5 of lepidolite weight
Times, it is obtained by filtration containing lithium, the solution of rubidium and kaliophilite product, wherein lithium recovery rate is up to 94.7%, and rubidium recovery rate is up to 95.9%.
(3) sodium phosphate is added by precipitation reaction in the solution containing lithium, rubidium for obtaining step (2), obtain after sinker liquid and
Lithium phosphate product.
(4) t-BAMBP extraction and recovery rubidium is added in liquid after the sinker for obtaining step (3).
The above is a preferred embodiment of the present invention, it is noted that for those skilled in the art
For, without departing from the principles of the present invention, several improvements and modifications can also be made, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (3)
1. a kind of method for extracting lithium, rubidium and by-product zeolite or kaliophilite from lepidolite ore, it is characterised in that: including following step
It is rapid:
(1) lepidolite ore is added in reactor with sodium hydroxide solution or potassium hydroxide solution and is stirred, in condition of normal pressure
Lower control temperature appropriate carries out the reaction of mine phase transition；
(2) water is added in the ore pulp of step (1) after the reaction was completed to be diluted, the solution containing lithium, rubidium is obtained by solid-liquor separation
And zeolite or kaliophilite product；
(3) sodium carbonate is added in the solution containing lithium, rubidium for obtaining step (2) or sodium phosphate carries out precipitation reaction, after obtaining sinker
Liquid and lithium carbonate or lithium phosphate product.
(4) t-BAMBP extraction and recovery rubidium is added in liquid after the sinker that step (3) obtains.
2. the method according to claim 1 for extracting lithium, rubidium and by-product zeolite or kaliophilite from lepidolite ore, feature
Be: lepidolite contains Li 0.1~3%, Rb 0.05~1% in the step (1), and granularity is 100 mesh hereinafter, reaction temperature is
260~350 DEG C, reactor is normal pressure operation, and naoh concentration or concentration of potassium hydroxide are 50~90%, sodium hydroxide or hydrogen
The weight ratio of potassium oxide and lepidolite ore is 1:1~10:1, and the reaction time is 0.5~3h.
3. the method according to claim 1 for extracting lithium, rubidium and by-product zeolite or kaliophilite from lepidolite ore, feature
Be: the weight that water used is diluted in the step (2) is 2~10 times of lepidolite weight.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811340951.8A CN109321748B (en) | 2018-11-12 | 2018-11-12 | Method for extracting lithium and rubidium from lepidolite ore and by-producing zeolite or kaliophilite |
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| CN201811340951.8A CN109321748B (en) | 2018-11-12 | 2018-11-12 | Method for extracting lithium and rubidium from lepidolite ore and by-producing zeolite or kaliophilite |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103290217A (en) * | 2013-06-20 | 2013-09-11 | 江西省科学院应用化学研究所 | Technology for extracting lithium by processing lithium ores through high-pressure steaming process |
| CN107381605A (en) * | 2017-07-18 | 2017-11-24 | 昊青薪材（北京）技术有限公司 | A kind of NaOH decomposes the method that spodumene prepares lithium carbonate by-product analcime |
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- 2018-11-12 CN CN201811340951.8A patent/CN109321748B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103290217A (en) * | 2013-06-20 | 2013-09-11 | 江西省科学院应用化学研究所 | Technology for extracting lithium by processing lithium ores through high-pressure steaming process |
| CN107381605A (en) * | 2017-07-18 | 2017-11-24 | 昊青薪材（北京）技术有限公司 | A kind of NaOH decomposes the method that spodumene prepares lithium carbonate by-product analcime |
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