CN108677006B - Method for extracting rubidium chloride from kaolin tailings - Google Patents
Method for extracting rubidium chloride from kaolin tailings Download PDFInfo
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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
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts 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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- 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
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/10—Hydrochloric acid, other halogenated acids or salts thereof
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- 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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- 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
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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Abstract
The invention discloses a method for extracting rubidium chloride from kaolin tailings, which comprises the steps of firstly, carrying out disc grinding and crushing on the kaolin tailings, sieving to obtain kaolin fine mineral powder, uniformly mixing the kaolin fine mineral powder with a leaching agent, pouring the uniformly mixed powder into a preheated acid solution, carrying out acid leaching to obtain an acid leaching solution, adjusting the pH of the obtained leaching solution to be close to neutral, then carrying out calcium removal to obtain a rubidium-containing leaching solution, extracting by adopting a 4-tert-butyl-2- (α -methylbenzyl) phenol solution after adding sulfonated kerosene for dilution, carrying out processes such as back extraction by adopting a hydrochloric acid solution and the like to obtain a crude rubidium salt product, dissolving and recrystallizing the crude rubidium salt product to obtain a high-purity rubidium salt product.
Description
Technical Field
The invention belongs to the field of mineral purification, and particularly relates to a method for extracting rubidium chloride from kaolin tailings.
Background
Because rubidium has unique performance, the rubidium plays an important role in both the traditional field and the new application field, and particularly has an increasingly obvious role in the high-tech field, so that the rubidium has wide application range and occupies an important position in national economy. In the traditional fields, such as catalyst, special glass, electronic devices, biological materials, etc., the development has been greatly increased in recent years. In new fields, such as rubidium atomic clock, magnetohydrodynamic power generation, energy and other fields, powerful vitality is further shown. At present, in developed countries, the ratio of rubidium used in high and new fields reaches 80%, and the ratio of rubidium used in traditional fields is 20%. Rubidium is an important raw material for manufacturing electronic devices (photomultiplier tubes and photoelectric tubes), spectrophotometers, automatic control, spectrometry, color movies, color televisions, radars, lasers, glass, ceramics, electronic clocks and the like; in terms of space technology, ion thrusters and thermionic energy converters require large amounts of rubidium; rubidium hydroxide and boride can be used as high-energy solid fuel; the radioactive rubidium can measure the mineral age; in addition, rubidium compounds are applied to the pharmaceutical industry and the paper making industry; rubidium may also act as a getter for vacuum systems.
Rubidium is a very active rare alkali metal, has a content of 0.028% in the earth crust, is extremely dispersed, has no separate mineral deposit, and is mainly present in lepidolite [ KRbLi (OH, F) Al2Si3O10Carnallite [ KCl MgCl ]2·6H2O, solid ore and salt lake brine. 55% of rubidium resources in China are stored in lepidolite, and Jiangxi Yichun, Hunan, Hubei, Henan, Guangdong, Sichuan and the like are main enrichment places of the rubidium resources in China. The content of rubidium in salt lake brine of Qinghai, Tibet plateau and other places and underground brine is also very rich, but the chemical property of rubidium is similar to the property of other coexisting metal ions, so that the industrial separation is difficult, the full utilization of rubidium resources is limited, and the yield of rubidium is low.
At present, enterprises for producing rubidium chloride and other rubidium salts in China are more, the yield is not large, the main preparation method is to extract the rubidium chloride and other rubidium salts from byproducts in the lithium salt smelting process and kaolin tailings, the extraction method is mainly to mix and granulate the rubidium chloride and then roast the rubidium chloride, the roasted minerals are crushed and then leached by water, and then processes such as calcium removal, extraction, back extraction and the like are carried out to prepare the rubidium salt product.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides the method for extracting rubidium chloride from kaolin tailings, which has the advantages of short process flow, low cost, small environmental pollution and the like.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a method for extracting rubidium chloride from kaolin tailings comprises the following steps:
(1) crushing and sieving kaolin tailings to obtain kaolin fine mineral powder;
(2) acid leaching the kaolin fine mineral powder, filtering and washing to obtain acid leaching liquid;
(3) removing calcium from the acid leaching solution to obtain a rubidium-containing leaching solution;
(4) alkalifying and extracting the rubidium-containing leachate to obtain a rubidium-rich solution;
(5) and purifying the solution rich in rubidium to obtain refined rubidium chloride.
In the above method, preferably, in the step (2), the acid used in the acid leaching process is sulfuric acid with a concentration of 10-50% or 0.5-4mol/L hydrochloric acid solution; the purpose of adding sulfuric acid or hydrochloric acid solution is to add H+. The leaching agent adopted in the acid leaching process is CaF2、NaCl、CaCl2、CaSO4And Na2SO4At least one of; crushing the leaching agent, and sieving with a 300-mesh sieve to obtain the-300-mesh leaching agent. The temperature of acid leaching is 70-95 ℃, and the leaching time is 3-10 h; the leaching temperature is increased and the leaching time is prolonged to facilitate leaching, the temperature of 70-95 ℃ is high enough for the aqueous solution under the condition of low energy consumption, and exploration experiments show that the leaching rate is not further improved after the leaching time is more than 10 hours. The mass of the leaching agent is 2-20% of the mass of the kaolin fine mineral powder, and the dosage of the acid is 50-500 ml. The exploration experiment shows that the leaching agent proportion is continuously increased, the leaching rate improving effect is not obvious, and the economic effect is not high. Through the erosion reaction of the leaching agent and acid, rubidium ions in the kaolin tailings enter the solution.
Preferably, in the step (2), in the acid leaching process, the kaolin fine ore powder and the leaching agent are uniformly mixed, and then the mixture reacts with the acid solution heated to 70-95 ℃. In the acid leaching process, the acid and the leaching agent need to be added separately, and if the acid and the leaching agent are mixed before, the acid and the leaching agent react firstly, so that the mineral decomposition effect cannot be achieved. The mineral powder and the leaching agent are mixed firstly, and then the acid solution is added to react together, so that the mineral decomposition effect is achieved.
In the above method, preferably, in the step (2), the specific operations of filtering and washing are as follows: and (3) carrying out primary vacuum filtration on the obtained solution under the condition of incomplete cooling, pulping and washing the obtained leaching residue for 20-40min, wherein the liquid-solid volume ratio is 4: 1-1: 1, followed by a second vacuum filtration with a rinse of deionized water and collection of the filtrate. The solution is filtered at high temperature, and the obtained leaching residue is pulped and washed, so that the leaching rate is further improved.
In the above method, preferably, in the step (1), the kaolin fine ore powder is fine ore powder with a-300 mesh content of more than 95%. The fine powder is beneficial to improving the leaching rate, and the leaching rate improving effect is not obvious by continuously reducing the powder granularity.
In the above method, preferably, in the step (3), the specific operation of removing calcium from the acid leachate is as follows: adding strong base into the acid leaching solution to neutralize hydrogen ions in the solution to enable the solution to be neutral, then adding carbonate or bicarbonate into the solution to enable residual calcium ions in the solution to precipitate, and stopping adding after the solution is transparent.
Preferably, in the step (4), the extracting agents adopted in the extracting process are 4-tert-butyl-2- (α -methylbenzyl) phenol and sulfonated kerosene, the back extracting agent adopted in the extracting process is hydrochloric acid solution, the concentration of the extracting agent is 0.8-1.5mol/L, the concentration of the back extracting agent hydrochloric acid solution is 0.5-3mol/L, the extracting efficiency of the extracting agent for extracting rubidium ions is highest, the cost of the sulfonated kerosene adopted as a diluent is lowest, the concentration range of the extracting agent is obtained by exploration experiments, and the cost is controlled while the extracting rate is ensured.
In the above method, in the step (4), the volume ratio of the rubidium-containing leachate to the extractant is preferably 1: 1-1: 4; the volume ratio of the obtained organic phase to the stripping agent is that the organic phase/water phase (O/A) is 4: 1-1: 1. the extraction rate and the economic effect reach the best compromise value at the ratio. The specific operation is as follows: mixing the rubidium-containing leachate with an extracting agent according to the ratio of organic phase/aqueous phase (O/A) to 1: 1-1: 4, stirring, standing, waiting for complete separation of an aqueous phase and an organic phase, respectively collecting the aqueous phase and the organic phase, mixing and stirring the obtained aqueous phase and a new organic phase, mixing and stirring the obtained organic phase and the new aqueous phase, performing the previous steps until the aqueous phase and the organic phase are completely separated, and repeating the steps until the aqueous phase does not contain rubidium ions any more, and extracting the organic phase to saturation to obtain a loaded organic phase. Mixing the obtained organic phase with a stripping solution, and performing organic phase/aqueous phase (O/A) ratio of 4: 1-1: 1, mixing and stirring, standing until the water phase and the organic phase are completely separated, respectively collecting the water phase and the organic phase, respectively mixing and stirring the obtained organic phase and new stripping solution, mixing and stirring the water phase and the new organic phase, repeating the steps until the water phase and the organic phase are completely separated, sampling and analyzing the organic phase until no rubidium ions are contained, and finally combining the obtained aqueous solutions to obtain a rubidium-rich solution.
In the above method, preferably, in the step (5), the specific operation of purifying the rubidium-rich solution to obtain purified rubidium chloride is as follows: evaporating and crystallizing the solution rich in rubidium to obtain a crude rubidium salt product, adding water into the crude rubidium salt product, heating and dissolving, alkalifying, extracting and back-extracting to obtain a back-extraction solution, concentrating, crystallizing and filtering to ensure that most of sodium chloride and potassium are left in a mother solution; based on the principle that potassium chloride and sodium chloride are slightly soluble and rubidium chloride is insoluble in anhydrous alcohol, rubidium chloride crystals are washed twice with anhydrous alcohol to obtain refined rubidium chloride.
Compared with the prior art, the invention has the advantages that:
1. the invention adopts a direct acid leaching mode, omits the common granulating and roasting processes, shortens the process flow, saves the cost, reduces the energy consumption in the sintering process, reduces the pollution of chlorine gas generated in the chlorination roasting process to the air, is more beneficial to the environmental protection and is suitable for industrialization.
2. The leaching rate of the common acid leaching is lower, generally lower than 50 percent. The invention improves the acid leaching rate by adopting the modes of grinding and crushing the tailings before acid leaching, mixing the minerals and a leaching agent, then mixing the minerals and an acid solution, filtering the solution at high temperature, pulping and washing the leached slag and the like.
3. The invention obtains the optimal process condition of direct acid leaching through a series of exploration experiments, thereby reducing the economic cost to the maximum extent while ensuring the leaching rate.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a SEM photograph of kaolin tailings of example 1 of the present invention: (a) amplifying by 100 times; (b) magnification is 1000 times.
FIG. 2 is a flow diagram of the acid direct leach of example 1 of the present invention.
FIG. 3 is a photograph of an X-ray diffraction analysis of kaolin tailing according to example 1 of the present invention.
FIG. 4 is an X-ray diffraction analysis photograph of the leached residues in example 1 of the present invention.
FIG. 5 is a scanning electron micrograph of rubidium chloride prepared in example 1 of the present invention.
FIG. 6 is a photograph of an X-ray diffraction analysis of rubidium chloride prepared in example 1 of the present invention.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
the experiment adopts rubidium-containing mineral produced by mineral processing technology provided by Changsha mining and metallurgy research institute, the mineral sample is dried and ground, and the bulk density of the mineral sample is 1.13g/cm3The true density is 2.4g/cm3The morphology of the ore sample is shown in figure 1, the acid leaching process is shown in figure 2, the phase composition is shown in figure 3, and the ore sample contains 0.2% of rubidium according to ICP analysis of national emphasis laboratory of powder metallurgy research institute of the university of Central and south China.
The method for extracting rubidium chloride from kaolin tailings comprises the following steps:
(1) adding the ore sample into a vibration disc mill, performing vibration milling for 4min, and sieving with a 300-mesh sieve to obtain 95% ore powder of-300 meshes; leaching agent CaF2Grinding with a disc mill, and sieving with a 300-mesh sieve; 200g of mineral powder and 30g of CaF are taken2Mixing leaching agents, and then adding the mixture into 400ml of sulfuric acid solution with the mass fraction of 40%;
(2) leaching conditions are as follows: sulfuric acid with the mass fraction of 40 percent and calcium fluoride with the mass fraction of 15 percent (the mass ratio of the calcium fluoride to the mineral powder) are leached, and the calcium fluoride is added to react with the sulfuric acid to release F-，F-The powder is decomposed at a liquid-solid ratio (sulfuric acid (ore powder + calcium fluoride)) of 2:1, a leaching temperature of 95 ℃ and a leaching time of 6h (the mass of the added sulfuric acid and the added calcium fluoride is based on the mass of rubidium-containing minerals), so that rubidium ions in the mixture are sufficiently leached, and the X-ray diffraction analysis result of the filtered powder sample is shown in FIG. 4, wherein the main component is SiO2；
The reaction taking place in the high temperature zone with calcium fluoride and sulphuric acid as leaching agent may be:
3Rb2O+2CaF2+4SiO2+2Al2O3+H2SO4＝2CaAl2Si2O8+4RbF+Rb2SO4+H2O
3Rb2O+2SiO2+2CaF2+H2SO4＝2CaSiO3+4RbF+Rb2SO4+H2O
7Rb2O+6CaF2+2Al2O3+H2SO4＝2Ca3Al2O6+12RbF+Rb2SO4+H2O
(3) vacuumizing and filtering the solution obtained in the step (2) under the condition of incomplete cooling, pulping and washing the obtained leaching residue for 30min once (the liquid-solid volume ratio is 1.5:1), and then performing second vacuumizing and filtering, and leaching twice with hot water (the leaching water amount is about 50mL each time) to obtain colorless and transparent leaching solution;
(4) adding NaOH into the leaching solution obtained in the step (3), and neutralizing the leaching solution until the pH value is 7;
(5) adding 400mL of leachate into the soda solution slowly while stirring, gradually adjusting the pH of the solution to be slightly more than 7.0, controlling the end-point pH, continuing stirring for 50min after stabilization, standing for 10min, then performing vacuum filtration, and leaching the calcium-removing residues with 100mL of water for three times;
(6) evaporating and concentrating 500mL of leachate obtained in the step (5) to 50mL to obtain rubidium-enriched leachate;
(7) through the processes of crushing, acid leaching, washing, neutralizing, calcium removal and evaporation, the recovery rate of rubidium reaches 83 percent, and the metal rate is higher;
(8) the concentrated solution is added with 20g/L sodium hydroxide to be alkalized to be used as extraction feed liquid, the organic phase is composed of t-BAMBP and sulfonated kerosene, and the concentration of the t-BAMBP is 1.2 mol/L. Preparing 450mL of extraction phase according to the formula, and preparing 200mL of 5g/L of LNaOH solution as a detergent and 300mL of 1mol/L of HCl stripping solution at the same time;
(9) mixing the prepared extracting agent and the concentrated solution according to the volume ratio of O/A to 1: 3, mixing and stirring, standing for layering, respectively collecting an aqueous phase and an organic phase, and then mixing a new organic phase and the aqueous phase according to the proportion of 1: 3, mixing and stirring, standing for layering, collecting a water phase and an organic phase respectively, and repeatedly performing countercurrent extraction for 3 times to obtain a loaded organic phase;
(10) mixing and washing the loaded organic phase obtained in the step (9) and the detergent prepared in the step (8) according to the ratio of O/A to 8:1 for 5min, repeatedly washing twice, and returning washing water to the step (6) for crystallization;
(11) and (3) mixing the washed organic phase with the stripping solution obtained in the step (8) according to the volume ratio of O/A to 3: 1, mixing and stirring for 5min, standing for layering, respectively collecting a water phase and an organic phase, then mixing and stirring a new stripping solution and the organic phase for 5min, standing for layering, respectively collecting the water phase and the organic phase, and repeating countercurrent stripping for 3 times to obtain a rubidium-enriched water phase;
(12) through multi-stage countercurrent extraction, washing and countercurrent back extraction, the recovery rate of rubidium reaches 97%, and the loss of rubidium in the extraction process is small;
(13) evaporating and crystallizing the water phase obtained in the step (11) to obtain crude rubidium chloride with higher impurity content compared with refined rubidium chloride;
(14) adding water into the crude rubidium salt product obtained in the step (13), heating to dissolve, alkalizing, extracting, back extracting to obtain a back extraction solution, concentrating, crystallizing, and filtering to enable most of sodium chloride and potassium to be remained in the mother liquor. Based on the principle that potassium chloride and sodium chloride are slightly soluble and rubidium chloride is insoluble in anhydrous alcohol, rubidium chloride crystals are washed twice with anhydrous alcohol to obtain refined rubidium chloride. The scanning electron micrograph is shown in FIG. 5, and the X-ray diffraction analysis is shown in FIG. 6. The purity of purified rubidium chloride is shown in table 1.
TABLE 1 purity of refined rubidium chloride
Recovery of rubidium-containing minerals at each stage: in the stages of crushing, acid leaching, washing, neutralizing, calcium removal and evaporation, the recovery rate of rubidium reaches 83%; in the extraction-washing-reverse quenching stage, the recovery rate of rubidium reaches 97 percent; in the concentrating, crystallizing and purifying stage, the recovery rate of rubidium reaches 98.8%; the total recovery rate of the rubidium-containing mineral test in the whole process reaches 79.54 percent.
Example 2:
the difference between the example and the example 1 is the step (2), the sulfuric acid with the mass fraction of 40% is replaced by the sulfuric acid with the mass fraction of 30%, and through test analysis and acid leaching operation, the leaching rate of rubidium in the mineral is 75%, and most of rubidium is leached.
Example 3:
the difference between the example and the example 1 is that in the step (2), 15% of calcium fluoride is replaced by 10% of calcium fluoride, and through test analysis and acid leaching operation, the leaching rate of rubidium in mineral powder is 73%, and most of rubidium is leached.
Example 4:
the difference of the example from the example 1 is that in the step (2), sulfuric acid with the mass fraction of 40% is replaced by 2mol/L HCl, and through detection and analysis and acid leaching operation, the leaching rate of rubidium in mineral powder is 20%, and compared with the method without adding an acid leaching agent, the leaching rate of rubidium is slightly improved.
Example 5:
this example differs from example 1 in step (2) in that 15% of the calcium fluoride is replaced by the same mass fraction of NaCl, CaCl2、CaSO4And Na2SO4Through detection and analysis and acid leaching operation, the leaching rate of rubidium in the mineral powder is improved compared with that of the mineral powder without adding a leaching agent.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A method for extracting rubidium chloride from kaolin tailings is characterized by comprising the following steps:
(1) crushing and sieving kaolin tailings to obtain kaolin fine mineral powder;
(2) acid leaching the kaolin fine mineral powder, filtering and washing to obtain acid leaching liquid;
(3) removing calcium from the acid leaching solution to obtain a rubidium-containing leaching solution;
(4) alkalifying and extracting the rubidium-containing leachate to obtain a rubidium-rich solution;
(5) purifying the solution rich in rubidium to obtain refined rubidium chloride;
in the acid leaching process, firstly, uniformly mixing fine kaolin mineral powder and a leaching agent, and then reacting with an acid solution; the leaching agent is NaCl and CaCl2、CaSO4And Na2SO4At least one of; the acid adopted in the acid leaching process is sulfuric acid with the concentration of 10-50% or hydrochloric acid solution with the concentration of 0.5-4 mol/L; the mass of the leaching agent is 2-20% of that of the kaolin fine mineral powder; the temperature of acid leaching is 70-95 ℃, and the leaching time is 3-10 h;
in the step (2), the specific operations of filtering and washing are as follows: and (3) carrying out primary vacuum filtration on the obtained solution under the condition of incomplete cooling, pulping and washing the obtained leaching residue for 20-40min, wherein the liquid-solid volume ratio is 4: 1-1: 1, followed by a second vacuum filtration with a rinse of deionized water and collection of the filtrate.
2. The method for extracting rubidium chloride from kaolin tailings as claimed in claim 1, wherein in the step (2), the amount of acid is 50-500 ml.
3. The method for extracting rubidium chloride from kaolin tailings according to claim 1, wherein in the acid leaching process in the step (2), the kaolin fine ore powder and the leaching agent are uniformly mixed, and then the mixture reacts with an acid solution heated to 70-95 ℃.
4. The method for extracting rubidium chloride from kaolin tailings according to claim 1, wherein in the step (1), the kaolin fine ore powder is a fine ore powder with a-300-mesh content of more than 95%.
5. The method for extracting rubidium chloride from kaolin tailings according to claim 1, wherein in the step (3), the specific operation of removing calcium from the acid leachate comprises: adding strong base into the acid leaching solution to neutralize hydrogen ions in the solution to enable the solution to be neutral, then adding carbonate or bicarbonate into the solution to enable residual calcium ions in the solution to precipitate, and stopping adding after the solution is transparent.
6. The method for extracting rubidium chloride from kaolin tailings according to claim 1, wherein in the step (4), the extracting agents adopted in the extracting process are 4-tert-butyl-2- (α -methylbenzyl) phenol and sulfonated kerosene, the back-extracting agent adopted in the extracting process is a hydrochloric acid solution, the concentration of the extracting agent is 0.8-1.5mol/L, and the concentration of the back-extracting agent is 0.5-3 mol/L.
7. The method for extracting rubidium chloride from kaolin tailings according to claim 1, wherein in the step (4), the volume ratio of the rubidium-containing leachate to the extracting agent is 1: 1-1: 4; the volume ratio of the obtained organic phase to the stripping agent is that the organic phase/water phase (O/A) is 4: 1-1: 1.
8. the method for extracting rubidium chloride from kaolin tailings according to claim 1, wherein in the step (5), the specific operation of purifying the rubidium-rich solution to obtain refined rubidium chloride is as follows: and (2) carrying out evaporative crystallization on the solution rich in rubidium to obtain a crude rubidium salt product, adding water into the obtained crude rubidium salt product, heating and dissolving, alkalifying, extracting and back-extracting to obtain a back-extraction solution, and carrying out crystallization and filtration after concentration to obtain refined rubidium chloride.
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| CN109777948B (en) * | 2019-02-25 | 2020-09-01 | 广东省矿产应用研究所 | Technological method for extracting rubidium by flash cycle leaching of silicate |
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| CN104313349A (en) * | 2014-10-10 | 2015-01-28 | 李宇龙 | Method of extracting lithium salt from lepidolite |
| CN105154670B (en) * | 2015-08-28 | 2018-01-12 | 武汉理工大学 | A kind of method from separation and concentration rubidium in mine tailing containing rubidium |
| CN106086470B (en) * | 2016-06-12 | 2017-12-22 | 宋玉军 | A kind of method that rubidium salt is obtained using Kaolin Tailings as raw material |
| CN106319245B (en) * | 2016-09-19 | 2018-05-04 | 福州大学 | A kind of method that lepidolite successive reaction carries lithium |
| CN107344725B (en) * | 2017-06-29 | 2019-02-26 | 周宇 | Sulfuric acid straight dipping process extracts the preparation process of elemental lithium in lithium ore |
| CN107354323B (en) * | 2017-07-26 | 2019-01-08 | 河北工程大学 | A method of separation and Extraction rubidium, caesium from coal |
| CN107739039A (en) * | 2017-10-16 | 2018-02-27 | 福州大学 | A kind of method that defluorinate lepidolite pipeline dissolution carries lithium |
| CN107841637A (en) * | 2017-11-28 | 2018-03-27 | 北京科技大学 | A kind of method of collaboration extraction rubidium potassium in ore from rubidium |
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