CN115821059A - Method for efficiently extracting rubidium from rubidium-containing ore through microwave-ultrasonic synergy - Google Patents

Method for efficiently extracting rubidium from rubidium-containing ore through microwave-ultrasonic synergy Download PDF

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CN115821059A
CN115821059A CN202211502080.1A CN202211502080A CN115821059A CN 115821059 A CN115821059 A CN 115821059A CN 202211502080 A CN202211502080 A CN 202211502080A CN 115821059 A CN115821059 A CN 115821059A
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rubidium
leaching
microwave
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张利波
林国
胡途
王仕兴
李世伟
夏洪应
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Kunming University of Science and Technology
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Abstract

The invention provides a method for efficiently extracting rubidium from rubidium-containing ore by microwave-ultrasonic synergy, which comprises the steps of uniformly mixing rubidium-containing mineral powder obtained by grinding into a roasting raw material with calcium chloride by adopting a combined process of chlorination microwave roasting-short-time ultrasonic water leaching, heating to a preset temperature under the action of microwaves, preserving heat, cooling to room temperature after the reaction is finished, and grinding into powder to obtain a leaching raw material; and mixing the leaching raw material with water according to a preset solid-to-liquid ratio, carrying out ultrasonic enhanced leaching treatment at a preset temperature, and filtering to obtain a rubidium-containing leaching solution and leaching residues. Through the mode, the method can be used for efficiently extracting rubidium from rubidium-containing ore, is simple in extraction process operation, low in energy consumption, short in time, high in leaching rate and free of pollution, effectively overcomes the technical defects of long leaching time and low leaching rate of a conventional extraction mode, and has high practical application value.

Description

Method for efficiently extracting rubidium from rubidium-containing ore through microwave-ultrasonic synergy
Technical Field
The invention relates to the technical field of metallurgy and mineral extraction, in particular to a method for efficiently extracting rubidium from rubidium-containing ore through microwave-ultrasonic synergy.
Background
Rubidium is an indispensable rare metal for national economic development, is an extremely soft silver white waxy metal and has very active chemical properties. Electrons are easy to be released under the action of light; the catalyst can take violent action when meeting water, generates a large amount of heat and generates hydrogen and rubidium hydroxide; in addition, complex oxides are easily formed by the reaction with oxygen. Due to the active chemical property of rubidium, the rubidium is widely applied to various industries, and mainly relates to the fields of electronic devices, energy sources, catalysts, special glass, medical treatment and the like. Particularly in the high-end technical field, rubidium has extremely excellent photoelectric effect and special performance which cannot be replaced by other substances, and is widely applied to photoelectric tubes, magnetohydrodynamic power generation, ion propulsion engines and the like in recent years. It can be seen that rubidium resources play an important role in rapidly developing industrial technologies.
Rubidium is often found in minerals such as leucite, pollucite, carnallite and lepidolite, and the abundance in earth crust is at the 23 rd position in all elements. China has abundant rubidium resources, and the rubidium resources are mainly stored in lepidolite and salt lake brine, and the content of rubidium in the lepidolite accounts for 55% of national rubidium resource reserves. In addition, rubidium resources are complete in types and distributed nationwide, are most abundant in Yichun reserves in Jiangxi, and are the main source of rubidium products in China. With the continuous expansion of the demand of rubidium and its compounds, the extraction technology is continuously developed, but most of the currently developed technologies have the defects of complex operation, high energy consumption, environmental pollution and the like, so that it is necessary to develop a new extraction technology.
The invention patent with publication number CN107034355A provides a method for extracting rubidium and cesium from lepidolite ore. The method mainly comprises the following steps: placing the alpha type lepidolite in a microwave device, roasting for 20-30 min at 780 ℃, converting into beta type lepidolite, mixing sulfuric acid, and carrying out sulfating roasting for 5-15 min in the microwave device; then soaking sulfated and roasted beta-type lepidolite mineral powder in water, ultrasonically stirring, standing until all particles are settled, and filtering to obtain a leaching solution; and finally, collecting rubidium metal from the leachate through an ion exchange resin exchange column. However, the method has the technical defects of complex process operation, large sulfuric acid consumption, easy corrosion of equipment, possible environmental pollution and the like, the overall extraction efficiency is low, and the leaching rate of rubidium still needs to be improved.
In view of the above, there is a need for an improved method for extracting rubidium with high efficiency to solve the above problems.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for efficiently extracting rubidium from rubidium-containing ore by microwave-ultrasonic synergy, which is simple in operation, low in energy consumption, short in leaching time, high in leaching rate and free of pollution.
In order to achieve the purpose, the invention provides a method for efficiently extracting rubidium from rubidium-containing ore by microwave-ultrasonic synergy, which comprises the following steps:
s1, carrying out ore grinding pretreatment on rubidium-containing ore to obtain rubidium-containing ore powder; fully mixing calcium chloride with the rubidium-containing mineral powder according to a preset mass ratio to obtain a roasting raw material;
s2, heating the roasting raw material obtained in the step S1 to a preset temperature under the action of microwaves, preserving heat, and cooling to room temperature after the reaction is finished to obtain a roasted material; grinding the roasted material into powder to obtain a leaching raw material;
and S3, mixing the leaching raw material with water according to a preset solid-to-liquid ratio, carrying out ultrasonic enhanced leaching treatment at a preset temperature, and filtering to obtain a rubidium-containing leaching solution and leaching residues.
As a further improvement of the invention, after the leaching residue obtained in the step S3 is washed, dried and weighed, the content of rubidium in the leaching residue is measured by a chemical analysis method and is used for calculating the leaching rate of rubidium.
As a further improvement of the invention, in step S1, the calcium chloride and the rubidium-containing mineral powder are mixed according to a mass ratio of 0.8-2.5; preferably, the mass ratio of the calcium chloride to the rubidium-containing mineral powder is 1.5.
In a further improvement of the present invention, in step S2, the microwave power under the action of the microwaves is 900 to 1100W, preferably 1000W.
As a further improvement of the present invention, in step S2, the predetermined temperature is 750 to 850 ℃, preferably 800 to 850 ℃.
As a further improvement of the invention, the time for heat preservation is 16-28 min, preferably 20-24 min.
As a further improvement of the present invention, in step S3, the solid-to-liquid ratio of the leaching raw material to water is 1.5 to 4.5g/mL, preferably 1.
As a further improvement of the present invention, in step S3, the predetermined temperature is 25 to 40 ℃, preferably 35 ℃.
As a further improvement of the present invention, in step S3, the ultrasonic power of the ultrasonic-enhanced leaching treatment is 80 to 200W, preferably 120 to 160W.
As a further improvement of the present invention, in step S3, the leaching time of the ultrasonic enhanced leaching treatment is 14 to 26min, preferably 18 to 22min.
The invention has the beneficial effects that:
1. according to the method for efficiently extracting rubidium from rubidium-containing ore by microwave-ultrasonic synergy, provided by the invention, calcium chloride is used as a mixed raw material to be mixed with the rubidium-containing mineral powder and then subjected to microwave roasting by adopting a combined process of chlorination microwave roasting-short-time ultrasonic water leaching, a chlorination environment can be provided for a system under a high-temperature condition, the reaction rate of the calcium chloride and rubidium can be accelerated, and rubidium elements in minerals can be converted into rubidium chloride with excellent solubility from an oxidation state to the maximum extent, so that conditions are created for subsequent leaching work, and the rubidium leaching rate is favorably improved. Meanwhile, microwave is used as a heating mode for converting microwave energy absorbed by an object into heat energy and heating the whole body of the microwave oven, dipole molecules inside the material do high-frequency reciprocating motion to generate 'internal friction heat', so that the temperature of the heated material is raised, the heating speed is high and uniform, the generated rubidium chloride also has certain wave-absorbing property, the reaction system can be further heated in the reaction process, the whole rapid heating of the reaction system is realized, the time required by heating is effectively shortened, the temperature distribution in the reaction system is more uniform, the chlorination process is more fully reacted, the generation of intermediate products can be avoided, and the roasting efficiency is greatly improved.
2. The method for efficiently extracting rubidium from rubidium-containing ore by microwave-ultrasonic synergy provided by the invention further realizes the purpose of efficiently improving the leaching rate in a short time by adopting ultrasonic water leaching on the basis of roasting by chlorination microwaves. On one hand, the rubidium element in the mineral is converted into rubidium chloride with excellent solubility from an oxidation state through chlorination microwave roasting treatment, so that favorable conditions are created for the water leaching process; on the other hand, the cavitation effect caused by the ultrasonic wave can generate instantaneous high temperature and high pressure in the system, so that the thermodynamic and kinetic conditions of the leaching system can be improved, and the leaching effect is enhanced. Meanwhile, the mechanical effect generated in the ultrasonic action process plays a role in stirring, so that the leaching raw materials can be uniformly distributed in the system, the agglomeration phenomenon is avoided, and the leaching effect is enhanced; in addition, the ultrasonic waves can also change the microscopic morphology of the mineral powder, the surfaces of the particles can be gradually peeled off to expose the inner layer under the action of the ultrasonic waves, and the leaching effect is more thorough.
3. According to the method for efficiently extracting rubidium from rubidium-containing ore through microwave-ultrasonic synergy, provided by the invention, the purpose of rapidly and efficiently extracting rubidium from the rubidium-containing ore is realized by further regulating and controlling the process conditions in the extraction process, the technical defects of long conventional leaching time and low leaching rate are avoided, and the leaching rate is higher.
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FIG. 1 is a schematic flow diagram of a method for efficiently extracting rubidium from rubidium-containing ore by microwave-ultrasonic synergy.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in detail with reference to the accompanying drawings and specific embodiments.
It should be noted that, in order to avoid obscuring the present invention with unnecessary details, only the structures and/or processing steps closely related to the solution of the present invention are shown in the drawings, and other details not closely related to the present invention are omitted.
In addition, it is also to be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention provides a method for efficiently extracting rubidium from rubidium-containing ore by microwave-ultrasonic synergy, which comprises the following steps:
s1, carrying out ore grinding pretreatment on rubidium-containing ore to obtain rubidium-containing ore powder; fully mixing calcium chloride with the rubidium-containing mineral powder according to a preset mass ratio to obtain a roasting raw material;
s2, heating the roasting raw material obtained in the step S1 to a preset temperature under the action of microwaves, preserving heat, and cooling to room temperature after the reaction is finished to obtain a roasted material; grinding the roasted material into powder to obtain a leaching raw material;
and S3, mixing the leaching raw material with water according to a preset solid-to-liquid ratio, carrying out ultrasonic enhanced leaching treatment at a preset temperature, and filtering to obtain a rubidium-containing leaching solution and leaching residues.
As a further improvement of the invention, after the leaching residue obtained in the step S3 is washed, dried and weighed, the content of rubidium in the leaching residue is measured by a chemical analysis method and is used for calculating the leaching rate of rubidium.
In step S1, the calcium chloride and the rubidium-containing ore powder are mixed in a mass ratio of 0.8 to 2.5. When the proportion of calcium chloride is too low, the rubidium in the rubidium-containing mineral powder is difficult to be fully chlorinated, so that the leaching rate is influenced; the proportion of calcium chloride is too high, and the leaching rate is not improved greatly. Preferably, the mass ratio of the calcium chloride to the rubidium-containing mineral powder is 1.5.
In step S2, the microwave power under the action of the microwaves is 900 to 1100W, preferably 1000W. The preset temperature is 750-850 ℃, the insufficient chlorination of rubidium is caused by too low temperature, but after the temperature reaches 800 ℃, the leaching rate is not improved greatly by further increasing the temperature, and the energy consumption is increased, and the temperature is preferably 800-850 ℃. The heat preservation time is 16-28 min, and the leaching rate can be influenced by too low temperature or too high temperature, preferably 20-24 min.
In step S3, the solid-to-liquid ratio of the leaching raw material to water is 1.5 to 4.5g/mL, the predetermined temperature is 25 to 40 ℃, the ultrasonic power of the ultrasonic enhanced leaching treatment is 80 to 200W, and the leaching time of the ultrasonic enhanced leaching treatment is as follows. The leaching rate can be further improved by properly increasing the proportion of water, the preset temperature, the ultrasonic power and the leaching time within a certain range, so that the solid-liquid ratio of the leaching raw material to water is preferably 1.5 g/mL, the preset temperature is 35 ℃, the ultrasonic power of ultrasonic enhanced leaching treatment is 120-160W, and the leaching time of the ultrasonic enhanced leaching treatment is 18-22 min.
The method for efficiently extracting rubidium from rubidium-containing ore by the synergy of microwave and ultrasound provided by the invention is described below by combining specific examples.
Example 1
The embodiment provides a method for efficiently extracting rubidium from rubidium-containing ore through microwave-ultrasonic synergy, which specifically comprises the following steps:
s1, carrying out ore grinding pretreatment on rubidium-containing ore (the content of rubidium is 0.1%) by using an ore grinding machine to obtain rubidium-containing ore powder; fully mixing calcium chloride with the rubidium-containing mineral powder according to a mass ratio of 0.8;
s2, heating the roasted raw material obtained in the step S1 to 750 ℃ in a 1000W microwave device, preserving heat for 16min, and cooling to room temperature after the reaction is finished to obtain a roasted material; grinding the roasted material into powder to obtain a leaching raw material;
s3, taking 40g of the leaching raw material, adding deionized water according to a solid-to-liquid ratio of 1.5 in a beaker, carrying out ultrasonic enhanced leaching treatment at 25 ℃, carrying out ultrasonic treatment at an ultrasonic power of 80W for 14min, and carrying out solid-liquid separation to obtain a rubidium-containing leaching solution and leaching residues.
Washing the leached residues with deionized water for multiple times, drying and weighing, determining the content of rubidium in the leached residues by adopting a chemical analysis method, and then calculating the leaching rate of rubidium according to the following formula:
Figure BDA0003968146370000061
wherein m is 0 The mass of the raw material rubidium-containing ore is expressed in g, omega 0 The content of rubidium in the raw material rubidium-containing ore is expressed in unit; m is a unit of 1 The mass of the leached slag is expressed in g, omega 1 The content of rubidium in the leaching residue is expressed in unit;
in this example, the experimental data gave m 1 =22.89g,ω 1 =0.0256%, and the leaching rate was 85.3% according to the calculation formula.
Examples 2 to 15
Embodiments 2 to 15 respectively provide a method for efficiently extracting rubidium from rubidium-containing ore through microwave-ultrasound synergy, and compared with embodiment 1, the method is different in that process parameters of an extraction process are changed, and the remaining steps are the same as those in embodiment 1, and are not described herein again. The parameters and the leaching rates measured and calculated for the respective examples are shown in table 1.
TABLE 1 Process parameters and Leaching rates for examples 2-15
Figure BDA0003968146370000062
Figure BDA0003968146370000071
As can be seen from Table 1, the mass ratio, solid-to-liquid ratio, microwave conditions, ultrasonic conditions and other parameters in the extraction process all affect the extraction rate of rubidium. According to the invention, by regulating and optimizing the process conditions in the extraction process, the purpose of extracting rubidium efficiently in a short time can be realized under the low-temperature condition, the leaching rates are all above 88.5%, and can reach above 99%, the purpose of extracting rubidium from rubidium-containing ore rapidly and efficiently is realized, and the technical defects of long conventional leaching time and low leaching rate are avoided.
In conclusion, the invention provides a method for efficiently extracting rubidium from rubidium-containing ore by microwave-ultrasonic synergy, which comprises the steps of uniformly mixing rubidium-containing mineral powder obtained by grinding with calcium chloride to obtain a roasting raw material by adopting a combined process of chlorination microwave roasting-short-time ultrasonic water leaching, heating to a preset temperature under the action of microwaves, preserving heat, cooling to room temperature after the reaction is finished, and grinding into powder to obtain a leaching raw material; and mixing the leaching raw material with water according to a preset solid-to-liquid ratio, carrying out ultrasonic enhanced leaching treatment at a preset temperature, and filtering to obtain a rubidium-containing leaching solution and leaching residues. Through the mode, the method can be used for efficiently extracting rubidium from rubidium-containing ore, is simple in extraction process operation, low in energy consumption, short in time, high in leaching rate and free of pollution, effectively overcomes the technical defects of long leaching time and low leaching rate of a conventional extraction mode, and has high practical application value.
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the spirit and scope of the present invention.

Claims (10)

1. A method for efficiently extracting rubidium from rubidium-containing ore through microwave-ultrasonic synergy is characterized by comprising the following steps:
s1, carrying out ore grinding pretreatment on rubidium-containing ore to obtain rubidium-containing ore powder; fully mixing calcium chloride with the rubidium-containing mineral powder according to a preset mass ratio to obtain a roasting raw material;
s2, heating the roasting raw material obtained in the step S1 to a preset temperature under the action of microwaves, preserving heat, and cooling to room temperature after the reaction is finished to obtain a roasted material; grinding the roasted material into powder to obtain a leaching raw material;
and S3, mixing the leaching raw material with water according to a preset solid-to-liquid ratio, carrying out ultrasonic enhanced leaching treatment at a preset temperature, and filtering to obtain a rubidium-containing leaching solution and leaching residues.
2. The method for efficiently extracting rubidium from rubidium-containing ore by microwave-ultrasonic synergy according to claim 1, characterized by comprising the following steps: and (4) washing, drying and weighing the leaching residues obtained in the step (S3), and then measuring the content of rubidium in the leaching residues by adopting a chemical analysis method for calculating the leaching rate of rubidium.
3. The method for efficiently extracting rubidium from rubidium-containing ore by microwave-ultrasonic synergy according to claim 1, characterized by comprising the following steps: in the step S1, mixing the calcium chloride with the rubidium-containing mineral powder according to a mass ratio of 0.8-2.5; preferably, the mass ratio of the calcium chloride to the rubidium-containing mineral powder is 1.5.
4. The method for efficiently extracting rubidium from rubidium-containing ore by microwave-ultrasonic synergy according to claim 1, characterized by comprising the following steps: in step S2, the microwave power under the action of the microwaves is 900 to 1100W, preferably 1000W.
5. The method for efficiently extracting rubidium from rubidium-containing ore by microwave-ultrasonic synergy according to claim 1, characterized by comprising the following steps: in step S2, the predetermined temperature is 750 to 850 ℃, preferably 800 to 850 ℃.
6. The method for efficiently extracting rubidium from rubidium-containing ore by microwave-ultrasonic synergy according to claim 1, characterized by comprising the following steps: the heat preservation time is 16-28 min, preferably 20-24 min.
7. The method for efficiently extracting rubidium from rubidium-containing ore by microwave-ultrasonic synergy according to claim 1, characterized by comprising the following steps: in step S3, the solid-to-liquid ratio of the leaching raw material to water is 1.5 to 4.5g/mL, preferably 1.
8. The method for efficiently extracting rubidium from rubidium-containing ore by microwave-ultrasonic synergy according to claim 1, characterized by comprising the following steps: in step S3, the predetermined temperature is 25 to 40 ℃, preferably 35 ℃.
9. The method for efficiently extracting rubidium from rubidium-containing ore by microwave-ultrasonic synergy according to claim 1, characterized by comprising the following steps: in step S3, the ultrasonic power of the ultrasonic-enhanced leaching treatment is 80 to 200W, preferably 120 to 160W.
10. The method for efficiently extracting rubidium from rubidium-containing ore by microwave-ultrasonic synergy according to claim 1, characterized by comprising the following steps: in step S3, the leaching time of the ultrasonic enhanced leaching treatment is 14 to 26min, preferably 18 to 22min.
CN202211502080.1A 2022-11-28 2022-11-28 Method for efficiently extracting rubidium from rubidium-containing ore through microwave-ultrasonic synergy Pending CN115821059A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005054211A (en) * 2003-08-06 2005-03-03 Mitsubishi Materials Corp Method for recovering rubidium from dust
CN101323909A (en) * 2008-07-17 2008-12-17 东北大学 Method of microwave selective reduction roasting-dilute acid leaching nickel oxide ore
CN101392320A (en) * 2008-10-31 2009-03-25 东北大学 Method for treating nickel-containing laterite by microwave reducing roasting-goethite precipitation conversion method
CN103820633A (en) * 2014-02-28 2014-05-28 金川集团股份有限公司 Processing method of rubidium-containing ore
CN107267777A (en) * 2017-06-09 2017-10-20 北京矿冶研究总院 Novel method for extracting rubidium from rubidium-containing ore
US20210236956A1 (en) * 2021-03-19 2021-08-05 Sichuan Normal University Microwave chemical method for totally extracting fluorine and rare earth from bastnaesite concentrate
CN113337734A (en) * 2021-04-25 2021-09-03 武汉科技大学 Method for ultrasonic reinforced extraction of rubidium from rubidium-containing ore

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005054211A (en) * 2003-08-06 2005-03-03 Mitsubishi Materials Corp Method for recovering rubidium from dust
CN101323909A (en) * 2008-07-17 2008-12-17 东北大学 Method of microwave selective reduction roasting-dilute acid leaching nickel oxide ore
CN101392320A (en) * 2008-10-31 2009-03-25 东北大学 Method for treating nickel-containing laterite by microwave reducing roasting-goethite precipitation conversion method
CN103820633A (en) * 2014-02-28 2014-05-28 金川集团股份有限公司 Processing method of rubidium-containing ore
CN107267777A (en) * 2017-06-09 2017-10-20 北京矿冶研究总院 Novel method for extracting rubidium from rubidium-containing ore
US20210236956A1 (en) * 2021-03-19 2021-08-05 Sichuan Normal University Microwave chemical method for totally extracting fluorine and rare earth from bastnaesite concentrate
CN113337734A (en) * 2021-04-25 2021-09-03 武汉科技大学 Method for ultrasonic reinforced extraction of rubidium from rubidium-containing ore

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