CN113957267A - Method for extracting rubidium salt from soil - Google Patents

Method for extracting rubidium salt from soil Download PDF

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Publication number
CN113957267A
CN113957267A CN202010707872.7A CN202010707872A CN113957267A CN 113957267 A CN113957267 A CN 113957267A CN 202010707872 A CN202010707872 A CN 202010707872A CN 113957267 A CN113957267 A CN 113957267A
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rubidium salt
soil
extracting
rubidium
salt
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范志东
杨瑞臣
耿小丕
王英新
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Chengde Petroleum College
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Chengde Petroleum College
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B26/00Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/10Obtaining alkali metals
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00Preliminary treatment of ores or scrap
    • C22B1/02Roasting processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • Chemical & Material Sciences (AREA)
  • Geology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Environmental & Geological Engineering (AREA)
  • Materials Engineering (AREA)
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Abstract

The invention provides a method for extracting rubidium salt from soil, fills the blank of the field of extracting rubidium salt from soil at home and abroad, has an epoch-spanning significance, and compared with the extraction of rubidium salt from ore, the extraction of soil is more convenient and faster than the extraction and utilization of ore, the production cost is low, the pollution is lower, and the method has good popularization value. The method specifically comprises the following steps: s1: crushing soil to form soil particles; s2: the soil particles and the displacing agent are uniformly mixed according to a proportion; s3: performing rubidium salt reduction treatment on the mixture obtained in S2 to obtain a rubidium salt reduced product; s4: subjecting the rubidium salt reduced product to liquid leaching treatment; s5: filtering the solution of step S4 to obtain a rubidium salt solution; s6: and extracting the rubidium salt solution to obtain solid rubidium salt.

Description

Method for extracting rubidium salt from soil
Technical Field
The invention relates to the technical field of metallurgy and mineral extraction, in particular to a method for extracting rubidium salt from soil.
Background
The content of rubidium in earth crust is 5.1 × 10-5—3.1×10-4And 16 positions respectively according to the abundance arrangement of elements. It has long been recognized that rubidium resources are primarily found in granite pegmatite, brines and potash deposits. People mainly develop and recover rubidium from granite pegmatite ore beds, and the main industrial mineral is lepidolite. The content of rubidium in lepidolite is about 3.75% rubidium content in seawater is 0.12 g/ton, and many formation water and salt lake brine also contain rubidium.
Rubidium is between potassium and cesium, is extremely active in nature, is a silver white waxy metal, is soft and light, can immediately lose the color of the metal when exposed to air, is severely oxidized by oxygen, and can cause spontaneous combustion of rubidium. The reaction is quite violent when exposed to water and even when exposed to ice at-100 ℃. Rubidium is more chemically reactive and more reactive than sodium and potassium.
Rubidium has irreplaceable use in many fields due to its unique physicochemical properties. With the development of high and new technology industries such as energy industry, atomic energy industry, bioengineering, aerospace industry, national defense industry and the like, rubidium metal and compounds thereof have great development in the traditional application fields such as biochemistry, catalysts, molecular biology, electronic devices, phototubes, special glass, medicines and the like in recent ten years; rubidium also shows strong vitality in new application fields such as magnetohydrodynamic power generation, thermionic conversion power generation, ion propulsion engines, and laser energy conversion electric energy devices.
In China, rubidium ores are mainly distributed in mountainous areas of Hunan and Sichuan, the rubidium ores are difficult to mine and have high cost, and the rubidium concentration in salt lakes and brine in China is low, so that the rubidium ores coexist with a large amount of lithium, sodium, potassium and cesium with similar chemical properties, and the industrial separation is difficult.
However, in the prior art, the rubidium extraction technology is extracted from various tailings, or ores or salt lake brine, a large amount of acid-base solution is used in the extraction process, the production cost is high, the production of rubidium ore becomes a new pollution source of the natural environment, and meanwhile, the rubidium crust content is low, so that the price is high, the rubidium resource is deficient, and the development of modern industry is limited.
Actual exploration shows that the soil in a partial region of Hebei Chengdu area is rich in rubidium elements and has mining value, no technical scheme for extracting rubidium salt from the soil exists in the prior art, and in view of the special physicochemical characteristics of the soil, how to provide a method for extracting rubidium salt from the soil fills the blank in the field, which is a technical problem to be solved by the technical staff in the field.
Disclosure of Invention
In view of the above, the present invention provides a method for extracting rubidium salt from soil, which solves the problems in the prior art, and the specific scheme is as follows:
a method for extracting rubidium salt from soil, comprising the steps of:
s1: crushing soil to form soil particles;
s2: the soil particles and the displacing agent are uniformly mixed according to a proportion;
s3: performing rubidium salt reduction treatment on the mixture obtained in S2 to obtain a rubidium salt reduced product;
s4: subjecting the rubidium salt reduced product to liquid leaching treatment;
s5: filtering the solution of step S4 to obtain a rubidium salt solution;
s6: and extracting the rubidium salt solution to obtain solid rubidium salt.
Specifically, the soil is selected from red clay, the displacer adopted in the step S2 is calcium chloride, and the liquid immersion treatment adopted in the step S4 is water immersion treatment.
Specifically, deionized water is used for the water immersion treatment in step S4.
Specifically, the component ratio of the calcium chloride to the red clay particles is 1: 0.5-1: 2.
Specifically, the component ratio of the calcium chloride to the red clay particles is 1: 1.3-1: 2.
Specifically, the calcium chloride is ground before being mixed with the red clay particles.
Specifically, the reduction treatment is reduction roasting, and the temperature of the reduction roasting is 700-1000 ℃.
Specifically, the reduction roasting temperature is 750-950 ℃.
Specifically, a grinding process is further provided between the steps S3 and S4.
Specifically, the soil formation red clay particles are specifically realized through the following steps:
s1-1: primary crushing;
s1-2: drying;
s1-3: ball milling and crushing;
s1-4: and (6) sieving.
The method for extracting rubidium salt from soil provided by the invention fills the blank of the field of extracting rubidium salt from soil at home and abroad, has an epoch-spanning significance, and compared with the extraction of rubidium salt from ore, the extraction of soil is more convenient and faster than the extraction and utilization of ore, the production cost is low, the pollution is lower, and the method has good popularization value.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required in the description of the embodiments or the prior art will be briefly introduced below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic diagram of a process for extracting rubidium mineral salt from soil provided by the invention.
FIG. 2 is a schematic diagram of a process for extracting rubidium mineral salt from soil according to an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the invention claims a method for extracting rubidium salt from soil, comprising the following steps:
s1: crushing soil to form red clay particles;
s2: the soil particles and the displacing agent are uniformly mixed according to a proportion;
s3: performing rubidium salt reduction treatment on the mixture obtained in S2 to obtain a rubidium salt reduced product;
s4: subjecting the rubidium salt reduced product to liquid leaching treatment;
s5: filtering the solution of step S4 to obtain a rubidium salt solution;
s6: and extracting the rubidium salt solution to obtain solid rubidium salt.
The substitution agent can be calcium chloride, sodium chloride, potassium chloride, salts of other halogen elements, or acidic substances such as hydrochloric acid, nitric acid, sulfuric acid and the like.
As a specific embodiment of the present invention, referring to fig. 2, the substitution agent used in step S2 is calcium chloride, the soil is red clay specific to the chender region, the liquid leaching used in step S4 is water leaching, the water is immersed in a dedicated water leaching device, and the water leaching is performed using deionized water or distilled water, so as to prevent water quality with different ph values from affecting the water leaching effect and the leaching of rubidium salt and rubidium chloride.
Specifically, the component ratio of the calcium chloride to the red clay particles is 1: 0.5-1: 2. In order to obtain the optimal clay component ratio, a plurality of groups of experiments are carried out on red clay and calcium chloride with different components under the same condition to obtain different leaching rates of the greening rubidium, wherein the representative groups of data are as follows:
Figure DEST_PATH_IMAGE001
from the table above, the leaching rate of rubidium chloride increases with the increase of calcium chloride, and the ratio of industrial use components is recommended to be 1: 1.3-1: 2.
The calcium chloride with through grinding before the red clay granule mixes, the calcium chloride solid particle after grinding is more tiny, takes place comparatively even and comprehensive chemical reaction with red clay granule easily in follow-up technology, and the calcium chloride passes through the blender misce bene with red clay granule after smashing. In view of the deliquescent nature of calcium chloride, the above described grinding and mixing process laboratory can be carried out in a drying oven, and the industrial production line can strictly control the air humidity of the operating plant (the air humidity should be within 10%), thus ensuring an efficient rubidium salt extract.
The reduction treatment is reduction roasting, and the temperature of the reduction roasting is 700-1000 ℃. Setting the ratio of the red clay to the calcium chloride to be constant, and the other conditions to be unchanged, roasting the mixture obtained in the step S2 at different temperatures at the temperature of 700-1000 ℃, observing the leaching rate, and selecting representative rubidium salt leaching data as follows:
Figure DEST_PATH_IMAGE002
as can be seen from the above table, the rubidium salt leaching rate increases with increasing temperature, reaches a maximum value at 900 ℃, and then decreases with increasing temperature.
The reduction roasting temperature is recommended to be 750-950 ℃ in industrial production.
Further, a grinding process is provided between the steps S3 and S4. Various elements in the soil exist, and through a reduction reaction, various salts may exist in the rubidium salt mixture obtained in step S3, and the various salts may show an aggregation state, so that leaching of rubidium chloride is inhibited in the water leaching process, and in order to ensure that the rubidium salt can be sufficiently dissolved into water, the granular or blocky rubidium salt mixture is ground again, the grinding particle size is recommended to be 0.15mm-0.045mm, and each production enterprise may also perform grinding according to actual conditions, the smaller the grinding particle size is, the better the leaching effect is, and ideally, the rubidium salt dissolution rate may be as high as 95.6% or more.
Specifically, as a further improvement of this embodiment, the formation of the red clay particles by the red clay is achieved by the following steps:
s1-1: the primary grinding can be carried out by using agricultural mills or other grinding facilities which can meet the particle size requirements. If the red clay is in a wet state and cannot be crushed, primary crushing can be performed after primary drying. Here, the particle size of the crushed red clay is required to be within 0.15 mm.
S1-2: and (4) drying, namely drying the red clay particles with the granularity of 0.15mm in drying equipment, and performing subsequent processes when the detected water content is lower than 5%.
S1-3: and (3) ball milling and crushing, namely crushing the dried red clay particles of S1-2 by using a ball milling crusher for not less than 2 h.
S1-4: and (6) sieving. And (4) sieving the red clay particles obtained in the step (S1-3) to obtain the red clay particles with the particle size within 0.075 mm.
The soil quality in the method is not limited to red clay, and can be loess or black soil and the like, so that the method is suitable for the soil with the rubidium element content not lower than 50g/T, and the rubidium-containing soil with the rubidium element content lower than the rubidium element content has no mining value.
While the present invention has been described with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, which are illustrative and not restrictive, and it will be apparent to those skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (10)

1. A method for extracting a rubidium salt from soil, comprising the steps of:
s1: crushing soil to form soil particles;
s2: the soil particles and the displacing agent are uniformly mixed according to a proportion;
s3: performing rubidium salt reduction treatment on the mixture obtained in S2 to obtain a rubidium salt reduced product;
s4: subjecting the rubidium salt reduced product to liquid leaching treatment;
s5: filtering the solution of step S4 to obtain a rubidium salt solution;
s6: and extracting the rubidium salt solution to obtain solid rubidium salt.
2. The method for extracting rubidium salt from soil according to claim 1, wherein: the soil is selected from red clay, the displacer adopted in the step S2 is calcium chloride, and the liquid immersion treatment adopted in the step S4 is water immersion treatment.
3. The method for extracting rubidium salt from soil according to claim 2, wherein: deionized water is adopted for water immersion treatment in the step S4.
4. The method for extracting rubidium salt from soil according to claim 2, wherein: the component ratio of the calcium chloride to the red clay particles is 1: 0.5-1: 2.
5. The method for extracting rubidium salt from soil according to claim 4, wherein: the component ratio of the calcium chloride to the red clay particles is 1: 1.3-1: 2.
6. The method for extracting rubidium salt from soil according to claim 2, wherein: the calcium chloride is ground before being mixed with the red clay particles.
7. The method for extracting rubidium salt from soil according to claim 2, wherein: the reduction treatment is reduction roasting, and the temperature of the reduction roasting is 700-1000 ℃.
8. The method for extracting rubidium salt from soil according to claim 2, wherein: the reduction roasting temperature is 750-950 ℃.
9. The method for extracting rubidium salt from soil according to claim 2, wherein: a grinding process is also provided between the steps S3 and S4.
10. Method for extracting rubidium salt from soil according to any one of claims 1 to 9, characterised in that said soil is formed into said red clay granules by two steps:
s1-1: primary crushing;
s1-2: drying;
s1-3: ball milling and crushing;
s1-4: and (6) sieving.
CN202010707872.7A 2020-07-21 2020-07-21 Method for extracting rubidium salt from soil Pending CN113957267A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4597955A (en) * 1985-05-01 1986-07-01 Carus Corporation Process for recovering cesium from cesium ore
CN103966460A (en) * 2013-02-01 2014-08-06 中国科学院广州地球化学研究所 Roasting leaching treatment process for recovery of metal rubidium resources from copper sulfur tailings
CN105803188A (en) * 2016-05-30 2016-07-27 江西旭锂矿业有限公司 Method for preferential segregation of potassium, rubidium and cesium through chloridizing roasting treatment of lepidolite
CN106086470A (en) * 2016-06-12 2016-11-09 宋玉军 A kind of method obtaining rubidium salt with Kaolin Tailings for raw material
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
CN107475513A (en) * 2016-07-11 2017-12-15 广州市光鼎矿业集团有限公司 The method that rubidium potassium aluminium is leached from MICA containing rubidium
CN108677006A (en) * 2018-06-06 2018-10-19 中南大学 A method of extracting rubidium chloride from Kaolin Tailings

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4597955A (en) * 1985-05-01 1986-07-01 Carus Corporation Process for recovering cesium from cesium ore
CN103966460A (en) * 2013-02-01 2014-08-06 中国科学院广州地球化学研究所 Roasting leaching treatment process for recovery of metal rubidium resources from copper sulfur tailings
CN105803188A (en) * 2016-05-30 2016-07-27 江西旭锂矿业有限公司 Method for preferential segregation of potassium, rubidium and cesium through chloridizing roasting treatment of lepidolite
CN106086470A (en) * 2016-06-12 2016-11-09 宋玉军 A kind of method obtaining rubidium salt with Kaolin Tailings for raw material
CN107475513A (en) * 2016-07-11 2017-12-15 广州市光鼎矿业集团有限公司 The method that rubidium potassium aluminium is leached from MICA containing rubidium
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
CN108677006A (en) * 2018-06-06 2018-10-19 中南大学 A method of extracting rubidium chloride from Kaolin Tailings

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