CN111560513A - Method for extracting cesium from pollucite based on chloridizing roasting method - Google Patents
Method for extracting cesium from pollucite based on chloridizing roasting method Download PDFInfo
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- CN111560513A CN111560513A CN202010617817.9A CN202010617817A CN111560513A CN 111560513 A CN111560513 A CN 111560513A CN 202010617817 A CN202010617817 A CN 202010617817A CN 111560513 A CN111560513 A CN 111560513A
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
- C22B1/08—Chloridising roasting
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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
- 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
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a method for extracting cesium from pollucite based on a chloridizing roasting method, which comprises the steps of grinding ores by a sampling machine to obtain pollucite mineral powder, and heating and melting calcium chloride into an aqueous solution; uniformly mixing the ground pollucite ore powder with the dissolved calcium chloride solution; adding the uniformly mixed materials into a ceramic crucible, and roasting in a muffle furnace; grinding the roasted material, stirring with water, heating for leaching, filtering to obtain a leaching solution, and conveying the leaching solution to an extraction process to extract a high-grade cesium product. According to the invention, the calcium chloride solution is heated and dissolved to treat the pollucite ore powder, the roasted material after roasting has a good leaching effect, the recovery rate of cesium metal reaches more than 95%, an acid system is not required for roasting and leaching, the equipment corrosion is low, and the leaching solution is a cesium chloride system and can be directly used for extraction and separation.
Description
Technical Field
The invention relates to the technical field of chemical production, in particular to a method for extracting cesium from pollucite.
Background
Cesium is a light golden active metal, has a low melting point, is very easily oxidized in air, can react violently with water to generate hydrogen and explode. Cesium has no elemental form in nature and is only rarely distributed in the form of salts in land and sea. Cesium is an important material for manufacturing vacuum devices, photoelectric cells, and the like.
Cesium-133 is not radioactive, but uranium-235, upon fission, produces long-lived cesium-137. Cesium-137 has a half-life of 30.17 years, radiates both beta and gamma radiation, and is useful as a beta and gamma radiation source for industrial and agricultural uses and medical uses.
Cesium is the most active among the alkali metals and reacts violently with oxygen to form a variety of cesium oxides. In humid air, the heat of oxidation is sufficient to melt and burn the cesium. Cesium does not react with nitrogen but can combine with hydrogen at high temperatures to form a fairly stable hydride. Cesium reacts violently with water and if placed in a water tank containing water, it can explode. Even with ice at temperatures as low as-116 c, can react violently to produce hydrogen gas, cesium hydroxide, which is the most basic of the non-radioactive hydroxides. With halogens, stable halides can also be formed, due to the large ionic radius. Cesium and organic species also react similarly to other alkali metals, but are more reactive. The oxidation of cesium in air yields not only cesium oxide and cesium peroxide, but also complex, non-integral compounds such as cesium superoxide and cesium ozonide.
The cesium salts are dissolved in all salt solutions as are the potassium and sodium salts. But the perchlorate is insoluble. Cesium salts are generally colorless unless the anion is colored (e.g., cesium permanganate is purple). Many simple salts are deliquescent, but are weaker than other alkali metals which are lighter. The acetates, carbonates, halides, oxides, nitrates and sulfates of cesium are soluble in water. Double salts are generally less soluble and the less soluble nature of cesium aluminum sulfate is often used to purify cesium from ores. Double salts formed with antimony (e.g., CsSbCl4), bismuth, cadmium, copper, iron, and lead are generally less soluble.
Cesium hydroxide (CsOH) is a strong base with strong water absorption. It can rapidly etch the surface of a semiconductor material (e.g., silicon). In the past chemists have considered CsOH to be the "strongest base", but many compounds are much more basic (protic) than CsOH, such as n-butyllithium, cesium hydride and sodium amide.
Cesium has been or is being used in a wide variety of high-tech fields due to its unique properties. Such as photoelectric primary devices, atomic clocks, high-performance batteries, catalysts (inorganic or organic synthesis), display screen coating films, high-grade glass ceramics and the like.
Cesium is a rare element on earth, mainly present in seawater, but at very low concentrations of only one in ten-thousandth. But also in some solid minerals such as pollucite, spodumene, lepidolite, lithium iron clouds. Currently, pollucite is the main raw material used in the world for the production of cesium salts, followed by lepidolite. The relatively pure pollucite is an aluminosilicate mineral containing 20% cesium and 4% other alkali metals, and has a composition of 2Cs2O·2A12O3·9SiO2·H2O, methods for producing cesium salts using pollucite are classified into two major types, acid method and baking method. Examples of the acid method include a hydrochloric acid method and a sulfuric acid method; examples of the roasting method include a sodium carbonate roasting method, a calcium oxide and calcium chloride roasting method, a calcium chloride and ammonium chloride roasting method, and the like.
Disclosure of Invention
The invention provides a method for extracting cesium from pollucite by a chlorination roasting method, which treats pollucite ore by heating and dissolving calcium chloride solution, has good roasting material leaching effect, has cesium metal recovery rate of more than 95 percent, does not need to adopt an acid system for roasting and leaching, has small corrosion to equipment, and can be directly used for extraction and separation because the leaching solution is a cesium chloride system.
The reaction principle of the invention is as follows: in the case of high-temperature calcination, calcium chloride reacts with pollucite, the reaction equation is as follows:
2Cs2O·2A12O3·9SiO2·H2O+2CaCl2→4CsCl+A12O3·4SiO2+CaO·SiO2+CaO·A12O3·4SiO2
the invention is realized by the following technical scheme. A method for extracting cesium from pollucite based on a chloridizing roasting method comprises the following steps:
(1) grinding ores: milling the ore by a sampling machine to obtain pollucite ore powder;
(2) calcium chloride dissolution: heating and melting calcium chloride into an aqueous solution;
(3) mixing materials: uniformly mixing the pollucite ore powder ground in the step (1) with the calcium chloride solution melted in the step (2);
(4) adding the uniformly mixed material obtained in the step (3) into a ceramic crucible, and roasting in a muffle furnace;
(5) filtering and taking out the materials subjected to the step (4), grinding and weighing;
(6) stirring the roasted material obtained in the step (5) with water and heating for leaching;
(7) carrying out suction filtration and leaching on the leached slurry in the step (6), and combining a washing liquid with the leached liquid to obtain the leached liquid and leached residues;
(8) and (4) measuring the leaching solution produced in the step (7), sampling and analyzing, putting leaching residues into an oven for drying, cooling, weighing, sampling and analyzing.
(9) And (4) conveying the measured and sampled leachate obtained in the step (8) to an extraction process to extract a high-grade cesium product.
Further preferably, in the step (1), the granularity grade of the pollucite ore powder is 160-200 meshes.
Further preferably, in the step (3), the pollucite ore powder and 1.3-1.6 times of calcium chloride solution (CaCl) by weight are mixed2·6H2O is heated and melted) and mixed.
Further preferably, in the step (4), the reaction is carried out for 20 to 60 minutes by heating to 750 to 850 ℃.
Further preferably, in the step (5), the reactant is ground to 120-160 meshes.
Further preferably, in the step (6), the liquid-solid ratio is 2.5-3.5: 1, heating to 80-90 ℃ to carry out leaching reaction for 1-2 hours.
Further preferably, in the step (7), the slag washing liquid-solid ratio is 1:1 to 2.
The invention has the following effects: 1. the pollucite ore is treated by a chloride roasting method, and calcium chloride is cheap and easily available. 2. Calcium chloride is heated and dissolved into water solution, and then the water solution is mixed with pollucite ore powder, so that the mixing is more uniform, and the roasting conversion is facilitated; 3. the leaching effect is good, the process conditions are adjusted, and the recovery rate of cesium metal reaches more than 95%; 4. because no acid participates in the reaction process, the corrosion to equipment is low. 5. The leaching solution is a cesium chloride system and can be directly used for extraction and separation to obtain high-purity cesium products and rubidium products. 6. The leaching slag is aluminosilicate neutral harmless substances, so that the method is safer and more environment-friendly.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will be explained in further detail with reference to examples.
Example 1
(1) Grinding ores: grinding pollucite with a sample preparation machine to obtain a powder with a particle size of D50When 97.1um (about 160 mesh) pollucite powder was sampled, the caesium grade was 20.56%.
(2) Calcium chloride dissolution: 130 g of crystalline calcium chloride (CaCl)2·6H2O) is heated to 50 ℃ to be dissolved into an aqueous solution.
(3) Mixing materials: mixing 100 g of pollucite ore powder ground in the step (1) with 130 g of calcium chloride solution melted in the step (2) in a ratio of 1: the ratio of 1.3 was sufficiently mixed in a porcelain crucible.
(4) Putting the materials uniformly mixed in the step (3) and loaded in a porcelain crucible into a muffle furnace for roasting; the roasting temperature is controlled at 750 ℃, and the roasting time is controlled at 1 hour.
(5) Filtering and taking out the material obtained in the step (4), and grinding the material in a sampling machine to D5095um (about 160 mesh) and a weight of 159 g.
(6) And (3) leaching the roasted material obtained in the step (5) by stirring with 398 ml of water, wherein the liquid-solid ratio is 2.5: 1, heating to 80 ℃, and keeping the temperature for 2 hours;
(7) carrying out suction filtration on the leached slurry in the step (6) to obtain 349ml of leached liquid, weighing, adding 386g of water into 193g of wet residues according to the liquid-solid ratio of 1:2 for leaching, and carrying out suction filtration to obtain 385ml of washing liquid to obtain 193g of wet leached residues;
(8) and (4) putting the wet leaching residue produced in the step (7) into an oven, drying for 2 hours at a constant temperature of 200 ℃, cooling, taking out, and weighing, wherein the weight is 136.3 g.
(9) 734ml of leaching solution (including washing liquid) and 136.3g of leaching residue (dry basis) produced in the steps (7) and (8) are sampled and analyzed.
(10) The cesium content in the leaching solution is 24.77g/l, the cesium content in the leaching residue is 1.66%, and the recovery rate of the leaching solution is 88.43%.
Example 2
(1) Grinding ores: grinding pollucite with a sample preparation machine to obtain a powder with a particle size of D50When 97.1um (about 160 mesh) pollucite powder was sampled, the caesium grade was 20.56%.
(2) Calcium chloride dissolution: 140 g of crystalline calcium chloride (CaCl)2·6H2O) is heated to 50 ℃ to be dissolved into an aqueous solution.
(3) Mixing materials: mixing 100 g of pollucite ore powder ground in the step (1) with 140 g of calcium chloride solution melted in the step (2) in a ratio of 1: the ratio of 1.4 was sufficiently mixed in a porcelain crucible.
(4) Putting the materials uniformly mixed in the step (3) and loaded in a porcelain crucible into a muffle furnace for roasting; the roasting temperature is controlled at 750 ℃, and the roasting time is controlled at 1 hour.
(5) Filtering and taking out the material obtained in the step (4), and grinding the material in a sampling machine to D50114um (about 130 mesh) and a weight of 168.3 g.
(6) And (3) stirring and leaching the roasted material obtained in the step (5) by using 510 ml of water, wherein the liquid-solid ratio is 3: 1, heating to 80 ℃, and keeping the temperature for 1.5 hours;
(7) carrying out suction filtration on the leached slurry in the step (6) to obtain 456ml of leached liquid, weighing 205g of wet slag, adding 205g of water according to the liquid-solid ratio of 1:1 for leaching, and carrying out suction filtration to obtain 204ml of washing liquid, thus obtaining 205.5g of washed wet leached slag;
(8) and (4) putting the wet leaching residue produced in the step (7) into an oven, drying for 2 hours at the constant temperature of 200 ℃, cooling, taking out, and weighing, wherein the weight is 152.3 g.
(9) 660ml of leachate (comprising washing liquid) and 144.9g of leaching residue (dry basis) produced in the steps (7) and (8) are sampled and analyzed.
(10) The cesium content in the leaching solution is 28.85g/l, the cesium content in the leaching residue is 0.97%, and the recovery rate of the leaching solution is 92.60%.
Example 3
(1) Grinding ores: grinding pollucite with a sample preparation machine to obtain a powder with a particle size of D50When 91um (about 170 mesh) pollucite powder was sampled, the caesium grade was 20.56%.
(2) Calcium chloride dissolution: 150 g of crystalline calcium chloride (CaCl)2·6H2O) is heated to 50 ℃ to be dissolved into an aqueous solution.
(3) Mixing materials: mixing 100 g of pollucite ore powder ground in the step (1) with 150 g of calcium chloride solution melted in the step (2) in a ratio of 1: the ratio of 1.5 was sufficiently mixed in a porcelain crucible.
(4) Putting the materials uniformly mixed in the step (3) and loaded in a porcelain crucible into a muffle furnace for roasting; the roasting temperature is controlled at 800 ℃, and the roasting time is controlled at 1 hour.
(5) Filtering and taking out the material obtained in the step (4), and grinding the material in a sampling machine to D50113um (about 130 mesh) weighing 175.1 g.
(6) And (3) stirring and leaching the roasted material obtained in the step (5) by using 525 ml of water, wherein the liquid-solid ratio is 3: 1, heating to 80 ℃, and keeping the temperature for 1.5 hours;
(7) carrying out suction filtration on the leached slurry in the step (6) to obtain 441ml of leached liquid, weighing, adding 213g of water into the leached liquid with the wet residue weight of 213g according to the liquid-solid ratio of 1:1, carrying out suction filtration to obtain 212ml of washing liquid, and obtaining 214g of washed wet leached residue;
(8) and (4) putting the wet leaching residue produced in the step (7) into an oven, drying for 2 hours at a constant temperature of 200 ℃, cooling, taking out, and weighing, wherein the weight is 150.7 g.
(9) And (3) sampling and analyzing 681ml of leaching solution (comprising washing liquid) and 150.7g of leaching residue (dry basis) produced in the step (7) and the step (8).
(10) The cesium content in the leaching solution (containing washing liquid) is 29.80g/l, the cesium content in the leaching residue is 0.55%, and the recovery rate based on the leaching solution is 95.38%.
Example 4
(1) Grinding ores: grinding pollucite with a sample preparation machine to obtain a powder with a particle size of D50When 81.3um (about 180 mesh) pollucite powder, the cesium grade was 20.56% by sampling analysis.
(2) Calcium chloride dissolution: 155 g of crystalline calcium chloride (CaCl)2·6H2O) is heated to 50 ℃ to be dissolved into an aqueous solution.
(3) Mixing materials: mixing 100 g of pollucite ore powder ground in the step (1) with 155 g of calcium chloride solution melted in the step (2) in a ratio of 1: the ratio of 1.55 was sufficiently mixed in a porcelain crucible.
(4) Putting the materials uniformly mixed in the step (3) and loaded in a porcelain crucible into a muffle furnace for roasting; the roasting temperature is controlled at 830 ℃, and the roasting time is controlled at 1 hour.
(5) Cooling the material obtained in the step (4), taking out, and grinding the material in a sampling machine to D50112.6um (about 135 mesh) weighing 178 g.
(6) And (3) leaching the roasted material obtained in the step (5) by using 534 ml of water with a liquid-solid ratio of 3: 1, heating to 80 ℃, and keeping the temperature for 1.5 hours;
(7) carrying out suction filtration on the leached slurry in the step (6) to obtain 466ml of leachate, weighing, adding 215g of water into the wet residue with the weight of 215.6g, carrying out leaching by using the liquid-solid ratio of 1:1, and carrying out suction filtration to obtain 214ml of washing liquid to obtain 216g of washed wet leached residue;
(8) and (4) putting the wet leaching residue produced in the step (7) into an oven, drying for 2 hours at a constant temperature of 200 ℃, cooling, taking out, and weighing, wherein the weight is 153.8 g.
(9) 693ml of leachate (including washing liquid) and 153.8g of leaching residue (dry basis) produced in the steps (7) and (8) are sampled and analyzed.
(10) The cesium content in the leaching solution is 28.73g/l, the cesium content in the leaching residue is 0.36%, and the recovery rate of the leaching solution is 96.83%.
Example 5
(1) Grinding ores: grinding pollucite with a sample preparation machine to obtain a powder with a particle size of D50When 81.3um (about 180 mesh) pollucite powder, the cesium grade was 20.56% by sampling analysis.
(2) Calcium chloride dissolution: 160 g of crystalline calcium chloride (CaCl)2·6H2O) is heated to 50 ℃ to be dissolved into an aqueous solution.
(3) Mixing materials: mixing 100 g of pollucite ore powder ground in the step (1) with 160 g of calcium chloride solution melted in the step (2) in a ratio of 1: the ratio of 1.6 was sufficiently mixed in a porcelain crucible.
(4) Putting the materials uniformly mixed in the step (3) and loaded in a porcelain crucible into a muffle furnace for roasting; the roasting temperature is controlled at 850 ℃, and the roasting time is controlled at 40 minutes.
(5) The material from step (4) was cooled and removed, ground in a sample preparation mill to 150 mesh and weighed 179.4 g.
(6) And (3) stirring and leaching the roasted material obtained in the step (5) by using 625 ml of water, wherein the liquid-solid ratio is 3.5: 1, heating to 90 ℃, and keeping the temperature for 1 hour;
(7) carrying out suction filtration on the leached slurry in the step (6) to obtain 558ml of leached liquid, weighing, adding 218g of water into 217.6g of wet residues according to the liquid-solid ratio of 1:1 for leaching, and carrying out suction filtration to obtain 217ml of washing liquid to obtain 218g of wet leached residues;
(8) and (4) putting the wet leaching residue produced in the step (7) into an oven, drying for 2 hours at a constant temperature of 200 ℃, cooling, taking out, and weighing, wherein the weight is 164.9 g.
(9) 785ml of the leachate (including the washing liquid) produced in the step (7) and the leachate (dry basis) produced in the step (8) and 154.6g of the leaching residue were sampled and analyzed.
(10) The cesium content in the leaching solution is 25.70g/l, the cesium content in the leaching residue is 0.19%, and the recovery rate of the leaching solution is 98.12%.
Example 6
(1) Grinding ores: grinding pollucite with a sample preparation machine to obtain a powder with a particle size of D50When 81.3um (about 180 mesh) pollucite powder, the cesium grade was 20.56% by sampling analysis.
(2) Calcium chloride pretreatment: 155 g of crystalline calcium chloride (CaCl)2·6H2O) loosening.
(3) Mixing materials: mixing 100 g of pollucite ore powder ground in the step (1) and 155 g of calcium chloride solid loosened in the step (2) in a ratio of 1: the ratio of 1.55 was sufficiently mixed in a porcelain crucible.
(4) Putting the materials uniformly mixed in the step (3) and loaded in a porcelain crucible into a muffle furnace for roasting; the roasting temperature is controlled at 830 ℃, and the roasting time is controlled at 1 hour.
(5) Cooling the material obtained in the step (4), taking out the cooled material, and preparing the sample in a sampling machineGrinding to D50112.6um (about 135 mesh) and weigh 178.3 g.
(6) And (3) stirring and leaching the roasted material obtained in the step (5) by using 535 ml of water, wherein the liquid-solid ratio is 3: 1, heating to 80 ℃, and keeping the temperature for 1.5 hours;
(7) carrying out suction filtration on the leached slurry in the step (6) to obtain 474ml of leached liquid, weighing 219g of wet residues, adding 219g of water to the liquid-solid ratio of 1:1 for leaching, and carrying out suction filtration to obtain 218ml of washing liquid to obtain 219.6g of washed wet leached residues;
(8) and (4) putting the wet leaching residue produced in the step (7) into an oven, drying for 2 hours at a constant temperature of 200 ℃, cooling, taking out, and weighing, wherein the weight is 162.7 g.
(9) 692ml of leaching solution (comprising washing solution) produced in the step (7) and 158.7g of leaching residue (dry basis) are sampled and analyzed.
(10) The cesium content in the leaching solution is 25.33g/l, the cesium content in the leaching residue is 1.85%, and the recovery rate is 85.24% by the leaching solution.
Claims (7)
1. A method for extracting cesium from pollucite based on a chloridizing roasting method is characterized by comprising the following steps:
(1) grinding ores: milling the ore by a sampling machine to obtain pollucite ore powder;
(2) calcium chloride dissolution: heating and melting calcium chloride into an aqueous solution;
(3) mixing materials: uniformly mixing the pollucite ore powder ground in the step (1) with the calcium chloride solution melted in the step (2);
(4) adding the uniformly mixed material obtained in the step (3) into a crucible, and roasting by using a muffle furnace;
(5) filtering and taking out the materials subjected to the step (4), grinding and weighing;
(6) stirring the roasted material obtained in the step (5) with water and heating for leaching;
(7) carrying out suction filtration and leaching on the leached slurry in the step (6), and combining a washing liquid with the leached liquid to obtain the leached liquid and leached residues;
(8) measuring, sampling and analyzing the leachate produced in the step (7);
(9) and (4) conveying the measured and sampled leachate obtained in the step (8) to an extraction process to extract a high-grade cesium product.
2. The method for extracting cesium from pollucite based on chloridizing roasting method as claimed in claim 1, wherein in step (1), the particle size of pollucite ore powder is ground to 160-200 mesh.
3. The method for extracting cesium from pollucite based on chloridizing roasting method according to claim 1, wherein in step (3), pollucite ore powder is mixed with 1.3-1.6 times by weight of calcium chloride solution.
4. The method for extracting cesium from pollucite based on the chloridizing roasting method according to claim 1, wherein in step (4), heating to 750-850 ℃ for reaction for 20-60 minutes.
5. The method for extracting cesium from pollucite based on the chloridizing roasting method according to claim 1, wherein in step (5), the reactants are ground to 120-160 mesh.
6. The method for extracting cesium from pollucite based on the chloridizing roasting method according to claim 1, wherein in step (6), the liquid-solid ratio is 2.5-3.5: 1, heating to 80-90 ℃ to carry out leaching reaction for 1-2 hours.
7. The method for extracting cesium from pollucite based on the chloridizing roasting method according to claim 1, wherein in step (7), the liquid-solid ratio of the washing residue is 1:1 to 2.
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