CN113046554A - Method for leaching weathering crust elution-deposited rare earth ore by using metabolite of microorganism - Google Patents
Method for leaching weathering crust elution-deposited rare earth ore by using metabolite of microorganism Download PDFInfo
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Abstract
The invention discloses a method for leaching weathering crust elution-deposited rare earth ore by using metabolites of microorganisms, which comprises the following steps: 1) culturing of the microorganisms: selecting one or more of the following three groups of microorganisms, and independently culturing in a proper liquid culture medium and a proper culture condition, and obtaining a bacterial suspension after culturing for a set time; 2) extraction of metabolites: crude extraction is carried out on the bacterial suspension in the step 1) to obtain a solid metabolite; 3) leaching: mixing the metabolic products obtained in the step 2) with the weathered crust elution type rare earth ore subjected to ball milling according to a set proportion, and then leaching under a set leaching condition to obtain a leaching solution. The key metabolite of the microorganism selected by the invention not only can not cause environmental pollution, but also is beneficial to ecological restoration and improvement. The method has the advantages of high efficiency, environmental protection, low cost, simple operation and the like, and is suitable for popularization and application.
Description
Technical Field
The invention belongs to the field of hydrometallurgy and mineral processing, and particularly relates to a method for leaching weathering crust elution type rare earth ore by using metabolites of microorganisms.
Background
Rare earth, called as "industrial vitamin", is an important strategic resource, has irreplaceable effects in many fields such as electronics, communication, superconduction and the like, is a key basic material for upgrading the traditional industry and developing new industries, and has wide application in equipment development and production in the field of national defense.
The rare earth resources in China are rich, the reserves are large, the distribution is wide, and the mineral varieties are complete. Through the development of more than 50 years in China, a relatively complete rare earth industrial chain and an industrial system are established, the development of rare earth mining, smelting separation and application technology is greatly improved, the industrial scale is continuously expanded, and the rare earth is developed into the first major country for rare earth production, export and consumption in the world and has a very important position in the world. Particularly, the weathering crust eluviation type (ionic type) rare earth ore which is special in China contains more key medium and heavy rare earth elements, and is an important strategic mineral resource in China.
However, the problems of repeated illegal exploitation, insufficient smelting separation capacity, serious ecological environment damage and resource waste, disordered export order and the like still exist in the development of the rare earth industry, and the sustainable development of the rare earth industry is seriously influenced. With the rapid development of rare earth industry in China, the consumption speed of rare earth mineral resources is accelerated, the resource utilization rate is low in the rare earth extraction process, and the problems of environmental pollution are increasingly serious. How to efficiently and environmentally extract rare earth, improve the utilization rate and the application added value of rare earth resources, realize the balanced application of rare earth elements and the like is an urgent problem to be solved in rare earth science and technology and industrial development in China.
The weathering crust leaching type rare earth ore is usually leached by ammonium sulfate and other salt ions, and the obtained rare earth leachate is subjected to ammonium bicarbonate impurity removal and oxalic acid precipitation recovery, but the existing rare earth precipitation recovery process has the serious environmental protection problems of low rare earth recovery rate, high consumption of chemical reagents, ammonia nitrogen pollution and the like, and is limited to be applied. In recent years researchers have attempted to find leachants that replace ammonium sulfate. Other salt ions (sulfuric acid or chloride of potassium, sodium, calcium, magnesium and the like) are used for leaching, but the leaching effect, the cost, the environmental protection and other factors cannot be applied industrially, and particularly, the high-concentration and high-dosage salt ions inevitably cause environmental pollution, soil and ecological damage.
The microbial biological metallurgy (leaching) is an important technology for clean and efficient extraction of complex mineral resources, mineral elements are leached by using metabolites generated by microorganisms, but the metabolites of different microorganisms have large difference, so that the selection of the metabolites of suitable microorganisms has great influence on the leaching of minerals. At present, few reports are related to leaching weathering crust elution type (ionic type) rare earth by using metabolites of microorganisms, so that the development of a process for leaching weathering crust elution type (ionic type) rare earth by using microorganisms has great research significance.
Disclosure of Invention
The invention aims to provide a method for leaching weathering crust elution-type rare earth ore by using metabolites of microorganisms, which solves the problems of high production cost, large dosage of leaching agent, easy generation of environmental pollution, soil and ecological damage and the like commonly existing in the chemical leaching process of weathering crust elution-type rare earth ore.
The method for leaching weathering crust elution-deposited rare earth ore by using metabolites of microorganisms comprises the following steps:
1) culturing of the microorganisms: selecting one or more of the following three groups of microorganisms, and independently culturing in a proper liquid culture medium and a proper culture condition, and obtaining a bacterial suspension after culturing for a set time;
2) extraction of metabolites: crude extraction is carried out on the bacterial suspension in the step 1) to obtain a solid metabolite;
3) leaching: mixing the metabolite in the step 2) with the weathered crust elution type rare earth ore according to a set liquid-solid ratio, and then leaching under a set leaching condition to obtain a leaching solution;
the three groups of microorganisms in the step 1) are respectively: a first group: pseudomonas aeruginosa, yarrowia lipolytica, Zygosaccharomyces rouxii and Bacillus subtilis; second group: nitrite monad, Vickers nitrobacter; third group: lactobacillus plantarum, propionibacterium, acetobacter, saccharomyces cerevisiae, pediococcus acidilactici and escherichia coli.
Preferably, the microorganisms are two of the three groups of microorganisms, after the two groups of microorganisms are respectively cultured, bacterial suspensions are mixed according to the volume ratio of 1 (0.5-1.5), and then metabolites are extracted; further preferably, the two microorganisms are from different groups.
Preferably, the microorganisms are three of three groups of microorganisms, after the three groups of microorganisms are respectively cultured, bacterial suspensions are mixed according to the volume ratio of 1 (0.5-1.5) to (0.5-1.5), and then metabolites are extracted; it is further preferred that the three microorganisms are from different groups, i.e. one microorganism from each of the first, second and third groups.
In the step 1), the culture medium matrixes of the microorganisms are respectively: substrates of pseudomonas aeruginosa, escherichia coli, bacillus subtilis, nitrosomonas nitrite and nitrobacter winogradskyi are tryptone, yeast extract and NaCl; the culture medium of Lactobacillus plantarum, Propionibacterium, Acetobacter, Saccharomyces cerevisiae, Lactobacillus lactis and yarrowia lipolytica is sucrose, urea, MgSO4NaCl, Tween 80; the culture medium of Zygosaccharomyces rouxii is sucrose and soybean peptone; the setting time is 5-12 days.
In the step 2), the crude extraction process is one or more of centrifugation, extraction, adsorption, ion exchange, membrane separation, electrodialysis and esterification.
In the step 3), the solid ratio of the leaching solution is 1: 1-10: 1; the leaching conditions are as follows: the leaching temperature is 15-75 ℃, and the potential of a leaching system is controlled to be 350-850 mV relative to a saturated silver/silver chloride electrode; the leaching pH is 1-6.
The principle of the invention is as follows: the acids contained in the first group of microbial metabolites adopted by the invention mainly comprise citric acid, malic acid, gluconic acid and ascorbic acid; the metabolites of the second group of microorganisms contain a large amount of siderophores (hydroxamate type, catechol type, and carboxylate type); the third group of microorganism metabolites contains tartaric acid, salicylic acid, and itaconic acid; the metabolites of the above microorganisms may also contain various proteases and polysaccharides; the metabolic products of the microorganisms, such as organic acid, siderophore, protease and the like, are mixed with the ore of the weathering crust elution type rare earth ore for leaching, the metabolic products, such as organic acid (salt) and siderophore, can efficiently leach ionic rare earth through the complexation and chelation of functional groups, such as hydroxyl, carboxyl and the like, biological enzyme and polysaccharide generated by metabolism also have certain corrosive effect on the ore, and the metabolic products of the microorganisms have biological activity and obviously higher effect than chemical reagents; thereby achieving the effect of leaching rare earth elements in the ores of the weathering crust elution-deposited rare earth ores.
The invention has the beneficial effects that: the invention adopts metabolites of special microorganisms as leaching reagents, key metabolites of the microorganisms are mainly organic acids (salts) containing functional groups such as carboxyl, hydroxyl and the like, siderophores, protease and polysaccharide, wherein the organic acids mainly comprise citric acid, gluconic acid, lactic acid, malic acid, pyruvic acid, ascorbic acid, salicylic acid and the like and salts thereof, and the siderophores mainly comprise siderophores including hydroxamate type, catechol type, carboxylate type and the like. These metabolites can efficiently leach out ionic rare earths through complexation or chelation, and due to biological activity, the effect is often remarkable due to chemical agent leaching. The key metabolite of the microorganism selected by the invention not only can not cause environmental pollution, but also is beneficial to ecological restoration and improvement. The method has the advantages of high efficiency, environmental protection, low cost, simple operation and the like, and is suitable for popularization and application.
Detailed Description
The liquid-solid ratio is mL/g, and the grade is the mass fraction of elements.
Example 1
Inoculating Pseudomonas aeruginosa (purchased Pseudomonas aeruginosa ATCC27853) into a culture medium (10 g/L of tryptone and 5g/L, NaCl 0.5.5 g/L of yeast extract), culturing at pH of 4.5 and temperature of 30 ℃ for 7 days, and testing strain concentration which is more than or equal to 1.0 × 107Obtaining pseudomonas aeruginosa suspension after the strain/mL is qualified;
yarrowia lipolytica (purchase Yar)Rowialipotica ATCC30162) was inoculated into a medium (yeast powder 10g/L, glucose 10g/L, K2HPO4Is 0.6g/L, MgSO40.4g/L), culturing at 30 deg.C and pH of 4.5 for 7 days, and testing strain concentration to 1.0 × 107The cell/mL is qualified; obtaining yarrowia lipolytica suspension;
mixing the pseudomonas aeruginosa suspension and the yarrowia lipolytica suspension according to the volume ratio of 1:1, then centrifuging, extracting supernatant, and then further filtering the supernatant to obtain a solution, namely a metabolite.
Mixing the metabolite and weathered crust eluviation type rare earth ore (rare earth grade is 0.12%) according to a liquid-solid ratio of 1:1, and controlling the potential of a leaching system at 510mV relative to a saturated silver/silver chloride electrode at a leaching temperature of 30 ℃; leaching for 12 hours under the leaching condition that the leaching pH is 4.5, after leaching, measuring the concentration of the rare earth element and calculating the leaching rate by an ICP-OES method, wherein the leaching rate of the aluminum impurity element is 14.5%. The final rare earth element recovery rate of 94.31 percent is obtained.
Example 2
Lactobacillus plantarum ATCC8014 was inoculated to the medium (yeast powder 10g/L, glucose 10g/L, K)2HPO4Is 0.6g/L, MgSO40.4g/L), culturing at 30 deg.C and pH of 10.0 for 7 days, and testing strain concentration to 1.0 × 107Obtaining lactobacillus plantarum bacterial suspension after the strain/mL is qualified;
propionibacterium (Propionibacterium acidipropionici ATCC4875) was inoculated into a medium (yeast powder 10g/L, glucose 10g/L, K)2HPO4Is 0.6g/L, MgSO40.4g/L), culturing at 30 deg.C and pH of 10.0 for 7 days, and testing strain concentration to 1.0 × 107The cell/mL is qualified; obtaining a propionibacterium suspension;
mixing the lactobacillus plantarum suspension and the propionibacterium suspension according to the volume ratio of 1:1, filtering, and obtaining a metabolite after filtering.
Mixing the metabolite and weathered crust eluviation type rare earth ore (rare earth grade is 0.12%) according to a liquid-solid ratio of 2:1, and controlling the potential of a leaching system at 536mV relative to a saturated silver/silver chloride electrode at a leaching temperature of 30 ℃; leaching for 12h under the leaching condition that the leaching pH is 3.0, measuring the concentration of the rare earth element by using an ICP-OES method after leaching is finished, and calculating the leaching rate, wherein the leaching rate of the aluminum impurity element is 13.4%. The recovery rate of the final rare earth element is 96.35 percent.
Example 3
Acetobacter aceti (Acetobacter aceti ATCC15973 purchased) was inoculated into a medium (tryptone 10g/L, yeast extract 5g/L, NaCl 0.5g/L, glucose 10g/L, K g/L)2HPO40.6g/L), at the temperature of 30 ℃ and the pH of 7.2-7.5, after culturing for 7 days, testing the strain concentration, wherein the strain concentration is more than or equal to 1.0 multiplied by 107Obtaining the bacillus aceticus suspension after the strain/mL is qualified;
saccharomyces cerevisiae ATCC20499 purchased was inoculated to a medium (yeast powder 10g/L, glucose 10g/L, K)2HPO4Is 0.6g/L, MgSO40.4g/L), at the temperature of 30 ℃ and the pH of 7.2-7.5, after culturing for 7 days, testing the strain concentration, wherein the strain concentration is more than or equal to 1.0 multiplied by 107The cell/mL is qualified; obtaining saccharomyces cerevisiae suspension;
pediococcus acidilactici (purchased Pediococcus acidilactii ATCC8018) was inoculated into the culture medium NaNO33g/L of cane sugar and 30g/L, K of cane sugar2HPO4Is 1g/L, MgSO40.5g/L, KCl 0.5.5 g/L), at pH 7.3 and 30 deg.C for 7 days, testing strain concentration to be not less than 1.0 × 107The cell/mL is qualified; obtaining pediococcus acidilactici bacterial suspension;
mixing acetic acid bacillus suspension, saccharomyces cerevisiae suspension and pediococcus acidilactici suspension according to the volume ratio of 1:1:1, filtering, and obtaining a metabolite after filtering.
Mixing the metabolite and weathered crust eluviation type rare earth ore (rare earth grade is 0.12%) according to a liquid-solid ratio of 5:1, and controlling the potential of a leaching system at 527mV relative to a saturated silver/silver chloride electrode at a leaching temperature of 30 ℃; leaching for 12h under the leaching condition that the leaching pH is 2.5, measuring the concentration of the rare earth element by using an ICP-OES method after leaching is finished, and calculating the leaching rate, wherein the leaching rate of the aluminum impurity element is 12.5%. The recovery rate of the final rare earth element is 98.21 percent.
Example 4
Pediococcus acidilactici (purchased Pediococcus acidilactii ATCC8018) was inoculated into a medium (NaNO)33g/L of cane sugar and 30g/L, K of cane sugar2HPO4Is 1g/L, MgSO40.5g/L, KCl 0.5.5 g/L), at the pH of 7.2-7.5 and the temperature of 30 ℃, after culturing for 7 days, testing the strain concentration, wherein the strain concentration is more than or equal to 1.0 multiplied by 107The cell/mL is qualified; obtaining pediococcus acidilactici bacterial suspension;
escherichia coli (purchased Escherichia coli ATCC25922) was inoculated into a medium (tryptone 10g/L, yeast extract 5g/L, NaCl 0.5.5 g/L, glucose 10g/L, K g/L)2HPO40.6g/L), culturing at 30 deg.C and pH of 10.2 for 7 days, and testing strain concentration to 1.0 × 107The cell/mL is qualified; obtaining Escherichia coli bacterial suspension;
mixing the lactic acid bacteria pellet bacterial suspension and the Escherichia coli bacterial suspension according to the volume ratio of 1:1, filtering, and obtaining a metabolite after filtering.
Mixing the metabolite and weathered crust eluviation type rare earth ore (rare earth grade is 0.12%) according to a liquid-solid ratio of 7:1, and controlling the potential of a leaching system at 568mV relative to a saturated silver/silver chloride electrode at a leaching temperature of 30 ℃; leaching for 12h under the leaching condition that the leaching pH is 3.0, measuring the concentration of the rare earth element by using an ICP-OES method after leaching is finished, and calculating the leaching rate, wherein the leaching rate of the aluminum impurity element is 12.7%. The final rare earth element recovery rate of 95.57 percent is obtained.
Example 5
Zygosaccharomyces rouxii (Saccharomyces rouxii ATCC14679 purchased) was inoculated into a medium (sucrose 10g/L, MgSO)40.5g/L, KCl 0.5.5 g/L), at pH of 5.6-7.3 and 30 deg.C for 7 days, testing strain concentration to be not less than 1.0 × 107The cell/mL is qualified; obtaining zygosaccharomyces rouxii suspension;
bacillus subtilis (purchased Bacillus)subtilis ATCC6633) was inoculated into a medium (tryptone 10g/L, yeast extract 5g/L, NaCl 0.5g/L, glucose 10g/L, K2HPO40.6g/L), at the temperature of 30 ℃ and the pH of 5.6-7.3, after culturing for 7 days, testing the strain concentration which is more than or equal to 1.0 multiplied by 107The cell/mL is qualified; obtaining bacillus subtilis suspension;
mixing the zygosaccharomyces rouxii suspension and the bacillus subtilis suspension according to the volume ratio of 1:1, filtering, and obtaining a metabolite after filtering.
Mixing the metabolite and weathered crust eluviation type rare earth ore (rare earth grade is 0.12%) according to a liquid-solid ratio of 8:1, and controlling the potential of a leaching system at 563mV relative to a saturated silver/silver chloride electrode at a leaching temperature of 30 ℃; leaching for 12h under the leaching condition that the leaching pH is 3.5, measuring the concentration of the rare earth element by using an ICP-OES method after leaching is finished, and calculating the leaching rate, wherein the leaching rate of the aluminum impurity element is 18.5%. The final recovery rate of the rare earth elements is 94.85 percent.
Example 6
Bacillus subtilis ATCC6633 purchased from Bacillus subtilis was inoculated into a medium (tryptone 10g/L, yeast extract 5g/L, NaCl 0.5g/L, glucose 10g/L, K g/L)2HPO40.6g/L), at the temperature of 30 ℃ and the pH of 5.6-7.3, after culturing for 7 days, testing the strain concentration which is more than or equal to 1.0 multiplied by 107The cell/mL is qualified; obtaining bacillus subtilis suspension;
inoculating nitrobacter winogradsky (purchased as Nitrobacter winogradsky ATCC25391) into a culture medium (sodium nitrite 1g/L magnesium sulfate 0.03g/L manganese sulfate 0.01g/L dipotassium phosphate 0.75g/L anhydrous sodium carbonate 1g/L sodium dihydrogen phosphate 0.25g/L), culturing at 30 ℃ and pH of 5.6-7.3 for 7 days, and testing the strain concentration, wherein the strain concentration is more than or equal to 1.0 multiplied by 107The cell/mL is qualified; obtaining nitrobacter winogradskyi bacterial suspension;
saccharomyces cerevisiae ATCC20499 purchased was inoculated to a medium (yeast powder 10g/L, glucose 10g/L, K)2HPO4Is 0.6g/L, MgSO40.4g/L), at a pH of 7.2 to 7.5 and a temperature of 30 ℃ for 7 daysTesting the strain concentration, wherein the strain concentration is more than or equal to 1.0 multiplied by 107The cell/mL is qualified; obtaining saccharomyces cerevisiae suspension;
mixing the bacillus subtilis, the nitrobacter winogradskyi and the saccharomyces cerevisiae suspension according to the volume ratio of 1:1:1, filtering, and obtaining a metabolite after filtering.
Mixing the metabolite and weathered crust eluviation type rare earth ore (rare earth grade is 0.12%) according to a liquid-solid ratio of 10:1, and controlling the potential of a leaching system at 563mV relative to a saturated silver/silver chloride electrode at a leaching temperature of 30 ℃; leaching for 12h under the leaching condition that the leaching pH is 4.0, measuring the concentration of the rare earth element by using an ICP-OES method after leaching is finished, and calculating the leaching rate, wherein the leaching rate of the aluminum impurity element is 14.2%. The recovery rate of the final rare earth element is 95.35 percent.
Claims (8)
1. A method for leaching weathering crust elution-deposited rare earth ore by using metabolites of microorganisms comprises the following steps:
1) culturing of the microorganisms: selecting one or more of the following three groups of microorganisms, and independently culturing in a proper liquid culture medium and a proper culture condition, and obtaining a bacterial suspension after culturing for a set time;
2) extraction of metabolites: crude extraction is carried out on the bacterial suspension in the step 1) to obtain a solid metabolite;
3) leaching: mixing the metabolic products obtained in the step 2) with the weathered crust elution type rare earth ore ores subjected to ball milling according to a set proportion, and then leaching under a set leaching condition to obtain a leaching solution;
the three groups of microorganisms in the step 1) are respectively: a first group: pseudomonas aeruginosa, yarrowia lipolytica, Zygosaccharomyces rouxii and Bacillus subtilis; second group: nitrite monad, Vickers nitrobacter; third group: lactobacillus plantarum, propionibacterium, acetobacter, saccharomyces cerevisiae, pediococcus acidilactici and escherichia coli.
2. The method for leaching the weathering crust eluviation type rare earth ore by using the metabolites of the microorganisms according to claim 1, wherein the microorganisms are two of three groups of microorganisms, after the two groups of microorganisms are respectively cultured, the bacterial suspensions are mixed according to the volume ratio of 1 (0.5-1.5), and then the metabolites are extracted.
3. The method of leaching rare earth ores of the weathering crust elution type using metabolites of microorganisms according to claim 2, wherein the two microorganisms are from different groups.
4. The method for leaching the weathering crust eluviation type rare earth ore by using the metabolites of the microorganisms according to claim 1, wherein the microorganisms are three of three groups of microorganisms, and after the microorganisms are respectively cultured, the bacterial suspensions are mixed according to the volume ratio of 1 (0.5-1.5) to (0.5-1.5), and then the metabolites are extracted.
5. The method of leaching rare earth ore of the weathering crust elution type using metabolites of microorganisms according to claim 4, wherein the three microorganisms are from different groups, i.e., one microorganism selected from each of the first, second and third groups.
6. The method for leaching weathering crust elution type rare earth ore by using the metabolite of the microorganism according to claim 1, wherein in the step 1), the culture medium matrixes of the microorganism are respectively: substrates of pseudomonas aeruginosa, escherichia coli, bacillus subtilis, nitrosomonas nitrite and nitrobacter winogradskyi are tryptone, yeast extract and NaCl; the culture medium of Lactobacillus plantarum, Propionibacterium, Acetobacter, Saccharomyces cerevisiae, Lactobacillus lactis and yarrowia lipolytica is sucrose, urea, MgSO4NaCl, Tween 80; the culture medium of Zygosaccharomyces rouxii is sucrose and soybean peptone; the setting time is 5-12 days.
7. The method for leaching rare earth ore of the weathering crust elution type using metabolites of microorganisms according to claim 1, wherein in the step 2), the crude extraction process is one or more of centrifugation, extraction, adsorption, ion exchange, membrane separation, electrodialysis and esterification.
8. The method for leaching the weathering crust elution-type rare earth ore by using the metabolite of the microorganism according to claim 1, wherein in the step 3), the solid-to-solid ratio of the leaching solution is 1: 1-10: 1; the leaching conditions are as follows: the leaching temperature is 15-75 ℃, and the potential of a leaching system is controlled to be 350-850 mV relative to a saturated silver/silver chloride electrode; the leaching pH is 1-6.
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| CN115491490A (en) * | 2022-09-23 | 2022-12-20 | 中南大学 | Method for enhancing permeability of bioleaching agent in leaching process of ionic rare earth ore |
| CN115505736A (en) * | 2022-09-23 | 2022-12-23 | 中南大学 | Method for bioleaching ionic rare earth ore in neutral or partial neutral environment |
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| CN115491490A (en) * | 2022-09-23 | 2022-12-20 | 中南大学 | Method for enhancing permeability of bioleaching agent in leaching process of ionic rare earth ore |
| CN115505736A (en) * | 2022-09-23 | 2022-12-23 | 中南大学 | Method for bioleaching ionic rare earth ore in neutral or partial neutral environment |
| CN115505736B (en) * | 2022-09-23 | 2024-04-19 | 中南大学 | Method for bioleaching ionic rare earth ore in neutral or near-neutral environment |
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