CN110607442B - Method for applying heavy saponification removal wastewater to rare earth in-situ leaching - Google Patents
Method for applying heavy saponification removal wastewater to rare earth in-situ leaching Download PDFInfo
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- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/10—Hydrochloric acid, other halogenated acids or salts thereof
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- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
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- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
- C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
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- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
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- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
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- C22B59/00—Obtaining rare earth metals
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Abstract
The invention discloses a method for applying heavy saponification removal wastewater to rare earth in-situ leaching, which comprises four steps of preparing a leaching agent, in-situ leaching, removing impurities from a rare earth leaching solution and extracting rare earth, wherein the heavy saponification removal wastewater and magnesium oxide are compounded to prepare the leaching agent, then the leaching agent is used for performing rare earth in-situ leaching, after the impurities are removed from the leaching solution, an extracting agent is added for extraction, a loaded organic phase containing rare earth ions and a raffinate aqueous phase are obtained after standing and clarification, then the loaded organic phase containing the rare earth ions is back-extracted by hydrochloric acid with the same volume to obtain a mixed rare earth chloride solution, and then the mixed rare earth chloride solution is subjected to conventional concentration and crystallization to obtain a mixed rare earth chloride product. The method recycles the calcium saponification wastewater, solves the problem of water hardness increase in the environment caused by calcium saponification wastewater discharge, realizes effective utilization of waste resources, and reduces the cost of rare earth in-situ mineral leaching production.
Description
Technical Field
The invention belongs to the technical field of saponification wastewater recycling, and particularly relates to a method for applying heavy saponification wastewater to rare earth in-situ ore leaching.
Background
In-situ leaching, referred to as "ground leaching", is a mining technique in which, under the condition of natural production of ore, leaching liquid is injected into the ore bed through liquid injection holes, the leaching liquid selectively leaches useful components in the ore, and the generated soluble compounds enter the leaching liquid flow and are lifted to the earth surface through liquid extraction holes for processing and extracting metals. Compared with the conventional mining and smelting method, the ground soaking method mainly has the advantages of low capital investment, short construction period, low production cost, good environmental protection, no damage to farmlands and mountain forests, no environmental pollution and the like. Compared with the traditional pond leaching and heap leaching modes, the rare earth in-situ leaching method has the advantages of no damage to vegetation on the earth surface of an ore body, no stripping of surface soil, protection of ecological environment, high rare earth recovery rate, less excavation and carrying work in production, reduction of working strength, production cost saving and the like, so the rare earth mining method for rare earth in-situ leaching is pushed at home and abroad at present.
Rare earth can be recovered by rare earth extraction separation of rare earth leachate obtained by in-situ leaching of rare earth, at present, the rare earth is extracted and separated by a solvent extraction method, three solvents, namely a cation extractant represented by acid phosphate, such as a P204 rare earth extractant and a P507 rare earth extractant, or an anion exchange solution N1923 represented by amine and a solvent extractant represented by neutral phosphate such as TBP, P350 and the like, are used, and the rare earth is purified by matching with equipment such as a mixer-settler, a centrifugal extractor and the like. In the process of extracting rare earth, H is continuously dissociated in the process of combining the extracting agents such as P507 and P204 with rare earth ions+The extraction efficiency is reduced, so the extraction agent needs to be saponified in the extraction process, ammonia water, calcium oxide and the like are commonly used, and the calcium saponification technology is more widely used because ammonia saponification can generate ammonia nitrogen wastewater. The calcium saponification wastewater contains part of heavy metal ions, organic phosphorus and Ca2+And the heavy metal ions are removed by the treatment of the environmental protection facility, and the obtained heavy saponification removal wastewater still contains a large amount of Ca2+If the waste rare earth is directly discharged, the hardness of the water body is increased, so the saponified waste liquid after weight removal is used for blending and in-situ leaching of rare earth, the recycling of waste resources is realized, and the method has great practical value and significance.
Disclosure of Invention
Aiming at the defects, the invention discloses a method for applying heavy saponification removal wastewater to rare earth in-situ ore leaching, which recycles calcium saponification wastewater, solves the problem of water hardness increase in the environment caused by calcium saponification wastewater discharge, realizes effective utilization of waste resources and reduces the production cost of rare earth in-situ ore leaching.
The invention is realized by adopting the following technical scheme:
a method for applying heavy saponification wastewater to rare earth in-situ leaching comprises the following steps:
(1) preparing an ore leaching agent: adding magnesium oxide into the heavy saponification removal wastewater under the stirring condition, respectively counting by calcium oxide and magnesium oxide, stopping adding the magnesium oxide when the mass ratio of calcium element to magnesium element in the heavy saponification removal wastewater is adjusted to (8-10): 1, and then continuously stirring for 20-30 min to obtain a solution A; adding hydrochloric acid into the solution A to adjust the pH value to 3-4, and obtaining an ore leaching agent; the content of calcium element in the heavy saponification removal wastewater is 100-160 g/L calculated by calcium oxide, and the pH value of the heavy saponification removal wastewater is 4-6;
(2) in-situ leaching: injecting the mineral leaching agent obtained in the step (1) into the injection point, wherein the liquid-solid ratio of the mineral leaching agent to the rare earth ore is 1000kg (0.4-1) kg, when the concentration of REO in the leachate is lower than 0.1g/L, stopping injecting the mineral leaching agent into the injection point, and then injecting top water into the injection point, wherein the liquid-solid ratio of the top water to the rare earth ore is 1000kg (0.3-1) kg;
(3) removing impurities from the rare earth leachate: adding a sodium bicarbonate solution into the leachate collected in the step (2) to adjust the pH value to 5-6, stirring for 2-3 h, standing, and filtering to remove precipitates to obtain a filtrate;
(4) rare earth extraction: and (3) mixing the filtrate obtained in the step (3) with an extracting agent in an equal volume, stirring for 30-40 min, standing for clarification to obtain a loaded organic phase containing rare earth ions and an extracted water phase, performing back extraction on the loaded organic phase containing the rare earth ions by using hydrochloric acid in an equal volume to obtain a mixed rare earth chloride solution, and performing conventional concentration and crystallization on the mixed rare earth chloride solution to obtain a mixed rare earth chloride product.
Further, the stirring speed in the step (1) is 600-800 r/min.
Further, the mass concentration of the sodium bicarbonate solution in the step (3) is 20-25%.
Further, the extracting agent in the step (4) is obtained by stirring and mixing a solvent, a dispersing agent, calcium oxide and pure water at normal temperature according to the mass ratio of 1:1.5:0.02: 10; the solvent is any one or mixture of P507 and P204; the dispersant is kerosene.
Further, the stirring speed in the step (4) is 500-600 r/min, the stirring speed during extraction is controlled, the diffusion speed of the rare earth ions in the loaded organic phase is increased, the time for reaching balance is greatly shortened, the extraction efficiency is improved, and the problem that the solvent of the loaded organic phase is dissolved into the water phase due to the fact that the stability of the loaded organic phase is damaged due to the excessively high stirring speed is avoided.
Compared with the prior art, the technical scheme has the following beneficial effects:
1. the heavy saponification removal wastewater and the magnesium oxide are compounded in proportion, the pH value is adjusted by hydrochloric acid to obtain the mineral leaching agent for rare earth in-situ mineral leaching, and the liquid-solid ratio is adjusted according to the mineral leaching agent to obtain high rare earth leaching rate.
2. The method is simple to operate, can realize effective utilization of waste resources, and reduces the cost of rare earth in-situ leaching production.
Detailed Description
The invention is further illustrated by the following examples, which are not to be construed as limiting the invention thereto. The specific experimental conditions and methods not indicated in the following examples are generally conventional means well known to those skilled in the art.
Example 1:
a method for applying heavy saponification wastewater to rare earth in-situ leaching comprises the following steps:
(1) preparing an ore leaching agent: adding magnesium oxide into the heavy saponification wastewater under the stirring condition that the stirring speed is 700r/min, respectively counting by calcium oxide and magnesium oxide, stopping adding the magnesium oxide when the mass ratio of calcium element to magnesium element in the heavy saponification wastewater is adjusted to 9:1, and then continuously stirring for 30min to obtain a solution A; adding hydrochloric acid into the solution A to adjust the pH value to 3.5, thus obtaining the mineral leaching agent; the content of calcium element in the heavy saponification wastewater is 160g/L and the pH value of the heavy saponification wastewater is 4, wherein the calcium oxide is counted in the heavy saponification wastewater;
(2) in-situ leaching: injecting the mineral leaching agent obtained in the step (1) into the injection point, wherein the liquid-solid ratio of the mineral leaching agent to the rare earth ore is 1000kg:0.8kg, when the concentration of REO in the leachate is lower than 0.1g/L, stopping injecting the mineral leaching agent into the injection point, and then injecting top water into the injection point, wherein the liquid-solid ratio of the top water to the rare earth ore is 1000kg:0.6 kg;
(3) removing impurities from the rare earth leachate: adding a sodium bicarbonate solution with the mass concentration of 20% into the leachate collected in the step (2) to adjust the pH value to 5.5, stirring for 3 hours, standing, and filtering to remove precipitates to obtain a filtrate;
(4) rare earth extraction: mixing the filtrate obtained in the step (3) with an extracting agent in the same volume, stirring for 40min at the stirring speed of 500r/min, standing for clarification to obtain a loaded organic phase containing rare earth ions and a raffinate water phase, performing back extraction on the loaded organic phase containing the rare earth ions by using hydrochloric acid in the same volume to obtain a mixed rare earth chloride solution, and then performing conventional concentration and crystallization on the mixed rare earth chloride solution to obtain a mixed rare earth chloride product; the extractant is obtained by stirring and mixing a solvent, a dispersant, calcium oxide and pure water at normal temperature according to the mass ratio of 1:1.5:0.02: 10; the solvents are P507 and P204 which are mixed according to the volume ratio of 3: 1; the dispersant is kerosene.
Example 2:
a method for applying heavy saponification wastewater to rare earth in-situ leaching comprises the following steps:
(1) preparing an ore leaching agent: adding magnesium oxide into the heavy saponification wastewater under the stirring condition that the stirring speed is 600r/min, respectively counting by calcium oxide and magnesium oxide, stopping adding the magnesium oxide when the mass ratio of calcium element to magnesium element in the heavy saponification wastewater is adjusted to 8:1, and then continuously stirring for 25min to obtain a solution A; adding hydrochloric acid into the solution A to adjust the pH value to 4, thus obtaining an ore leaching agent; the content of calcium element in the heavy saponification wastewater is 100g/L and the pH value of the heavy saponification wastewater is 6, wherein the calcium oxide is counted in the heavy saponification wastewater;
(2) in-situ leaching: injecting the mineral leaching agent obtained in the step (1) into the injection point, wherein the liquid-solid ratio of the mineral leaching agent to the rare earth ore is 1000kg:1kg, when the concentration of REO in the leachate is lower than 0.1g/L, stopping injecting the mineral leaching agent into the injection point, and then injecting top water into the injection point, wherein the liquid-solid ratio of the top water to the rare earth ore is 1000kg:0.3 kg;
(3) removing impurities from the rare earth leachate: adding a sodium bicarbonate solution with the mass concentration of 25% into the leachate collected in the step (2) to adjust the pH value to 6, stirring for 2.5h, standing, and filtering to remove precipitates to obtain a filtrate;
(4) rare earth extraction: mixing the filtrate obtained in the step (3) with an extracting agent in the same volume, stirring for 30min at the stirring speed of 600r/min, standing for clarification to obtain a loaded organic phase containing rare earth ions and a raffinate water phase, performing back extraction on the loaded organic phase containing the rare earth ions by using hydrochloric acid in the same volume to obtain a mixed rare earth chloride solution, and then performing conventional concentration and crystallization on the mixed rare earth chloride solution to obtain a mixed rare earth chloride product; the extractant is obtained by stirring and mixing a solvent, a dispersant, calcium oxide and pure water at normal temperature according to the mass ratio of 1:1.5:0.02: 10; the solvent is P507; the dispersant is kerosene.
Example 3:
a method for applying heavy saponification wastewater to rare earth in-situ leaching comprises the following steps:
(1) preparing an ore leaching agent: adding magnesium oxide into the heavy saponification wastewater under the stirring condition that the stirring speed is 800r/min, respectively counting by calcium oxide and magnesium oxide, stopping adding the magnesium oxide when the mass ratio of calcium element to magnesium element in the heavy saponification wastewater is adjusted to 10:1, and then continuously stirring for 20min to obtain a solution A; adding hydrochloric acid into the solution A to adjust the pH value to 3, thus obtaining an ore leaching agent; the content of calcium element in the heavy saponification wastewater is 120g/L by calcium oxide, and the pH value of the heavy saponification wastewater is 5;
(2) in-situ leaching: injecting the mineral leaching agent obtained in the step (1) into the injection point, wherein the liquid-solid ratio of the mineral leaching agent to the rare earth ore is 1000kg:0.4kg, when the concentration of REO in the leachate is lower than 0.1g/L, stopping injecting the mineral leaching agent into the injection point, and then injecting top water into the injection point, wherein the liquid-solid ratio of the top water to the rare earth ore is 1000kg:0.4 kg;
(3) removing impurities from the rare earth leachate: adding a sodium bicarbonate solution with the mass concentration of 22% into the leachate collected in the step (2) to adjust the pH value to 5, stirring for 2 hours, standing, and filtering to remove precipitates to obtain a filtrate;
(4) rare earth extraction: mixing the filtrate obtained in the step (3) with an extracting agent in the same volume, stirring for 35min at the stirring speed of 550r/min, standing for clarification to obtain a loaded organic phase containing rare earth ions and a raffinate water phase, performing back extraction on the loaded organic phase containing the rare earth ions by using hydrochloric acid in the same volume to obtain a mixed rare earth chloride solution, and performing conventional concentration and crystallization on the mixed rare earth chloride solution to obtain a mixed rare earth chloride product; the extractant is obtained by stirring and mixing a solvent, a dispersant, calcium oxide and pure water at normal temperature according to the mass ratio of 1:1.5:0.02: 10; the solvent is P204; the dispersant is kerosene.
Experimental example:
carrying out column leaching experiments on the mineral leaching agents described in examples 1-3, and simultaneously carrying out the same column leaching experiments by taking an ammonium sulfate solution with the concentration of 0.2mol/L, a calcium chloride solution with the concentration of 0.2mol/L and a magnesium chloride solution with the concentration of 0.3mol/L as comparative mineral leaching agents; the column leaching experiment is to take 5kg of ionic rare earth ore with 0.356 per mill ion item grade of Chonglevu six-soup mine, crush the ionic rare earth ore and then load the crushed ionic rare earth ore into an ore leaching column with the diameter of 30cm and the height of 150cm, then select one ore leaching agent from the ore leaching agents to carry out the column leaching experiment, control the flow rate by a peristaltic pump to be 0.6ml/L, wash the ore leaching solution with top water when the concentration of REO in mother liquor of the leaching solution is lower than 0.1g/L, and respectively measure the rare earth leaching rate obtained by column leaching by adopting various ore leaching agents, wherein the specific result is shown in Table 1.
TABLE 1 rare earth leaching rates obtained with different leaching agents
According to the results, the leaching agent of the invention is used for column leaching under the same conditions, the leaching rate of the obtained rare earth is not much different from the leaching effect of the leaching agent of ammonium sulfate, and the leaching effect is obviously improved compared with the leaching effect of single calcium chloride and magnesium chloride leaching agents; meanwhile, the mineral leaching agent does not contain ammonium sulfate, so that the environmental pollution caused by ammonia nitrogen wastewater is avoided; therefore, the method not only realizes the recycling of calcium saponification wastewater, solves the problem of water hardness increase in the environment caused by calcium saponification wastewater discharge, but also eliminates the pollution of ammonia nitrogen wastewater to the environment, reduces the cost of rare earth in-situ leaching production, and simultaneously can obtain high rare earth leaching rate.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (4)
1. A method for applying heavy saponification wastewater to rare earth in-situ leaching is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing an ore leaching agent: adding magnesium oxide into the heavy saponification removal wastewater under the stirring condition, respectively counting by calcium oxide and magnesium oxide, stopping adding the magnesium oxide when the mass ratio of calcium element to magnesium element in the heavy saponification removal wastewater is adjusted to (8-10): 1, and then continuously stirring for 20-30 min to obtain a solution A; adding hydrochloric acid into the solution A to adjust the pH value to 3-4, and obtaining an ore leaching agent; the content of calcium element in the heavy saponification removal wastewater is 100-160 g/L calculated by calcium oxide, and the pH value of the heavy saponification removal wastewater is 4-6;
(2) in-situ leaching: injecting the mineral leaching agent obtained in the step (1) into the injection point, wherein the liquid-solid ratio of the mineral leaching agent to the rare earth ore is 1000kg (0.4-1) kg, when the concentration of REO in the leachate is lower than 0.1g/L, stopping injecting the mineral leaching agent into the injection point, and then injecting top water into the injection point, wherein the liquid-solid ratio of the top water to the rare earth ore is 1000kg (0.3-1) kg;
(3) removing impurities from the rare earth leachate: adding a sodium bicarbonate solution into the leachate collected in the step (2) to adjust the pH value to 5-6, stirring for 2-3 h, standing, and filtering to remove precipitates to obtain a filtrate;
(4) rare earth extraction: mixing the filtrate obtained in the step (3) with an extracting agent in an equal volume, stirring for 30-40 min, standing for clarification to obtain a loaded organic phase containing rare earth ions and an extracted water phase, performing back extraction on the loaded organic phase containing the rare earth ions by using hydrochloric acid in an equal volume to obtain a mixed rare earth chloride solution, and performing conventional concentration and crystallization on the mixed rare earth chloride solution to obtain a mixed rare earth chloride product;
the extractant is obtained by stirring and mixing a solvent, a dispersant, calcium oxide and pure water at normal temperature according to the mass ratio of 1:1.5:0.02: 10; the solvent is any one or mixture of P507 and P204; the dispersant is kerosene.
2. The method for applying the heavy saponification wastewater in rare earth in-situ leaching according to claim 1, wherein: the stirring speed in the step (1) is 600-800 r/min.
3. The method for applying the heavy saponification wastewater in rare earth in-situ leaching according to claim 1, wherein: the mass concentration of the sodium bicarbonate solution in the step (3) is 20-25%.
4. The method for applying the heavy saponification wastewater in rare earth in-situ leaching according to claim 1, wherein: the stirring speed in the step (4) is 500-600 r/min.
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Effective date of registration: 20230511 Address after: No. 21 Honghua Street, Honghua Town, Zhongshan County, Hezhou City, Guangxi Zhuang Autonomous Region, 542600 Patentee after: Hezhou Rare Earth Mining Co.,Ltd. Address before: Floor 16, building 3, Xingning Pioneer Park, 31 Songbai Road, Xingning District, Nanning City, Guangxi Zhuang Autonomous Region, 530012 Patentee before: CHINALCO GUANGXI NONFERROUS RARE EARTH DEVELOPMENT CO.,LTD. |