CN114107706B - Method for purifying and removing impurities from ion type rare earth ore leaching solution - Google Patents
Method for purifying and removing impurities from ion type rare earth ore leaching solution Download PDFInfo
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- CN114107706B CN114107706B CN202111437204.8A CN202111437204A CN114107706B CN 114107706 B CN114107706 B CN 114107706B CN 202111437204 A CN202111437204 A CN 202111437204A CN 114107706 B CN114107706 B CN 114107706B
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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
- C22B59/00—Obtaining rare earth metals
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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Abstract
The invention provides a method for purifying and removing impurities from an ion type rare earth ore leaching solution, which comprises the following steps: and (3) stirring and mixing the ion type rare earth ore leaching solution uniformly, adding cocoyl glucoside as a impurity removing agent to regulate the pH value of the leaching solution, and carrying out solid-liquid separation after the reaction is completed to obtain purified leaching solution and precipitation slag. The purification and impurity removal method can remarkably solve the problems of high impurity ion content, difficult removal, high rare earth loss rate, serious ammonia nitrogen pollution and the like in the rare earth leaching solution, is a novel purification and impurity removal method for the rare earth leaching solution, which is safe and environment-friendly, has low impurity removal cost, high purification efficiency, no ammonia nitrogen pollution and low rare earth loss rate, and is suitable for popularization and application.
Description
Technical Field
The invention belongs to the field of dressing and smelting, and particularly relates to a method for purifying and removing impurities from an ion type rare earth ore leaching solution.
Background
Rare earth is the general name of seventeen metal elements of lanthanide elements and scandium and yttrium in the periodic table, 250 rare earth ores exist in nature, but only more than 10 industrial minerals suitable for the current dressing and smelting conditions exist. Rare earths have special physical and chemical properties. The rare earth ions are not filled with different energy level orbitals, which is favorable for receiving lone electron pairs, and forms hybridization to enable pi electrons to be delocalized, so that the magnetism, the dispersity, the mass transfer and the oxygen storage/release (nitrogen/sulfur) performance of the material are improved, and the rare earth material plays an important role in modern high and new technology industries and industrialization of information, biology, catalysis, energy sources, environmental protection and the like. In particular, the application of rare earth in the field of national defense brings great leap to military science and technology, and the ionic rare earth ore is the most prominent, so that the ionic rare earth ore becomes one of the decisive factors for getting the victory of modern war.
The rare earth elements in the ionic rare earth ore and the impurity elements have similar occurrence characteristics, and are all adsorbed on the surface of the weathered clay mineral or substituted in crystal lattices. In the rare earth leaching process, the leaching agent is subjected to exchange reaction with rare earth ions and Al on the surface of clay minerals 3+ 、Fe 3+ Isoimpurity(s)The ion reaction is carried out, and then the ion reaction enters the rare earth leaching solution, so that the ion content of the ion type rare earth ore leaching impurity is increased, the purity of rare earth products is influenced, the production period of rare earth is seriously influenced, and the consumption of precipitant is increased.
The ion type rare earth ore leaching process in China sequentially uses sodium chloride, ammonium sulfate and magnesium sulfate as leaching agents, and uses oxalic acid, ammonium bicarbonate, ammonia water and the like as precipitants to precipitate, crystallize and separate rare earth ions. The existing production process uses ammonium bicarbonate, ammonia water, sodium sulfide and the like to remove impurity metal ions in the leachate. However, long-term production practice shows that the ammonia nitrogen content in the leachate wastewater is increased due to the large amount of ammonium bicarbonate and ammonia water, the wastewater treatment difficulty is increased, and the ecological environment is seriously deteriorated. Although some scholars research macromolecular organic medicaments such as ion exchange resins, macromolecular colloid substances and modified adsorbents for removing impurity ions, the selectivity is poor, the removing efficiency is low, the medicament dosage is large, the cost is high, and the medicaments only stay in a laboratory research stage and cannot be applied industrially on a large scale.
Disclosure of Invention
Aiming at the problems of low purification and impurity removal efficiency, high cost, serious ammonia nitrogen pollution, high rare earth loss rate and the like of the ion type rare earth ore leaching liquid, the invention aims to provide a novel purification and impurity removal method which is safe, environment-friendly, low in consumption, high in efficiency, free of ammonia nitrogen pollution, high in impurity removal rate and low in rare earth loss rate.
The aim of the invention is achieved by the following technical scheme.
A method for purifying and removing impurities from ion type rare earth ore leaching liquid comprises the steps of adding a liquid phase impurity removing agent cocoyl glucoside for removing impurities.
As a further improvement of the method for purifying and removing impurities from the leaching solution of the ionic rare earth ore, the steps of the purifying and removing impurities process comprise:
(1) Mixing and stirring the ion type rare earth ore leaching solution uniformly;
(2) Adding a liquid phase impurity removing agent cocoyl glucoside into the leaching solution in the step (1), and regulating and controlling the pH value of the leaching solution;
(3) And (3) carrying out solid-liquid separation after impurity removal reaction of the leaching solution to obtain purified leaching solution and precipitation slag.
The invention relates to a method for purifying and removing impurities from an ion type rare earth ore leaching solution, wherein the strength of the leaching solution which is uniformly mixed and stirred is 200-400 r/min.
The invention relates to a method for purifying and removing impurities from an ion type rare earth ore leaching solution, which is characterized in that the concentration of a impurity removing agent cocoyl glucoside in the leaching and impurity removing process is 50-60 percent, and the pH value of the leaching solution is regulated and controlled to be 5.1-5.3.
The method for purifying and removing impurities from the leaching solution of the ionic rare earth ore has the leaching solution impurity removal reaction time of 15-20 min.
The invention overcomes the defects of the prior art, and provides a method for purifying and removing impurities from ion type rare earth ore leaching liquid, which has the following technical characteristics:
(1) Aiming at the problems of low purification and impurity removal efficiency, high cost, serious ammonia nitrogen pollution, high rare earth loss rate and the like of the existing ionic rare earth ore leaching solution, the invention adopts coco glucoside as the impurity removal agent of the rare earth leaching solution for the first time, and solves the problems of difficult impurity removal, low purification efficiency and obvious ammonia nitrogen pollution in the leaching solution. The cocoyl glucoside can stably regulate and control the pH value of the solution, realizes the regulation and removal of impurity ions, ensures the removal efficiency of the impurity ions, effectively solves the problem of serious rare earth loss, avoids the problems of environmental pollution, harmful gas release and the like caused by the use of the existing impurity removing agents such as ammonium bicarbonate, sodium sulfide and the like, and realizes the efficient, green purification and clean production of the ion type rare earth ore leaching solution.
(2) The impurity removing agent cocoyl glucoside used in the invention has strong complexing reaction capability on metal ions, and can be matched with Fe in leaching solution 3+ 、Al 3+ The plasma impurity ions form stable complex, so that the purification and removal of the impurity ions are enhanced; meanwhile, cocoanut glucoside has weak complexing ability with rare earth ions, so that rare earth ion loss can not be caused in the impurity removal process, and the recovery rate of the rare earth ions can be improved.
(3) The impurity removing agent cocoyl glucoside used in the invention is a natural organic matter with a long carbon chain structure, has good foaming performance, can enhance the dispersion force of cocoyl glucoside in the solution, promotes the full action of the impurity removing agent and impurity ions, avoids the loss of rare earth caused by non-selective flocculation in the impurity removing process of the rare earth leaching solution, and greatly improves the impurity removing and separating efficiency of the rare earth.
The invention provides a purifying agent and a purifying and impurity removing method which are not disclosed in the field of ionic rare earth ores and are unique and innovative, and is a novel purifying and impurity removing method which is safe and environment-friendly, low in cost, free of ammonia nitrogen pollution, capable of being degraded naturally, high in impurity removing rate, low in rare earth ion loss rate and free of influence on rare earth products.
Drawings
FIG. 1 is a comparison of experimental results of purification and impurity removal of an ionic rare earth mine leachate, wherein FIG. (a) is an experimental result of impurity removal using coco-based glucoside of the present invention; and the graph (b) is an experimental result of impurity removal of ammonium bicarbonate adopted in industrial production. The comparison experiment results show that: the coco glucoside of the invention has obviously higher impurity removal efficiency, and not only Fe 3+ 、Al 3+ The impurity removal rate is greatly increased, the rare earth loss rate is obviously reduced, and the dosage of the impurity removing agent cocoyl glucoside is lower.
FIG. 2 is a reaction mechanism of coco glucoside, impurity ions and rare earth ions, wherein the graph (a) is a composition distribution diagram of leaching liquid when the pH value is changed, and research results show that: when coco glucoside adjusts the pH value of the leaching solution to 5.2, impurity Al 3+ With Al (OH) 3 The rare earth element is still in an ion form, so that the rare earth loss rate is lower in the purification and impurity removal process; FIG. b shows coco-based glucoside (CG) and Al (OH) respectively 3 、Y 3+ A model diagram of the reaction product, and the research result shows that: cocoyl glucoside and Al (OH) 3 Generating a new firm Al-O bond to react with Y 3+ The Y-O bond is formed, so that the cocoyl glucoside has higher impurity removal efficiency.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
A method for purifying and removing impurities from ion type rare earth ore leaching liquid is characterized in that cocoyl glucoside is added as an impurity removing agent in the purifying and removing process.
The invention relates to a method for purifying and removing impurities from an ion type rare earth ore leaching solution, which comprises the following steps:
(1) Mixing and stirring the ion type rare earth ore leaching solution in a beaker;
(2) Adding a liquid phase impurity removing agent cocoyl glucoside into the leaching solution in the step (1), and regulating and controlling the pH value of the leaching solution;
(3) And (3) carrying out solid-liquid separation after impurity removal reaction of the leaching solution to obtain purified leaching solution and precipitation slag.
The method for purifying and removing impurities from the ion type rare earth ore leaching solution has the strength of 200-400 r/min after uniform mixing and stirring; the concentration of the impurity removing agent cocoyl glucoside is 50-60%, and the pH value of the leaching solution is regulated and controlled to be 5.1-5.3; the impurity removal reaction time of the leaching solution is 15-20 min.
Table 1 shows the pharmaceutical composition and Al (OH) 3 、Y 3+ The related parameters such as the reaction adsorption binding energy and the like show that when the pH value is 5.2, cocoyl glucoside and Al (OH) are proved 3 The adsorption binding energy of (C) is-111.87 KJ/mol, which is far higher than that of Y 3+ The binding energy of the impurity removing agent cocoyl glucoside is-28.76 KJ/mol, so that the impurity removing agent cocoyl glucoside can be subjected to chemical reaction with impurity ions preferentially, and the impurity ion selective removal effect is better.
Table 1: parameter table such as medicament-ion reaction adsorption binding energy
Example 1
The ion type rare earth ore leaching liquid adopted in the impurity removal test is from a rare earth mine of Ganzhou city of Jiangxi province, wherein the total amount of rare earth ions in the leaching liquid is 685.43mg/L, and the impurity Al is 3+ The content is 235.58mg/L, and the impurity Fe 3+ The content is 56.72mg/L. Impurity Al in leaching solution obtained by traditional impurity removal process method 3+ The removal rate is 86.32 percent, fe 3+ The removal rate is 81.28%, and the loss rate of rare earth in the precipitated slag is 8.74%.
The impurity removal process comprises the steps of adding cocoyl glucoside as an impurity remover, wherein the impurity removal step comprises the following steps:
(1) Uniformly mixing and stirring the ion type rare earth ore leaching solution in a beaker, wherein the stirring intensity is 200r/min;
(2) Adding 50% of liquid phase impurity removing agent cocoyl glucoside into the leaching solution in the step (1), and regulating the pH value of the leaching solution to be 5.1;
(3) And (3) carrying out solid-liquid separation after leaching impurity removal reaction for 15min to obtain purified leaching liquid and precipitation slag.
Impurity Al in the leachate obtained in this example 3+ The removal rate is 95.88 percent, fe 3+ The removal rate is 91.75 percent, and the loss rate of rare earth in the precipitated slag is 4.53 percent.
Example 2
The ion type rare earth ore leaching liquid adopted in the impurity removal test is from a rare earth mine of Ganzhou city of Jiangxi province, wherein the total amount of rare earth ions in the leaching liquid is 648.26mg/L, the impurity aluminum ion content is 214.45mg/L, and the impurity iron ion content is 48.66mg/L. Impurity Al in leaching solution obtained by traditional impurity removal process method 3+ The removal rate is 88.53 percent, fe 3+ The removal rate is 84.31%, and the loss rate of rare earth in the precipitated slag is 7.15%.
The impurity removal process comprises the steps of adding cocoyl glucoside as an impurity remover, wherein the impurity removal step comprises the following steps:
(1) Uniformly mixing and stirring the ion type rare earth ore leaching solution in a beaker, wherein the stirring intensity is 300r/min;
(2) Adding 55% of liquid phase impurity removing agent cocoyl glucoside into the leaching solution in the step (1), and regulating the pH value of the leaching solution to be 5.3;
(3) And (3) carrying out solid-liquid separation after leaching impurity removal reaction for 20min to obtain purified leaching liquid and precipitation slag.
Impurity Al in the leachate obtained in this example 3+ The removal rate is 97.58 percent, fe 3+ The removal rate is 92.45 percent, and the loss rate of rare earth in the precipitated slag is 4.33 percent.
Example 3
The ion type rare earth ore leaching liquid adopted in the impurity removal test is from a rare earth mine of Ganzhou city of Jiangxi province, wherein the total amount of rare earth ions in the leaching liquid is 672.48mg/L, the impurity aluminum ion content is 232.76mg/L, and the impurity iron ion content is 52.15mg/L. Impurity Al in leaching solution obtained by traditional impurity removal process method 3+ The removal rate is 85.26 percent, fe 3+ The removal rate is 83.15%, and the loss rate of rare earth in the precipitated slag is 8.27%.
The impurity removal process comprises the steps of adding cocoyl glucoside as an impurity remover, wherein the impurity removal step comprises the following steps:
(1) Uniformly mixing and stirring the ion type rare earth ore leaching solution in a beaker, wherein the stirring intensity is 200r/min;
(2) Adding 60% of liquid phase impurity removing agent cocoyl glucoside into the leaching solution in the step (1), and regulating the pH value of the leaching solution to be 5.2;
(3) And (3) carrying out solid-liquid separation after leaching impurity removal reaction for 20min to obtain purified leaching liquid and precipitation slag.
Impurity Al in the leachate obtained in this example 3+ The removal rate is 96.72 percent, fe 3+ The removal rate is 92.83%, and the loss rate of rare earth in the precipitated slag is 4.16%.
The invention provides a method for purifying and removing impurities from an ion type rare earth ore leaching solution, which comprises the following steps: and (3) stirring and mixing the ion type rare earth ore leaching solution uniformly, adding cocoyl glucoside as a impurity removing agent to regulate the pH value of the leaching solution, and carrying out solid-liquid separation after the reaction is completed to obtain purified leaching solution and precipitation slag. The purification and impurity removal method can remarkably solve the problems of high impurity ion content, difficult removal, high rare earth loss rate, serious ammonia nitrogen pollution and the like in the rare earth leaching solution, is a novel purification and impurity removal method for the rare earth leaching solution, which is safe and environment-friendly, has low impurity removal cost, high purification efficiency, no ammonia nitrogen pollution and low rare earth loss rate, and is suitable for popularization and application.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (2)
1. The method for purifying and removing impurities from the leaching solution of the ionic rare earth ore is characterized by comprising the following steps of:
(1) Mixing and stirring the ion type rare earth ore leaching solution uniformly; the total amount of rare earth ions in the leaching solution is 600-700 mg/L;
(2) Adding a liquid phase impurity removing agent cocoyl glucoside into the leaching solution in the step (1), and regulating and controlling the pH value of the leaching solution to be 5.1-5.3;
(3) And (3) carrying out solid-liquid separation after impurity removal reaction of the leaching solution to obtain purified leaching solution and precipitation slag.
2. The method for purifying and removing impurities from the leaching solution of the ionic rare earth ore according to claim 1, wherein the intensity of uniform mixing and stirring is 200-400 r/min; the concentration of the impurity removing agent cocoyl glucoside is 50-60%; the impurity removal reaction time of the leaching solution is 15-20 min.
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