CN114323828A - Method for measuring concentration of leaching agent for leaching ion adsorption type rare earth mineral - Google Patents
Method for measuring concentration of leaching agent for leaching ion adsorption type rare earth mineral Download PDFInfo
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- 238000002386 leaching Methods 0.000 title claims abstract description 192
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 138
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 131
- 229910052500 inorganic mineral Inorganic materials 0.000 title claims abstract description 61
- 239000011707 mineral Substances 0.000 title claims abstract description 61
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 39
- 238000001179 sorption measurement Methods 0.000 title abstract description 53
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- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
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- 229910002651 NO3 Inorganic materials 0.000 description 5
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- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 4
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 4
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 3
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Abstract
The invention relates to a method for measuring the concentration of a leaching agent for leaching ion-adsorption type rare earth minerals, which is characterized by comprising the following steps of: dispersing the primary rare earth mineral sample in an aqueous solution to obtain a solution to be analyzed, wherein the liquid-solid ratio of the solution to be analyzed is preset to be R1(ii) a Adding a leaching agent solution into the solution to be analyzed for several times to carry out trickle leaching on rare earth ions, and analyzing the rare earth concentration of the supernatant of the solution to be analyzed after each trickle leaching; stopping the dripping when the rare earth concentration of the supernatant after the Nth dripping is increased by less than 1 percent compared with the rare earth concentration of the supernatant after the N-1 th dripping, so as to obtain the optimal leaching agent concentration C1 of the leaching agent for the equilibrium leaching of the primary rare earth mineral sample under the liquid-solid ratio, wherein the optimal leaching agent concentration C1 is the concentration of the sum of the leaching agent solutions used from the 1 st time to the Nth time in the solution to be analyzed; calculating to obtain the leaching agent for the primary rare earth mineral sample according to a formulaThe leaching concentration of the mineral is C2 when the mineral is used for non-equilibrium leaching. The method has the advantages of simple steps, short flow and low consumption.
Description
Technical Field
The invention belongs to the technical field of rare earth hydrometallurgy and environmental protection, and relates to a process for selecting an ore leaching agent in an ion adsorption type rare earth leaching process and evaluating the correlation between the ore leaching agent and mineral characteristics and the risk of tailing landslide.
Background
During decades of exploitation of ion-adsorption type rare earth, researchers have conducted a great deal of research on leaching conditions, and the research work of the last 50 years is described in detail in book of ion-adsorption type rare earth resource and green extraction thereof. The selection of mineral characteristics and leaching agents was the most important in all studies. In the research of selecting mineral leaching agents, the most popular method is an on-column leaching method. The method has large workload, large error caused by the heterogeneity of the ore sample, long flow path and high consumption when determining leaching conditions.
Disclosure of Invention
Therefore, in view of the above-mentioned problems, it is an object of the present invention to provide a method for measuring the concentration of a leaching agent for leaching an ion-adsorbing type rare earth mineral, which is short in process and low in consumption.
A method for determining the concentration of a leaching agent for leaching an ion-adsorbing rare earth mineral comprises the following steps:
dispersing the primary rare earth mineral sample in an aqueous solution to obtain a solution to be analyzed, wherein the liquid-solid ratio of the solution to be analyzed is preset to be R1；
Adding a leaching agent solution into the solution to be analyzed for several times to carry out trickle leaching on rare earth ions, and analyzing the rare earth concentration of the supernatant of the solution to be analyzed after each trickle leaching;
stopping the dripping when the rare earth concentration of the supernatant after the Nth dripping is increased by less than 1 percent compared with the rare earth concentration of the supernatant after the N-1 th dripping, so as to obtain the optimal leaching agent concentration C1 of the leaching agent for the equilibrium leaching of the primary rare earth mineral sample under the liquid-solid ratio, wherein the optimal leaching agent concentration C1 is the concentration of the sum of the leaching agent solutions used from the 1 st time to the Nth time in the solution to be analyzed;
calculating the leaching concentration C2 of the leaching agent to the mineral of the primary rare earth mineral sample when the mineral is used for non-equilibrium leaching according to the following formula,
wherein K is a correction coefficient, and the range of K is 0.1-0.6.
Preferably, the particle size of the primary rare earth mineral sample is 200-800 meshes.
Preferably, the liquid-solid ratio R1Is 10-50.
Preferably, the method further comprises the following steps: the rare earth ion leaching was performed on a zeta potential analyzer.
Preferably, the method further comprises the following steps: after dispersing the primary rare earth mineral sample in an aqueous solution, measuring one, two or more of zeta potential, pH value and electric conductivity value of the liquid to be analyzed.
Preferably, after each drip, one, two or more of the zeta potential of the clay mineral particles in the suspension at equilibrium, the pH value and the electrical conductance value of the solution are measured; and filtering the solution to be analyzed after the Nth dripping to obtain a filter cake, re-dispersing the filter cake into water, and measuring one or two or more of zeta potential, pH value and electric conductivity of the suspension.
The invention solves the problems of long flow, much consumption, large error and the like when the leaching condition is determined by the existing on-column leaching mode; in addition, the specific method for reducing the waste water yield and the water and soil loss can be determined simultaneously.
Compared with the traditional column leaching method, the method can realize continuous drop leaching without replacing mineral samples every time, and solves the problems of long flow, high consumption and the like; furthermore, the zeta potential, the pH value and the conductance value during each leaching balance and the zeta potential, the pH value and the pollutant concentration after the tailing particles are dispersed in water after rare earth leaching can be simultaneously measured, the data can be utilized to research the relationship between the rare earth leaching efficiency and the zeta potential, the pH value and the conductance, study the leaching exchange law, preferably leach reagents and the optimal concentration range thereof, and further determine the concentrations of pollutants such as electrolyte, leached rare earth and heavy metal in the solution after each water leaching and the pH value of the solution and the generation amount of wastewater generated when the discharge standard is reached. Because the zeta potential value of the clay mineral particles is related to the suspension dispersibility of the clay mineral particles in water, and the suspension property of the clay mineral is related to the difficulty of water and soil loss of the clay mineral, the tailing wastewater yield and the landslide risk after rare earth leaching of each leaching agent can be evaluated, and a specific method for reducing water and soil loss is provided.
The more times a water wash is required when discharge standards are met, the greater the amount of waste water produced.
When the absolute value of the Zeta potential of the clay mineral after mineral leaching is larger than the absolute value of the Zeta potential of the raw mineral, landslide is likely to occur, and the more the absolute value of the Zeta potential is close to zero, the more stable the Zeta potential is, the more the landslide is unlikely to occur.
Drawings
FIG. 1: the Zeta potential value of the clay mineral after the three mineral samples are leached in a balanced manner and are soaked in water is related to the size of the clay mineral particles.
FIG. 2: six kinds of sulfate are used as electrolyte to continuously titrate Zeta potential of the south ion adsorption type rare earth sample at a certain concentration during each titration balance.
FIG. 3: six kinds of sulfate are used as electrolyte to continuously titrate the pH value of the south ion adsorption type rare earth sample at a certain concentration during each titration balance.
FIG. 4: six kinds of sulfate are used as electrolyte to continuously titrate the conductance value of the south ion adsorption type rare earth sample at a certain concentration during each titration balance.
FIG. 5: six kinds of sulfate are used as electrolyte to continuously titrate the rare earth leaching rate of the south ion adsorption type rare earth sample at a certain concentration during each titration balance.
FIG. 6: six kinds of sulfate are used as electrolyte to continuously drip and soak the Zeta potential of the Longnan ion adsorption type rare earth sample under a certain concentration when the equilibrium is titrated each time.
FIG. 7: six kinds of sulfate are used as electrolyte to continuously drip the pH value of the southernwood ion adsorption type rare earth sample at a certain concentration during each titration balance.
FIG. 8: six kinds of sulfate are used as electrolyte to continuously drip the conductivity value of the Longnan ion adsorption type rare earth sample under a certain concentration when the balance is titrated each time.
FIG. 9: six kinds of sulfate are used as electrolyte to continuously drip and leach the southeast ion adsorption type rare earth ore sample under a certain concentration, and the rare earth leaching rate is obtained when each time of titration balance.
FIG. 10: the seven chlorides are used as electrolytes to continuously titrate the Zeta potential of the south ion adsorption type rare earth sample at a certain concentration during each titration balance.
FIG. 11: the seven chlorides are used as electrolytes to continuously titrate the pH value of the south ion adsorption type rare earth sample at a certain concentration during each titration balance.
FIG. 12: the seven chlorides are used as electrolytes to continuously titrate the conductance value of the south ion adsorption type rare earth sample at a certain concentration during each titration balance.
FIG. 13: the seven chlorides are used as electrolytes to continuously titrate the rare earth leaching rate of the south ion adsorption type rare earth sample at a certain concentration during each titration balance.
FIG. 14: the seven chlorides are used as electrolytes to continuously drip and soak the Zeta potential of the Longnan ion adsorption type rare earth sample under a certain concentration during each titration balance.
FIG. 15: the seven chlorides are used as electrolytes to continuously drip and soak the pH value of the southernwood ion adsorption type rare earth sample at a certain concentration during each titration balance.
FIG. 16: the seven chlorides are used as electrolytes to continuously drip and soak the southeast ion adsorption type rare earth sample under a certain concentration, and the conductance value of the southeast ion adsorption type rare earth sample is obtained during each titration balance.
FIG. 17: the rare earth leaching rate of the southeast ion adsorption type rare earth sample is continuously leached by using seven chlorides as electrolytes under a certain concentration during each titration balance.
FIG. 18: seven nitrates are used as electrolytes to continuously titrate the Zeta potential of the south ion adsorption type rare earth sample at a certain concentration during each titration balance.
FIG. 19: the seven nitrates are used as electrolytes to continuously titrate the pH value of the south ion adsorption type rare earth sample at a certain concentration during each titration balance.
FIG. 20: seven nitrates are used as electrolytes to continuously titrate the conductance value of the south ion adsorption type rare earth sample at a certain concentration during each titration balance.
FIG. 21: the leaching rate of the south ion adsorption type rare earth ore sample is continuously titrated under certain concentration by using seven nitrates as electrolytes at each titration balance.
FIG. 22: seven nitrates are used as electrolytes to continuously dip the Zeta potential of the Longnan ion adsorption type rare earth sample at a certain concentration during each titration balance.
FIG. 23: seven nitrates are used as electrolytes to continuously drip and soak the pH value of the southernwood ion adsorption type rare earth sample at a certain concentration during each titration balance.
FIG. 24: seven nitrates are used as electrolytes to continuously dip the conductivity value of the southernwood ion adsorption type rare earth sample at a certain concentration during each titration balance.
FIG. 25: the leaching rate of the rare earth is obtained by continuously dripping the southeast ion adsorption type rare earth sample as electrolyte at a certain concentration during each titration balance.
FIG. 26: six kinds of sulfate are used as electrolyte to continuously drip and dip the Zeta potential after the south ion adsorption type rare earth sample is soaked in the tailing water under certain concentration.
FIG. 27 is a schematic view showing: six kinds of sulfate are used as electrolyte to continuously drip and dip the conductivity value of the solution after the south ion adsorption type rare earth sample is soaked in the tailing water under certain concentration.
FIG. 28: six kinds of sulfate are used as electrolyte to continuously dip the southernwood ion adsorption type rare earth sample under a certain concentration, and the Zeta potential is obtained after the tailings are soaked in water.
FIG. 29: six kinds of sulfate are used as electrolyte to continuously dip the Longnan ion adsorption type rare earth sample under a certain concentration, and then the conductivity value of the solution is obtained after the tailings are soaked in water.
FIG. 30: seven chlorides are used as electrolytes to continuously drip and dip the Zeta potential after the south ion adsorption type rare earth sample is soaked in the tailing water under certain concentration.
FIG. 31: seven chlorides are used as electrolytes to continuously drip and dip the conductivity value of the south ion adsorption type rare earth sample after tailing water leaching under certain concentration.
FIG. 32: seven chlorides are used as electrolytes to continuously dip the southernwood ion adsorption type rare earth sample under a certain concentration, and the Zeta potential is obtained after the tailings are soaked in water.
FIG. 33: seven chlorides are used as electrolytes to continuously dip the southeast ion adsorption type rare earth sample under a certain concentration, and then the conductivity value of the tailings is obtained after water leaching.
FIG. 34: seven nitrates are used as electrolytes to continuously drip and leach the Zeta potential after the south ion adsorption type rare earth sample is soaked in the tailings water under certain concentration.
FIG. 35: seven nitrates are used as electrolytes to continuously drip and leach the conductivity value of the south ion adsorption type rare earth sample after tailing water leaching under certain concentration.
FIG. 36: seven nitrates are used as electrolytes to continuously dip the southernwood ion adsorption type rare earth sample under a certain concentration, and the Zeta potential is obtained after the tailings are soaked in water.
FIG. 37: seven nitrates are used as electrolytes to continuously dip the Longnan ion adsorption type rare earth sample under a certain concentration, and then the conductivity value of the tailings is obtained after water leaching.
FIG. 38: six inorganic salts are used as electrolytes to determine the concentration of the south ion adsorption type rare earth ore sample, and the liquid-solid ratio is 1: 1 rare earth leaching rate in leaching on the column.
FIG. 39: six inorganic salts are used as electrolytes to adsorb the Longnan ion type rare earth ore sample under a certain concentration according to the liquid-solid ratio of 1: 1 rare earth leaching rate in leaching on the column.
FIG. 40: the method comprises the following steps of taking five inorganic salts as electrolytes, and carrying out liquid-solid ratio 1: leaching rate of rare earth when leaching on the 1 and 2:1 columns.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In addition, the descriptions related to "first", "second", etc. in the present invention are for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.
The method for completely leaching ionic rare earth and measuring the content of the rare earth, which is published in rare metal in 1985, proposes to solve the problem of non-uniformity of an ore sample by ore blending. Although the workload of sample treatment is increased, the repeatability of the determination result is good, the error range is greatly reduced, and the method is applied to determination of the rare earth content in the raw ore. However, in the selection of ore leaching reagents and conditions, most of researches do not adopt an ore blending method, and in addition, the selection of ore leaching conditions has specific requirements on the liquid-solid ratio in ore leaching, and the error caused by the nonuniformity of ore samples is larger. Therefore, there are contradictory reports on the study of the influence of the type of leaching agent and its concentration on leaching efficiency. High and low, or even out of order. It is difficult to determine whether leaching agent or column layer non-uniformity is a problem.
In addition, when the leaching condition is optimized, the leaching rate of the leaching agent to the rare earth is considered, and the safety performance of the tailings is also considered. The safety of the tailings is mainly considered from two aspects of pollutant discharge and soil erosion. In earlier researches, a novel method for researching the correlation between the types and the concentrations of leaching agents and leaching efficiency based on the zeta potential change of a leaching tailing clay mineral is provided. Zeta potential can be used to explain many surface phenomena such as particle accumulation and deposition. By comparing the effects of different leaching agents and the change of the concentration of the leaching agents on the rare earth leaching rate and the zeta potential, the leaching efficiency and the zeta potential are correspondingly changed along with the change of the concentration of a specific agent, and a linear relation exists between the leaching efficiency and the zeta potential. The slope of the straight line is related to the leaching capability of the leaching reagent, so that the leaching capabilities of different leaching reagents on rare earth can be compared and judged, and an evaluation method for leaching efficiency and tailing landslide risk based on Zeta potential measurement is provided. In the experimental method, a leaching experiment, the determination of the rare earth concentration and the zeta potential of the tailings are required to be carried out independently under each concentration condition, so that a series of experiments are required for each reagent, the sample amount and the reagent consumption are large, and due to the uniformity problem of the sample, parallel experiments are required to calculate experiment errors, and the workload is large.
The applicant further investigated the effect of liquid-solid ratio in the suspension on zeta potential during the experiment and the results of the determination of the leached rare earths. The liquid-solid ratio is reduced, the absolute value of the zeta potential can be improved, and the experimental error is reduced. Meanwhile, the amount of the leached rare earth is increased, and the error of the rare earth concentration measurement is favorably reduced. Therefore, after each leaching, the whole leaching solution or most of the leaching solution is not required to be used for measuring the concentration of the rare earth, and only a small amount of the solution is required to be taken to complete the measurement of the concentration of the rare earth. Accordingly, a continuous drop leaching method for determining leaching characteristics of ion-adsorption type rare earth and optimizing leaching conditions is proposed. For each reagent, only one continuous titration leaching experiment is needed to determine the relationship between the concentration of the leached rare earth and the concentration of the leaching agent. Meanwhile, the zeta potential of the clay mineral, the pH value and the conductivity of the solution are measured, and the main characteristic parameters of the leaching process can be measured. The magnitude and order of leaching capacity of each leaching agent can be determined by comparing the results of the leaching experiments with different leaching agents. Provides direct basis for selecting leaching reagent and concentration condition.
The application provides a method for measuring the concentration of a leaching agent for leaching ion-adsorption type rare earth minerals, which comprises the following steps:
dispersing the primary rare earth mineral sample in an aqueous solution to obtain a solution to be analyzed, wherein the liquid-solid ratio of the solution to be analyzed is preset to be R1；
Adding a leaching agent solution into the solution to be analyzed for several times to carry out trickle leaching on rare earth ions, and analyzing the rare earth concentration of the supernatant of the solution to be analyzed after each trickle leaching;
stopping the dripping when the rare earth concentration of the supernatant after the Nth dripping is increased by less than 1 percent compared with the rare earth concentration of the supernatant after the N-1 th dripping, so as to obtain the optimal leaching agent concentration C1 of the leaching agent for the equilibrium leaching of the primary rare earth mineral sample under the liquid-solid ratio, wherein the optimal leaching agent concentration C1 is the concentration of the sum of the leaching agent solutions used from the 1 st time to the Nth time in the solution to be analyzed;
calculating the leaching concentration C2 of the leaching agent to the mineral of the primary rare earth mineral sample when the mineral is used for non-equilibrium leaching according to the following formula,
wherein K is a correction coefficient, and the range of K is 0.1-0.6.
Preferably, the particle size of the primary rare earth mineral sample is 200-800 meshes.
Preferably, the liquid-solid ratio R1Is 10-50.
Preferably, the method further comprises the following steps: the rare earth ion leaching was performed on a zeta potential analyzer.
Preferably, the method further comprises the following steps: after dispersing the primary rare earth mineral sample in an aqueous solution, measuring one, two or more of zeta potential, pH value and electric conductivity value of the liquid to be analyzed.
Preferably, after each drip, one, two or more of the zeta potential of the clay mineral particles in the suspension at equilibrium, the pH value and the electrical conductance value of the solution are measured; and filtering the solution to be analyzed after the Nth dripping to obtain a filter cake, re-dispersing the filter cake into water, and measuring one or two or more of zeta potential, pH value and electric conductivity of the suspension.
The invention solves the problems of long flow, much consumption, large error and the like when the leaching condition is determined by the existing on-column leaching mode; in addition, the specific method for reducing the waste water yield and the water and soil loss can be determined simultaneously.
Compared with the traditional column leaching method, the method can realize continuous drop leaching without replacing mineral samples every time, and solves the problems of long flow, high consumption and the like; furthermore, the zeta potential, the pH value and the conductance value during each leaching balance and the zeta potential, the pH value and the pollutant concentration after the tailing particles are dispersed in water after rare earth leaching can be simultaneously measured, the data can be utilized to research the relationship between the rare earth leaching efficiency and the zeta potential, the pH value and the conductance, study the leaching exchange law, preferably leach reagents and the optimal concentration range thereof, and further determine the concentrations of pollutants such as electrolyte, leached rare earth and heavy metal in the solution after each water leaching and the pH value of the solution and the generation amount of wastewater generated when the discharge standard is reached. Because the zeta potential value of the clay mineral particles is related to the suspension dispersibility of the clay mineral particles in water, and the suspension property of the clay mineral is related to the difficulty of water and soil loss of the clay mineral, the tailing wastewater yield and the landslide risk after rare earth leaching of each leaching agent can be evaluated, and a specific method for reducing water and soil loss is provided.
The more times a water wash is required when discharge standards are met, the greater the amount of waste water produced.
When the absolute value of the Zeta potential of the clay mineral after mineral leaching is larger than the absolute value of the Zeta potential of the raw mineral, landslide is likely to occur, and the more the absolute value of the Zeta potential is close to zero, the more stable the Zeta potential is, the more the landslide is unlikely to occur.
The ion adsorption type raw rare earth ore used in the examples is taken from both places of Dingnan and Longnan, samples are prepared from raw ore samples by a wet sieving method, and clay particles larger than 800 meshes are screened out and dried and ground at 80 ℃ for standby.
If no special description is provided, the volume of each electrolyte titration is 2ml except for 4ml of sodium salt, and after the titration is finished once in the continuous dripping and dipping process and the balance is reached, the supernatant of the corresponding titration volume is taken to analyze the content of the rare earth, and the content of the rare earth is determined by adopting an azoarsine III spectrophotometry.
In the experiment, the leaching rate of the maximum rare earth content in each ore sample is 100 percent, the maximum rare earth content in the Minnan ore sample is 2039.38ug/g, and the maximum rare earth content in the Longnan ore sample is 1219.6 ug/g.
Example 1
And (3) continuously dripping and leaching six kinds of sulfate as electrolyte under certain concentration to obtain rare earth leaching rates of the south ion adsorption type rare earth ore sample and the south ion adsorption type rare earth ore sample: dispersing 25 g of a south/south fixing clay ore sample with the particle size of more than 800 meshes in 250ml of aqueous solution, carrying out balanced oscillation in a constant-temperature oscillation tank at the temperature of 25 ℃ for 30 minutes, and then measuring a zeta potential, a pH value and a conductivity value on a zeta potential analyzer; then using a sulfate solution with a certain concentration (0.9 mol/lNa)2SO4、0.6ml/lK2SO4、0.6mol/l(NH4)2SO4、0.6mol/lZnSO4、 0.6mol/lMgSO4、0.05mol/lAl2(SO4)3) Continuously dripping and leaching the rare earth for a plurality of times, measuring the zeta potential, the pH value, the conductance and other characteristic parameters when each dripping and leaching reaches the balance, and taking supernatant with corresponding volume to analyze the concentration of the rare earth; the rare earth leaching rate is calculated and plotted against the electrolyte concentration in the equilibrium solution to determine the optimum leaching agent species and concentration conditions. The experimental results are shown in fig. 2-fig. 10, and the experimental results show that: for the Dingnan and Longnan mineral samples, the mineral leaching effect of aluminum sulfate is the best, the optimal concentration of the aluminum sulfate of the Dingnan mineral sample is 2.8mmol/l, and the optimal concentration of the aluminum sulfate of the Longnan mineral sample is 2.4 mmol/l. The optimum concentrations for the other sulfates were, respectively, denna ore samples: the optimal concentration of ammonium sulfate is 28.8mmol/l, the optimal concentration of potassium sulfate is 33.6mmol/l, the optimal concentration of magnesium sulfate is 48mmol/l, the optimal concentration of zinc sulfate is 52.8mmol/l, and the optimal concentration of sodium sulfate is 158.4 mmol/l. And (3) Longnan mineral sample: the optimal concentration of the ammonium sulfate is 33.6mmol/l, the optimal concentration of the potassium sulfate is 28.8mmol/l, the optimal concentration of the magnesium sulfate is 52.8mmol/l, the optimal concentration of the zinc sulfate is 52.8mmol/l, and the optimal concentration of the sodium sulfate is 158.4 mmol/l.
Example 2
And (3) continuously dripping and leaching the rare earth leaching rates of the south ion adsorption type rare earth ore sample and the Longnan ion adsorption type rare earth sample by using seven chlorides as electrolytes under certain concentration: the electrolyte solutions used were 1.8mol/l NaCl, 1.8mol/l KCl, 1.2mol/lNH4Cl, 0.45mol/l CaCl2, 0.6mol/l ZnCl2, 0.6mol/l MgCl2, 0.1mol/l AlCl3, respectively. The experimental results are shown in fig. 11-18, and the experimental results show that: for the Dingnan and Longnan ore samples, the ore leaching effect of aluminum chloride is the best, the optimal concentration of the aluminum chloride of the Dingnan ore sample is 8.8mmol/l, and the optimal concentration of the aluminum chloride of the Longnan ore sample is 5.6 mmol/l. The optimum concentrations for the other chlorides were, respectively, ding nan ore sample: the optimal concentration of ammonium chloride is 105.6mmol/l, the optimal concentration of potassium chloride is 115.2mmol/l, the optimal concentration of calcium chloride is 43.2mmol/l, the optimal concentration of magnesium chloride is 57.6mmol/l, the optimal concentration of zinc chloride is 57.6mmol/l, and the optimal concentration of sodium chloride is 345.6 mmol/l. And (3) Longnan mineral sample: the optimal concentration of ammonium chloride is 96mmol/l, the optimal concentration of potassium chloride is 100.8mmol/l, the optimal concentration of calcium chloride is 43.2mmol/l, the optimal concentration of magnesium chloride is 57.6mmol/l, the optimal concentration of zinc chloride is 57.6mmol/l, and the optimal concentration of sodium chloride is 345.6 mmol/l.
Example 3
And (3) continuously dripping and leaching the leaching amount and the leaching rate of rare earth of two ion adsorption type rare earth ore samples of south and south as the electrolyte by using seven nitrates at a certain concentration: the electrolyte solutions used are respectively 1.8mol/l NaNO3, 1.8mol/l KNO3, 1.2mol/lNH4NO3, 0.45mol/lCa (NO3)2, 0.6mol/lZn (NO3)2, 0.6mol/lMg (NO3)2 and 0.1mol/lAl (NO3)3, the experimental results are shown in the figure 19-figure 26, and the experimental results show that: for the Dingnan and Longnan ore samples, the ore leaching effect of aluminum nitrate is the best, the optimal concentration of the aluminum nitrate of the Dingnan ore sample is 7.2mmol/l, and the optimal concentration of the aluminum nitrate of the Longnan ore sample is 5.6 mmol/l. The optimum concentrations for the other nitrates were, respectively, denna ore samples: the optimal concentration of ammonium nitrate is 115.2mmol/l, the optimal concentration of potassium nitrate is 115.2mmol/l, the optimal concentration of calcium nitrate is 39.6mmol/l, the optimal concentration of magnesium nitrate is 57.6mmol/l, the optimal concentration of zinc nitrate is 57.6mmol/l, and the optimal concentration of sodium nitrate is 345.6 mmol/l. And (3) Longnan mineral sample: the optimal concentration of ammonium nitrate is 115.2mmol/l, the optimal concentration of potassium nitrate is 115.2mmol/l, the optimal concentration of calcium nitrate is 43.2mmol/l, the optimal concentration of magnesium nitrate is 57.6mmol/l, the optimal concentration of zinc nitrate is 57.6mmol/l, and the optimal concentration of sodium nitrate is 345.6 mmol/l.
Example 4
Comparing the electrolyte concentration and the suspension property of clay particles after the tailings are soaked after the different mineral leaching agents are dripped: after the dripping and soaking are finished, filtering; re-dispersing the filter cake into 250ml of water, measuring the Zeta potential, pH value, conductance and other characteristic parameters after stirring and dispersing, observing the clarification condition, taking a certain volume of supernatant to analyze the concentration of rare earth and electrolyte,
and repeating the steps for 3 times, and evaluating the amount of wastewater generated by leaching the tailings by rainwater after each leaching agent leaches the rare earth and the risk of water and soil loss. The rare earth content in the solution of the tailings after water leaching is less after the different mineral leaching agents are dripped, so the conductivity value measured after stirring and dispersing can reflect the concentration of the electrolyte in the solution after water leaching to a great extent, and the larger the conductivity value is, the larger the electrolyte concentration is; and the suspension property of the clay particles can be reflected to a great extent by measuring the Zeta potential value after stirring and dispersing, and the larger the absolute value of the Zeta potential is, the better the suspension property of the clay particles is, and the larger the risk of water and soil loss is.
The experimental results are shown in fig. 27-38, and the experimental results show that: for ion adsorption type ore samples in both Dingnan and Longnan places, the electrolyte concentrations of tailings after water leaching are similar after different mineral leaching agents are dripped, and the electrolyte concentrations of tailings after water leaching are all as follows: the concentration of the electrolyte in the solution after water leaching is related to the concentration of the dripping electrolyte, and the concentration of the electrolyte in the solution after water leaching is higher when the dripping concentration is higher; the concentration difference of electrolytes in the solution after the first water leaching is large, the concentration difference of each electrolyte in the solution after the second water leaching and the solution after the third water leaching is not large, particularly the concentration of each electrolyte in the solution after the third water leaching is very close, and the difference of the concentration of each electrolyte in the solution after the third water leaching and the conductivity value of the solution is not large. For suspension of clay particles after leaching of tailings after dripping of different leaching agents: the suspension property of clay particles after tailings are soaked in water after electrolytes of different systems of sulfate, chloride and nitrate are soaked is related to the cations of the electrolytes soaked in water, the suspension property of the cations with the same valence state is similar, the suspension property of a Longnan mineral sample in a sulfuric acid system, a chlorination system and a nitric acid system is K, Na, NH4 & gt Mg, Zn and Ca & gt Al, the suspension property of a Dingnan mineral sample in the chlorination system and the nitric acid system is K, Na, NH4 & gt Al & gt Mg, Zn and Ca, and the suspension property of the Dingnan mineral sample in the sulfuric acid system is K, Na, NH4 & gt Mg, Zn and Ca & gt Al.
Example 5
Ammonium sulfate, magnesium sulfate, aluminum sulfate, ammonium chloride, magnesium chloride and aluminum chloride are selected as mineral leaching agents, and the liquid-solid ratio is 1: 1, the longnan and ding-nan ore samples below 20 meshes are taken to carry out an on-column leaching experiment, and the influence of the two ore samples on the leaching efficiency when different concentrations of different leaching agents are used is compared. The experimental results are shown in fig. 39 and fig. 40, and the experimental results show that the ore leaching effect of the aluminum sulfate is the best for the Dingnan and Longnan ore samples, the optimal concentration of the aluminum sulfate of the Dingnan ore sample is 33.3mmol/l, and the optimal concentration of the aluminum sulfate of the Longnan ore sample is 6.6 mmol/l. The optimal concentrations for the other mineral leaching agents were, respectively, given south mine samples: the optimal concentration of magnesium sulfate is 192mmol/l, the optimal concentration of ammonium sulfate is 128mmol/l, the optimal concentration of calcium chloride is 192mmol/l, the optimal concentration of magnesium chloride is 192mmol/l, and the optimal concentration of ammonium chloride is 384 mmol/l. And (3) Longnan mineral sample: the optimal concentration of magnesium sulfate is 160mmol/l, the optimal concentration of ammonium sulfate is 96mmol/l, the optimal concentration of calcium chloride is 192mmol/l, the optimal concentration of magnesium chloride is 128mmol/l, and the optimal concentration of ammonium chloride is 320 mmol/l. The sequence of the leaching and leaching effects on the column is similar to the continuous dripping and leaching effects.
See Table 1 for example to obtain C1Then, C is obtained by calculation according to the formula of the invention2(ii) a In addition, the optimum leaching agent concentration C is experimentally measured by adopting a non-balanced leaching method0. Comparison C2And C0It can be seen that the determination of the lixiviant concentration for leaching the ion-adsorbing rare earth mineral using the method of the present application is reliable.
TABLE 1
The above description is only a preferred embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which can be directly or indirectly applied to other related technical fields without departing from the spirit of the present invention, are included in the scope of the present invention.
Claims (7)
1. A method for determining the concentration of a leaching agent for leaching an ion-adsorbing rare earth mineral, comprising the steps of:
dispersing the primary rare earth mineral sample in an aqueous solution to obtain a solution to be analyzed, wherein the liquid-solid ratio of the solution to be analyzed is preset to be R1；
Adding a leaching agent solution into the solution to be analyzed for several times to carry out trickle leaching on rare earth ions, and analyzing the rare earth concentration of the supernatant of the solution to be analyzed after each trickle leaching;
stopping the dripping when the rare earth concentration of the supernatant after the Nth dripping is increased by less than 1 percent compared with the rare earth concentration of the supernatant after the N-1 th dripping, so as to obtain the optimal leaching agent concentration C1 of the leaching agent for the equilibrium leaching of the primary rare earth mineral sample under the liquid-solid ratio, wherein the optimal leaching agent concentration C1 is the concentration of the sum of the leaching agent solutions used from the 1 st time to the Nth time in the solution to be analyzed;
calculating the leaching concentration C2 of the leaching agent to the mineral of the primary rare earth mineral sample when the mineral is used for non-equilibrium leaching according to the following formula,
wherein K is a correction coefficient, and the range of K is 0.1-0.6.
2. The method according to claim 1, wherein the particle size of the primary rare earth mineral sample is 200-800 mesh.
3. The method of claim 1, wherein the liquid-to-solid ratio R is1Is 10-50.
4. The assay method of claim 1, further comprising: the rare earth ion leaching was performed on a zeta potential analyzer.
5. The assay method of claim 1, further comprising: after dispersing the primary rare earth mineral sample in an aqueous solution, measuring one, two or more of zeta potential, pH value and electric conductivity value of the liquid to be analyzed.
6. The assay method according to claim 1, wherein one, two or more of a zeta potential of the clay mineral particles in the suspension at equilibrium, a pH value and a conductivity value of the solution are measured after each dipping; and filtering the solution to be analyzed after the Nth dripping to obtain a filter cake, re-dispersing the filter cake into water, and measuring one or two or more of zeta potential, pH value and electric conductivity of the suspension.
7. The assay method of claim 1, wherein the primary rare earth mineral sample has a particle size of greater than 800 mesh.
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| CN104573210A (en) * | 2014-12-30 | 2015-04-29 | 南昌大学 | Method for determining permeability and rare earth recovery rate of ion-adsorption-type rare earth deposit |
| CN111180017A (en) * | 2020-01-09 | 2020-05-19 | 江西理工大学 | Method for calculating dosage of ionic rare earth mineral leaching agent |
| CN111926180A (en) * | 2020-08-14 | 2020-11-13 | 南昌大学 | Method for extracting ion adsorption type rare earth |
| CN112964611A (en) * | 2021-02-01 | 2021-06-15 | 攀枝花学院 | Real-time monitoring method for ion type rare earth heap leaching seepage efficiency |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104573210A (en) * | 2014-12-30 | 2015-04-29 | 南昌大学 | Method for determining permeability and rare earth recovery rate of ion-adsorption-type rare earth deposit |
| CN111180017A (en) * | 2020-01-09 | 2020-05-19 | 江西理工大学 | Method for calculating dosage of ionic rare earth mineral leaching agent |
| CN111926180A (en) * | 2020-08-14 | 2020-11-13 | 南昌大学 | Method for extracting ion adsorption type rare earth |
| CN112964611A (en) * | 2021-02-01 | 2021-06-15 | 攀枝花学院 | Real-time monitoring method for ion type rare earth heap leaching seepage efficiency |
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