CN111180017A - Method for calculating dosage of ionic rare earth mineral leaching agent - Google Patents

Method for calculating dosage of ionic rare earth mineral leaching agent Download PDF

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CN111180017A
CN111180017A CN202010021120.5A CN202010021120A CN111180017A CN 111180017 A CN111180017 A CN 111180017A CN 202010021120 A CN202010021120 A CN 202010021120A CN 111180017 A CN111180017 A CN 111180017A
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秦磊
王观石
李琪
罗嗣海
彭陈亮
胡世丽
余茜
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Abstract

The invention relates to a method for calculating the dosage of an ionic rare earth leaching agent, which is suitable for parameter design of the dosage of the leaching agent during ionic rare earth leaching. The invention integrates the consumption of three forms of ammonium in the ion type rare earth leaching, divides the consumption of the leaching agent into three parts, describes the leaching process by a binary equilibrium desorption model, considers the exchange effect of cations in ore soil, the obligatory adsorption effect of ammonium and the consumption of the leaching agent caused by maintaining the concentration of reaction equilibrium solution, provides a calculation model aiming at the consumption of the ammonium sulfate of the leaching agent under different ore soils and different target leaching rates, and provides a theoretical basis for reasonably determining the dosage of the leaching agent. The usage amount of the mineral leaching agent determined by the invention is scientific and reasonable, and the error of the leaching rate of the rare earth obtained by the invention and the actually obtained rare earth is only within 1.14 percent.

Description

Method for calculating dosage of ionic rare earth mineral leaching agent
Technical Field
The invention relates to a method for calculating the dosage of an ionic rare earth leaching agent, which is suitable for parameter design of the dosage of the leaching agent during ionic rare earth leaching.
Background
Because of its unique physicochemical properties, the ionic rare earth cannot be extracted by traditional reselection, magnetic separation and flotation processes, and needs to be extracted by a chemical leaching method (see "rare earth" 2016,37(3):129-133. in "evaluation on ionic rare earth mining and extraction process development [ J ]"), that is, rare earth is leached by an ion exchange method by an ore leaching agent. The ionic rare earth mining is subjected to three-generation processes of pond leaching, heap leaching and in-situ leaching (see rare earth 2018,39(01):132-141, namely 'ionic adsorption type rare earth mining process and theoretical research status [ J ]'), but the dosage of an ore leaching agent in any process is always the most critical factor for influencing the leaching effect. The use amount of the mineral leaching agent is too small, the cation and the rare earth are insufficiently exchanged, the recovery rate of the rare earth is influenced, and the resource waste is caused; the use amount of the mineral leaching agent is too large, so that production raw materials are wasted, the production cost is increased, more ammonia nitrogen and the like can be remained in the mineral soil, and the surrounding environment of a mining area is polluted. Therefore, the determination of the usage amount of the mineral leaching agent has important significance for the exploitation of the ionic rare earth.
At present, the related documents and patents related to the mining of the ionic rare earth are relatively few, and in the technical specification (promissory draft) of in-situ leaching mining of the ionic rare earth ore, the method proposes that the usage amount of an ore leaching agent is determined according to the volume of ore and the liquid-solid ratio of 0.33:1 and the concentration of ammonium sulfate of 1% -2%, and the specific usage amount is determined according to actual production. Although the dosage range of the mineral leaching agent is given, the actual operation still depends on the experience of workers, and no more specific embodiment is provided; the patent "method for calculating the dosage of ammonium sulfate for in-situ leaching of ionic rare earth" (patent No. 2017103708364) provides a method for calculating the dosage of an ore leaching agent according to the reaction equilibrium principle, but the method only considers the consumption of the ore leaching agent for replacing rare earth and lacks the consumption for replacing other impurity ions, so the method has certain errors. At present, the calculation mode of the amount of the mineral leaching agent required by the exploitation of ionic rare earth with different properties can be accurately reflected is still to be further improved.
In the ionic rare earth mining, research on determining the usage of the mineral leaching agent according to local conditions is less, and the determination of the usage of the mineral leaching agent lacks a theory for guiding practical engineering. Therefore, a scientific and reasonable method for calculating the usage amount of the mineral leaching agent is theoretically established, so that the defects of empiric meaning can be overcome, a reliable basis can be provided for engineering standardization, and the method has important significance for practical production.
Disclosure of Invention
During the extraction of the ionic rare earth, the reaction of ammonium on the surface of the mineral soil can comprise reversible ion exchange reaction and irreversible obligate adsorption reaction, so that a binary equilibrium desorption model (DED) can be used for describing the adsorption and desorption process of ammonium ions on the surface of the ionic rare earth mineral. The expression is shown in formula (1),
Figure BDA0002360785750000021
in formula (1): q is the total adsorption capacity of ammonium ions on the ore soil, and the unit is as follows: t/t; q1stThe unit is the reversible part ammonium ion adsorption capacity: t/t; q2ndThe unit is irreversible partial ammonium ion adsorption quantity: t/t; k1Is the ion exchange partial equilibrium constant; k2Is the irreversible adsorption partial partition coefficient;
Figure BDA0002360785750000022
is the maximum adsorption capacity of the ammonium ion of the irreversible fraction, unit: t/t; f (f is more than or equal to 0 and less than or equal to 1) is the filling degree of the irreversible chamber; c is the ammonium ion concentration at reaction equilibrium, unit: g/L.
The research on the adsorption and desorption process of ammonium ions on the surface of rare earth and cations such as rare earth can be realized by performing indoor adsorption and desorption tests on specific rare earth mine soil and fitting by adopting the formula (1) to obtain a relevant parameter K for describing the exchange of ammonium ions, rare earth and other cations of the mine1、K2N and
Figure BDA0002360785750000023
value, thereby characterizing the process.
The present research① the ① research ① shows ① that ① the ① consumption ① of ① ore ① leaching ① agent ① (① ammonium ① ion ①) ① in ① the ① ion ① type ① rare ① earth ① ore ① leaching ① process ① is ① mainly ① divided ① into ① three ① parts ①, ① namely ①, ① ammonium ① ion ① consumption ① m ① of ① ion ① exchange ① reaction ① between ① the ① ion ① leaching ① agent ① and ① rare ① earth ① cations ①1② the consumption m of the special adsorption ammonium ion generated on the surface of the ore soil2thirdly, the ammonium ion consumption m for maintaining the concentration of the leaching agent3. The total consumption of ammonium ions is thus m ═ m1+m2+m3。
m1Is the sum of the consumption of ammonium ions by each cation in the ore soil, corresponding to Q in the formula (1)1st. In the process of rare earth mining, ammonium and main cations such as rare earth and the like are subjected to ion exchange in the formula (2), and according to the principle of charge conservation, the dosage of ammonium ions consumed when a single cation is completely leached
Figure BDA0002360785750000031
Can be represented by the formula (3). M can be obtained by considering the target leaching rate epsilon of the rare earth and considering that the leaching rates of other cations are approximately equal to the rare earth1The expression (4) of (a),
Figure BDA0002360785750000032
in formula (2): a. theiRepresents the ith cation; x represents a soil solid phase; biIs the charge number of the ith cation.
Figure BDA0002360785750000033
In formula (3): is the amount of ammonium ion consumed by the ith cation in units of: t/t;
Figure BDA0002360785750000034
is the relative molecular mass of the ith cation, in units: g/mol; mNHis the relative molecular mass of ammonium ion, in g/mol,. alpha.iIs the ionic phase grade of the ith cation on the sample, unit: mg/g.
Figure BDA0002360785750000035
In formula (4): m is1Is the sum of the consumption of ammonium ions by each cation in the ore soil, and the unit is as follows: t/t; ε is the leaching rate, in units: % of the total weight of the composition.
m2Consumption of the obligatory adsorbed ammonium ions generated on the surface of the ore soil, corresponding to that in formula (1)
Figure BDA0002360785750000036
Namely, see the formula (5),
Figure BDA0002360785750000037
in formula (5): m is2The consumption of the obligate adsorbed ammonium ions is unit: t/t.
m3the consumption of ammonium ions for maintaining the concentration of the leaching agent can be determined from the ion concentration c at the equilibrium of the reaction in the formula (1), see formula (6), and the liquid-solid volume ratio β in the leaching process, see formula (7)
Figure BDA0002360785750000041
m3＝cβ (7)
In formula (7): m is3the dosage of ammonium ions for maintaining the concentration of the mineral leaching agent is t/t, β is the liquid-solid volume ratio, and m is the unit3/m3。
Therefore, the total consumption of ammonium ions is shown in formula (8), the dosage of the ammonium sulfate serving as the mineral leaching agent is shown in formula (9),
Figure BDA0002360785750000042
in formula (8): m is the total consumption of ammonium ions, unit: t/t.
Figure BDA0002360785750000043
In formula (9):
Figure BDA0002360785750000044
the dosage of the ammonium sulfate of the mineral leaching agent is as follows: t/t;
Figure BDA0002360785750000045
is the relative molecular mass of ammonium sulfate, unit is g/mol, αREOThe unit is the rare earth ion phase grade in the ore soil: mg/g.
The invention aims to provide a method for calculating the dosage of an ionic rare earth leaching agent.
The technical scheme of the invention is as follows: a method for calculating the dosage of an ionic rare earth leaching agent is characterized in that the dosage of ammonium sulfate as a leaching agent is calculated by the formula (9):
Figure BDA0002360785750000046
in formula (9):
Figure BDA0002360785750000051
the dosage of the ammonium sulfate of the mineral leaching agent is as follows: t/t;
Figure BDA0002360785750000052
is the relative molecular mass of ammonium sulfate, unit is g/mol, αREOThe unit is the rare earth ion phase grade in the ore soil: mg/g; mNHRelative molecular mass of ammonium ion, unit: g/mol; m is the total consumption of ammonium ions, unit: t/t.
The total consumption m of ammonium ions was calculated from formula (8):
Figure BDA0002360785750000053
in formula (8): m is the total consumption unit of ammonium ions: t/t; m is1Is the sum of the consumption of ammonium ions by each cation in the ore soil, and the unit is as follows: t/t; m is2The dosage of the obligate adsorption ammonium ion is as follows: t/t; m is3the dosage of ammonium ion for maintaining the concentration of ore-leaching agent is t/t, the extraction rate is epsilon, and alphaiIs the positive of the ith cation in the oreIon grade, unit: permillage; mNHRelative molecular mass of ammonium ion, unit: g/mol;
Figure BDA0002360785750000054
relative molecular mass of the ith cation, unit: g/mol; biThe number of charges carried by the ith cation;
Figure BDA0002360785750000055
t/t is the maximum irreversible adsorption capacity, c is the ammonium ion concentration in the reaction equilibrium and g/L is the unit, β is the liquid-solid volume ratio and m is the unit3/m3。
The invention integrates the consumption of three forms of ammonium ions in ion type rare earth leaching, divides the consumption of the leaching agent into three parts, describes the leaching process by a binary equilibrium desorption model, considers the exchange effect of cations in ore soil, the obligatory adsorption effect of ammonium ions and the consumption of the leaching agent caused by maintaining the concentration of reaction equilibrium solution, provides a calculation model aiming at the consumption of the ammonium sulfate of the leaching agent under different ore soils and different target leaching rates, and provides a theoretical basis for reasonably determining the dosage of the leaching agent. The usage amount of the mineral leaching agent determined by the invention is scientific and reasonable, and the error of the leaching rate of the rare earth obtained by the invention and the actually obtained rare earth is only within 1.14 percent.
Drawings
FIG. 1 is a graph showing the isothermal adsorption of ammonium ions in the ore of the examples.
FIG. 2 is an adsorption curve showing the amount of irreversible ammonium ion adsorption in examples.
Detailed Description
The invention carries out undisclosed experiment in certain rare earth mining area in Gannan, and takes ore samples in different places from the field to mix to prepare the representative ionic rare earth ore sample. And performing an adsorption and desorption test on the ore sample to obtain key parameters, performing a column leaching test by taking the calculated result as a test condition, and verifying the reliability of the calculated result.
The specific implementation steps of the embodiment are as follows:
firstly, testing parameters;
the raw rare earth ore grade is 1.31mg/g, the sodium ion content is 0.080mg/g, the potassium ion content is 0.046mg/g, the aluminum ion content is 0.016mg/g, and the magnesium ion content is 0.035mg/g according to the test of the prior art.
Secondly, performing adsorption test;
twelve parts of ore soil are taken, ammonium sulfate solutions with different concentrations are added according to the solid-liquid mass ratio of 1:5, the ammonium sulfate solutions with the mass concentrations of 0.01%, 0.02%, 0.03%, 0.05%, 0.07%, 0.1%, 0.2%, 0.5%, 1%, 2%, 3% and 4% are added, the mixture reacts for 12 hours at the temperature of 25 ℃, a centrifugal machine is adopted for solid-liquid separation, and the isothermal adsorption curve of ammonium ions in the ore soil is obtained and is shown in figure 1.
Step three, carrying out a step desorption test;
adopting KCl solution with mass concentration of 2% for adsorption solids under different ammonium sulfate concentrations obtained in the second adsorption test, performing a stepwise desorption test according to a solid-liquid mass ratio of 1:5 until ammonium ions can not be desorbed on the solid surface to obtain irreversible adsorption amounts of the ammonium ions adsorbed on the solid surface under different ammonium sulfate concentrations, drawing an adsorption curve of the irreversible adsorption amounts of the ammonium ions as shown in figure 2, and obtaining the maximum irreversible adsorption amount of the ammonium ions
Figure BDA0002360785750000061
It was 0.2894 mg/g.
Fourthly, determining K in the DED model1N and K2；
According to the third step of fractional desorption test to obtain
Figure BDA0002360785750000062
At 0.2894mg/g, f is taken to be 1, and the parameter K is obtained by mathematically fitting the formula (1) based on the isothermal adsorption curve obtained in the adsorption test in the second step1Is 0.2471, n is 0.4053 and K2Is 0.1054.
Figure BDA0002360785750000071
The fifth step: calculating ion exchange consumption m of mineral leaching agent1；
According to the first step of parameter test, the grade of the obtained rare earth raw ore is 1.31mg/g, the sodium ion content is 0.080mg/g, the potassium ion content is 0.046mg/g, the aluminum ion content is 0.016mg/g, the magnesium ion content is 0.035mg/g, and m is obtained from the formula (4) under the set target leaching rate epsilon1＝0.5472εt/t。
Figure BDA0002360785750000072
Sixthly, calculating the specific adsorption consumption m of the mineral leaching agent2；
Obtaining m according to the third step of fractional desorption test result by the formula (5)2＝0.2894t/t，
Figure BDA0002360785750000073
The seventh step, calculating the consumption m of the mineral leaching agent for maintaining the concentration of ammonium ions in the solution3；
the equilibrium concentration c of the leaching agent is calculated by the formula (6) to be (0.5472 epsilon/0.2471) ^ (1/0.4053), and the specific adsorption consumption m of ammonium ions is calculated by the formula (7) to be β to be 0.333＝0.33*(0.5472ε/0.2471)^(1/0.4053)t/t，
Figure BDA0002360785750000074
m3＝cβ (7)
Eighthly, calculating the using amount of the ammonium sulfate serving as the mineral leaching agent;
the consumption of ammonium sulfate obtained by the following formulae (8) and (9) was determined to be 132.14, taking out the relative molecular weight of ammonium sulfate
Figure BDA0002360785750000081
Figure BDA0002360785750000082
Figure BDA0002360785750000083
Figure BDA0002360785750000084
The experimental effect is as follows:
the invention carries out column leaching test on the ore sample in Gannan, calculates the consumption of the ammonium sulfate as the leaching agent through a model under the condition that the target leaching rates of rare earth are respectively 85%, 90% and 95%, carries out ore leaching by adopting an ammonium sulfate solution with the concentration of 2%, and then injects top water, wherein other specific parameters and test results are shown in a table 1. According to the calculation formula, for Jiangxinan this mineral, K10.2471, n is 0.4053, the grade of raw ore is 1.31 per mill, when the rare earth target leaching rate is 85%, 90% and 95%, the consumption of ammonium sulfate is calculated to be 7.9t/t, 8.7t/t and 9.7t/t as the dosage of ammonium sulfate in the column leaching process, and the leaching rate in the actual column leaching is 85.97%, 90.55% and 95.14%. The maximum error between the calculated value and the measured value is 1.14%, which shows that the calculation method of the invention has close actual condition and higher practical value.
Table 1:
Figure BDA0002360785750000085
。

Claims (2)

1. a method for calculating the dosage of an ionic rare earth leaching agent is characterized in that the dosage of ammonium sulfate as the leaching agent is calculated by the formula (9):
Figure FDA0002360785740000011
in formula (9):
Figure FDA0002360785740000012
the dosage of the ammonium sulfate of the mineral leaching agent is as follows: t/t;
Figure FDA0002360785740000013
is the relative molecular mass of ammonium sulfate, unit is g/mol, αREOIs the rare earth ion phase grade in the ore soilBit: mg/g; mNHRelative molecular mass of ammonium ion, unit: g/mol; m is the total consumption of ammonium ions, unit: t/t.
2. The method for calculating the dosage of the ionic rare earth leaching agent according to claim 1, which is characterized in that: the total consumption m of ammonium ions was calculated from formula (8):
Figure FDA0002360785740000014
in formula (8): m is1Is the sum of the consumption of ammonium by each cation in the ore soil, unit: t/t; m is2The unit is the dosage of the obligate adsorption ammonium: t/t; m is3the concentration of the ore leaching agent is maintained, the unit is t/t, the unit is epsilon, the unit is percent of leaching rate, and alphaiIs the cation grade of the ith cation in the ore, unit: permillage; mNHRelative molecular mass of ammonium ion, unit: g/mol;
Figure FDA0002360785740000015
relative molecular mass of the ith cation, unit: g/mol; biThe number of charges carried by the ith cation;
Figure FDA0002360785740000016
t/t is the maximum irreversible adsorption capacity, c is the ammonium ion concentration in the reaction equilibrium and g/L is the unit, β is the liquid-solid volume ratio and m is the unit3/m3。
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CN114323828A (en) * 2021-10-22 2022-04-12 南昌大学 Method for measuring concentration of leaching agent for leaching ion adsorption type rare earth mineral

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