Method for determining component composition and cryolite ratio of solid samples of potassium-containing electrolyte of aluminium production by xpa method

FIELD: metallurgy.

SUBSTANCE: method involves sampling of an electrolyte from a bath, grinding of the sample and addition of sodium fluoride to the ground sample. Then, the sample is sintered and cryolite ratio and concentration of fluorides in the sample is determined. After sintering is completed, the sample is subject to additional heat treatment till balanced phase composition of Na3AlF6, K2NaAlF6, CaF2, NaF is achieved, and cryolite ratio and concentration of fluorides in the sample is determined by means of an X-ray phase analysis.

EFFECT: improving accuracy of determination of a cryolite ratio.

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The invention relates to electrolytic production of aluminum and can be used in determining the composition of the potassium-containing electrolyte for the regulation of technological parameters of the process.

Control of the electrolyte composition is an important technological procedure in the electrolytic production of aluminum. In operation, the electrolytic bath composition and properties of electrolyte change. In this regard, the electrolyte is about once every three days is analyzed on the basis of what is correction of electrolyte composition of each bath. The number of monitored characteristics of the composition include: cryolite ratio (CR) is the ratio of the total content of sodium fluoride to aluminum fluoride ([NaF]/[AlF3]), the content of KF and, in some cases, CaF2, MgF2. Cryolite ratio is responsible for such important parameters of the electrolyte, temperature of crystallization, the solubility of alumina, conductivity, viscosity and others. The composition produced by the method of quantitative x-ray phase analysis (xrpa) selected from the baths of the crystallized samples of the electrolyte. The required accuracy of the determination is TO Δ=±0,04 units TO.

Phase composition of the solid sample of potassium-containing electrolytes mainly includes phase Na5Al3F14, K2NaAl3F12, K NaAlF6. However, as shown by the XRD, the sample optionally may be present phase, the composition of which is unknown. Ignoring the latter in the analysis skews the result TO determine.

Distortion of the results of the analysis can be eliminated using the method of doping the composition of the analyzed samples. The method consists in the fact that in the analyzed samples is added to a known quantity of another substance with subsequent heat treatment, with the aim of changing the phase composition of the samples and receive samples of known crystalline phases.

Known method of preparing samples of calcium-containing electrolytes for subsequent analysis of the XRF method (Patent RF №2418104, M. CL. C25C 3/06, 3/20, publ. 10.05.2011), namely that the samples of the electrolyte undergo heat treatment in a furnace at temperatures of 480-520°C for 20-40 minutes to improve the diffraction properties secretaryoffice phase before performed quantitative XRF.

This method focuses on the analysis of the potassium-containing electrolyte, since the applied heat treatment does not allow to improve the measuring conditions for the quantitative x-ray fluorescence analysis.

The known method of determination of cryolite ratio of electrolyte aluminum electrolytic cells (USSR Author's certificate No. 548809, M. CL G01N 31/16,C01F 7/54, publ. 28.02.1977), which is that the original sample of the electrolyte containing the additive of magnesium fluoride and lithium, is sintered with sodium fluoride at temperatures of 600-650°C, leached obtained peck and titration of the resulting solution of 0.05 n solution of nitrate of thorium determine the amount of unreacted NaF. Next, is calculated TO the original sample.

Method can not be applied to the analysis of electrolytes containing potassium fluoride, and to determine the composition of samples of the electrolyte.

The known method of determination of cryolite ratio of the electrolyte (Patent RF №2424379, M. CL. SS 3/06, publ. 20.07.2011), which is that the sample of electrolyte containing additives of fluorides of magnesium and calcium, analyzed x-ray fluorescence method and by measuring the intensity of fluorescent radiation by Co, the lines of Na, F, Ca, Mg carried out to determine the concentrations of elements Na, F, Ca, Mg and carry out the determination of cryolite ratio on the concentrations of Na, F, Ca, Mg. For construction of calibration parameters for Na, F, Ca, Mg use industry standard samples of the electrolyte the electrolytic production of aluminum. This method cannot be applied to the analysis of electrolytes containing potassium fluoride, and to determine the concentration of K.

Known publication devoted to the determination of cryolites�th relations in electrolytes rentgenoradiometricheskim method (Kirik S. D., Kulikova N. N., Yakimov I. S., Klyuev, T. I., Baranov I. A., bushunow V. Y., Goloshchapov V. G. non-ferrous metals, 1996, No. 9, pp. 75-77; S. N. Arkhipov, A. A., Glass, G. A. Lutinska, L. N. Maksimova, L. A. Pyankov. Factory laboratory. Diagnostics of materials, 2006, volume 72, No. 9, pp. 34-36). The method consists in determining the crystalline phases of the components in a cooled sample of the electrolyte with subsequent recalculation in accordance with stoichiometry in value TO and content of CaF2and MgF2. The basis for quantitative diffraction analysis of fluoride content on external standard method, which involves calculating the concentrations of the phases on a pre-constructed calibration curves, the total content of calcium fluoride is determined by the fluorescent channel. This method cannot be applied to potassium-containing electrolytes, as in the samples of potassium-containing electrolyte has a phase of unknown composition.

Known methods of analysis of potassium-containing electrolytes ["Method for determining molecular ratio of acidic KF-NaF-AlF3 electrolyte systems Yan, Hengwei; Yang, Jianhong; Li, Wangxing; Chen, Shazi; Bao, Shengchong; Liu, Dan From Faming Zhuanli Shenqing (2012), CN 102507679 A 20120620], which is that the sample to a solid electrolyte is added to the suspension of NaF in 1:2 ratio to the mass of the original sample, followed by sintering the sample at a temperature of 600-700°C for 15-50 min, further leached received �EC and by measuring the conductivity of the solution determine the amount of unreacted NaF. Next, is calculated TO the original sample. This method does not allow to determine the composition of samples of the electrolyte. This method of analysis potassium-containing electrolyte is taken as a prototype.

The objective of the proposed method is to increase the accuracy of determination of CO to a value ±0,04% abs. CO.

The technical result, which directed the present invention is the controlled variation of the phase composition of the sample, based on the doping of the sample and subsequent thermal treatment, to obtain samples with known crystalline phases, which is necessary to determine the composition of the electrolyte with the desired precision.

Said technical result is achieved in that in the method of determining the component composition and cryolite ratio of potassium-containing electrolyte, comprising a sample of electrolyte from the bath, grinding of the sample, add to ground sample of sodium fluoride, the sintering of the sample and the definition of cryolite ratio and the concentration of fluoride in the sample, according to the inventive method after sintering, the sample is subjected to a further heat treatment to achieve the equilibrium phase composition of Na3AlF6, K2NaAlF6, CaF2, NaF, and the definition of cryolite ratio and the concentration of fluoride in the sample perform quantitative�th by x-ray analysis.

Method clarify additional points.

Sodium fluoride is added in a 1:2 ratio to the mass of the sample, and the sintering of the sample is carried out at 650-750°C for 20-40 minutes.

The sample is subjected to a further heat treatment at 420-450°C for 15-30 minutes.

The proposed method differs from the prototype in that in selected from the baths of the crystallized sample is added to a known amount of sodium fluoride. The samples sintered at temperatures of 650-750°C for 20-40 minutes and at 420-450°C for 15-30 minutes.

In solid samples potassium-containing electrolytes have been the following phases: K2NaAl3F12, Na5Al3F14, K2NaAlF6, KCaAl2F9also present phase of unknown composition. As the dopant used was sodium fluoride (NaF) mark "chemically pure". During sintering of the samples with sodium fluoride occur following chemical reaction:

K2NaAl3F12+6NaF→K2NaAlF6+2Na3AlF6,

Na5Al3F14+4NaF→3Na3AlF6,

2KCaAl2F9+10NaF→2CaF2+K2NaAlF6+3Na3AlF6,

and in the presence of magnesium fluoride also

Na2MgAlF7+2NaF→NaMgF3+Na3AlF6.

The final phase composition doped with sodium fluoride sample is represented by two main phases: Na3AlF6, K2NaAlF6 and excess NaF, in the samples containing calcium, the calcium ions are present in the phase of CaF2in samples containing magnesium, the magnesium ions are present in the phase NaMgF3.

The resulting phases are crystalline.

Experiments have shown that for areas with compositions lying in the area of CR≥0,8, rather the introduction of additives, sodium fluoride, equal to half the original weight of the sample. The introduction of a smaller amount of sodium fluoride does not allow to obtain the desired phase composition with the magnitude TO≈3.

The need for additional heat treatment was due to the fact that radiographs doped samples weighing up to 3 g, sintered at temperatures of 650-750°C, have broadened the analytical line, are unsuitable for quantitative XRF analysis. Additional thermal treatment of doped samples at a temperature of 420-450°C allows to obtain a chest x-ray with narrow permitted analytical lines.

The drawing shows the fragments of x-ray patterns of the solid sample of potassium-containing electrolyte source doped and doped with additional thermal processing, where: the lower x-ray - of potassium-containing electrolyte (original); the average x-ray - doped potassium-containing electrolyte, heat treatment at 750°C (wider line); upper roentgenol�Amma - subsequent heat treatment at 450°C (analytical line narrow, with greater intensity).

The original sample is multi-phase, in addition to the basic compounds Na5Al3F14, K2NaAl3F12, K2NaAlF6there are phases, the composition of which is unknown (on the x-ray lines of unknown phases are marked by question marks). The controlled doping and additional heat treatment of the sample changes its phase composition. After this operation, the samples consist only of known crystalline phases (Na3AlF6, K2NaAlF6, CaF2, NaF). Additional heat treatment leads to improved radiographic characteristics of phase - lines become narrow, their intensity increases.

In the course of the research it is established that optimum conditions for sintering the sample of electrolyte with sodium fluoride are the temperatures of 650-750°C and calcination time of 20-40 minutes.

The increase of thermal treatment temperature of 750°C could lead to the departure of compounds NaAlF4, AlF3, KAlF4and changing the composition of the sample. The heat treatment temperature less than 650°C requires too more time to complete the reactions between the phases, are part of the sample, and the fluoride of sodium.

It was established experimentally that 20 minutes, just barely�sharpening for the full course of all reactions between the phases, part of the sample, and sodium fluoride. The increase in the duration of heat treatment for more than 40 minutes is impractical since this time is sufficient for the occurrence of all reactions between the phases, are part of the sample, and sodium fluoride at any degree of mixing.

Subsequent heat treatment of the doped sample at a temperature of 420-450°C leads to improved radiographic characteristics (decrease of the half-width and increase the intensity of the analytical lines). The heat treatment temperature less than 420°C is impractical because it is experimentally established that the improvement of crystallinity is much slower. The heat treatment temperature of over 450°C does not lead to a significant improvement of radiographs.

It was established experimentally that thermal treatment time is less than 15 minutes is not enough to improve the crystallinity of the doped sample. Heat treatment for more than 30 minutes is impractical because of the increased analysis time.

Thus, the doping should be carried out under the following conditions: a suspension of milled sample was stirred with a suspension of sodium fluoride, taken in the ratio 1:2 by weight of the sample. The mixture was placed in a closed crucible in the furnace, heated to a temperature of 650-750°C and kept at it for 20-40 minutes. Next, the doped specimen is placed� in the oven, heated to a temperature of 420-450°C and incubated in it for 15-30 minutes. Then the sample is removed, cooled in air and analyze the phase composition by any method of quantitative x-ray fluorescence analysis with consideration of the amount of sodium fluoride. The use of doping with subsequent heat treatment of the doped sample allows to obtain samples of the equilibrium phase composition and good okristallizovannymi phases, which is a necessary condition for the application of methods for quantitative XRF analysis.

These conclusions were made for samples of electrolytes synthesized in the laboratory, and samples of electrolytes selected from the experimental pots. The mass loss during heat treatment of the samples under these conditions does not exceed 1 wt.%.

Calculation of CO and concentrations of KF and CaF2initial samples potassium - and calcium-containing electrolytes can be made from the quantitative data of XPA-doped samples by the following method:

1) by means of XPA for example, using calibration graphs are determined by the concentration of the phases of the doped sample Cd(Na3AlF6), Cd(K2NaAlF6), Cd(CaF2), Cd(NaF);

2) calculated concentration (wt.%) fluoride doped sample Cd(NaF), Cd(KF), Cd(AlF3), C(CaF2):

3) �assy fluorides m d(NaF), md(KF), md(AlF3), md(CaF2in the doped sample:

m(sample) is the sample mass,

m(EXT.NaF) is the mass added to the sample of sodium fluoride;

4) cryolite ratio (CR) and the concentration of fluoride in the initial sample:

Examples of the method.

As the test materials used were samples of potassium-containing electrolyte with additives of calcium fluoride, selected from the test cells in a conical mold.

Example 1

Samples of the electrolyte, taken in a conical mold from the test cell were carefully crushed and grinded with hitch NaF brand "chemically pure". Weight of sodium fluoride was 2 times less than the mass of the original sample. Further components were placed in a closed platinum crucible in an oven at a temperature of 650-750°C and was kept in her 20-40 min. Initial and final weight was recorded. The mass loss was less than 1 wt.%. Control of the composition of the samples was performed using x-ray fluorescence analysis on estandartes method of "corundum numbers" (diffractometer X pert Pro (PANalytical, the Netherlands)). Arbitrage is the method to control the composition of the samples used x-ray spectral analysis method based on the determination of the elemental with�tava on the relevant calibrations (automated wave x-ray fluorescence spectrometer of the company Shimadzu XRF-1800 (with Rh-anode)).

In table 1, as an example, the phase composition of four samples of potassium-containing electrolytes with additives of calcium fluoride and phase compositions corresponding doped samples. The original samples are multiphase (more than 6 phases), including that they contain phase, the composition of which is unknown, almost all phase contain sodium fluoride and/or aluminum. For the calculation necessary TO determine the content of each phase and to know its chemical composition. In doped samples contain only four of the crystalline phase, and composition of these phases is known.

Table 1
PhaseThe original sampleDoped samples
12341234
Na5Al3F14++++
K2NaAlF6++++++++
K2NaAl3F12++++
AlF3+++
KCaAl2F9++++
KAlF4++
NaCaAlF6+
unknown. phase++++
Na3AlF6++++
CaF2++++
NaF+ +++

Table 2 shows the values of KO (unit CO) samples potassium-containing electrolytes with additives of calcium fluoride obtained by the formula 4 from the composition of the doped samples. Below the accuracy TO determine in the original samples.

Table 2
No.KO, obtained by the formula 4
PCAXPA
10,860,91
21,021,09
30,90,98
41,030,99
50,820,89
61,161,2
71,191,22
81,121,17
91,111,13
101,241,2
111,151,19
121,271,31
131,271,29
141,311,33
1.1,331,38
CP.Val. Δ (XRD-XRF)-0,03
SKO Δ0,03

TO samples, calculated according to the XRD of doped samples as sodium fluoride, is overestimated by 0.03 units relative TO values according TO the PCA, while the RMSE varied from 0.03% TO.

Table 3 shows the concentrations of fluorides of potassium and calcium (wt.%) for samples of potassium-containing electrolytes, obtained by the formula 3 composition of doped samples. Below, the accuracy of determination of fluoride content of potassium and calcium in the original sample.

Table 3No.C (KF)C (CaF2)PCAXPAPCAXPA117,5615,661,101,1216,5016,121,301,3318,0715,143,343,5416,1613,853,463,5517,8917,202,852,969,206,103,883,82716,68 13,664,124,178Of 8.075,59A 4.53Of 3.9897,806,314,524,001011,9611,075,665,7011Of 12.559,955,846,11129,476,414,764,78138,025,395,27Is 5.3314The 7.256,225,485,49158,686,76To 5.05Of 5.32 CP.Val. With (XRD-XRF)2,030,01RMS AC0,930,23

The obtained RMSE reflect the cumulative error of 2 techniques and XRF and XRD.

The method of doping with sodium fluoride solid sample of electrolyte at a temperature of 650-750°C with subsequent heat treatment 420-450°C can be successfully used for analysis of potassium-containing electrolytes.

As can be seen from the above examples, the use of doping samples of the electrolyte with subsequent heat treatment to ensure good okristallizovannymi phases and reproducibility of the phase composition of the analyzed samples, which is necessary for the application of methods of quantitative x-ray fluorescence analysis.

The results of experiments on the doping and subsequent thermal treatment of industrial electrolytes allow to recommend this method in the preparation and analysis of samples with the required accuracy TO determine Δ=±0,04 units TO.

1. Method for determination of component composition and cryolite ratio of potassium-containing electrolyte, comprising a sample of electrolyte from the bath, grinding of the sample, add to ground sample of sodium fluoride, the sintering of the sample and determination of cu�ricovero relations and the concentration of fluoride in the sample, characterized in that after sintering, the sample is subjected to a further heat treatment to achieve the equilibrium phase composition of Na3AlF6, K2NaAlF6, CaF2, NaF, and the definition of cryolite ratio and the concentration of fluoride in the sample perform quantitative x-ray phase analysis.

2. The method of determination according to claim 1, characterized in that adding sodium fluoride in a 1:2 ratio to the mass of the sample, and the sintering of the sample is carried out at 650-750°C for 20-40 minutes.

3. The method of determination according to claim 1, characterized in that the sample is subjected to a further heat treatment at 420-450°C for 15-30 minutes.



 

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1 tbl, 1 ex

FIELD: measuring engineering.

SUBSTANCE: invention refers to X-ray equipment. The method consists in the following: by calculation and before an experiment there is selected an optimal value of θ angle between velocity of fast electrons and direction of quantum escape whereat spectre of slowing-down radiation is concentrated in the region of low frequencies. Also position of maximum of coherent spike is measured experimentally. Additionally, position of this maximum as function of dimension and shape of grain is calculated theoretically. Notably, values of theoretical parametres are chosen to achieve the best concurrence of spectres of calculated and measured spikes.

EFFECT: evaluation of grain dimension in ultra-fine-dispersed medium (nano material).

2 dwg

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