2022. Т. 26. № 2. С.

348–356 ISSN 2782-4004 (print)

2022;26(2):348-356 ISSN 2782-6341 (online)

METALLURGY

Original article
https://doi.org/10.21285/1814-3520-2022-2-348-356

Physicochemical parameters of a hydrochemical

technology employing sodium chloride to obtain
cryolite used in aluminium production

Khaydar Safiev1 , Nosir A. Naimov2, Jura R. Ruziev3, Ibrokhim Sh. Akhmadshoev4,

A’zamjon M. Juraqulov5, Asror Murodiyon6, Nina V. Nemchinova7
1,2,4,5,6
Scientific Research Institute of Metallurgy JSC TAlCo, Dushanbe, Tajikistan
3
Tajik National University, Dushanbe, Tajikistan
7
Irkutsk National Research Technical University, Irkutsk, Russia
1
inmet.talco@mail.ru
2
nosser2016@outlook.com, https://orcid.org/0000-0003-0405-1537
3
gyra71@mail.ru
4
ibrohim.ahmadshoev@mail.ru, https://orcid.org/0000-0003-4623-8287
5
naza1995naz@gmail.com
6
inmet.talco@mail.ru
7
ninavn@yandex.ru, https://orcid.org/0000-0001-9895-1709

Abstract. The paper aims to study the physicochemical parameters of a hydrochemical technology employing hydro-
fluoric acid and local mineral resources (sodium chloride) to obtain cryolite used in the electrolysis of cryolite-alumina
melts. In order to determine the elemental chemical and phase compositions of initial, intermediate, and final products,
titration and X-ray diffraction analysis (using an upgraded Dron-2 unit) were employed. The conducted studies indicate
that the proposed process of cryolite production from hydrofluoric acid at 28–30% concentration using aluminium hydrox-
ide and a concentrated sodium chloride solution occurs at 25°С for 10–15 min. The yield of cryolite reaches 87.6%, while
~12% of cryolite remains dissolved in the hydrochloric acid solution. With the temperature rising from 25°С to 95°С, the
cryolite yield is shown to decrease from 87.6% to 69.3% due to its higher solubility in the formed hydrochloric acid. The
cryolite production process was validated via X-ray diffraction analysis. The analysed sample was found to be consistent
with the cryolite reference, i.e., indicating an interaction between sodium chloride and fluoroaluminic acid. The conducted
studies served as a basis for developing a process flow diagram of hydrochemical cryolite production using hydrofluoric
acid, aluminium hydroxide, and sodium chloride. The conducted studies revealed that the technology of cryolite produc-
tion employing sodium chloride is easy to implement and cost-effective due to the use of local mineral resources and low
energy consumption.
Keywords: aluminum production, cryolite, aluminum hydroxide, sodium chloride, electrolyte, hydrofluoric acid
For citation: Safiev Kh., Naimov N. A., Ruziev J. R., Akhmadshoev I. Sh., Juraqulov A. M., Murodiyon A., Nemchi-
nova N. V. Physico-chemical aspects of the technology for obtaining the cryolite used for the production of aluminum by
a hydrochemical method using common salt. iPolytech Journal. 2022;26(2):348-356. https://doi.org/10.21285/1814-3520-
2022-2-348-356.

© Safiev Kh., Naimov N. A., Ruziev J. R., Akhmadshoev I. Sh., Juraqulov A. M., Murodiyon A., Nemchinova N. V., 2022
348 https://ipolytech.ru
Safiev Kh., Naimov N. A., Ruziev J. R. et al. Physico-chemical aspects of the technology for obtaining the cryolite …
Сафиев Х., Наимов Н. А., Рузиев Дж. Р и др.Физико-химические аспекты технологии получения криолита…

МЕТАЛЛУРГИЯ

Научная статья
УДК 66.012.2:66.012.3

Физико-химические аспекты технологии получения криолита,

используемого для производства алюминия, гидрохимическим
способом с использованием поваренной соли
Хайдар Сафиев1 , Носир Абдурахмонович Наимов2, Джура Рахимназарович Рузиев3,
Иброхим Шарифович Ахмадшоев4, Аъзамджон Мусурмонкулович Джуракулов5,
Асрор Муродиѐн6, Нина Владимировна Немчинова7
1,2,4,5,6
Научно-исследовательский институт металлургии ОАО «ТАлКо»,
г. Душанбе, Республика Таджикистан
3
Таджикский национальный университет, г. Душанбе, Республика Таджикистан
7
Иркутский национальный исследовательский технический университет,
г. Иркутск, Россия
1
inmet.talco@mail.ru
2
nosser2016@outlook.com, https://orcid.org/0000-0003-0405-1537
3
gyra71@mail.ru
4
ibrohim.ahmadshoev@mail.ru, https://orcid.org/0000-0003-4623-8287
5
naza1995naz@gmail.com
6
inmet.talco@mail.ru
7
ninavn@yandex.ru, https://orcid.org/0000-0001-9895-1709

Резюме. Цель – изучение физико-химических параметров технологии производства криолита, используемого

при электролизе криолит-глиноземных расплавов, гидрохимическим способом с применением производимой
плавиковой кислоты и местного минерального сырья – хлорида натрия. Употреблены титриметрический и рент-
геноструктурный (с использованием модернизированной установки Дрон-2) методы анализа с целью определе-
ния химического элементного и фазового составов исходного, промежуточного и конечного продуктов. Пров е-
денные исследования показали, что процесс получения криолита предлагаемым способом из плавиковой кисло-
ты 28–30% концентрации с использованием гидроксида алюминия и концентрированного раствора хлорида
натрия протекает при температуре 25°C в течение 10–15 мин. При этом выход криолита достигает 87,6%, а ~
12% криолита остается в растворе соляной кислоты в растворенном виде. Показано, что с повышением темпер а-
туры в интервале от 25°С до 95°С наблюдается снижение выхода криолита с 87,6% до 69,3%, связанное с пов ы-
шением его растворимости в образующейся соляной кислоте. Достоверность протекания процесса получения
криолита с применением поваренной соли подтверждена результатами рентгенофазового анализа. Установлено,
что анализируемая проба соответствует эталону криолита, свидетельствуя о взаимодействии хлорида натрия и
фторалюминиевой кислоты. На основе проведенных исследований была разработана принципиальная технол о-
гическая схема производства криолита гидрохимическим способом с применением плавиковой кислоты, гидро к-
сида алюминия и поваренной соли. В результате проведенных исследований установлено, что технология полу-
чения криолита с применением поваренной соли проста в осуществлении и экономически эффективна за счет
использования местного минерального сырья и малой энергозатратности производства.
Ключевые слова: производство алюминия, криолит, гидроксид алюминия, хлорид натрия, электролит, пла-
виковая кислота
Для цитирования: Сафиев Х., Наимов Н. А., Рузиев Дж. Р., Ахмадшоев И. Ш., Джуракулов А. М., Муродиѐн А.,
Немчинова Н. В. Физико-химические аспекты технологии получения криолита, используемого для производства
алюминия, гидрохимическим способом с использованием поваренной соли // iPolytech Journal. 2022. Т. 26. № 2.
С. 348–356 (In Eng.). https://doi.org/10.21285/1814-3520-2022-2-348-356.

INTRODUCTION nearly 70 million tonnes of aluminium. For over

Aluminium is one of the world’s most in- 120 years, it has been produced using the Hall–
demand metals. Due to its low density and high Héroult process8
strength, aluminium is widely used in construc- [1–12].
tion, as well as in the manufacture of car parts, The electrolyte in electrolyzers used for alu-
aircraft, etc., which results in an annual output of minium production performs several essential
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2022;26(2):348-356 ISSN 2782-6341 (online)

functions such as charge transfer, dissolution, duced during the sulphatisation of fluorite. Thus,
and mass transfer of electrode products. The the hydrochemical production of cryolite using
proper performance of these functions depends hydrofluoric acid at 30% and sodium chloride
solely on physicochemical properties, namely was studied.
electrical conductance, viscosity, vapour pres- Under laboratory conditions, parameters for
sure, solidus and liquidus temperatures, density, processing hydrofluoric acid at 28–30% concen-
surface tension, the solubility and dissolution tration using aluminium hydroxide to produce
rate of aluminium oxide, carbon oxide, and vari- fluoroaluminic acid were determined as per the
ous compounds, as well as the following operat- following equation:
ing parameters: temperature, current density,
anode-cathode distance, etc. The electrolyte 6HF + Al(OH)3 = H3AlF6 + 3H2O. (1)
affects the current output and cell voltage, which
determine the specific energy consumption and The resulting fluoroaluminic acid was treated
the overall cost of aluminium [13–20]. with sodium chloride to produce cryolite
Fluoride salts – cryolite and aluminium fluo- according to the reaction equation:
ride – constitute essential electrolyte compo-
nents. Since natural cryolite is rare, it is pro- H3AlF6 + 3NaCl = Na3AlF6 + 3HCl. (2)
duced synthetically from fluorite to meet the
needs of the aluminium industry [21–25]. The main parameters in the production of
fluoroaluminic acid include temperature and
SUBJECT MATTER OF THE STUDY process duration.
In Tajikistan, hydrofluoric acid is currently The temperature dependence of the fluoro-
produced from local minerals (fluorspar) by aluminic acid yield was investigated within a
TALCO Chemical, which is used to obtain cryo- temperature range of 25°С to 95°С at a constant
lite employing imported aluminium and sodium process duration of 10 min. Within this
hydroxides [26]. temperature range, a yield reduction from 97.5%
At this plant, along with concentrated hydro- to 74.8% was observed (fig. 1 a).
fluoric acid, acid at 30% concentration is pro-

a b

Fig. 1. Dependence of the fluoroaluminic acid yield on temperature (a) and process duration (b)
Рис. 1. Зависимость выхода фторалюминиевой кислоты от температуры (а) и продолжительности процесса (b)
It can be seen in fig. 1 a that the yield of fluoroaluminic acid decreases at higher process
___________________________________
8
Zelberg B. I., Ragozin L. V., Barantsev A. G., Yasevich O. I., Grigoriev V. G., Baranov A. N. Metallurgist's Handbook.
Production of aluminum and alloys based on it. St. Petersburg: MANEB; 2013, 143 p. / Зельберг Б. И., Рагозин Л. В.,
Баранцев А. Г., Ясевич О. И., Григорьев В. Г., Баранов А. Н. Справочник металлурга. Производство алюминия и
сплавов на его основе. СПб.: МАНЭБ, 2013. 143 c.

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Safiev Kh., Naimov N. A., Ruziev J. R. et al. Physico-chemical aspects of the technology for obtaining the cryolite …
Сафиев Х., Наимов Н. А., Рузиев Дж. Р и др.Физико-химические аспекты технологии получения криолита…

temperatures, which can be attributed to the yield was also studied (fig. 2 a) at a constant
partial evaporation of hydrofluoric acid. process duration of 10 min. Here, with a tem-
Hydrofluoric acid starts to evaporate from the perature increase from 25°С to 95°С, a reduc-
solution at 50–60°С, with the process tion in the cryolite yield from 87.6% to 69.3% is
intensifying at temperatures above 95℃. observed.
Fig. 1 b shows the dependence between the With rising temperature (see fig. 2 a), the
yield of fluoroaluminic acid and the process yield of cryolite decreases due to its higher sol-
duration. With the process duration varying from ubility in hydrochloric acid formed in (2).
5 to 45 min, a decrease in the yield of fluoro- The dependence of the cryolite yield on pro-
aluminic acid from 97.3% to 69.5% is observed. cess duration was also examined. With the in-
The exothermic reaction between aluminium teraction time of reactants increasing from 10 to
hydroxide and hydrofluoric acid exhibits a 50 min, a reduction in the cryolite yield from
reduction in the yield of fluoroaluminic acid as 87.6% to 82.1% is observed (see fig. 2 b). At a
the temperature reaches 60°С or higher due to longer process duration, a slight decrease in the
the evaporation of hydrofluoric and cryolite yield is clearly also attributable to the
fluoroaluminic acids. dissolution of cryolite in the hydrochloric acid.
Thus, the rational parameters of Thus, the following rational parameters for
fluoroaluminic acid production via the interaction hydrochemical cryolite production from hydroflu-
of hydrofluoric acid and aluminium hydroxide are oric acid using aluminium hydroxide and sodium
as follows: initial temperature of 25–40°С; chloride are determined: temperature – 25°С;
duration of 10–15 min. duration – 10–15 min; concentration of sodium
Experiments were carried out to produce chloride solution – 25%. Under these conditions,
cryolite through the interaction of a fluoroalu- the yield of cryolite reaches 87.6%, while ~12%
minic acid solution with a 25% sodium chloride of cryolite remains dissolved in hydrochloric acid.
solution in a stoichiometric ratio according to (2). Of note is that the used hydrofluoric acid so-
The interaction of fluoroaluminic acid with so- lution contains up to 1.5% of hexafluorosilicic
dium chloride produces hydrochloric acid, whose acid that reacts with the aluminium hydroxide to
concentration amounts to 10–12%. produce silica gel and an aluminium fluoride so-
Of note is that hydrochloric acid comprises lution. Following the separation of silica gel via
from 10% to 27% of produced cryolite in dis- filtration, the aluminium fluoride remains in the
solved state. solution.
The temperature dependence of cryolite

a b

Fig. 2. Dependence of the cryolite yield on temperature (a) and process duration (b)
Рис. 2. Зависимость выхода криолита от температуры (а) и продолжительности процесса (b)

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Fig. 3. XRD pattern of synthetic cryolite obtained using sodium chloride

(upper graph – analysed sample; lower reference graph – cryolite)
Рис. 3. Рентгенограмма синтетического криолита, полученного с использованием хлорида натрия
(верхний график – анализируемая проба, нижний эталонный график – криолит)

Fig. 4. Process flow diagram for the production of cryolite using sodium chloride
Рис. 4. Принципиальная технологическая схема получения криолита с использованием хлорида натрия

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Safiev Kh., Naimov N. A., Ruziev J. R. et al. Physico-chemical aspects of the technology for obtaining the cryolite …
Сафиев Х., Наимов Н. А., Рузиев Дж. Р и др.Физико-химические аспекты технологии получения криолита…

In order to validate the cryolite production chloride solution is prepared followed by the de-
process that employs sodium chloride, an X-ray composition of fluoroaluminic acid at room tem-
diffraction (XRD) analysis was performed using perature for 15–20 min. The resulting slurry is
an upgraded Dron-2 unit (fig. 3). separated via filtration, while the solids are
The obtained XRD pattern shows that the dried.
analysed sample (upper graph) is consistent The liquid part comprising 10–12% HCl and
with the reference sample (lower graph), which 12% Na3AlF6 in dissolved form can be directly
confirms the interaction between sodium chlo- applied as an acidic composition to treat the bot-
ride and fluoroaluminic acid resulting in the for- tom-hole zone of hot water reservoirs. Cryolite
mation of cryolite. used in the electrolytic production of aluminium
Thus, the conducted studies served as a ba- is obtained by evaporating the solution, while
sis for developing a process flow diagram of hy- acid vapours condense or are absorbed by wa-
drochemical cryolite production using hydrofluor- ter to produce commercial hydrochloric acid.
ic acid, aluminium hydroxide, and sodium chlo-
ride (fig. 4). CONCLUSION
According to the provided process flow dia- The conducted studies revealed that the
gram, the first step involves the decomposition technology of cryolite production using sodium
of aluminium hydroxide with hydrofluoric acid to chloride is easy to implement and cost-effective
obtain fluoroaluminic acid; the process occurs at due to the use of local mineral resources and
25–30°С for 10–15 min. Then, a 25% sodium low energy consumption.

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INFORMATION ABOUT THE AUTHORS ИНФОРМАЦИЯ ОБ АВТОРАХ

Khaydar Safiev, Сафиев Хайдар,

Dr. Sci. (Chem.), Professor, доктор химических наук, профессор,
Academician of the National Academy of Sciences академик Национальной Академии наук
of Tajikistan, Таджикистана,
Director, директор,
Scientific Research Institute of Metallurgy Научно-исследовательский институт металлургии
JSC TAlСo, ОАО «ТАлКо»,
17 Kh. Khakimzade St., Dushanbe 734003, Republic of 734003, г. Душанбе, ул. Х. Хакимзаде, 17,
Tajikistan. Республика Таджикистан

Nosir A. Naimov, Наимов Носир Абдурахмонович,

Cand. Sci. (Eng.), кандидат технических наук,
Deputy Director for Research, заместитель директора по научной работе,
Scientific Research Institute of Metallurgy Научно-исследовательский институт металлургии
JSC TAlСo, ОАО «ТАлКо»,
17 Kh. Khakimzade St., Dushanbe 734003, Republic 734003, г. Душанбе, ул. Х. Хакимзаде, 17,
of Tajikistan. Республика Таджикистан

https://ipolytech.ru 355
 2022. Т. 26. № 2. С. 348–356 ISSN 2782-4004 (print)
2022;26(2):348-356 ISSN 2782-6341 (online)

Jura R. Ruziev, Рузиев Джура Рахимназарович,

Dr. Sci. (Eng.), Professor, доктор технических наук, профессор,
Professor of the Department of Applied Chemistry, профессор кафедры прикладной химии,
Tajik National University, Таджикский национальный университет,
17, Rudaki Ave., Dushanbe 734025, Republic 734025, г. Душанбе, пр. Рудаки, 17,
of Tajikistan Республика Таджикистан

Ibrokhim Sh. Akhmadshoev, Ахмадшоев Иброхим Шарифович,

Dr. PhD, доктор PhD,
Acting Head of the Laboratory of исполняющий обязанности заведующего
Environmental Research and Industrial Waste Recycling, Лабораторией
Research Institute of Metallurgy экологических исследований и переработки
JSC TAlСo, промышленных отходов,
17 Kh. Khakimzade St., Dushanbe 734003, Republic of Научно-исследовательский институт металлургии
Tajikistan. ОАО «ТАлКо»,
734003, г. Душанбе, ул. Х. Хакимзаде, 17,
Республика Таджикистан

A’zamjon M. Juraqulov, Джуракулов Аъзамджон Мусурмонкулович,

Process Engineer, инженер-технолог,
Scientific Research Institute of Metallurgy Научно-исследовательский институт металлургии
JSC TAlСo, ОАО «ТАлКо»,
17 Kh. Khakimzade St., Dushanbe 734003, Republic of 734003, г. Душанбе, ул. Х. Хакимзаде, 17,
Tajikistan. Республика Таджикистан

Asror Murodiyon, Муродиѐн Асрор,

Dr. Sci. (Eng.), Associate Professor, доктор технических наук, доцент,
Scientific Research Institute of Metallurgy Научно-исследовательский институт металлургии
JSC TAlСo, ОАО «ТАлКо»,
17 Kh. Khakimzade St., Dushanbe 734003, Republic of 734003, г. Душанбе, ул. Х. Хакимзаде, 17,
Tajikistan. Республика Таджикистан

Nina V. Nemchinova, Немчинова Нина Владимировна,

Dr. Sci. (Eng.), Professor, доктор технических наук, профессор,
Head of the Department of Non-Ferrous Metals заведующая кафедрой металлургии цветных
Metallurgy, металлов,
Irkutsk National Research Technical University, Иркутский национальный исследовательский
83, Lermontov St., Irkutsk 664074, Russia технический университет,
664074, г. Иркутск, ул. Лермонтова, 83, Россия

Contribution of the authors Вклад авторов

Juraqulov A. M., Naimov N. A., Akhmadshoev I. Sh. con- Джуракулов А. М., Наимов Н. А. Ахмадшоев И. Ш. –
ducted the experiments and processed data. Safiev Kh., проведение экспериментов и обработка данных;
Ruziev J. R., Murodiyon A., Nemchinova N. V. were re- Сафиев Х., Рузиев Дж. Р., Муродиѐн А., Немчинова
sponsible for the scientific supervision and research con- Н. В. – научное руководство, концепция исследова-
cept. ний.

Conflict of interests Конфликт интересов

The authors declare that there is no conflict of interests Авторы заявляют об отсутствии конфликта интере-
regarding the publication of this paper. сов.

The final manuscript has been read and approved by all Все авторы прочитали и одобрили окончательный
the co-authors. вариант рукописи.

Information about the article Информация о статье

The article was submitted 03.02.2022; approved after Статья поступила в редакцию 03.02.2022; одобрена
reviewing 07.04.2022; accepted for publication после рецензирования 07.04.2022; принята к публи-
17.06.2022. кации 17.06.2022.

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