Thermodynamic Modelling of Oxide Conversion Processes for Metals of Life
In the presented work, the environmentally friendly production processes of pure metals via reduction from the respective oxides in the atmosphere of ultra-low oxidation potential (PO₂=10¹⁶—10²⁶ atm) are offered. We propose the formation of such an environment by injection of ethyl alcohol in the re...
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Інститут металофізики ім. Г.В. Курдюмова НАН України
2015
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irk-123456789-1117102017-01-14T03:03:16Z Thermodynamic Modelling of Oxide Conversion Processes for Metals of Life Mikadze, O.I. Bagdavadze, J.I. Dzigrashvili, T.A. Maisuradze, N.I. Дефекты кристаллической решётки In the presented work, the environmentally friendly production processes of pure metals via reduction from the respective oxides in the atmosphere of ultra-low oxidation potential (PO₂=10¹⁶—10²⁶ atm) are offered. We propose the formation of such an environment by injection of ethyl alcohol in the reactor and interaction of its vapour with oxygen. Such conditions promote dissociation of oxides of almost any kind. Using this method, the pure, so-called ‘metals of life’ are obtained: Cu, Fe, Ni, and Co, which are used in medicine as the essential nutrients. In the case of chromium conversion, this process is completed with the synthesis of carbide phases. Production of pure Cr is possible by using the similar methodology with the help of oxygen pump. For identification of the reduced products, an X-ray phase analysis is used. The purity of the converted products is characterized by spectrochemical analysis. The experimental data are in a good conformity with the thermodynamic calculations of optimal temperature ranges of conversion reactions and the ratio of the initial ingredients. У запропонованій роботі розглянуто екологічно безпечні процеси одержання чистих металів шляхом їх відновлення з відповідних оксидів у атмосфері з ультранизьким окиснювальним потенціялом (PO₂=10¹⁶—10²⁶атм.). Ми пропонуємо створення такого середовища інжекцією етилового спирту в замкнений контур реактора внаслідок взаємодії пари спирту з киснем. Такі умови сприяють дисоціяції оксидів майже будь-якого виду. Цією методою одержано так звані «метали життя»: Cu, Fe, Ni и Co, які використовуються в медицині як поживні нутрієнти. У випадку конверсії оксиду хрому процес завершується синтезою карбідних фаз. Одержання чистого Cr можливе застосуванням подібної методології за допомогою кисневої помпи. Ідентифікація продуктів конверсії відбувається рентґенофазовою структурною аналізою, а їхня чистота контролюється спектрохемічною методою. Експериментальні дані добре узгоджуються з термодинамічними обчисленнями оптимальних температур конверсійних реакцій і молярних часток початкових інґредієнтів. В предложенной работе рассмотрены экологически безопасные процессы получения чистых металлов путём их восстановления из соответствующих оксидов в атмосфере с ультранизким окислительным потенциалом (PO₂=10¹⁶—10²⁶ атм.). Мы предлагаем создание такой среды инжекцией этилового спирта в замкнутый контур реактора в результате взаимодействия паров спирта с кислородом. Такие условия способствуют диссоциации оксидов почти любого вида. Этим методом получены так называемые «металлы жизни»: Cu, Fe, Ni и Co, применяемые в медицине как питательные нутриенты. В случае конверсии оксида хрома процесс завершается синтезом карбидных фаз. Получение чистого Cr возможно применением подобной методологии с помощью кислородного насоса. Идентификация продуктов конверсии происходит рентгенофазовым структурным анализом, а их чистота контролируется спектрохимическим методом. Экспериментальные данные находятся в хорошем согласии с термодинамическими вычислениями оптимальных температур конверсионных реакций и молярных долей начальных ингредиентов. 2015 Article Thermodynamic Modelling of Oxide Conversion Processes for Metals of Life / O. I. Mikadze, J. I. Bagdavadze, T. A. Dzigrashvili, N. I. Maisuradze // Металлофизика и новейшие технологии. — 2015. — Т. 37, № 1. — С. 115-120. — Бібліогр.: 5 назв. — англ. 1024-1809 PACS: 61.72.sd, 64.75.Lm, 68.47.Gh, 81.05.Je, 81.65.Mq, 82.30.Lp, 82.80.Ej http://dspace.nbuv.gov.ua/handle/123456789/111710 en Металлофизика и новейшие технологии Інститут металофізики ім. Г.В. Курдюмова НАН України |
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Digital Library of Periodicals of National Academy of Sciences of Ukraine |
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| language |
English |
| topic |
Дефекты кристаллической решётки Дефекты кристаллической решётки |
| spellingShingle |
Дефекты кристаллической решётки Дефекты кристаллической решётки Mikadze, O.I. Bagdavadze, J.I. Dzigrashvili, T.A. Maisuradze, N.I. Thermodynamic Modelling of Oxide Conversion Processes for Metals of Life Металлофизика и новейшие технологии |
| description |
In the presented work, the environmentally friendly production processes of pure metals via reduction from the respective oxides in the atmosphere of ultra-low oxidation potential (PO₂=10¹⁶—10²⁶ atm) are offered. We propose the formation of such an environment by injection of ethyl alcohol in the reactor and interaction of its vapour with oxygen. Such conditions promote dissociation of oxides of almost any kind. Using this method, the pure, so-called ‘metals of life’ are obtained: Cu, Fe, Ni, and Co, which are used in medicine as the essential nutrients. In the case of chromium conversion, this process is completed with the synthesis of carbide phases. Production of pure Cr is possible by using the similar methodology with the help of oxygen pump. For identification of the reduced products, an X-ray phase analysis is used. The purity of the converted products is characterized by spectrochemical analysis. The experimental data are in a good conformity with the thermodynamic calculations of optimal temperature ranges of conversion reactions and the ratio of the initial ingredients. |
| format |
Article |
| author |
Mikadze, O.I. Bagdavadze, J.I. Dzigrashvili, T.A. Maisuradze, N.I. |
| author_facet |
Mikadze, O.I. Bagdavadze, J.I. Dzigrashvili, T.A. Maisuradze, N.I. |
| author_sort |
Mikadze, O.I. |
| title |
Thermodynamic Modelling of Oxide Conversion Processes for Metals of Life |
| title_short |
Thermodynamic Modelling of Oxide Conversion Processes for Metals of Life |
| title_full |
Thermodynamic Modelling of Oxide Conversion Processes for Metals of Life |
| title_fullStr |
Thermodynamic Modelling of Oxide Conversion Processes for Metals of Life |
| title_full_unstemmed |
Thermodynamic Modelling of Oxide Conversion Processes for Metals of Life |
| title_sort |
thermodynamic modelling of oxide conversion processes for metals of life |
| publisher |
Інститут металофізики ім. Г.В. Курдюмова НАН України |
| publishDate |
2015 |
| topic_facet |
Дефекты кристаллической решётки |
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http://dspace.nbuv.gov.ua/handle/123456789/111710 |
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Thermodynamic Modelling of Oxide Conversion Processes for Metals of Life / O. I. Mikadze, J. I. Bagdavadze, T. A. Dzigrashvili, N. I. Maisuradze // Металлофизика и новейшие технологии. — 2015. — Т. 37, № 1. — С. 115-120. — Бібліогр.: 5 назв. — англ. |
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Металлофизика и новейшие технологии |
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115
PACS numbers:61.72.sd, 64.75.Lm,68.47.Gh,81.05.Je,81.65.Mq,82.30.Lp, 82.80.Ej
Thermodynamic Modelling of Oxide Conversion Processes
for Metals of Life
O. I. Mikadze, J. I. Bagdavadze*, T. A. Dzigrashvili,
and N. I. Maisuradze
Georgian Technical University,
77 Kostava Str.,
0175 Tbilisi, Georgia
*Ferdinand Tavadze Institute of Metallurgy and Materials Science,
15 Kazbegi Ave.,
0160 Tbilisi, Georgia
In the presented work, the environmentally friendly production processes of
pure metals via reduction from the respective oxides in the atmosphere of
ultra-low oxidation potential (
2
16
O
10P 26
10 atm) are offered. We propose
the formation of such an environment by injection of ethyl alcohol in the re-
actor and interaction of its vapour with oxygen. Such conditions promote
dissociation of oxides of almost any kind. Using this method, the pure, so-
called ‘metals of life’ are obtained: Cu, Fe, Ni, and Co, which are used in med-
icine as the essential nutrients. In the case of chromium conversion, this pro-
cess is completed with the synthesis of carbide phases. Production of pure Cr
is possible by using the similar methodology with the help of oxygen pump.
For identification of the reduced products, an X-ray phase analysis is used.
The purity of the converted products is characterized by spectrochemical
analysis. The experimental data are in a good conformity with the thermody-
namic calculations of optimal temperature ranges of conversion reactions
and the ratio of the initial ingredients.
У запропонованій роботі розглянуто екологічно безпечні процеси одер-
жання чистих металів шляхом їх відновлення з відповідних оксидів у ат-
мосфері з ультранизьким окиснювальним потенціялом (
2
16
O
10P 26
10
атм.). Ми пропонуємо створення такого середовища інжекцією етилового
спирту в замкнений контур реактора внаслідок взаємодії пари спирту з
киснем. Такі умови сприяють дисоціяції оксидів майже будь-якого виду.
Цією методою одержано так звані «метали життя»: Cu, Fe, Ni и Co, які
використовуються в медицині як поживні нутрієнти. У випадку конверсії
оксиду хрому процес завершується синтезою карбідних фаз. Одержання
чистого Cr можливе застосуванням подібної методології за допомогою ки-
сневої помпи. Ідентифікація продуктів конверсії відбувається рентґено-
Металлофиз. новейшие технол. / Metallofiz. Noveishie Tekhnol.
2015, т. 37, № 1, сс. 115—120
Оттиски доступны непосредственно от издателя
Фотокопирование разрешено только
в соответствии с лицензией
2015 ИМФ (Институт металлофизики
им. Г. В. Курдюмова НАН Украины)
Напечатано в Украине.
116 O. I. MIKADZE, J. I. BAGDAVADZE, T. A. DZIGRASHVILI et al.
фазовою структурною аналізою, а їхня чистота контролюється спектро-
хемічною методою. Експериментальні дані добре узгоджуються з термо-
динамічними обчисленнями оптимальних температур конверсійних реа-
кцій і молярних часток початкових інґредієнтів.
В предложенной работе рассмотрены экологически безопасные процессы
получения чистых металлов путём их восстановления из соответствую-
щих оксидов в атмосфере с ультранизким окислительным потенциалом
(
2
16
O
10P 26
10 атм.). Мы предлагаем создание такой среды инжекцией
этилового спирта в замкнутый контур реактора в результате взаимодей-
ствия паров спирта с кислородом. Такие условия способствуют диссоциа-
ции оксидов почти любого вида. Этим методом получены так называемые
«металлы жизни»: Cu, Fe, Ni и Co, применяемые в медицине как пита-
тельные нутриенты. В случае конверсии оксида хрома процесс заверша-
ется синтезом карбидных фаз. Получение чистого Cr возможно примене-
нием подобной методологии с помощью кислородного насоса. Идентифи-
кация продуктов конверсии происходит рентгенофазовым структурным
анализом, а их чистота контролируется спектрохимическим методом.
Экспериментальные данные находятся в хорошем согласии с термодина-
мическими вычислениями оптимальных температур конверсионных ре-
акций и молярных долей начальных ингредиентов.
Key words: metals of life, oxides, ethyl alcohol, conversion.
(Received June 3, 2014; in final version, August 14, 2014)
1. INTRODUCTION
In contrast to the classical methods of metallurgical and chemical pro-
cessing of ores connected with significant energy consumption and eco-
logical stress, we would like to recommend a different, energy-saving
and environmentally friendly technology affording production of pure
‘metals of life’ adopted in pharmaceutical industry [1]. These biologi-
cally active metals of life take up position side by side in the fourth pe-
riod of the Periodic Table of elements:
24Cr,
25Mn,
26Fe,
27Co,
28Ni,
29Cu,
30Zn. Content of most of them is negligible in the body, but absence of
these elements leads to ailments. As a basis for the offered technology
of pure metals, production from the corresponding oxides is the princi-
pal possibility of creating gas environments with ultra-low partial pres-
sure of oxygen in the closed volume of a reactor [2]. The accessibility
level of rarefaction of oxygen (up to 10
28
atm) is significantly lower
than dissociation tension of the oxides of any considered metals.
2. EXPERIMENTAL
Since the purity of converted products is altered depending on purity
THERMODYNAMIC MODELLING OF OXIDE CONVERSION PROCESSES 117
of initial materials (in our case, oxides), the basic oxide powders of the
analytical purity ( 99.9%) is used. An installation for the creation
and maintenance of partial pressure of oxygen (
2OP ) within the re-
quired range of 10
16—10
26
atm had been designed by the authors and
described recently in [3]. The dynamics of the abrupt decrease of
2OP in
the closed contour is a function of the reactor temperature and practi-
cally is in progress up to the depressurization temperature of the reac-
tor material. The optimal consumption of the ethyl alcohol is 0.2 mg
per 1 litre of a closed atmosphere and its heating to 800C provides fall
of
2OP to 10
22
atm. Increase of operating temperatures up to 1500C
stipulates achievement of fine and deep rarefaction of oxygen,
10
28
atm. In such conditions, dissociation of practically each oxide
becomes possible. At the same time, duration of the exposure process
at fixed temperature does not influence the level of
2OP , and the most
possible rarity is achieved at given instant. X-ray phase analysis of the
converted oxides was performed using the HZG-4 diffractometer for
X-ray powder diffraction analysis. Diffraction patterns are obtained
using the CuK X-rays ( 1.542 Å). The complete thermodynamic
analysis of the reductive processes for these oxides is performed using
the ASTRA-4 software.
3. RESULTS AND DISCUSSION
A computer simulation of thermodynamic processes at general atmos-
pheric pressure in the temperature range 1000—2000 K was performed
in the case of Cr2O3. During the simulation, the mole correlation of the
converted oxides and the reducing gas was chosen based on the follow-
ing reaction:
Cr2O3(cd) 4.5C2H5OH(gas).
Among the probable condensed (cd) components, the following were
considered: H2O, C, Cr, Cr2O3, CrO2, CrO3, Cr3C2, Cr7C3, and Cr23C6. Be-
cause of plenty of gaseous connections of C—H—O system, only some of
them were specified: Cr, CrO2, Cr2O3, CrN, and CrOH. The basic results
of complete thermodynamic analysis are presented in the diagram.
Concerning chromium conversion, it should be noted that we have not
found any information on the complete thermodynamic analysis of
Cr2O3 interaction with the ethyl alcohol.
As well known, chromium possesses such a high chemical sensitivity
to oxygen that it oxidizes at 1000C even in the condition of space
evacuation, where
2
20
O
10 atP [5]. Therefore, high temperature, ul-
tra-low partial pressure of oxygen, and the increased consumption of
the reducing agent are required for conversion of Cr2O3 (see reaction).
Preliminary thermodynamic analysis of alcohol dissociation showed
118 O. I. MIKADZE, J. I. BAGDAVADZE, T. A. DZIGRASHVILI et al.
that below 400 K gaseous methane, water vapour, and condensed car-
bon precipitate, while at 450 K a partial dissociation of the methane
takes place, and the content of the condensed carbon increases and ex-
ceeds that of the condensed carbon available in the system.
Since carbon exists among the possible condensed components, it is
highly probable to suppose that convenient conditions are created for
effective conversion of the oxides to pure metals or their carbide phas-
es. Figure 1 shows the results of the analysis only in the temperature
range 1000—2000 K because dissociation of chromium oxide does not
take place below 1300 K. In the Cr2O3 conversion process above 1350 K,
condensed chromium carbide Cr3C2 occurs, amounts to 30% of the
mass, and remains unchanged up to 2000 K. The abrupt decrease of the
condensed carbon content (from 20% to 0%) indicates at its inten-
sive consumption during the synthesis of Cr3C2 and is optimal for ter-
mination of the process.
In order to check the thermodynamic calculations, some relevant
results on NiO, CoO, CuO, and Fe2O3 conversions are shown in Table 1
as good examples of conversion of oxides of other metals of life [3].
However, the conversion process of chromium oxide completes via syn-
thesis of carbide phases instead of precipitation of metal substrate.
The matter is that in the case of ethyl alcohol injection, the presence of
free carbon in the reaction zone causes the carbidization of conversed
chromium.
As should be noted here, the constructed installation for conversion
of oxides allows creating a gaseous environment in two different ways:
1–using an oxygen pump [2], or 2–via injection of ethyl alcohol in
the closed contour of the reactor [5]. In spite of the nearly, the same
Fig. 1. Temperature dependence of the components concentration in the sys-
tem: 1–Cr2O3, 2–C, 3–Cr3C2, 4–CO, 5–H2O.
THERMODYNAMIC MODELLING OF OXIDE CONVERSION PROCESSES 119
evacuation rate of oxygen in the reactor, the deoxidizing abilities of
these methods are completely different (see Tables 1 and 2). As it is
clear from the Tables, the conversion process accelerates when the at-
mosphere in the reactor is formed via injection of alcohols (Table 1).
However, production of pure chromium is possible, if super-deep evac-
uation is achieved using oxygen pump (Table 2).
Taking into account the results shown in tables and the X-ray data,
the obtained results on the complete thermodynamic analysis of chro-
mium oxide conversion lead to the conclusion that the injection of
ethyl alcohol is an efficient method for the formation of Cu, Ni, Co,
and Fe condensates, while in the case of chromium oxide, the end prod-
uct of conversion is its carbide–Cr3C2, instead of pure metal (see
Fig. 2).
4. SUMMARY
For the first time, it has been carried out a multicomponent thermody-
TABLE 1. Parameters of metal complete reduction from their oxides by alco-
hol injection method.
Temperature,
C
Partial pressure
2O
,P atm
Duration, min
1 5 10 15 20 60
700 10
21 Fe2O3 CoO
800 10
22 NiO CuO
900 10
23 NiO CuO
1000 10
24 NiO CoO
TABLE 2. Parameters of metal complete reduction from their oxides by oxy-
gen pump method.
Temperature,
C
Partial pressure
2O
,P atm
Duration, h
0.5 1.0 1.5 2.5 3.0 5.0 5.5
800 10
20 Cu2O
900 10
21 Fe2O3
1000 10
21 Cu2O
1100 10
21 Fe2O3 NiO NiO
1200 10
22 Fe2O3 CoO
1300 10
26 Cr2O3
1400 10
27 Cr2O3
120 O. I. MIKADZE, J. I. BAGDAVADZE, T. A. DZIGRASHVILI et al.
namic simulation of chromium conversion process using ethyl alcohol.
It is determined that the highest output of conversion products corre-
spond to the temperature range 1350—1600 K. The molar ratio of
chromium and ethyl alcohol is 1:4.5.
During conversion of the active carbide-forming metals oxides, the
synthesis of carbide phases takes place simultaneously with their re-
duction. Production of such pure metal as chromium is possible using
the oxygen pump.
REFERENCES
1. E. Terletsky, Metals, Which Are Always with You (Moscow: Znanie: 1986)
(in Russian).
2. O. Mikadze, L. Rukhadze, and B. Bulia, Georgian Engineering News, 1: 90
(2000) (in Georgian).
3. O. Mikadze, A. Kandelaki, J. Bagdavadze, and L. Rukhadze, Bulletin of the
Georgian National Academy of Sciences, 7, No. 1: 37 (2013).
4. N. Vatolin, G. Moiseyev, and B. Trusov, Thermodynamic Modelling in
High-Temperature Inorganic Systems (Moscow: Metallurgy: 1994)
(in Russian).
5. E. Gulbransen and K. Andrew, J. Electrochem. Soc., 99, No. 10: 402 (1952).
Fig. 2. XRD patterns of samples reduced at 1300C.
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/NLD (Gebruik deze instellingen om Adobe PDF-documenten te maken die zijn geoptimaliseerd voor prepress-afdrukken van hoge kwaliteit. De gemaakte PDF-documenten kunnen worden geopend met Acrobat en Adobe Reader 5.0 en hoger.)
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/ENU (Use these settings to create Adobe PDF documents best suited for high-quality prepress printing. Created PDF documents can be opened with Acrobat and Adobe Reader 5.0 and later.)
>>
/Namespace [
(Adobe)
(Common)
(1.0)
]
/OtherNamespaces [
<<
/AsReaderSpreads false
/CropImagesToFrames true
/ErrorControl /WarnAndContinue
/FlattenerIgnoreSpreadOverrides false
/IncludeGuidesGrids false
/IncludeNonPrinting false
/IncludeSlug false
/Namespace [
(Adobe)
(InDesign)
(4.0)
]
/OmitPlacedBitmaps false
/OmitPlacedEPS false
/OmitPlacedPDF false
/SimulateOverprint /Legacy
>>
<<
/AddBleedMarks false
/AddColorBars false
/AddCropMarks false
/AddPageInfo false
/AddRegMarks false
/ConvertColors /ConvertToCMYK
/DestinationProfileName ()
/DestinationProfileSelector /DocumentCMYK
/Downsample16BitImages true
/FlattenerPreset <<
/PresetSelector /MediumResolution
>>
/FormElements false
/GenerateStructure false
/IncludeBookmarks false
/IncludeHyperlinks false
/IncludeInteractive false
/IncludeLayers false
/IncludeProfiles false
/MultimediaHandling /UseObjectSettings
/Namespace [
(Adobe)
(CreativeSuite)
(2.0)
]
/PDFXOutputIntentProfileSelector /DocumentCMYK
/PreserveEditing true
/UntaggedCMYKHandling /LeaveUntagged
/UntaggedRGBHandling /UseDocumentProfile
/UseDocumentBleed false
>>
]
>> setdistillerparams
<<
/HWResolution [2400 2400]
/PageSize [612.000 792.000]
>> setpagedevice
|