Reaction of a mixture of bismuth and iron oxides with chlorine and sulfur dioxide

Article abstract of DOI:10.1134/S1070363208100022

The processes in a heterogenous multicomponent system Bi₂O ₃-Fe₂O₃-Cl₂-SO₂. are explored. In the temperature range 300-700°C is clearly developed mutual influence of chemical reactions at introducing to the system of an additional component: chloridosublimation of both bismuth and iron in the presence of SO₂ and chloridosublimation of bismuth at adding iron oxide to bismuth oxide are accelerated. In the region of the higher temperatures the possible chemical reactions in the system proceed independently: SO₂ only dilutes chlorine and mutual influence of bismuth and iron oxides is not found.

Full text of DOI:10.1134/S1070363208100022

ISSN 1070-3632, Russian Journal of General Chemistry, 2008, Vol. 78, No. 10, pp. 1836–1842. © Pleiades Publishing, Ltd., 2008.
Original Russian Text © L.E. Derlyukova, M.V. Vinokurova, 2008, published in Zhurnal Obshchei Khimii, 2008, Vol. 78, No. 10, pp. 1598–1604.
Reaction of a Mixture of Bismuth and Iron Oxides
with Chlorine and Sulfur Dioxide
L. E. Derlyukova and M. V. Vinokurova
Institute of Problems of Chemical Physics, Russian Academy of Sciences,
pr. Akad. Semenova 1, Chernogolovka, Moscow oblast, 142432 Russia
e-mail: led@icp.ac.ru, alv@icp.ac.ru
Received April 10, 2008
Abstract—The processes in a heterogenous multicomponent system Bi2O3–Fe2O3–Cl2–SO2. are explored. In
the temperature range 300–700°С is clearly developed mutual influence of chemical reactions at introducing to
the system of an additional component: chloridosublimation of both bismuth and iron in the presence of SO2
and chloridosublimation of bismuth at adding iron oxide to bismuth oxide are accelerated. In the region of the
higher temperatures the possible chemical reactions in the system proceed independently: SO2 only dilutes
chlorine and mutual influence of bismuth and iron oxides is not found.
DOI: 10.1134/S1070363208100022
Revealing the optimal conditions for conducting a
chemical process in multicomponent heterogenous
system widely used in chemical technology meets a
problem defined by mutual influence of chemical
reactions. Change in the composition of reaction
mixture and, in particular, adding to the system of any
additional component leads to changes in both
equilibrium composition of reaction products and rates
of chemical processes [1].
presence of Fe2O3 [4, 5]. Variations in composition of
gas phase, in part, dilution of chlorine with sulfur
dioxide also leads to changes in the rate of chlorination
[6, 7].
In the present work we explored interactions in the
system Bi2O3–Fe2O3–Cl2–SO2 for the estimation of
variations in the rate of BiCl3 and FeCl3 formation at
the complication of the reaction system. Such
investigation are interesting not only for revealing
regularities of the processes in multicomponent
heterogenous systems but also for finding optimal
conditions of BiCl3 separation from the mixtures
containing Fe2O3. The importance of obtaining pure
BiCl3 is defined by its wide application in preparative
chemistry and in catalysis and because it is used as a
basic material for preparation of metallic bismuth [8, 9].
A convenient model for the investigation of mutual
influence of chemical reactions in heterogenous
systems “gas–condensed phase” is the process of
chemical sublimation. In such process a substance is
transformed from condensed phase into gas owing to
chemical reactions. A particular case of chemical
sublimation is the process of chlorination where only
gaseous reaction products are formed. In this case the
process kinetics is not complicated by diffusion of
gaseous components through the film formed by
reaction products.
Reaction of Bi2O3 with Cl2 proceeds even at room
temperature, the products are bismuth oxychloride
BiOCl and oxygen. Chemical sublimation of bismuth
trichloride at 25–250°С does not occur. The BiCl3
sublimate appears at 300°С. The chloridosublimation
completeness at the temperature below 400°С is only
5% or less (Table 1), the bismuth remains in the solid
phase in the form of oxychloride. We suggest possible
to conclude that BiOCl is an intermediate at the
chemical sublimation of BiCl3, and in the temperature
range 25–400°С the rate of BiOCl formation is much
higher than the rate of the bismuth chloridosublimation.
Investigations of chlorination of mixtures of oxides
have been carried out earlier mainly for revealing
optimal conditions for separating the components [2,
3]. In some works has been shown that certain
conclusions about kinetics of chlorination of mixtures
can not be achieved from the results obtained for
individual metal oxides: the rate of chlorination of
Ga2O3, In2O3 and ZnO increases noticeable in the
1836

REACTION OF A MIXTURE OF BISMUTH AND IRON OXIDES
1837
The isotherms of interaction of bismuth oxide with
chlorine at 500–650°С (Fig. 1) also show that the
process of BiCl3 formation consists of separate steps.
In the initial moment the sample mass increases due to
formation of BiOCl, and then decreases practically
lineary in mass due to sublimation of BiCl3. Above
650°С no increase in the initial mass is registered and
the process includes induction step whose duration
falls when temperature increases. The activation
energy of the process of BiCl3 chemical sublimation is
115 kJ mol–1.
Table 1. Completeness of chloridosublimation of bismuth
and iron at the chlorination of Bi2O3 and Fe2O3 (% to initial)
Bi, (% to initial)
Fe, (% to initial)
t, °С τ, min
Cl2
Cl2 + SO2
Cl2
Cl2 + SO2
300
350
400
450
30
60
90
30
60
90
30
60
90
30
60
90
30
60
30
60
30
30
30
1.2
1.5
4.4
7.4
0.3
0.5
0.5
0.8
1.0
0.9
1.0
1.5
1.7
1.8
2.3
2.4
3.2
5.4
3.8
6.2
8.8
18.8
36.6
19.1
23.0
25.2
20.0
22.0
26.5
22.0
23.1
28.0
22.5
27.3
29.5
25.6
30.6
–
1.5
10.3
6.5
1.6
Reaction of Bi2O3 with SO2 begins at 450°С and
proceeds with increase in the sample mass. By the data
of chemical analysis, content of sulfur in the solid
phase reaction products achieves 4.0% at the process
temperature 500°С and contact duration 5 h. The main
portion of sulfur is sulfate, that is, the total process can
be represented by the following equation:
2.3
8.6
2.7
11.8
7.0
2.6
3.9
10,6
12.5
21.8
34.4
46.3
24.5
38.2
37.3
52.5
61.0
82.6
–
5.2
4 Bi2O3 + 12 SO2 = 3 Bi2(SO4)3 + Bi2S3.
(1)
8.9
Under polythermic conditions (heating rate 15 deg/min)
the increase in mass occurs until ~650°С, but further
increase in temperature leads to decrease in the sample
mass, and the content of sulfur in the residue also falls.
The apparent activation energy of the process at the
contact duration 60 min in the temperature range 450–
550°С is 130 kJ mol–1. Formation of new solid phase
leads to sharp decrease in the rate of the process, and
even after 5 h contact of Bi2O3 with SO2 at 500°С the
process deepness is not higher than 20%. Elevating the
temperature leads to stepwise decomposition of
bismuth sulfate [10], content of sulfur in the solid
phase falls and at 900°С becomes equals to 0.9% only.
15.7
20.3
12.5
18.9
25.9
47.6
58.1
93.7
96.6
500
550
–
600
650
700
31.4
38.1
57.1
Reaction of Bi2O3 with a mixture of Cl2 and SO2
occurs even at room temperature, the reaction products
are predominantly bismuth sulfate and oxychloride.
4 Bi2O3 + 3 Cl2 + 3 SO2 = 6 BiOCl + Bi2(SO4)3.
(2)
Chemical sublimation of BiCl3 in this case occurs
at 300°С (Table 1). Completeness of chlorido-
sublimation raises practically lineary in time. The con-
densed phase consists mainly of BiOCl and Bi2(SO4)3
(Table 2). Formation of solid phase products in
conjunction with low volatility of BiCl3 vapor
decelerate further progress of the process. In the
temperature range 300–400°С the fraction of bismuth
in sulfate is higher than in trichloride. A considerable
increase in the degree of chloridosublimation occurs
only at the temperature above 400°С.
τ, min
80
20
40
60
0
–20
1
–40
2
–60
–80
3
6
5
4
–100
The reaction isotherms of Bi2O3 with Сl2 in the
presence of SO2 at 500–750°С resemble those of Bi2O3
Fig. 1. Isotherms of reaction of Bi2O3 with Cl2. (1) 500,
(2) 550, (3) 600, (4) 650, (5) 700, and (6) 750°С.
RUSSIAN JOURNAL OF GENERAL CHEMISTRY Vol. 78 No. 10 2008

1838
DERLYUKOVA, VINOKUROVA
Table 2. Distribution of bismuth between the products and solid residue at the chlorination of Bi2O3 and Fe2O3 with a mixture
of Cl2 and SO2
Bi, % to initial
BiOCl
Fe, % to initial
t, °C
τ, min
BiCl3
4.4
Bi2(SO4)3
19.5
20.2
22.6
24.1
20.1
21.2
22.5
18.9
19.9
23.2
19.4
20.5
20.2
Bi2O3
13.5
14.3
–
FeCl3
19.1
23.0
25.2
–
Fe2(SO4)3
18.8
22.0
24.7
–
Fe2O3
62.0
54.9
50.0
–
300
30
60
90
120
30
60
90
30
60
90
30
60
90
62.5
58.1
–
7.4
10.3
14.7
6.5
49.1
62.1
60.3
–
12.1
11.3
9.9
–
350
400
450
20.0
22.0
26.5
22.0
23.1
28.0
22.5
27.3
29.5
19.1
20.9
25.1
21.3
21.4
26.4
21.5
25.0
28.4
60.8
56.9
48.3
56.6
55.4
45.4
55.9
47.6
42.0
8.6
11.8
7.0
66.7
62.5
–
7.4
7.0
–
10.6
12.5
21.8
34.4
46.3
43.9
32.4
–
14.7
12.7
–
and SO2 mixture shows that dilution of chlorine with
sulfur dioxide accelerates chemical sublimation of
BiCl3 (Table 3).
chlorination with individual chlorine: at 500–600°С in
the first moment the sample mass increases due to
accumulation of the intermediate reaction products.
The further decrease in mass is explainable by
chemical sublimation of BiCl3 at the chlorination of
the intermediates.
Noteworthy that rate of Bi2(SO4)3 formation as a
result of reactions (2) and (3) is much higher than in
the atmosphere of sulfur dioxide alone. Thus, in the
reaction of Bi2O3 with the mixed Cl2 and SO2 both the
process, chloridosublimation of busmuth and forma-
tion of Bi2(SO4)3, accelerate. Increase in the
completeness of bismuth chloridosublimation is
promoted by decrease in stability of Bi2(SO4)3 with
increase in temperature. The accelerating action of SO2
in the region of high temperatures falls: at 750°С the
rates of bismuth chloridosublimation in the mixtures of
Cl2 with either argon or sulfur dioxide are practically
the same (Table 3).
6BiOCl + 3SO2 + 3Cl2 = 4BiCl3 + Bi2(SO4)3,
BiOCl + SO2 + Cl2 = BiCl3 + SO3.
(3)
(4)
Comparison of rates of chloridosublimation of
bismuth in the atmosphere of either Cl2 alone or Cl2
Table 3. Temperature dependence of the rate of bismuth
chloridosublimation
W, %/min
t, °C
Bi2O3
Bi2O3 + Fe2O3
Reaction of Fe2O3 with Cl2 with an appreciable rate
occurs only above 500°С [6], but chlorination of the
most active region on the surface occurs even at 300°С
(Table 1). The degree of passing FeCl3 to sublimate at
300°С is less than 0.5% practically regardless the
duration of the contact of oxide with chlorine. In the
chlorine flow the isotherms are convex toward ordinate
axis, the curves transform into one another at the
change in the scale along the time axis (affine
transform). This result shows that the process is
Cl2
0.3
Cl2 + Ar Cl2 + SO2
Cl2
2.6
Cl2 + SO2
500
550
600
650
700
750
0.2
0.5
0.7
2.0
2.7
6.2
0.9
6.5
2.6
1.4
3.6
7.8
7.3
4.0
2.5
5.0
10.8
16.1
24.0
8.2
9.6
5.0
8.0
12.2
15.5
23.1
11.6
11.1
RUSSIAN JOURNAL OF GENERAL CHEMISTRY Vol. 78 No. 10 2008

REACTION OF A MIXTURE OF BISMUTH AND IRON OXIDES
1839
limited by one and same step. The apparent activation
energy of FeCl3 chemical sublimation is 99 kJ mol–1,
as estimated from the temperature dependence of the
affine transform coefficients in the temperature range
600–800°С.
mass is a result of chemical sublimation of FeCl3 ·
Fe2(SO4)3 is not stable in the presence of chlorine. At
the temperature above 600°С the sample mass falls
monotonically. The iron chloridosublimation proceeds
according to the following equartion:
Unlike bismuth oxide, reaction of Fe2O3 with SO2
in the studied temperature range is restricted by
adsorption and no formation of voluminous substances
has been registered.
Fe2O3 + 3Cl2 + 3SO2 = 2FeCl3 + 3SO3.
(6)
The process apparent activation energy in the
temperature range 600–750°С is 62.8 kJ mol–1. The
dependence of chloridosublimation rate on the SO2/Cl2
ratio in gas phase is shown in Fig. 2. The accelerating
action of SO2 falls when the temperature raises, and at
800°С sulfur dioxide behaves as inert chlorine diluting
substance only.
In the reaction of Fe2O3 with a mixture of Cl2 and
SO2 formation of reaction products occurs even at 200°С.
At 300°С and above the iron chloridosublimation
proceeds with the rate higher than the rate of Fe2O3
chlorination in the atmosphere of Cl2 alone (Table 1).
Analysis of reaction products showed that the fractions
of iron converted into chloride and sulfate are
approximately equal (Table 2). The total process can
be described by the following equation:
Comparison of completeness of chemical
sublimation of individual bismuth and iron chlorides
showed that in the temperature range 400–700°С the
rate of chloridosublimation of bismuth is much higher
(Table 1).
2Fe2O3 + 3SO2 + 3Cl2 = Fe2Cl6 + Fe2(SO4)3.
(5)
In the mixture of Cl2 and SO2 the completeness of
iron chloridosublimation in the temperature range 300–
400°С is about those of bismuth, but at 500–700°С the
amount of BiCl3 passed to gas phase in a time unity is
considerably higher than for FeCl3.
Thus, introduction to the system of an additional
gaseous reagent (either Cl2 or SO2) results in appearing
of new reaction pathways and increases the degree of
Fe2O3 transformation. Like the case of Bi2O3,
accumulation of solid phase in the temperature range
300–450°С stepwise decelerates further chlorination of
Fe2O3, and reaction rate falls in time noticeable. At
600°С the essence of the process is changed. On the
chlorination isotherm in the initial moment is seen
increase in the sample mass and further it falls
practically lineary. Analysis of the reaction products
showed that increase in mass is defined by the
formation of Fe2(SO4)3 along the Eq. (5). Decrease in
The reaction isotherms for the Bi2O3–Fe2O3 mixture
with Cl2 (Fig. 3) are typical: at the temperature below
700°С after the induction period that is shorter at
higher temperature follows practically linear decrease
in the sample mass, the loss in mass is approximately
45%, and then the process sharply decelerates. We
have shown earlier that the decrease in mass is a result
of BiCl3 sublimation while iron remains in condensed
phase practically whole [11].
0
10
20
30
40
50 τ, min
0
–20
3.0
1
3
2.5
2
2
3
–40
2.0
1
4
1.5
–60
1.0
0.5
5
–80
6
–100
0
20
40
60
80
100 % SO2
Fig. 3. Isotherms of reaction of a mixture of Bi2O3 and
Fe2O3 with Cl2. (1) 500, (2) 550, (3) 600, (4) 650, (5) 700,
and (6) 750°С.
Fig. 2. Dependence of the rate of chloridosublimation on
the Cl2/SO2 ratio in gas phase. (1) 700, (2) 750, and (3) 800°С.
RUSSIAN JOURNAL OF GENERAL CHEMISTRY Vol. 78 No. 10 2008

1840
DERLYUKOVA, VINOKUROVA
amount of FeCl3. One can assume that iron trichloride
being adsorbed on the surface of BiOCl formed
intermediately at the chlorination of Bi2O3, promotes
BiCl3 formation.
Table 4. Distribution of bismuth and iron between the
product and solid residue at the chlorination of mixture of
Bi2O3 and Fe2O3 with a mixture of Cl2 with SO2
Bi (% to initial)
Fe (% to initial)
τ,
6BiOCl + 4FeCl3 = 6BiCl3+ 2Fe2O3.
(7)
t, °C
min
BiCl3
27.6
66.7
89.5
77.0
95.9
98.7
99.2
99.0
99.1
99.2
99.6
99.2
100
BiOCl
72.4
33.3
10.5
23.0
4.1
1.3
0.8
1.0
0.9
–
FeCl3 Fe2(SO4)3 Fe2O3
The significant difference in the rates of chemical
sublimation of BiCl3 and FeCl3 allows to perform the
process of selective bismuth chlorosublimation from
Bi2O3 and Fe2O3 mixtures in the atmosphere of
chlorine in the temperature range 500–700°С.
300
30
60
120
30
60
30
60
30
60
30
60
30
60
30
60
3.6
8.5
18.3
47.7
–
78.0
43.7
–
–
Reaction of a mixture of Bi2O3 and Fe2O3 with Cl2
in the presence of SO2 proceeds with a noticeable rate
even at 250°С and is accompanied with the increase in
the sample mass. At higher temperature after the initial
increase in the mass it becomes to fall.
350
400
450
500
600
650
14.4
27.0
27.2
26.6
26.5
28.0
25.6
30.6
–
55.7
52.4
53.2
54.7
47.6
49.0
51.8
45.1
–
29.8
20.5
19.6
18.7
25.8
23.0
22.6
24.3
–
The results of chemical and X-ray phase analysis
show that initial increase in the sample mass in the
chlorination process is a result of formation in
condensed phase of BiOCl and Fe2(SO4)3 (Table 4).
The further decrease in mass is a result of transfer of
metal chlorides to gas phase. At 300–700°С the rate of
chloridosublimation of bismuth is much higher that
that of iron.
–
0.8
0
31.4
–
47.7
–
20.8
–
The apparent activation energy of chemical
sublimation of BiCl3 estimated from the degree of
conversion for 15 min in the temperature range 300–
400°С is 83.7 kJ mol–1. The total chloridosublimation
of bismuth occurs under relatively mild conditions: at
400°С at the experiment duration 60 the bismuth
content in solid phase residue (as oxychloride) was
0.8%. There was no inreacted Bi2O3 in the residue.
99.3
100
0.7
0
48.6
2.7
48.7
The rate of chloridosublimation of bismuth throm
the mixture of oxides is much higher than in the case
of individual Bi2O3 (Table 3). The activation energy of
bismuth chloridosublimation in the presence of Fe2O3
is 95 kJ mol–1, while for the Bi2O3 alone is 115 kJ mol–1.
Decrease in activation energy and increase in the rate
of the process show that the reaction pathway is
changed. This can not be a result of contact
phenomena at the boards of grains because in the
mechanical mixture the sufficient contact between
oxides grains seems doubtful. Hence, effect of Fe2O3 is
realized through the gas phase.
Chemical sublimation of FeCl3 proceeds with a
noticeable rate at 300°С. But at the sublimation
completeness of BiCl3 below 30% (Table 4) the degree
of chloridosublimation of iron is less than 4%. At
removing bismuth from solid phase the completeness
of iron chloridosiblimation becomes higher. The
fraction of iron converted to sulfate is twice of that
passed to chloride.
The data obtained show that presence of Fe2O3
defines sharp increase in the amount of bismuth
transformed into BiCl3. Therewith, in condensed phase
is absent Bi2(SO4)3 whose formation in the reaction of
Bi2O3 with the mixture of Cl2 and SO2 led to
deceleration of the process of bismuth chloride-
sublimation. However, in the presence of Bi2O3
noticeable falls completeness of iron transfer into chlo-
ride but increases its fraction in the form of Fe2(SO4)3.
The decrease in activation energy can be defined by
essential influence of iron trichloride on the
chlorination process. Interaction with chlorine of the
most active areas on the Fe2O3 surface occurs at
enough low temperature (300°С). Acceleration of
chemical sublimation of BiCl3 in the presence of Fe2O3
occurs in a wide temperature range, that is the process
of bismuth chloridosublimation is affected by small
RUSSIAN JOURNAL OF GENERAL CHEMISTRY Vol. 78 No. 10 2008

REACTION OF A MIXTURE OF BISMUTH AND IRON OXIDES
1841
The observed increase in the content of Fe2(SO4)3 in
condenced phase and increase in the rate of bismuth
chloridosublimation in the temperature range 300–
500°С at the reaction of Cl2 and SO2 with the Bi2O3
and Fe2O3 mixture can be a result of exchange reaction:
Reaction of Bi2O3, Fe2O3 and their mixtures with
chlorine and sulfur dioxide in the temperature range
250–600°С was studied by a flow method [6]. A
weighted sample 0.60–0.90 g was placed to a heated
tubular reactor with an inert gas passing through it.
After achieving a given temperature the inert gas flow
was replaced by the flow of reacting gas. Volatile
products were trapped in cooled traps. The linear gas
speed was 0.02 m sec–1.
Bi2(SO4)3 + 2FeCl3 = 2BiCl3 + Fe2(SO4)3.
(8)
Increase in temperature leads to decrease in the role
of exchange reaction, probably owing to low thermal
stability of Bi2(SO4)3. At the temperature 550–750°С
unlike the region of low temperatures just after passing
of gas mixture into the reactor the sample mass falls
and to the vapor phase is passed not only BiCl3, but
also FeCl3. At 600°С still occurs formation of Fe2(SO4)3,
but longer duration leads to complete sublimation of
iron. This observation shows that Fe2(SO4)3 is formed
as an intermediate. At 650°С the condensed phase does
not contain sulfur (Table 4), and iron chloride-
sublimation proceeds mainly as the reaction (9):
The process regularities at 550–750°С were studied
by gravimetric method on an installation with
automatic recording of mass change in time [4].
Sensitivity of the installation is 0.001 g per one mm of
its scale. The sample weight was 0.180–0.200 g. Total
gas consumption was 150–200 ml min–1 at linear rate
0.05 m sec–1. Under such conditions the rate of gas
achieving the surface not limited the process. The
experiments were carried out mostly at the Cl2:SO2
ratio 1:1.
Fe2O3 + 3Cl2 + 3SO2 = 2FeCl3 + 3SO3.
(9)
In the work was used mechanical mixture of
bismuth and iron oxides with purity grade “extra
pure,” in weight ratio 1:1. For the characterization of
parent samples and reaction products were applied x-
ray phase analysis and commonly used procedures of
chemical analysis [12].
According to the data of Table 3, Fe2O3 accelerates
chloridosublimation of bismuth till up to 600°С. At
650–750°С the rates of transfer of BiCl3 to gas phase
from individual oxide and from the Bi2O3 and Fe2O3
mixtures are similar. Increase in temperature also
diminishes effect of SO2 on the bismuth chloridosub-
limation. At 750°С sulfur dioxide behaves as inert
diluting agent only.
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