Ethylene to Propylene Conversion over Ni-W/ZSM-5 Catalyst

Article abstract of DOI:10.1134/S1070427219080068

A ZSM-5 based catalyst was employed to produce light olefins in the process of converting ethylene to propylene, as well as Ni-W/ZSM-5 to improve the catalyst. After loading the Ni-W/ZSM-5 0.5, 1.0, 2.0 wt.% by inoculation, the modified catalyst was assessed for accurate determination of the specification by SEM, BET, FTIR analyzes. The activity of this catalyst was evaluated in the process of ethylene to propylene conversion in a constant reactor under operational conditions (temperature 400°C, pressure 1 atm, and feed flow rate of 0.5 cm³/min of pure ethylene). The selectivity of ethylene and propylene over the modified catalyst increased as the temperature rises and the maximum selectivity was achieved at 400°C. The catalyst with 0.5 wt.% Ni/ZSM-5 had the highest conversion rate and better selectivity than that with other percentages. Also the catalyst with 2 wt.% Ni-W/ZSM-5 had the highest conversion rate and better selectivity than other percentages.

Full text of DOI:10.1134/S1070427219080068

ISSN 1070-4272, Russian Journal of Applied Chemistry, 2019, Vol. 92, No. 8, pp. 1094−1101. © Pleiades Publishing, Ltd., 2019.
CATALYSIS
Ethylene to Propylene Conversion over Ni-W/ZSM-5 Catalyst
Ehsan Kianfara,b,*
a Department of Chemical Engineering, Arak Branch, Islamic Azad University, Arak, Iran
b Young Researchers and Elite Club, Gachsaran Branch, Islamic Azad University, Gachsaran, Iran
*e-mail: e-kianfar94@iau-arak.ac.ir
Received February 1, 2019; revised June 25, 2019; accepted July 3, 2019
Abstract—A ZSM-5 base is used to produce light olefins in the process of converting ethylene to propylene, as
well as Ni-W/ZSM-5 to improve the catalyst. After loading the Ni-W/ZSM-5 0.5,1,2 wt % by inoculation, the
modified catalyst was investigated for accurate determination of the specification by SEM, BET, FTIR analyzes.
The activity of this catalyst was evaluated in the process of ethylene to propylene conversion in a constant reac-
tor under operational conditions (temperature 400°C, pressure 1 atm, and feed flow rate of 0.5 cm3/min of pure
ethylene), which also shows the results of tests of catalyst activity evaluation. The selectivity of ethylene and
propylene over the modified catalyst will increase as the temperature rises and the maximum selectivity will be
achieved at 400°C. The catalyst with 0.5 wt % Ni/ZSM-5 has the highest conversion rate and better selectivity
than that with other percentages, also the catalyst with 2 wt % Ni-W/ZSM-5 has the highest conversion rate and
better selectivity than other percentages.
Keywords: ethylene, propylene, fixed-bed reactor, catalyst ZSM-5, modified catalyst, Ni-W/ZSM-5
DOI: 10.1134/S1070427219080068
INTRODUCTION
propylene, such technologies as fluid catalytic cracking
(FCC) and thermal cracking of ethane are classified as the
methods with low efficiency. The effects of acidity, pore
size, pore structure, and crystal size of the zeolite, as well
as effect of operation reaction conditions upon product
selectivity, has been investigated. These investigations was
explained in [1]. World reserves of natural gas are approved
to be over 5 000 trillion cubic feet which are being grown
with a speed higher than that of approved reserved of crude
oil. Current gas reserves are about 83% equivalent to the
energy of approved oil reserves while 75% of these reserves
are occupied to crude oil with lower suitability [2, 3].About
3 000 trillion cubic feet of gas reserves are recognized as
stranded reserves due to the economically unsustainable
transition to consumer markets [3, 4]. Catalytic conversion
of methanol to hydrocarbons is promising and indirect
process to convert natural gas reservoirs to such valuable
products as gasoline and olefins [5–10]. The changes made
to the demand for petroleum products and petrochemicals
with better properties have had a significant impact on
the role of refinery and petrochemical processes in the
former industry and it is even expected that this will be
even more significant in the future. Therewith, in order to
satisfy the required changes, some researchers plan to use
Light olefins (ethylene and propylene), are considered
among the most crucial elements in petrochemical
industries, which are used for producing polymers and
diverse chemicals. As the main feed of petrochemical
processes, propylene is widely used. Olefins can be
produced through diverse processes and different raw
materials. The common point of all these processes is
production in a wide range of products and peripherals.
In addition to mentioned industrial processes, there
exist additional non-industrial technologies in diverse
development steps including oxidative coupling of methane
(OCM), propane dehydrogenation (PDH) for production
of propylene, low-value heavy olefins cracking exemplary
C4/C5, metathesis of ethylene and butylene to propylene,
and conversion of methanol to light olefins (MTP, MTO).
Concerning access to hydrocarbon resources in different
countries, diverse strategies are selected for production of
olefins so that upon discovery of such strategies, propylene
to ethylene ratio has been considerably decreased in
steam cracking units and this has resulted in complicated
propylene market. Although thermal cracking of naphtha
is the main process of light olefins production such as
1094

ETHYLENE TO PROPYLENE CONVERSION
Condenser
1095
Gas chromatograph (GC)
Liquid products
N2
Reactor
Preheater
Ethylene
MFC
Fig. 1. Schematic diagram of experimental setup.
new and more important technologies with new catalysts.
One of the most efficient methods is catalytic cracking
in the vicinity of zeolites. During the recent decade, the
advances in FCC area were considered in the sections of
alumina technology and stability of zeolite as well as of
acceptable limits of catalyst poisoning. The recent advances
in the catalyst technology meet environmental regulations
for illegal materials emissions such as SOx, CO, and NOx.
In addition, controlling the selectivity of light olefins has
been enhanced due to recent advances in stabilization
and combination of ZSM-5 basic additives [5–15]. Since
catalytic cracking has been recognized as an alternative way
to produce light olefins, although this process is still in the
development step, the results show that catalytic cracking
provides more advantages compared to thermal cracking.
The most important features of catalytic cracking include
the higher capacity to produce ethylene and propylene,
lower emissions of greenhouse gases, considerable energy
saving as well as the capability to reduce invaluable heavy
products [16]. In this section, the cracking process will be
discussed initially and then catalytic cracking of olefins
preparation will be pointed out [17–20, 34–36]. Overview
of catalytic results for the ethylene to propylene reaction
using selectivity zeolite catalysts is in Table 1. Zeolites
as catalysts have many unique properties such as acidity,
shape-selectivity, high surface area and structural stability.
The destination of this article is using the ZSM-5 catalytic
process for producing light olefins. The purpose of this
work is to synthesize and determine the characteristics of
Ni/SM-5 and W/ZSM-5 catalysts and evaluate their role
in the conversion of ethylene to propylene. Therewith,
the direct conversion of ethylene to propylene can be an
effective way to respond to global demand. In the study
ethylene was used as a feed. In addition, insemination of
the modified zeolite with nickel and tungsten leads to the
production of propylene with a higher conversion rate and
selectivity.
EXPERIMENTAL
Materials. Sodium aluminate (technical grade) was
purchased from Riedel-deHaen. Silicic acid (96.6%),
tetrapropylammonium bromide (98%), sodium hydroxide
(97.5%), methanol (99.9%), ethanol (96%), ammonium
nitrate (99.95%), ethylene (99.9%), nickel(II) nitrate
(99%), sodium tungstate (99%) were supplied by Merck.
All materials used were of experimental purity grade and
suitable purity.
ZSM-5 catalyst synthesis. Initially the desired amount
of sodium aluminate was added to hydroxide sodium
solution and stirred for 60 min (solution A). In another
beaker, required amount of tetra-propyl-ammonium
bromide was added to sodium hydroxide solution and
stirred for 30 min. Silicic acid and deionized water were
slowly added and stirred for another 30 min (solution B).
Subsequently, solution A was mixed with solution B and
stirred for 60 min. Final gel was transferred to a Teflon-
lined stainless steel autoclave and heated at 180°C for
12 h. Finally, contents of reactor were filtered, washed,
and dried at 110°C for 12 h. The solid product was cal-
cined at 500°C for 5 h. Ion exchanging of ZSM-5 zeolite
was performed using ammonium nitrate solution (1 M).
Zeolite was mixed with solution and heated at 110°C for
6 h. In the following step, silica foam was added to the
solution while mixing. After 24 h of mixing, the derived
gel was poured into an autoclave reactor and heated at
RUSSIAN JOURNAL OF APPLIED CHEMISTRY Vol. 92 No. 8 2019

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EHSAN KIANFAR
Table 1. Role of reaction parameters during ETP reaction with zeolite catalysts
T,
°C
C1–C4,
wt %
C3=,
wt %
BTX,
wt %
Zeolite
Ni/MCM-41
Si/Al
C4=, wt %
C5+, wt %
References
–
60
–
400
450
350
50
–
48.0
44.0
56.0
49.0
32.0
47.5
14.1
43.4
38.5
43.8
31.5
45.4
32.3
19.1
41.8
43.4
75.4
84.7
68.3
63.0
79.5
78.7
40.0
43.0
54.0
35.0
50.0
56.0
14.4
5.1
<5
–
–
–
[23]
[24]
[25]
[26]
[27]
[28]
[29]
[30]
[30]
[31]
[29]
[30]
[30]
[29]
[29]
[31]
[31]
[31]
[31]
[30]
[30]
[32]
[33]
Ni/MCM-41
Ni/MCM-48
NiRe/γ-Al2O3
–
–
8
–
–
–
–
–
Ni/silica-alumina 12-MR 223
375
450
550
450
400
450
400
550
400
550
550
550
450
450
400
–
–
–
Beta
25
28.1
69.1
25.7
25.8
15.9
19.3
13.2
26.5
38.2
6.3
10.0
3.8
10.1
14.5
0
0
Beta
27
7.9
-
Beta
11.4
11.2
20
20.8
21.2
40.3
25.8
21.1
22.3
8.7
Mordenite
MCM-22
UZM-35a
EU-1
-
0
8.9
33
16.2
14.7
18.9
4.9
20.5
18.4
3.8
0
7.2
5.6
-
EU-1
10.3
35
ZSM-11
ZSM-22
ZSM-23
SAPO-44b
SAPO-34b
SAPO-34b
SAPO-34b
SAPO-34b
SAPO-18b
SAPO-18b
29.1
3.1
4.9
0
35
28.3
24.4
10.0
7.5
34
8.9
0.1
0.1
0.1
10.8
7.8
0
22.4
12.0
6.6
7.7
1.6
9.0
1.8
0
–
0.08 400
16.0
12.1
12.2
24.0
–
0.1
0.1
0.3
450
450
500
–
9.1
0
14.0
20.0
2.0
a K/Al = 0.09.
b Si/(Si + Al + P).
150°C for 6 days. Catalyst was dried at 110°C for 12 h
and calcined at 500°C for 5 h [21, 22].
pH was adjusted to 5 using the ammonia solution (1 M).
When the pH became stable, the mixture was placed in
an ultrasonic bath for 180 min. The resultant product was
filtered, washed, and dried at 110°C for 24 h and calcined
at 650°C for 3 h.
Preparation of catalyst Ni/ZSM-5. An appropriate
amount of 0.07 g nickel nitrate salt was used to make third
catalysts with 0.5, 1, and 2 wt % of Ni on ZSM-5 zeolite.
For each sample, 5 g salt was mixed with 2 cm3 water in a
beaker. ZSM-5 (0.05 g) was then added to the solution and
Preparation of catalyst Ni-W/ZSM-5. An appropriate
amount (0.155 g) of nickel nitrate and tungsten nitrate salt
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ETHYLENE TO PROPYLENE CONVERSION
1097
(B)
(C)
(A)
(E)
(D)
(F)
(G)
Fig. 2. SEM analysis: (A) ZSM-5, (B) 0.5 wt % Ni/ZSM-5, (C) 1 wt % Ni/ZSM-5, (D) 2 wt % Ni/ZSM-5, (E) 0.5 wt % Ni-W/ZSM-5,
(F) 1 wt % Ni-W/ZSM-5, (G) 2 wt % Ni-W/ZSM-5.
was used to make third catalysts with 0.5, 1, and 2 wt %
of Ni-W on ZSM-5 zeolite. For each sample, 5 g salt was
mixed with 2 cm3 water in a beaker. ZSM-5 (0.10 g) was
then added to the solution and pH was adjusted to 5 using
the ammonia solution (1 M). When the pH became stable,
the mixture was placed in an ultrasonic bath for 180 min.
The resultant product was filtered, washed, and dried at
110°C for 24 h and calcined at 650°C for 3 h.
with an FID indicator and Petrocol® DH capillary column
(L.: 100 m, Dia.: 0.25 mm, film thickness: 0.5 μm) and
helium as a carrier gas.
RESULTS AND DISCUSSION
SEM analysis results. Figure 2 shows SEM analysis
results for the calcined catalyst, which were photographed
with a zooming of 20 μm. The SEM analysis was used to
evaluate the morphology of modified catalysts. As it can
be seen in Fig. 2, the catalysts of 0.5, 1, 2% Ni/ZSM-5,
0.5, 1, and 2% Ni-W/ZSM-5 with a Si/Al ratio of 15 have
a fully porous and spongy structure.
Catalytic tests. Figure 1 shows ETP of the experi-
mental rig. Conversion of ethylene to propylene was
carried out in a fixed-bed reactor. For each experiment,
1.2 g of catalyst sample was placed in a stainless steel
tube (L: 500mm, ID: 7mm), and held in its place with
glass wool. Subsequently, a reactor was placed inside of
a tabular furnace, which was controlled by a PID tem-
perature controller. All experiments were carried out at
the temperature of 400°C and pressure of 1 bar. Nitrogen
was used as carrier gas for ethylene as well as providing
better distribution of reactant. Products are passed through
a condenser, which is held in cool water to reduce the
temperature of the effluent gas. Subsequently, gas and
liquid products are separated in a small cylinder. Liquid
products were analyzed using an online GC equipped
Results of FT-IR analysis. Figure 3 depicts the
results of FTIR on the catalysts 0.5, 1, 2% Ni/ZSM-5,
0.5, 1, 2% Ni-W/ZSM-5 with a Si/Al ratio of 15 in the
area of 400 to 2000 cm–1. The peak in the area 450 cm–1
is associated with Si–O–Si and Al–O–Al bonds and the
peaks 790 and 1100 cm–1 are, respectively, associated
with symmetric and asymmetric T–O–T bonds in the
structure of zeolite while T can be either Al or Si in the
structure of the zeolite. The peaks 790 and 1100 cm–1
are seen at almost all zeolites or crystalline materials
RUSSIAN JOURNAL OF APPLIED CHEMISTRY Vol. 92 No. 8 2019

1098
EHSAN KIANFAR
T, %
Table 2. BET results for different synthesized catalysts
1
2
3
4
5
6
7
BET surface
area, m2 g–1
Pore volume,
cm3 g–1
35
Catalysts
ZSM-5
300
0.39
0.33
0.31
0.30
0.35
0.33
0.31
Ni / ZSM-5 (0.5%)
Ni / ZSM-5 (1%)
Ni/ ZSM-5 (2%)
Ni-W/ ZSM-5 (0.5%)
Ni-W/ ZSM-5 (1%)
Ni-W/ ZSM-5 (2%)
286.97
270.02
272.15
257.38
271.97
275.85
25
15
5
containing silicon. The peaks available in 545 and
620 cm–1 indicate MFI structure and are visible only in
the zeolites with MFI structure. The peaks appeared in
the areas 1633 and 3451 cm–1 are, respectively, associated
with stretching vibration frequency ofAl–O bond and that
of hydroxyl group for the bond between Si andAl atoms.
The acidity of OH group in the area 3000 cm–1 means
a high absorptive frequency which has been appeared.
Accordingly, a sharp peak of OH group was removed
0
1000
2000
CM-1
3000
4000
Fig. 3. (Color online) FTIR analysis pattern results for prepared
catalyst. (1) ZSM-5, (2) 0.5 wt % Ni/ZSM-5, (3) 1 wt % Ni/ZSM-
5, (4) 2 wt % Ni/ZSM-5, (5) 0.5 wt % Ni-W/ZSM-5, (6) 1 wt %
Ni-W/ZSM-5, (7) 2 wt % Ni-W/ZSM-5.
80
0.5%
60
1%
2%
40
20
0
0
100
200
300
400
T, °C
Fig. 4. (Color online) Effect of temperature on the rate of ethylene conversion by Ni/ZSM-5 catalyst.
80
0.5%
60
40
20
1%
2%
0
0
100
200
T, °C
300
400
Fig. 5. (Color online) Effect of temperature on the rate of ethylene conversion by Ni-W/ZSM-5 catalyst.
RUSSIAN JOURNAL OF APPLIED CHEMISTRY Vol. 92 No. 8 2019

ETHYLENE TO PROPYLENE CONVERSION
1099
35
25
15
5
0.5%
1%
2%
0
100
200
T, °C
300
400
Fig. 6. (Color online) Effect of temperature on the selectivity of propylene with Ni/ZSM-5.
35
25
15
0.5%
1%
2%
5
0
0
100
100
200
200
300
300
400
400
T, °C
Fig. 7. (Color online) Effect of temperature on the selectivity of propylene with Ni-W/ZSM-5 catalyst.
in the area 3600 cm–1, which is associated with Al–OH
group, indicating removal of OH group and formation
of Ni–O. If a peak has appeared for Ni–O and W–Ni–O
compounds, then it should have appeared in the area
400–450 cm–1 which can be overlapped with the peaks
Si–O–Si and Si–O–Al.
The effect of temperature on rate of ethylene
conversion by Ni/ZSM-5 catalyst. Figure 4 shows
conversion rate of ethylene according to temperature
using Ni/ZSM-5 catalysts with 0.5, 1, and 2 wt %. The
percent conversion of ethylene to propylene at various
temperatures with Ni modified ZSM-5 catalysts is shown
in Fig. 4. With increasing temperature, the percentage of
ethylene conversion increases and the ascending trend
is observed. The maximum conversion rate can be seen
at 400°C and the lowest conversion rate, at 50°C. The
catalyst with 0.5% Ni has the highest conversion rate
than those of other percentages.
Results of BET analysis. Table 2 presents physical
and chemical properties of the catalyst of ZSM-5 and
Ni/ZSM-5 and Ni-W/ZSM-5 using BET analysis. Also,
BET analysis was conducted to be informed of specific
surface, size, and volume of pores. The specific surface
of the catalyst of Ni/ZSM-5 decreased from 286.97 to
272.15 m2 g–1 through increased amount of Ni from 0.5
to 2%. Also, total pores volume decreased from 0.33 to
0.30 cm3 per gram through increased amount of Ni from
0.5 to 2%, as well. The specific surface of the catalyst of
Ni-W/ZSM-5 increased from 257.35 to 275.85 m2 g–1
through increased amount of Ni-W from 0.5 to 2%.
Total pores volume decreased from 0.35 to 0.31 cm3 g–1
through increased Ni-W from 0.5 to 2%, as well.
The effect of temperature on rate of ethylene
conversion by Ni-W/ZSM-5 catalyst. Figure 5 shows
conversion rate of ethylene vs. temperature using Ni-W/
ZSM-5 catalysts with 0.5, 1 and 2 wt %. The percent
conversion of ethylene to propylene at various tempera-
tures with Ni-W modified ZSM-5 catalysts is shown in
Fig. 5. With increasing the temperature, the percentage
of ethylene conversion increases and the ascending trend
is observed. The maximum conversion rate can be seen
RUSSIAN JOURNAL OF APPLIED CHEMISTRY Vol. 92 No. 8 2019

1100
EHSAN KIANFAR
at 400°C and the lowest conversion rate at 50°C. The
catalyst with 2 wt % Ni-W has the highest conversion
rate than those of other percentages.
CONFLICT OF INTEREST
Conflict of interest the authors declare that they have
no conflict of interest
The effect of temperature on selectivity of propyl-
ene by Ni/ZSM-5 catalyst. Figure 6 presents an effect of
temperature on the selectivity of propylene on the ZSM-5
catalysts modified by Ni. Figure 6 shows diagram of se-
lectivity in terms of temperature using Ni/ZSM-5 catalysts
with 0.5, 1 and 2 wt %. In this regard, with increasing
temperature from 250°C, selectivity rate is enhanced with
an increasing trend. The highest and lowest selectivity
can be seen at 400°C and 50–150°C range. The catalyst
with 0.5 wt % Ni has the highest selectivity than those
of other percentages.
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