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Synthesis and Modification of Zeolite ZSM-5 Catalyst with Solutions of

Calcium Carbonate (CaCO3)and Sodium Carbonate(Na2CO3)for Methanol to
Gasoline Conversion

Article  in  International Journal of Chemical Reactor Engineering · December 2018

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 DE GRUYTER International Journal of Chemical Reactor Engineering. 2018; 20170229

Ehsan Kianfar1 / Mahmoud Salimi1 / Vahid Pirouzfar2 / Behnam Koohestani1

Synthesis and Modification of Zeolite ZSM-5

Catalyst with Solutions of Calcium Carbonate
(CaCO3) and Sodium Carbonate (Na2CO3) for
Methanol to Gasoline Conversion
1 Department of Chemical Engineering, Arak Branch, Islamic Azad University, Arak, Iran, E-mail: m-salimi@iau-arak.ac.ir
2 Department of Chemical Engineering, Central Tehran Branch, Islamic Azad University, Tehran, Iran

Abstract:
In this article, the ZSM-5 catalyst was used as the base catalyst and its structure was modified for conducting
Methanol to Gasoline reactions. ZSM-5 catalyst reacts to the solutions with diverse concentrations of calcium
carbonate (CaCO3 ) and sodium carbonate (Na2 CO3 ), and consequently, some changes were applied to its in-
ternal structure. Thus, Methanol to Gasoline (MTG) process was carried out under pressure of 1 atm, the tem-
perature of 400°C, and specific surface area of 300 m2g-1 on synthetic zeolite ZSM-5 catalyst by a fixed-bed
reactor. Structure and morphology of the synthesized catalyst were investigated by XRD, FT-IR, SEM, XRF and
BET analyses. The effect of CaCO3 and Na2 CO3 solutions used for catalyst modification on the distribution of
hydrocarbon products were studied and compared to ZSM-5 catalyst. The result of catalyst activity evaluation
tests shows that the modified catalyst with a 0.1 molar solution of CaCO3 and Na2 CO3 provides the highest
selectivity and efficiency compared to the hydrocarbons in boiling point range of C6+ gasoline.
Keywords: modification of ZSM-5 catalyst, structure and morphology, Methanol to Gasoline
DOI: 10.1515/ijcre-2017-0229
Received: November 26, 2017; Revised: January 14, 2018; Accepted: March 12, 2018

1 Introduction
The evidence indicates that the limited petroleum resources are not able to supply global energy demands.
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The general fuel consumption is about 133 million tons per day which are being increased with a growth of
higher than 3 %. Given this consumption rate, it will reach 162 million tons per day in 2020 (Mena Subiranas
and Schaub 2007; Hagey and de Lasa 2004; Ferreira, Al-Bogami, and de Lasa 2015; Sengupta, Ghosal, and Basu
2012). Conventional methods for gasoline production typically include distillation of crude oil and processes
such as alkylation, isomerization, and catalytic cracking. However, fuel production by coal (coal to liquid) is
also attracted by some countries with coal resources. Given the critical importance and urgent need of the fuel
as well as increased demand for fuel, some alternative methods should be sought. Methanol to Gasoline (MTG)
process that is a part of general Gas to Liquid process, is a suitable alternative process which recently has been
considerably paid attention to. MTG process was used for the first time in the 1970s by petroleum research
group of Mobil Co (Aghaei and Haghighi 2014; Amereh, Haghighi, and Estifaee 2018; Estifaee et al. 2014; Ra-
hemi et al. 2014). Since the late 1970s, plenty of studies has been conducted in the process. In 1982, production
of aromatics, light olefins and gasoline through methanol was studied on ZSM-5 catalyst (Svelle et al. 2006; Tes-
sonnier et al. 2008). Inui (1984) studied the relationship between the acidic characteristic of ZSM-5 catalyst and
catalyst performance in MTG process (Zhang et al. 2014). Production of fuel and other chemical compounds
through methanol by ZSM-5 catalyst was also investigated (Bjorgen et al. 2007). Joensen et al. studied the appli-
cation of soda for ZSM-5 catalyst modification in MTG reaction (Fellah and Onal 2011). The effect of acids on the
performance of MTG process catalysts and impact of phosphoric acid on acidic sites of ZSM-5 catalyst was spec-
ified (Rownaghi and Hedlund 2011). Rownaghi et al. examined the efficiency of hydrocarbons within gasoline
boiling point range and impact of ZSM-5 catalyst crystals size on the efficiency of the products (Bi et al. 2014).
The studies conducted so far include assessment of the process and catalysts as well as their modification and
optimization of operational conditions for doing MTG reactions. Among zeolite catalysts, ZSM-5 and SAPO-
34 are suitable to conduct the process reactions and were further studied. The main mechanism recognized
Mahmoud Salimi is the corresponding author.
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for MTG process includes equilibrium reaction of methanol dehydration to dimethyl ether after which light
olefins (e. g., ethylene and propylene) are produced by rehydrating dimethyl ether. These olefins are converted
to hydrocarbons inside the pores and then the greater hydrocarbons and such aromatics as Xylene, Toluene and
Benzene are produced (Du et al. 2014; Liu et al. 2015; Vo et al. 2012; Yan and Le Van Mao 2010; Al-Yassir and Le
Van Mao 2006; Li et al. 2007; Gregg and Sing 1982; 1967; Sing 1985; Shirazi and Jamshidi 2008; Fathi, Sohrabi,
and Falamaki 2014; Zaidi and Pant 2004; Kianfar et al. 2017). The present study employed ZSM-5 catalyst as
the base catalyst whose structure was modified for the accomplishment of MTG reactions. Performance of the
catalysts derived from the fixed-bed reactor was investigated and production of diverse hydrocarbons by them
was approved. The effect of the concentration of calcium carbonate (CaCO3 ) and sodium carbonate (Na2 CO3 )
solutions for modification of catalyst on conversion rate and efficiency of the hydrocarbons in gasoline boiling
point range was determined and compared to the conventional ZSM-5 catalyst. The modified ZSM-5 catalyst
with CaCO3 and Na2 CO3 solution leads to decrease Si/A1 ratio, namely, CaCO3 and Na2 CO3 solution cause to
remove Si from the catalyst structure. This is used due to the alkali properties of the solution which is able to
partly solve silicon catalyst structure and remove it. Moreover, with increased CaCO3 and Na2 CO3 concentra-
tion, Si/Al would be decreased in the catalyst which is a factor to increase heavier hydrocarbons production.
However, with decreased Si/Al, the specific surface of catalyst will also be decreased. The cause of specific
surface reduction following the increased concentration of CaCO3 and Na2 CO3 may be catalyst pores blockage
by deposits of CaCO3 and Na2 CO3.

2 Materials and methods

For modification of zeolite ZSM-5 catalyst, 30 ml of 0.05 and 0.1 molar solution of calcium carbonate (CaCO3 )
or sodium carbonate (Na2 CO3 ) (per 3 g of catalyst) was added to zeolite ZSM-5 catalyst and was completely
mixed for 3 h at a temperature of 70 °C. Then, the solution was separated from the catalyst by evaporation
under vacuum and the solid sample was dried in an oven. This operation was carried out once more and after
drying the catalyst, final acidification operation was also redone by ammonium nitrate solution (NH4 NO3 ).
Since some of the H+ s may have been missed while contact of catalyst to the solution of calcium carbonate
(CaCO3 ) and sodium carbonate (Na2 CO3 ), re-acidification may bring back them. Finally, calcination process
was carried for 3 h at a temperature of 550 °C. The obtained catalysts are named according to concentration of
solution of calcium carbonate CaCO3 and sodium carbonate Na2 CO3 and ion exchange in such a way that Z-0.05
is a catalyst modified by 0.05 molar solution of calcium carbonate CaCO3 and sodium carbonate Na2 CO3 and
Z-0.1 is the one modified by 0.1 molar solution of calcium carbonate CaCO3 and sodium carbonate Na2 CO3 .
Details on the reactor test characteristic methods are reported elsewhere.
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2.1 Experimental setup

Efficiency and stability in a specific reaction are of the most important criteria for catalyst selection. In this
regard, MTG reaction was simulated in a fixed-bed reactor to evaluate reactive performance of the generated
catalyst. Figure 1 shows a schema of the relevant experimental system.

Figure 1: Scheme of the reactor, and testing and analysis system.

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3 Results and discussion

3.1 XRD analysis

Figure 2 indicates the spectra associated with XRD analysis for Zeolite ZSM-5. The relative crystalline mode of
this catalyst was calculated according to a reference, considering prominent peaks within angles of 22–25°.

Figure 2: XRD pattern and results for ZSM-5 and modified catalysts.

3.2 FT-IR analysis

Figure 3 shows FT-IR spectroscopy analysis for ZSM-5 sample. Generally, in FT-IR spectrum of zeolites two
type of peaks are observed. One is dedicated to internal vibrations of TO4 in which T are the elements inside
the zeolite structure (e. g. Si and Al) which are linked to oxygen. Such peaks are typically in the range of 950–
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1250 cm−1 and 420–500 cm−1 which are attributed to T-O and O-T-O stretching vibrations, respectively. Other
one is the vibrations associated with tetrahedral connections. These peaks are appeared in the range of 500–
600 cm−1 and 1300–1700 cm−1 .

Figure 3: FT-IR results and analysis pattern for ZSM-5 and modified catalysts.

3.3 SEM analysis

Figure 4 shows SEM analysis results for a calcined catalyst which were photographed. As it can be seen from
micrograph, the sample crystals have a suitable dispersion and regular morphology.

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Figure 4: SEM images of ZSM-5 and modified catalysts with various percentage of CaCO3 and Na2 CO3 .

3.4 BET-XRF- NH3-TPD analysis results

Table 1 report physical and chemical characteristics of ZSM-5 using BET, XRF, NH3 -TPD analyses. Acidity of
Zeolite ZSM-5 linearly depends on concentration of aluminum at composition of the zeolite. Results of NH3 -
TPD analysis are compatible with the presence of aluminum at composition of zeolite.

Table 1: Results of surface area, Si/Al, Temperature programmed desorption, pore volume of various modified catalysts.
Catalysts SiO2/Al2O3 Si/Al BET Pore vol- NH3 capac-
surface ume(cm3/g) ity(mmol/g)
area(m2/g)
ZSM-5 30 15 300 0.379 0.8594
ZSM-5/CaCO3 (Z-0.05) 22 11 290 0.273 0.7058
ZSM-5/CaCO3 (Z-0.1) 20 10 284 0.177 0.7287
ZSM-5/Na2 CO3 (Z-0.05) 24 12 290 0.273 0.7428
ZSM-5/Na2 CO3 (Z-0.1) 22 11 292 0.281 0.7587
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Given the BET analysis results, the specific surface of calcium carbonate with the increased concentration of
calcium carbonate from 0 to 0.1 % while the total volume of pores was decreased from 0.379 to 0.177 cm3/g with
increased calcium carbonate from 0 to 0.1 %. Also, specific surface of catalyst ZSM-5/Na2 CO3 with increased
sodium carbonate from 0 to 0.1 %, initially decreased concentration of 0.05 % solution of sodium carbonate
and then increased 0.1 % sodium carbonate solution. In addition, volume of pores with increased amount of
sodium carbonate from 0 to 0.1 %, initially decreased concentration of 0.05 % solution of sodium carbonate and
then increased 0.1 % sodium carbonate solution. Temperature Programmed Desorption analysis with ammonia
(NH3 -TPD) was used to specify acidity of catalyst sample. Results of these analyses are presented in Table 1.
Acidity of Zeolite ZSM-5 linearly depends on concentration of aluminum at composition of the zeolite. Results
of NH3 -TPD analysis are compatible with presence of aluminum at composition of zeolite. Given the results,
acidity distribution approaches the sites with medium acidity (peak in a temperature of 400 °C) by adding
improver CaCO3 and Na2 CO3 . Accordingly, the rate of high-acidity sites (peak in a temperature of 400 °C) and
poor-acidity ones (peak in a temperature of about 200°C) was decreased (Sing).

3.5 Evaluation of modified calcium carbonate and sodium carbonate catalyst to convert methanol to
gasoline

As shown in Table 1, modified ZSM-5 catalyst with CaCO3 and Na2 CO3 solution leads to decrease Si/A1 ratio,
namely, CaCO3 and Na2 CO3 solution causes to remove Si from the catalyst structure. This is used due to the
alkali properties of the solution which is able to partly solve silicon of catalyst structure and remove it (Fathi,
Sohrabi, and Falamaki 2014; Shirazi and Jamshidi 2008). Moreover, with increased CaCO3 and Na2 CO3 concen-
tration, Si/Al would be decreased in the catalyst which is a factor to increase heavier hydrocarbons production.
However, with decreased Si/Al, the specific surface of catalyst will also be decreased. The cause of specific sur-

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 DE GRUYTER Kianfar et al.

face reduction following the increased concentration of CaCO3 and Na2 CO3 may be catalyst pores blockage by
deposits of CaCO3 and Na2 CO3 . Therefore, it makes sense to use a concentration which optimises these two
acidity increase factors along with decreased specific surface in order to produce the desired product. Figure 5,
Figure 6 and Table 2 present methanol conversion rates for diverse catalysts. Table 1 and Table 2 show that de-
creased Si/Al gives rise to relatively increase methanol conversion rate. Figure 5, Figure 6 and Table 2 indicate
the efficiency of the produced hydrocarbons within C6+ gasoline boiling point range among diverse catalyst
samples. Efficiency is more frequently seen in Z-0.1 sample compared to additional catalysts. This can be at-
tributed to the higher acidity of such a catalyst which leads to boost accomplishing oligomerization reactions.
Hence, the Z-0.1 catalyst was considered and studied under more experiments. The rate of the hydrocarbons
produced by catalyst Z-0.1 within C6+ gasoline boiling point range is higher than additional hydrocarbons. As
pointed out, the reason for the increased production of heavier hydrocarbons is the increased acidity of the
catalyst that results from the decreased Si/Al which leads to increase oligomerization reactions and produc-
tion of heavy hydrocarbons. The studies show that performance of modified catalyst was enhanced with alkali
solution for BTX production compared to the initial catalyst. The authors believe that Meso pores structure in
the Z-0.1 catalyst is the main cause of such behaviour (Zaidi and Pant 2004). Accordingly, given BET analysis
results, the contribution of Meso pores was relatively increased in this sample of the catalyst. The produced
BTXs are valuable with a high octane number. In some cases, BTX is separated from the products and is used
as the feed of petrochemical plants.

Figure 5: Products distribution on the catalysts surface for MTG reactions with consideration of CaCO3 .
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Figure 6: Products distribution on the catalysts surface for MTG reactions with consideration of Na2 CO3 .

Table 2: Distribution of hydrocarbons in synthesized gasoline.

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Catalysts Conversion CH4 C2 H4 C2 H6 C3 H6 C3 H8 i-C5 n-C5 C6+ -

(%) C7+ -
C8+
ZSM-5 99.5 4 % 20 % 3 % 21 % 15 % 13 % 3 % 20.5 %
ZSM-5/(0.05) CaCO3 84 3 % 17 % 1 % 35 % 2 % 8 % 3 % 15 %
ZSM-5/(0.1) CaCO3 99.65 7 % 18 % 2 % 20 % 5 % 5 % 4 % 38.65 %
ZSM-5/(0.05) Na2 CO3 79 3 % 16 % 1 % 35 % 2 % 8 % 3 % 11 %
ZSM-5/(0.1) Na2 CO3 99.8 6.90 % 17.95 % 2.70 % 19.80 % 4.93 % 4.97 % 3.95 % 38.6 %

4 Conclusion
ZSM-5 catalyst is used to carry out Methanol to Gasoline process reactions. Since the increased acidity of the
catalyst results in the increased oligomerization reactions and production of heavy hydrocarbons, the ZSM-
5 catalyst is applied with carbonate calcium and sodium carbonate solutions which provide alkali properties
to partly remove the silicones existing in catalyst structure. Results indicate that decrease of Si/Al affects the
catalyst performance and C6+ heavy hydrocarbons production was significantly increased. The results analysis
shows that Z-0.1 catalyst has a better performance to produce hydrocarbons with in C6+ gasoline boiling point
range.

NOMENCLATURE
T: temperature [°C]
id: internal diameter [mm]
FA0: molar flowrate of methanol [cc/min]
W: weight of catalyst [g]

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