Available online at http://ijcpe.uobaghdad.edu.iq and www.iasj.net

Iraqi Journal of Chemical and Petroleum
Engineering

Vol.20 No.4 (December 2019) 61 – 66
EISSN: 2618-0707, PISSN: 1997-4884

Corresponding Authors: Name: Halah M. Hussain , Email: Hala_muhammed@gmail.com , Name: Abdulhaleem A.K. Mohammed, Email:

prof.abdullhaleem@gmail.com
IJCPE is licensed under a Creative Commons Attribution-NonCommercial 4.0 International License.

Experimental Study of Iraqi Light Naphtha Isomerization over

Ni-Pt/H-Mordenite

Halah M. Hussain and Abdulhaleem A.K. Mohammed

Alfaraby University College / Baghdad-Iraq

Abstract

Hydroisomerization of Iraqi light naphtha was studied on prepared Ni-Pt/H-mordenite catalyst at a temperature range of 220-

300°C, hydrogen to hydrocarbon molar ratio of 3.7, liquid hourly space velocity (LHSV) 1 hr
-1

and at atmospheric pressure.

The result shows that the hydrisomerization of light naphtha increases with the increase in reaction temperature at constant LHSV.

However, above 270
0
C the isomers formation decreases and the reaction is shifted towards the hydrocracking reaction, a higher

octane number of naphtha was formed at 270 °C.

Keywords: Iraqi light naphtha isomerization, Nickel-Platinum over H-mordenite.

Received on 09/02/2019, Accepted on 03/04/2019, published on 30/12/1029

https://doi.org/10.31699/IJCPE.2019.4.10

1- Introduction

The utilization of an upgraded low-value refinery

stream to the gasoline pool might present a solution to the

problem, as it can considerably lower the cost of gasoline

production, while loses only some of its original quality,

but still remains environmentally friendly. The use of

bifunctional zeolite catalysts specifically designed to

enhance the octane number of light nuphtha through the

hydroisomerization process has already been

marketed.[1].

However, this application has not yet been

commercially extended to include the treatment of heavy

naphtha, which usually contains normal alkanes from the

Heptane range to Decane [2].

Isomerization, cracking and alkylation are acid-induced

reactions. The catalyzad hydrocarbon reactions are of

great importance nowadays and it is not surprising that

many studies have been devoted to this subject. However,

important questions remain regarding the mechanism and

effect of catalytic pore structure on the activity and

selectivity to answer. [3].

Isomerization of n-paraffin to branched paraffin is

important in petroleum refining industry for improving

motor fuels properties such as high gasoline octane

number [4], diesel fuel with high cetane number, low pour

point and high viscosity index. To accomplish high

isomerization selectivity; balance between the active

component (metal) and acid functions is needed [5].

More studies about isomerization to produce high

quality gasoline such as Vaudagna, [6] indicated that

loading of Pt on WO3/ZrO2 have positive effect on the

rate and selectivity of alkanes isomerisation in the

presence of hydrogen.

The Pt metal was impregnated into the WO3/ZrO2, so

that the catalysts contain 0.4wt. % of Pt and the Pt/

WO3/ZrO2 calcined to a temperature of 830
0
C (at 20 C

min
-1

) for 3 hours. The specific surface area was found to

increase to more than 350m
2
/g.

Al-Hassany M. [7] studied that Light naphtha treatment

achieved over 0.3wt%Pt loaded-alumina, HY-zeolite and

Zr/W/HY-zeolite catalysts at temperature range of 240-

370 °C, hydrogen to hydrocarbon mole ratio of 1-4 with

liquid hourly space velocity (LHSV) 0.75-3 hr
-1

, and at

atmospheric pressure. Results showed that Pt/Zr/W/HY is

the best catalyst for producing isoparffines due to its

higher acidity compared with Pt/HY. The Pt/Zr/W/HY

catalyst showed lower activity for aromatization of

naphtha to cyclopareffins and benzene selectivity than

Pt/HY.

A smaller pore volume leads to lower aromatization

activity and higher isomerization and cracking activity.

The maximum isoparaffins extent was achieved and

reached 78% at 300 °C and LHSV of 0.75 hr
-1

Pt/Zr/HY and aromatics extent was reached 10% at 370

°C and LHSV of 0.75 hr
-1

on Pt/ HY.

Al-Saraj M A A. et al. [8] studied light naphtha

isomerization over 0.3wt. % Pt / HMOR was the catalyst.

The operating condition was performed for all

temperature experiments from 200 to 350 ° C, pressure -

range from 3 to 15 bar, LHSV - range from 0.5-2.5hr
-1

and from hydrogen to naphtha - a ratio of 300. The results

show that the isomerization of the Iraqi light naphtha

increases with increasing reaction temperature and

decreases with an increase in LHSV. High research

octane number (93)was formed at 240 ° C.

https://doi.org/10.31699/IJCPE.2019.4.10

H. M. Hussain and A. A.K. Mohammed / Iraqi Journal of Chemical and Petroleum Engineering 20,4 (2019) 61 - 66

In this work the catalytic activity of the promoted

prepared catalyst (Pt-Ni/H-mordenite) using light naphtha

isomerization was studied at different operating

conditions and the chemical composition of produced

gasoline using PONA analysis was determined.

2- Experimental Work

2.1. Materials

a. Feedstock

Iraqi light naphtha supplied from Al-Dora Refinery was

used as a feedstock in hydroisomerization experiments.

The physical properties and PONA analysis of Iraqi light

naphtha are listed in Table 1.

Table 1. Physical Properties and PONA analysis of Iraqi

light naphtha

Physical proprties value

Specific gravity at 60
0
/60

0
F 0.6631

API gravity 80.6

Kinematic viscosity at 25
0
C, m

2
/s 7.2*10

-7

Research Octane number 60

Sulfur content ppm 1.5

Chemical Composition Wt.%

n-Paraffin 42.9

i-Paraffin 42.1

Olefin 0.3

Naphthene 9.1

Aromatic 5

b. Chemicals

The chemicals used for experimental work are tabulated

in Table 2.

Table 2. The chemicals used for experimental work
Chemical Source(company) Purity

Sodium Hydroxide Alpha Chemika 99%

Sulfuric Acid Sigma Aldrich 98%

Sodium aluminate Sigma Aldrich 50-56%

Ammonium
Chloride

BDH Limited Pool,
England

99%

Nickel nitrate Himedia, India 97%

Cloro platinic acid Sigma Aldrich 40%

Hydrogen gas Al-Dura Power station 99%

Nitrogen gas Al-Khalej Plant 99%

2.2. Synthesis of Na-mordenite (Na-MOR)

Na-MOR was synthesized from nano-silica. 38. 90 g of

NaOH was dissolved in 249.3 ml of water and then

divided into two equal portions. In one portion, 5.56 g of

nano-silica was completely dissolved. To the other

portion, 10.19 g of NaAlO2 was added to prepare a clear

aluminate solution. Then the silicate solution was slowly

poured into the aluminate solution with vigorous stirring,

and a homogenous gel resulted.

The resultant gel was stored in a water bath at room

temperature (T =25 ± 2°C), in a sealed poly tetra fluoro

ethylene (PTFE) bottle under stirrer at 250 rpm for 3 days

at pH 14. The solid product was separated by filtration

(Whatman No. 41 filter paper) using a Buckner funnel

with the aid of a vacuum pump, then washed more times

by distilled water until the pH value dropped to 8.69. The

product was left at room temperature overnight, dried at

110°C for 2 hr and calcined at 400
0
C for 2 hr. [9].

2.3. Synthesis of H-mordenite (H-MOR)

The hydrogen form of zeolite H-MOR was obtained

from Na-MOR exchange with a solution of 4 N NH4Cl.

Zeolite Na-MOR was slurred in an ammonium chloride

solutions with mixing at 70
o
C for 2 hr and then left at

room temperature overnight for ion exchange completion.

After that the exchanged zeolite was filtered off, washed

with distilled water. The product was left at room

temperature overnight, dried at 110
0
C for 2 hr and

calcined at 400
0
C for 2 hr. [10]

2.4. Preparation of Ni-Pt/H-MOR by impregnation

method

100g of H-MOR-zeolite as a powder was mixed with 10

wt. % bentonite clay as binder. The resulting mixture was

mixed with water to form a paste. Extrudates with 3-7

mm were formulated and dried over night at 110
º
C and

then calcined at 400
0
C for 2 hr.

To prepare 0.15wt % of Pt on 50 g of H-MOR pellets

the carrier catalyst H-MOR was dried at 110
º
C with air

for two hours and placed in impregnation under vacuum,

then the solution of chloroplatinic acid (0.205 g H2PtCl6

and 30 ml deionized water) was added drop by drop under

magnetic stirring then the vacuum cut off and the sample

left under mixing for about 2 hr to have a homogenous

distribution of metal precursors. The product was slurry

filter washed with distilled water, dried at 110
o
C

overnight and calcined at 400
o
C for two hours at a rate of

2ºC /min [11]. After calcination the catalyst was reduced

by hydrogen at 350
º
C for 3 hours. For preoare Ni-Pt/H-

MOR catalyst containing 0.215 wt. % of Ni, 50 g of Pt/H-

MOR was impregnated with 0.2 M Ni (NO3)2.2H2O

aqueous solution at 40
0
C for 2 hours. The obtained

filtrated, dried and calcined at 400
0
C for 2 hours.

2.5. Catalytic Activity Test

The catalytic activity test was achieved in a continuous

flow at fixed-bed reactor. Figure 1 shows the process flow

diagram of unit. 30 g Ni-Pt/H-MOR was charged to the

reactor between two layers of inert ceramic particles. The

platinum containing catalyst was reduced with H2 at

350°C for 3 hr.

The catalytic reaction was carried out with LHSV of 1

hr
-1

, at temperature range of 220-300°C, hydrogen to feed

mole ratio of 3.7 and at atmospheric pressure.

The reactor was flushed with nitrogen to purge the air

from the system.

H. M. Hussain and A. A.K. Mohammed / Iraqi Journal of Chemical and Petroleum Engineering 20,4 (2019) 61 - 66

Meanwhile, the reactor is heated to the desired

temperature. After reaching the reaction temperature, the

nitrogen valve was closed.

A pre-specified flow rate of light naphtha was set on.

Vaporization of the feed occurs in the evaporator.

The vapor of light naphtha was mixed with specified

flow rate of hydrogen in the mixing section. The mixture

entered the reactor from the top, and reacted on the

surface of catalyst. The final condensed product was

collected only after steady state operation was established

while initial products were discarded.

Fig. 1. Process flow diagram of the catalytic experimental

unit

3- Results and Discussion

3.1 Characterization of Na-MOR and H-MOR.

a. XRD Analysis

Fig. 2 shows that the X-ray diffraction patterns of

synthesized Na-MOR. These crystal was similar to that

obtained by R. Szostak [12] and M. Mohamed et al, [13].

This means that the synthesized sample is Na-MOR

crystals.

Fig. 2. X-ray powder pattern of prepared Na-MOR zeolite

The exchange technique was used in this work is one

step impregnation under a constant temperature to convert

Na-MOR zeolite to H-MOR zeolite. Fig. 3, illustrates the

XRD patterns of the synthesized zeolite H-MOR. XRD

phase is found to match with the show peaks at 2θ = 6.57,

9.77, 19.65, 22.36, 25.72 and 26.36. These peaks are

characteristic for H-MOR zeolite. It can be seen from

Figure 4, that the synthesized sample showed the

formation of H-MOR phase [13]. The relative crystnality

of H-MOR was calculated by equation 1 and it was 118

Relative crystnality of zeolite= Sx/Sy *100 (1)

Where:

Sx = sum of integral peak intensities for the prepared

catalyst.

Sy = sum of integral peak intensities for the standard

catalyst.

Fig. 3. X-ray powder pattern of prepared H-MOR zeolite

b. Surface Area and Pore Distribution Analysis

H-MOR was characterized using N2 sorption to

determine their surface area and pore volume. Surface

area and pore volume depend mainly on the structure of

the solid. It was found that the BET surface area and pore

size of H-MOR were 336.7 m
2
/g and 2.49 nm,

respectively. The surface area obtained in this work was

higher than those obtained by Hisham M. et al, (52.14

m
2
/g) [14] and Heman et al, (254.38 m

2
/g) [15].

3.2. Isomerization Conversion

Isomerization conversion was determined by equation 2,

while percentage decreasing of naphthenic and aromatic

calculation by equation 3.

* 100% (2)

* 100% (3)

200

400

600

800

1000

1200

1400

1600

5 10 15 20 25 30 35 40 45 50 55 60

IN
T

E
N

C
IT

2 THETA

H. M. Hussain and A. A.K. Mohammed / Iraqi Journal of Chemical and Petroleum Engineering 20,4 (2019) 61 - 66

Table 3 shows the chemical composition of produced

gasoline using PONA analysis in order to evaluate the

catalyst performance. The hydroconversion involves three

main reactions hydroisomerization, dealkylation and

hydrogenation.

Table 3. PONA analysis for isomerization of Iraqi light

naphtha at LHSV = 1 hr
-1

and different T
T

0
C

wt. %

220
0
C 240

0
C 270

0
C 300

0
C

n-paraffin 29.4 28.1 26.1 28

i-paraffin 57.2 62.7 65.2 62.7

Olefin - 0.2 0.2 0.2

Naphthen 8.7 5.8 5.4 5.8

Aromatic 4.7 3.2 3.1 3.3

Fig. 4 shows the effect of temperature on the

isomerization reaction.

The isomerization conversion, as shown in this figure,

increases with temperature increasing up to 270
0
C. This

is due to n-paraffin isomerization. This agrees with an

investigation reported by Mohammed et al, [8] and Maha

H. [7] obtained for hydroisomerization light naphtha

using Pt-Ni/H-mordenite.

Furthermore, the lower reaction temperature increases

the percentage of branch alkane at thermodynamic

equilibrium as mentioned by Fahim M A et al. [16].

Fig. 4. Effect of temperature on isomerizate conversion of

Iraqi light naphtha on Pt-Ni/H-mordenite catalyst at

LHSV = 1 hr
-1

Fig. 5 and Fig. 6 show the relationship between

percentage change of naphthene and aromatic with

temperature, respectively.

The increasing of temperature firstly, promote aromatic

hydrogenation to cyclo-paraffin and cyclo-paraffin

hydroisomerization to iso-paraffin and secondly, higher

temperature change the thermodynamic equilibrium

forward decreasing hydroisomerization as mentioned by

Al-Hassany M. [7] at different temperature 220-300
0
C ,

constant LHSV = 1 hr
-1

and H2/hydrocarbon mole ratio =

3.7

Fig. 5. Effect of temperature on naphthene percent

decreas of Iraqi light naphtha on Pt-Ni/H-mordenite

catalyst at LHSV = 1 hr
-1

Fig. 6. Effect of temperature on aromatic percent decrease

of Iraqi light naphtha on Pt-Ni/H-mordenite catalyst at

LHSV = 1 hr
-1

Fig. 7 shows the octane number of produced light

naphtha at different temperature. This figure shows that

the octane number of produced light naphtha

(isomerization) more higher than the light naphtha (RON

= 60) and the maximum octane number (92) obtained at

270
0
C. The isomeizate obtained at 270

0
C can be easy

used as high octane component for producer lead free

automobile gasoline.

Fig. 7. The highr of temperature on the RON at LHSV 1

hr
-1

200 220 240 260 280 300 320

Is
o

m
e

ri
za

te
C

o
n

ve
rs

io
n

t.
%

Temperature 0C

200 220 240 260 280 300 320

N
a

p
h

th
e

n
e

P
e

rc
e

n
t

d
e

cr
e

a
se

s
w

t.
%

Temperature 0C

200 220 240 260 280 300 320A
ro

m
a

ti
c

P
e

rc
e

n
t

d
e

cr
e

a
se

s
w

t.
%

Temperature 0C

200 250 300 350

R
O

Tempreature 0C

H. M. Hussain and A. A.K. Mohammed / Iraqi Journal of Chemical and Petroleum Engineering 20,4 (2019) 61 - 66

4- Conclusions

The prepared catalyst Ni-Pt/H-mordenite exhibits a high

hydroisomerization activity within the studied range of

operating conditions. The hydroisomerization reaction is

temperature dependent, and the lower temperature the

greater hydrosiomerization selectivity and in turn high

RON value. The isomerizate at 270
0
C and LHSV = 1 hr

-1

has RON = 92 and can be used as component for lead free

gasoline production.

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https://books.google.iq/books?hl=en&lr=&id=UcFsv1mMFHIC&oi=fnd&pg=PP1&dq=%5B16%5D%09Fahim,+Mohamed+A.,+Taher+A.+Al-Sahhaf,+and+Amal+Elkilani.+Fundamentals+of+petroleum+refining.+Elsevier,+2009.&ots=E1ath-yFrw&sig=OsClqaZMMrHbDWcfrXFbCiSSUI4&redir_esc=y#v=onepage&q=%5B16%5D%09Fahim%2C%20Mohamed%20A.%2C%20Taher%20A.%20Al-Sahhaf%2C%20and%20Amal%20Elkilani.%20Fundamentals%20of%20petroleum%20refining.%20Elsevier%2C%202009.&f=false
https://books.google.iq/books?hl=en&lr=&id=UcFsv1mMFHIC&oi=fnd&pg=PP1&dq=%5B16%5D%09Fahim,+Mohamed+A.,+Taher+A.+Al-Sahhaf,+and+Amal+Elkilani.+Fundamentals+of+petroleum+refining.+Elsevier,+2009.&ots=E1ath-yFrw&sig=OsClqaZMMrHbDWcfrXFbCiSSUI4&redir_esc=y#v=onepage&q=%5B16%5D%09Fahim%2C%20Mohamed%20A.%2C%20Taher%20A.%20Al-Sahhaf%2C%20and%20Amal%20Elkilani.%20Fundamentals%20of%20petroleum%20refining.%20Elsevier%2C%202009.&f=false
https://books.google.iq/books?hl=en&lr=&id=UcFsv1mMFHIC&oi=fnd&pg=PP1&dq=%5B16%5D%09Fahim,+Mohamed+A.,+Taher+A.+Al-Sahhaf,+and+Amal+Elkilani.+Fundamentals+of+petroleum+refining.+Elsevier,+2009.&ots=E1ath-yFrw&sig=OsClqaZMMrHbDWcfrXFbCiSSUI4&redir_esc=y#v=onepage&q=%5B16%5D%09Fahim%2C%20Mohamed%20A.%2C%20Taher%20A.%20Al-Sahhaf%2C%20and%20Amal%20Elkilani.%20Fundamentals%20of%20petroleum%20refining.%20Elsevier%2C%202009.&f=false

H. M. Hussain and A. A.K. Mohammed / Iraqi Journal of Chemical and Petroleum Engineering 20,4 (2019) 61 - 66

Ni-Pt / H-Mordenite دراسة عممية أليزوميتة النفتا العراقية الخفيفة عمى

محمد عبدالحميم عبدالكريم و حسين هالة محمد

العراق-بغداد-كمية الفارابي الجامعة

الخالصة
عند درجة حرارة Ni-Pt / H-mordeniteتمت دراسة عممية االزمرة من النفثا العراقية عمى محفزالمحضر

و في hr-1 1مع سرعة الفراغيه 3.3م ، نسبة الهيدروجين الى هيدروكاربون 0 322-222تتراوح بين
الضغط الجوي.

ثبوت السرعه ، في حين أن تكوين أظهرت النتائج ان تحول النفثا يزداد مع زيادة درجة حرارة التفاعل عند
ن. ارتفاع عدد األوكتين النفثا م ، يتم تحويل التفاعل نحو تفاعل التكسير بالهيدروجي0 232أيزومرات أعمى عند

.م0 232المتكون عند

.بالتينيوم عمى موردنايت-ه, نيكلأزمرة النفثا العراقية الخفيف: الدالةالكممات