Final Review

SYNTHESIS AND
CHARACTERIZATION OF
FISCHER TROPSCH REACTION
CATALYST(Fe / Mn / Al2O3)
GUIDED BY
Mr. ARUL JAYAN.M
ASST.PROFESSOR,SATHYABAMA
UNIVERSITY
CHENNAI.
NIKHIL RAJ.T R(3219167)
VARUN PAUL P(3219226)
DEPT.OF CHEMICAL ENGINEERING
SATHYABAMA UNIVERSITY,CHENNAI.
OUTLINE
 Aim
 Objective
 Introduction
 Work Plan
 Results and discussion
 References
AIM
 synthesis and characterization of Fischer

Tropsch reaction (Fe/ Mn /Al2O3) catalyst
for the conversion of syngas to hydro
carbons.
OBJECTIVE
 Developing a high temperature withstanding
iron catalyst in porous form.
 Understanding the impact of support on the

catalyst
 conversion rate of carbon monoxide to

hydrocarbons using promoted catalyst
INTRODUCTION
 F-T process is a set of chemical reactions that

converts syngas(CO+H2) to liquid hydrocarbons.
(2n+1)H2+ n CO C n H(2n+2)+ n H2O
 most of alkanes formed tend to diesel fuel &

small amount of alkenes provide alcohols and
other oxygenated hydrocarbons
WORK PLAN
Catalyst Synthesis
Most commonly used catalyst’s are ;
Iron (Fe) , Cobalt (CO), Nickel(Ni) , Ruthenium (Ru)
Catalyst Cost Basis Curve

CATALYST PREPARATION TECHNIQUES
 Impregnation
 Co-precipitation
 Sol-gel
Why we choose iron (Fe)… ?
 Low Cost
 Methane production can be reduced
 Able to generate high chain hydrocarbons
(diesel & waxes)
 High activity and attain stability
IMPREGNATION TECHNIQUE
 Contacting the support (Al2O3) with the
impregnating solution precursor.
 Drying the support to remove the imbibed liquid.
 Thermal decomposition, followed by activating the
catalyst by reduction or other appropriate
treatment like calcinations.

PROCESS FLOW SHEET
Remnants
Fe(No3)2 Al2O3 Heat 1000 C of Fe(No3)2
aqueous aqueous up to 14 + Mno2
solution + solution hours, aqueous
Mno2 aqueous magnetic solution
solution stirrer
Paste form
Keep it for dried at
Calcination 24hours at 120˚C, hot
Fe/ Mn /Al2O3 5000 C
catalyst room air oven
temp. for 12
hours
METHOD OF PREPARATION
 Prepare Fe(No3)2 (catalyst), Mno2 (promoter),
Al2O3 (support) to 100 ml water.
 Mix 80 ml Fe(No3)2 solution & 80 ml Mno2 solution to
100 ml Al2O3 support.
 Heat it for 14 hours at 1000C In Magnetic stirrer until
solution becomes saturated.
 Add 20 ml Remnants to the above remaining
solution
• Heat it again and make it into saturated

form
 Make it into paste form by keeping it in a Hot air
oven for 12 hours at 120oC
 Keep it at room temperature for 24 hours
 For further activation keep it in muffler furnace at 500oC
For 6 hours
 Fe/ Mn /Al2O3 catalyst is obtained in powdered form.
CHARACTERIZATION
TECHNIQUES
o X ray diffraction ( XRD )
o Thermo gravimetric analysis (TGA)
o Scanning electron microscope (SEM)
with eds
o Brunauer-Emmett-Teller (BET) Analysis

RESULTS AND DISCUSSION
X ray diffraction ( XRD )

 X-ray diffraction provide structural information, interatomic
distances and bond angles
 The XRD analyses were conducted on catalyst ,The highest

intensity peaks corresponds to Mno2(corundum) , Iron (
hematite ) & Al2O3 (Pyrolusite)
 From the XRD analysis it was inferred hematite that is cubic

and Al2O3 is orthorhombic and Mno2 is monoclinic
XRD PLOT
TGA PLOT
TGA(THERMO GRAVIMETRIC
ANALYSIS )
 Thermal analysis in which changes in physical and
chemical properties of materials are measured as a
function of increasing temperature
 A 6.950 mg sample of iron catalyst was analysed.
 Temperature Program = 30.00°C to 800.00°C at
20.00°C/min in Nitrogen atmosphere with a purge rate
of 20 mL/minute
 it is observed that there is only removal of adsorbed
water till 60°C & from 60°C to 615°C decomposition
of 0.67 mg occurs
 From 615oC to 650oC there is decomposition of MnO2

to Mn2O3 and Fe3O4 to Fe where having weight loss of
0.15 mg
 It is inferred from the analysis that the catalyst is

withstanding up to a temperature of 650oC.
Scanning electron microscope (SEM)
 Scanning electron microscopy with energy dispersive X-ray
spectroscopy (SEM/EDX) is the best known and most
widely-used of the surface analytical techniques
 High resolution images of surface topography, with

excellent depth of field, are produced using a highly-
focused, scanning (primary) electron beam
 The material morphology and elemental composition

analysis was performed with a Carl-Zeisis Supra-55
Scanning Electron Microscope equipped with an energy-
dispersive x-ray spectrometer.
SEM IMAGE
Sem under
Magnification
SEM WITH EDS
Brunauer-Emmett-Teller (BET)
Analysis
B E T S u r f a c e A re a P l o t
SURFACE AREA
 single point surface area at p/p0 = 0.300568810:
52.3674m2/g
 Bet surface area: 53.6636 m2/g
PORE VOLUME
 Single point adsorption total pore volume of pores less
than 2436.781 Å diameter at P/Po = 0.992011640: 0.116867
cm³/g
PORE SIZE
 Adsorption average pore width (4V/A by BET): 87.1106Å
CATALYST ACTIVITY
TEMPERATURE PROGRAMMED REDUCTION
o It’s a technique used in the field of heterogeneous
catalysis to find the most efficient reduction
conditions
o A simple container (U-tube) is filled with a solid or
catalyst is positioned in a furnace with temperature
control equipment
o A thermocouple is placed in the solid for
temperature measurement
 Temperature-programmed reduction using both
carbon monoxide (CO-TPR) and hydrogen (H2-
TPR) was used
 The sample in the oven is heated up on

predefined values. Heating values are usually
between 1 K/min and 20K/min
 A phase change occurs to the Fe2O3 to Fe3O4 .

REFERENCES
 Using different preparation methods to enhance fischer-tropsch products
over iron-based catalyst
(M. Sarkaria,b, F. Fazlollahib, H. Atashic, A. A. Mirzaeid, and W. C. Heckerb)
 Study of an iron-manganese fischer–tropsch synthesis catalyst promoted with

copper ( cheng-hua zhang a,b, yong yang A, bo- tao tenga, ting- zhen li A,
hong- yan zhenga,hong-wei xiang A, yong-wang li )
 Activation pressure studies with an iron-based catalyst for slurry fischer-

tropsch synthesis (Qinglan hao,liang bai, hongwei xiang, yong wang li) 10 june
2009
 Short history and present trends of fischer–tropsch synthesis (hans schulz)
 Highly selective iron based fischer tropsch catalyst activated by co2 containing
syngas ,(dong hyun chun, ji chan park, seok yong hong ) 9 june 2014
THANK YOU

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SYNTHESIS AND

 synthesis and characterization of Fischer

 Understanding the impact of support on the

 conversion rate of carbon monoxide to

 F-T process is a set of chemical reactions that

(2n+1)H2+ n CO C n H(2n+2)+ n H2O

 most of alkanes formed tend to diesel fuel &

Catalyst Cost Basis Curve

 Contacting the support (Al2O3) with the

impregnating solution precursor.

 Drying the support to remove the imbibed liquid.

 Thermal decomposition, followed by activating the

catalyst by reduction or other appropriate

treatment like calcinations.

• Heat it again and make it into saturated

o X ray diffraction ( XRD )

o Thermo gravimetric analysis (TGA)

o Scanning electron microscope (SEM)

o Brunauer-Emmett-Teller (BET) Analysis

X ray diffraction ( XRD )

 The XRD analyses were conducted on catalyst ,The highest

 From the XRD analysis it was inferred hematite that is cubic

 Thermal analysis in which changes in physical and

chemical properties of materials are measured as a

function of increasing temperature

 A 6.950 mg sample of iron catalyst was analysed.

 Temperature Program = 30.00°C to 800.00°C at

20.00°C/min in Nitrogen atmosphere with a purge rate

 From 615oC to 650oC there is decomposition of MnO2

 It is inferred from the analysis that the catalyst is

 High resolution images of surface topography, with

 The material morphology and elemental composition

 The sample in the oven is heated up on

 A phase change occurs to the Fe2O3 to Fe3O4 .

 Study of an iron-manganese fischer–tropsch synthesis catalyst promoted with

 Activation pressure studies with an iron-based catalyst for slurry fischer-

 Short history and present trends of fischer–tropsch synthesis (hans schulz)

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