Block diagram reduction techniques in control systems.ppt
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Studies of low temperature catalytic de-NOx emissions from lean burn engines
1. Presented by:
Kavaiya Ashish Rajeshkumar
(15042022)
Department Chemical Engineering & Technology
Indian Institute of Technology (BHU), Varanasi
U.P.-221005
âStudies of low temperature catalytic de-NOx
emissions from lean burn enginesâ
2. ďIntroduction
â˘Sources of Nox
â˘Effects of Nox
â˘Control Technologies for vehicular NOx
â˘Objectives
â˘Literature Review
ďExperimental Section
â˘Catalyst Preparation
â˘Experimental Setup
ďResults and Discussion
â˘Catalyst Activity Measurements
â˘Catalyst Characterization
ďConclusion
ďReference
ďAppendix
Outline
4. ďą Diesel engines are compression ignition
ďą Advantages:
ďź Fuel efficient
ďź High durability & reliability
ďź Low maintenance cost
ďź Low CO2 emission
ďą Disadvantages:
ďź High quantity of NOx and PM compared to gasoline (spark ignition) engines.
ďą NOx Constituents of ~ 95% NO, ~ 4.5% NO2 and very low N2O.
Diesel Particulate Filter (DPF) controls PM ~ 95% and diesel NOx
control is the major challenge. The challenges become more severe
during cold start of diesel exhausts. NOx can be separately controlled
by selective catalytic reduction (SCR).
5. Composition of Exhaust Gases in Diesel engines
Components Concentration
CO 100-1000 ppm
HC 50-500 ppm
NOx 30-1000 ppm
SOx
Proportional to fuel S
content
DPM 20-200 mg/m3
CO2 2-12 Vol %
6. Sources of NOx
ďNatural
â˘Marine Ecosystems
â˘Volcanoes
â˘Lightening and Fires
â˘Bacteria
ďAnthropogenic
â˘Highway Mobile Sources
â˘Non-Road Mobile Sources
⢠Industries
â˘Power Plants
Figure 1. Man- made sources of NOx
7. On Human Health
On
Environment
On
Vegetation
On
Material
Pulmonary fibrosis,
emphysema &
higher LRI
(lower respiratory tract
illness) in children
Aggravate existing
heart disease
Nose and eye
irritation
Pneumonia
Lung tissue damage
Pulmonary edema
(swelling)
Bronchitis Defense
mechanisms
Green House
Gas (N2O)
Acid Rain
Photochemical
Smog
PAN , PAH etc.
Vegetation
growth
reduction
Visible
Injury to
Leaves
Acidified
particle
deposition on
a surface
Discoloration
of wall &
ceiling of
monuments
Effects of NOx
Ground level
ozone
8. Emission Legislation of vehicular NOx
Year Reference
Light duty
Vehicles
(g/km)
Heavy duty
Vehicels
(g/kWh)
2000
Euro 1/I
India 2000 - 8.0
2005
Euro 2/II
Bharat Stage II - 7.0
2008
Euro 3/III
Bharat Stage III 0.50-0.78 5.0
2010
Euro 4/IV
Bharat Stage IV 0.25-0.33 3.5
2011 Euro 5/V 0.18-0.24 2.0
2014 Euro 6/VI 0.08 0.4
9.
10. Control Technologies for vehicular NOx
Pre-combustion
Fuel Treatment
Technologies
Post combustion
Exhaust Treatment
SCR Technology
Fuel Switching
Fuel Reforming NSCR Technology
EGR technology
Combustion
Modification
Dual Fueling
Low NOx burner
Staged Combustion
Reburning
Four Way Catalytic Systems
Three Way Catalytic Systems
NOx storage and Reduction
Simultaneous NOx & soot
Lean NOx Trap
13. ďTo develop the best possible low-cost and low-temperature active catalyst for the reduction
of NOx emissions using selective catalytic reduction (SCR) technology for diesel engines.
ďTo check the effect of different preparation methods on the activity of catalysts.
ďTo check the effect of doping of transition metal elements and 0.1% Rh doping on the
activity of catalysts.
ďTo check the effect of reducing agent on the activity of catalysts.
ďTo characterize the catalyst by various techniques: FTIR, XRD, BET, SEM, and EDX, etc.
ďTo evaluate the activity of various catalysts and find the most suitable for reduction of
NOx.
15. Sr.
No
Catalyst Preparation Method Exp. Conditions Catalyst Activity
% and Temp.
Author Year
NH3/Urea
1
Mn/TNT Alkaline Hydrothermal
Synthesis
Technique
900 ppm NO, 100 ppm NO2, 1000 ppm
NH3 and 10 vol.% O2 and ultra-high
purified helium (UHP helium
99.999%)
100-300 0C, 96-99 % Pappas et al
(2016) [1]
2 Fe-Cu-SSZ-13 Ion-exchange method 1000 ppm NO,1000 ppm NH3, 3% O2,
5% H2O (when used), and balance
with N2
95% NOx conversion ranges
from 150 to 450 âŚC
Zhang et al
(2015) [2]
3 NSUCH Fe-
ZSM-5)
Gel composition 600 ppm NO, 600 ppm NH3, and 6%
O2 in N2 balance.
100% NOx Conversion ranges
from 300 to 500 0C
Yan et al (2016)
[3]
4 Fe-containing
BEA zeolites
Ion exchange, post-
synthesis
[NO] = 0.1 vol.%, [NH3] = 0.1 vol.%,
[H2O] = 3.5 vol.%, [O2] = 8.0 vol.
higher temperature NO
conversion did not exceed 20%
JabĹoĹska et al
(2016) [4]
5 FeHBEA,
FeHZSM-5 and
FeHMOR
Ion Exchange and
Impregnation
procedures
[NO] = [NH3] = 0.25 vol.%, [O2] = 2.5
vol.% and [He] = 97 vol.%.
90% at temperature higher than
553 K.
Boron et al
(2015) [5]
6 MCM-41
modified with
iron
Template ion-exchange
(TIE) method.
[NO] = 0.25 vol.%, [NH3] = 0.25
vol.%, [O2] = 2.5 vol.% and
(b) in NH3-SCO: [NH3] = 0.5 vol.%,
[O2] = 2.5 vol.%, diluted in pure
helium
95 % conversation in the range
of 320- 350 0C
Kowalczyk et al
(2016) [6]
16. Sr.
No
Catalyst Preparation Method Exp. Conditions Catalyst Activity
% and Temp.
Author Year
7 CeO2âZrO2âWO3 Hydrothermal synthesis
method
0.06% NH3,0.06% NO, 5 vol.% O2,
and N2 as the balance gas
95% NOxconversion at 201â
459°C
Song et al (2016)
[7]
8 Fe/WO3âZrO2 Impregnation to
incipient wetness
12 mol% O2, 5% CO2, 10% H2O
(steam), 100 mol-ppm NH3and 100
ppm NO in nitrogen
90% NOx conversion at 350â
440°C
Foo et al (2016)
[8]
9 SBA-15 modified
with iron
Molecular designed
dispersion method and
ion-exchange method
[NO] = 0.25 vol.%, [NH3] = 0.25
vol.%, [O2] = 2.5 vol.% and [He] = 97
vol.%.
94% NOx conversion at 325â
400°C
Macina et al
(2016) [9]
10 CuâZeolite Commercial SDPF H2O = 5%(v/v), O2= 8%(v/v), NH3=
500 ppm NOx = 500 ppm
90% NOx conversion at 175â
350°C
Marchitti et al
(2016) [10]
11 VOx/CeO2 nanorod Impregnation method 100 mg of catalyst with 500 ppm NO,
500 ppmNH3, 3% O2, 5%H2O (when
used) and the balance was N2
V0.75Ce catalyst convert the
96% NOx at 225â350°C
Peng et al (2014)
[11]
12 WO3/CeOx-TiO2 Flame-spray synthesis 10 mg catalyst with 10 vol %,O2, 5 vol
% H2O, 1000 ppm of NO, 1200 ppm
of NH3 and
balance N2
99% NOx conversion at 350-
450 °C
Katarzyna et al
(2015) [12]
17. Sr.
No
Catalyst Preparation
Method
Exp. Conditions Catalyst Activity
% and Temp.
Author Year
13 MnâCeâTi Hydrothermal Method 500 ppm of NO, 500 ppm of NH3, 0
or 5% H2O, 0 or 50 ppm of SO2, 5%
O2, and helium as the balance gas
Mn0.2Ce0.1Ti0.7Ox catalyst
very active in the range of
150-350 0C with 85 %
conversation
Liu et al (2014)
[13]
14 CuCexZr1âx/TiO2 Wet
impregnation method
100 mg of catalyst with 500 ppm
NO, 500 ppm NH3, 3% O2, 5% H2O
(when used) and the balance was N2
More stable over
CuCe0.25Zr0.75/TiO2 over high
Temp.
Chen et al (2016)
[14]
15 CeO2 added
V2O5/TiO2
Chemical Vapor
Condensation or
Impregnation method
NO = NH3 = 500 ppm, O2 = 5 vol%,
without SO2 and water vapor
>90% NOx conversion
maintain from 200
to 350 0C
Cha et al (2016)
[15]
16 MnxCo3 â xO4 Nanocasting method 200 mg catalyst with 500 ppm NO,
500 ppm NH3, 5%O2, balanced N2
99 % conversation in the
range of 100 to 300 0C
Qiu et al (2015)
[16]
17 IronâCeriumâ
Titanium mixed
oxide
Co-precipitation
method
[NO] = [NH3] = 0.1%, [O2] = 3.0 %
and 3000 mL/min
Fe0.65Ce0.05Ti0.30Oz catalyst
gave >86% conversation in
the temp. range 150 â 300 0C
Zhi-bo et al
(2016) [17]
18 Co and Ce Doped
Mn/TiO2
Wet Impregnation
Method
0.15 g sample, 320 ppm NO, 320
ppm NH3, 5 vol.% O2,
MnâCoâCe/TiO2 exhibited
the highest catalytic
activity of 99 % at 573 K
Qiu et al (2015)
[18]
18. H2-Hydrocarbon and Hydrocarbon
Sr.
No
Catalyst Preparation Method Exp. Conditions Catalyst Activity
% and Temp.
Author Year
1 Ag supported Îł-
Al2O3
wetâ
impregnation method
200 mg catalyst 400 ppm NO,
1600 ppm CH4, 700 ppm CO,
6.5% O2, 10% H2O, and balanced
with He
23 % in the range 600-650 0C Azizi et al
(2016) [19]
2 1%wt Ruâ10%wt
AM/MO (AM = Ba
or K; MO =
Ce0.8Zr0.2O2, ZrO2,
Al2O3),
incipient wetness
impregnation
60 mg of catalyst NO (1000 ppm)
+ 3% v/v O2 in flowing He (lean
phase) with steps of H2 (4000
ppm) in He
N2 selectivity (74%, 83% and
67% for RuâK/Al,RuâK/Zr
and RuâK/CZ, respectively
in the presence of soot vs.
32%,71% and 41% in the
absence of soot) K-
containing catalysts 200- 230
0C
Matarrese et al
(2016) [20]
3. Pt Catalyst over
SiO2 and Al2O3
Aerosol Method 236 ppm NO, 440 ppm C3H6, and
5% O2 in He
Pt/SiO2 and Pt/Al2O3
catalysts are 29.8% and
55.8%, at 250°C.
Zahaf et al
(2015) [21]
4. Fe/zeolite catalysts wet
impregnation method
470 ppm NO, 5% O2 and N2 as the
balance gas; total flow rate: 370
mL min-1,
Fe/MOR > Fe/FER _
Fe/ZSM-5 > Fe/Beta at low
temperatures between 200 0C
and 300 0C.
Pan et al (2015)
[22]
19. Sr.
No
Catalyst Preparation Method Exp. Conditions Catalyst Activity
% and Temp.
Author Year
5. magnesia doped
Ag/Al2O3
impregnation method NO (1000 ppm), C3H6(2000
ppm), CO2(10%), O2(5%), 0 or
20 ppm SO2, 0 or 9% H2O and
balance helium
8% NO conversion with
100% selectivity for
N2was obtained at 350âŚC
with 7% Mg doping
More et al
(2013) [23]
6. Au Pd
nanoparticles
Using reducing
agents and stabilizer
ligands,
720 ppm NO,620 ppm toluene
(4340 as C1), 4.3% O2, 7.2%
H2O, 1% Kr was used with Ar
as balance
60% Conversation in the
250-300 0C temp. range
Hamill et al
(2014) [24]
7. PdâAu/TiO2 by H2 incipient wetness
impregnation
method
0.25% NO, 1% H2, and 5% O2
and helium as the balance gas
80% Conversation in the
175-250 0C temp. range
Duan et al
(2014) [25]
22. Sr.
No
Catalyst
Nomenclature
Catalyst Preparation methods
Calcinations
Temp
1
Cat-A Mn/TiO2 Reactive Grinding 500 °C for 5 h
2
Cat-B Mn/SiO2 Reactive Grinding 500 °C for 5 h
3
Cat-C Mn/ď§-Al2O3 Reactive Grinding 500 °C for 5 h
4
Cat-D V1W9Ti90 Wet impregnation 500°C for 5 h
5
Cat-E Co0.01V0.99W9Ti90 Wet impregnation 500°C for 5 h
6
Cat-F Ce0.01V0.99W9Ti90 Wet impregnation 500°C for 5 h
7
Cat-G NiCo2O4 Nano-casting method 500 °C for 5 h
8
Cat-H Cu/Al2O3 Co-Precipitation 500 °C for 5 h
9
Cat-I 0.1% Rh-Mn/TiO2 Reactive Grinding 500 °C for 5 h
10
Cat-J 0.1% Rh-NiCo2O4 Nano-casting method 500 °C for 5 h
11
Cat-K 0.1% Rh- Cu/Al2O3 Co-Precipitation 500 °C for 5 h
Table 1: Nomenclature of prepared catalysts
23. MnO2 Powder,
TiO2 (Cat-A)
/SiO2 (Cat-B)
/ď§-Al2O3 (Cat-C)
Planetary ball mill Ball Ratio 1:5, 240
rpm for 24h
Calcined in situ in a tubular reactor at
500°C for 5 h in Stagnant Air (SA) and
Flowing air (FA)
Cat-A, Cat-B, Cat-C
Catalyst
Reactive Grinding Method
*Cat-A(Mn/TiO2), Cat-B (Mn/SiO2), Cat-C (Mn/ď§-Al2O3 )
Figure 2: Reactive Grinding machine
24. 3.406g of sodium tungstate
(Na2WO4.2H2O) conc. HCl
was added to form white
precipitate. It is then washed
4-5 times with distilled water.
Light yellow precipitate was
obtained,
25.21g oxalic acid added to 200 ml water stirred and
mixed. 0.2571g of ammonium metavanadate
(NH4VO3)
0.8g of prepared WO3 was added to the solution and
stirred for 30 min
then add Subsequently TiO2 powder
and stirred for 7 h
heated to 110 °C for 12 h followed by
calcinations at 500°C for 5 h in air
Cat- D, Cat-E,
Cat-F catalyst
Wet impregnation method
*Cat-D(V1W9Ti90 ), Cat-E(Co0.01V0.99W9Ti90), Cat-F (Ce0.01V0.99W9Ti90)
25. 1 g KIT-6 dissolved in 70 ml n-
Hexane
1 ml aq.sol of 2.3 mmol
Ni(NO3)2¡4H2O and 4.6 mmol
Co(NO3)2¡4H2O
Vigorous stirring (over night), filtered and
dried at °C, followed by calcined in a muffle
furnace at 500 °C for 5 h
Washing with hot 2 M NaOH aqueous solution , then
centrifuged and dried at 80 °C
Cat- G catalyst
Nano-casting Method
*Cat-G (NiCo2O4)
26. 12.0 ml of 69% nitric acid + 3.75 g citric acid anhydrous + 15.30 g(15 mmol) of
alumininum iso-propoxide + 15 mol% of copper nitrate trihydrate
(Stirr to homogeneous solution)
8.325 ml PEG 300 dissolved in 150 ml ethanol
Vigorous stirring for 10 h
Filterd and dired at 60 °C
Final solution was dired in overnight at 110 °C
Calcination at static air at 500 °C for 5h
Mesoporous Cat-H
Co-Precipitation Method
*Cat-H (Cu/Al2O3)
34. ďA number of catalysts are prepared and evaluated for NO reduction with various
reductants such as NH3/LPG/H2-LPG.
ďThe order of NO reduction activity of the catalysts prepared by the reactive
gridding (RG) is given below:
Cat-A > Cat-B > Cat-C.
ďThe SCE activity order of the Rh-doped catalysts is as follows:
Cat-I > Cat-J > Cat-K.
ďThe SCR activity order of V-W-Ti catalyst is as follows:
Cat-E > Cat-F > Cat-D.
ďCo doped catalysts are accountable for maximum NO reduction over Cat-D
catalytic active site.
*Cat-A(Mn/TiO2), Cat-B (Mn/SiO2), Cat-C (Mn/ď§-Al2O3), Cat-D(V1W9Ti90 ), Cat-E(Co0.01V0.99W9Ti90), Cat-F (Ce0.01V0.99W9Ti90), Cat-I
(0.1% Rh-Mn/TiO2), Cat-J (0.1% Rh-NiCo2O4), Cat-K (0.1% Rh- Cu/Al2O3)
35. ď99 % NO reduction is achieved over the Cat-A and Cat-I catalysts with H2
assisted LPG-SCR.
ď0.1mol% Rh doping into Cat-I is enhancing the activity of catalyst and showed
better activity with the H2-LPG as compare the NH3.
ďThe orders of activity due to reductants are as follow:
H2-LPG > LPG >NH3.
ďActive SCR catalyst can be prepared by a one-step mechanical grinding using
green precursors, with the advantage that no aqueous waste is generated.
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40. Paper Published:
â˘Kavaiya A. R., Yadav, D., Singh P.,Prasad R., Promotional effects of Co and Ce on V-W-Ti catalyst for selective catalytic
reduction of NO, published in Asian Journal of Science and technology, 2017, 08, 4087-4092.
â˘Yadav, D., Kavaiya A. R., Prasad R., Low temperature SCR of NOx emissions by Mn doped Cu/ Al2O3 catalysts, in press in
Bulletin of Chemical Reaction and Catalysis, 2017.
â˘Kavaiya A. R., Yadav, D., Prasad R., Low temperature SCR of NO over MnO2/ TiO2 catalyst produced by reactive grinding,
paper accepted for Publication in Catalysis in Green Chemistry and Engineering, 2017.
Present in Conference:
â˘Kavaiya A. R., Yadav, D., Prasad R., Comparative study of transition metal M=Mn, Cu, Ni cobaltite for low temperature
NO reduction, Oral Presentation in Chemcon 2016, Dec. 27-30, 2016, IIT-Madars.
â˘Kavaiya A. R., S. Trivedi, Prasad R., Effect of Precipitatnts of NiCo2O4 catalyst for Oxidation of CO-CH4 mixture emitted
from CNG Vehicles, Poster Presentation in Chemcon 2016, Dec. 27-30, 2016, IIT-Madars.
â˘Kavaiya A. R., Yadav, D., Prasad R., Low temperature SCR of NO over MnO2/ TiO2 catalyst produced by reactive grinding,
Oral presentation in APCAT-7, Jan. 17-21, 2017, ICT Mumbai.
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