j b 2013 presentation tateo usui mod
TRANSCRIPT
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IX JAPAN-BRAZIL SYMPOSIUM ON
DUST PROCESSING - ENERGY - ENVIRONMENT
IN METALLURGICAL INDUSTRIES
September, 8-11, 2013
Gorceix Fundation Auditorium, Ouro Preto, Brazil
THE STATE-OF-THE-ART EMPLOYMENT OF WOODY
BIOMASS AND BIOGAS IN MANUFACTURING INDUSTRIES
CENTERING AROUND STEEL INDUSTRY
Tateo USUI ( Osaka Univ., Japan; now at Univ. Federal de Ouro Preto, Brazil )
Hirok azu KONISHI , Kazuh ira ICHKAWA , Hideki ONO, Hiroto sh i KAWABATA
( Graduate School of Engneering, Osaka Univ., Japan )
Paulo Santos A ss is ( Univ. Federal de Ouro Preto, Brazil)
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1. INTRODUCTION
The purpose of this paper is to show the
idea of an excellent employment of woody
biomass and biogas in manufacturingindustries centering around steel industry.
In the beginning, how come to recognize
the present research themeis explained by
looking back on our previous works.
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2. BACKGROUND FOR THE PRESENT WORK
The first author and coworkers used to be,carried out experimental studies on
carbonization of coal and wood in Graduate
School of Engineering, Osaka University, in order
to use both carbonization gas and coal-char or
charcoalin the following ironmaking processes.
semi-coal-charor semi-charcoal
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2.1 Pre-reductionof iron oxide pellets by
coal carbonization gas
( Iron bath smelting reduction process)
In the first step, three sorts of bituminous
coal were carbonized under various rising
temperature conditions (see Figs.1and 2).
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Carbonization experiment
Carbonization furnace
Gas
chromatograph
155 I.D.100
320
850
N2inlet
Thermocouple
81 I.D.
Heater
Coal particles
280
Alumina balls
Ribbon heater
Water inlet
(273 K)
Condenser
Exhaust
gas
Tar filter
Carbonization conditionsCarrier gas: N2 1.0 L/min (s.t.p.) Heating rate: 200 K/hTC, max: 823 K, 873 K, 973 K, 1073 K, 1273 K
Experimental apparatusFig. 1
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Coal Pellets
Backgrounds (Iron bath smelting
reduction total process Image )
Carbonization furnace Pre-reductionfurnace
Exhaust gas
Carbonization gas
Fe
Smelting furnace
Coal
Char
Fe2O3
Utilization of V.M. of coal
in an iron bath smelting
reduction total process
Iron bath smelting reduction total process
Fe3O4, FeO, Fe
Smelting furnace Smelting furnace
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Reference
T. Usui, T. Yokoyama, T. Nakahashi and Z. Morita, 1993 Ironmaking ConferenceProceedings (Iron and Steel Society), pp. 389-398.
Application
Fig. Mole fraction of carbonization gas before
reduction as a function of carbonization time.
Tc, max=1073 K
Carbonization conditions
Coal: Muswellbrook coalCarrier gas: N2 1.0 L/min (s.t.p.)Maximum carbonization temperature
(TC, max): 1073 K
Heating rate: 200 K/h
Utilization of volatilematter (V.M.) of coal
Pre-reduction of iron oxide inan iron bath smelting reduction
total process
Backgrounds(Pre-reduction of iron
oxide with carbonization gas of coal)
Fig. 3
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Fig. Variations of final fractional reductionsFandFH with reduction temperature TR.
Reduction temperature
1173, 1273 K
Reduction of iron oxide by
hydrogen in hydrocarbons
800 1000 1200
0
0.2
0.4
Reduction temperatureTR(K)
Fra
ctinalreduction
F,
FH
()
Muswellbrook coal
Fractional reduction
(gravimetric method)
Fractional reduction due to H
Tar filter: room temperature
800 1000 1200
0
0.2
0.4
Reduction temperature TR(K)
Frac
tinalreduction
F,
FH
()
Newlands coal
Fractional reduction (gravimetric method)
Fractional reduction due to H
Tar filter: room temperature
Final fractional reductions Fand FH
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2.2Carbon composite iron oxide pellets
using semi-coal-char
It was found in the above-mentioned carbonizationexperiments under rising temperature conditions that when the
carbonization was interrupted halfway, the volatile matter
release was interrupted corresponding to the interrupted
carbonizing temperature, i.e., the maximum carbonizing
temperature Tc,max ; and that when the carbonization was
started again the release of the residual volatile matter began
at the very interrupted carbonizing temperatureTc,max and the
same total amount of carbonization gas was released as the
one without interruption.
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From these findings we proposed the novel
carbon composite pellets, in which the semi-coal-char
including the residual volatile matter was used ascarbonaceous material. When we use fully
carbonized coal char as carbonaceous material, the
reduction of carbon composite pellets starts at first assolid / solid reaction under rising temperature
condition like in a blast furnace. Whereas, when we
use the semi-coal-char as carbonaceous material,the reduction of carbon composite pellets starts from
the beginning as gas / solid reaction just after the
reduction temperature arrives at Tc,max .
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Therefore, the first merit is the decrease instarting temperature of reaction and the second
one is the rate enhancement of reduction reaction
by the residual volatile matter (see Fig.5). The
decrease in starting temperature of reduction
reaction of iron ore in a blast furnace leads to thedecrease in consumption of reducing agent.
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Heating pattern
0 120 240 360
400
600
800
1000
1200
1400
Carbonization time (min)
Carb
onizationtemperatu
re(K)
Tc,max = 1273 K
873 K
1073 K
973 K
823 K
TC, max = 1273 K
Carbonization time t (min)
Carboniz
ationtemperatureT
C
(K)
In order to obtain the semi-coal-char, Newcastle blend coal wascarbonized from room temperature to TC, max= 823, 873, 973, 1073and 1273 Kat200 K/h, and kept at TC, maxuntil arrival time of 6 h.
Fig. 2
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0
0.05
0.1
0.15
0.2
0.25
0.3
823 873 973 1073 1273
Totalgasvolume
[m3(s.
t.p.)]
Maximum carbonization temperature TC, max (K)
H2
CO
CO2
CH4
C2H4
C2H6
C3H8
Carbonization experiment (total gas volume)
Total gas volume ( Newcastle blend coal )H2gas releases more than any other gasesat TC, max= 873, 973, 1073, 1273 K.The higher TC, maxis, the more H2gas releases.Char contained much hydrogen at TC, max = 823 K.
Fig. 4
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F.C. V.M. Ash S C H O N
72.2 15.9 11.9 0.53 75.3 2.87 7.31 2.06
TC, max823 KTable. Analysis of Char carbonized at Tc, max = 823 K
(mass%)
TC, max1073 K
TC, max1273 K
F.C. V.M. Ash S C H O N
82.7 4.43 12.9 0.42 81.5 1.54 1.91 1.74
Table. Analysis of Char carbonized at Tc, max = 1073 K(mass%)
F.C. V.M. Ash S C H O N
83.2 2.51 14.3 0.52 81.7 0.90 1.34 1.27
Table. Analysis of Char carbonized at Tc, max = 1273 K
(mass%)
Analysis of the char obtained by carbonization
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Reduction of carbon composite iron oxide pellets
Ar gas inlet
Alumina
crucible
Gas outlet
Pellets
Thermo-
couple
Preparation of carbon compositeiron oxide pelletsChar : Fe2O3 = 1 : 4BinderBentonite (1 mass added)Particle size: under 4563 mPellets size: about 15 mmKeeping at 378 K for 24 hto remove waterReduction experiment and analysisReduction conditionsAr or N2gas atmosphereHeating rate: 0 or 3K/minAnalysisGas chromatography, SEM, XRD
Electric
furnace
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Relation between fractional reduction and reduction time of
carbon composite pellets at 1073 K in N2atmosphere
Semi-coal-char
Reduction behavior of carbon composite pellet atTC, max= 823Kwas higher thanany other pellets by about 10 .When TC, maxwas lower, namelythe pellet had more residual
V.M., the reduction of carboncomposite pellet was muchenhanced.
TC, max = 823 K
TC, max = 1073 K
TC, max = 1273 K
Char
Fr
actionalreductionF
(-)
Reduction time t (min)
0 10 20 30 40 50 600
5
10
15
20
25
10TR= 1073 K
( Fig. 5 )
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TC, max = 823 K
TC, max = 1073 KTC, max = 1273 K
Semi-coal-char
Fractionalreducti
onF(-)
Reduction time t (min)0 20 40 60 80
0
20
40
60
80
100
Fig. 5. Reduction curves for semi-coal-char
composite pellets ( TR= 1173 K ).
TR= 1173 K
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0 10 20 30 40 50 600
20
40
60
80
100
Char (TC, max = 823 K) (V.M. 15.9 %)
Coke (V.M. 0.6 %)Graphite (Purity 98 %)
Reduction time t [min]
Fractionalre
ductionF
[%]
Early stageChar Coke, GraphiteLater stageChar, Coke Graphite
Reduction rate
Effect of V.M. and crystallization Reduction rate
Influence of several kinds of carbon materials
Reduction at 1273 K in
N2gas atmosphere
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2.3Carbon composite iron oxide
pellets using semi-charcoal
The above-mentioned carbonization
experiments on coal were expanded into
those on charcoal; semi-charcoal including
the residual volatile matter was used as
carbonaceous material in the novel carbon
composite pellets.
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The rate enhancement effect of reduction
for semi-charcoal composite pellets isstronger than that for semi-coal-charcomposite pellets, because the gasification
rate of semi-charcoal is higher than that of
semi-coal-char. This is caused by the
following reasons: amorphous nature of
semi-charcoal is stronger than that of semi-
coal-char (see Fig.6) and the activationenergyof semi-charcoal is lower than that of
semi-coal-char (see Table 1).
R d i f i id b d bi
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A lot of steel engineers
researched various meansto decrease coke in a blast
furnace in order to reduce
CO2emission.
Carbon neutral(No CO2emission)Rich resources
Biomass
Reduction of iron oxide by woody biomass
Woody biomass
Japanese
cedar
Application(Carbonaceous material)
Injection into a blast furnace
Preparation of carbon com-
posite iron ore agglomerateJapanese
cypressBiomass
waste
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Sample
F.C. V.M. Ash T.S T.C H O N
8.12 90.8 1.05 0.014 50.7 6.16 41.1 1.01
Carbonaceous materialJapanese cypressTable. Analysis of Japanese cypress (mass%)
Iron oxide: Reagent grade hematite (Fe2O3)
(95 mass%, Wako Pure Chemical Industries Ltd.)
Sample for carbonization experiment
Sample for reduction experiment of iron oxide pellets
SiO2 Al2O3 Fe2O3 CaO MgO K2O Na2O
58.79 14.27 2.99 0.70 1.28 0.70 3.42
Table. Chemical analysis of Bentonite (mass%)
BinderBentonite(1 mass% added)
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Heating pattern of carbonization of Japanese cypress
Carbonization time t (min)
In order to obtain the semi-charcoal, Japanese cypress was
carbonized from room temperature to TC, max= 823, 1073 and
1273 K at 200 K/h, and kept at TC, maxuntil arrival time of 6 h.
Carbonizationtem
peratureTC(K
)
823 K
0 120 240 360
800
1000
1200
600
400
1400
1073 K
TC, max = 1273 K
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Total gas volume generated by carbonization
Totalg
asvolume[m3(s.t.p.)]
Maximum carbonization temperature Tc, max (K)
H2
CO
CO2
CH4
C2H4
C2H6
C3H8
Total gas volume generated by carbonizationH2 gas was released more than any other gases at TC, max = 1273 K,but was released less than CO, CO2and CH4gases at TC, max= 823 K.
The higher TC, maxwas, the more H2gas was released.Semi-charcoal retained much V.M., namely H2gas, at Tc, max = 823 K.
823 1073 1273
0.01
0.02
0.03
0.04
0
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Table Analysis of semi-charcoal obtained by carbonization of Japanese cypress.
Tc, max =
823 KTc, max =
1073 K
Volatile matter
(V.M.)Hydrogen
Tc, max =
1273 K
(mass%)
Analysis of the semi-charcoal obtained by carbonization
It was confirmed that the semi-charcoal of TC, max= 823 K
retained much V.M., namely hydrogen.
0.04 0.824.810.5692.61.167.0091.80TC,max= 1273 K
0.03 0.555.891.3391.21.019.6489.35TC,max= 1073 K
0.01 0.609.892.9385.80.7618.6580.60TC,max= 823 KSemi-
charcoal
S NOHCAshV.M.F.C.Component
Coke 87.1 0.97 11.97 84.6 0.26 1.35 1.220. 60
0.01 41.11.016.1650.71.0890.88.12Japanesecypress
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Semi-charcoal has many micro pores with the size of about 10 m.
Semi-charcoal obtained by carbonization
Tc, max = 823 K Tc, max = 1073 KT
c, max = 1273 K
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Semi-charcoalTc, max = 823, 1073, 1273 KCO2 1.0 L/min (s.t.p.)TG= 1073, 1173, 1273 K
Experimental conditions
Reaction rate
Weight loss measurement
6375 mBinder 2 mass% Pellets
CO2N2
TG
R.T.
600 [K/h]
Fig. Schematic of reduction furnace.
Gasification of semi-charcoal
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TG= 1173 K TG= 1273 K
Tc, max is low Reaction rate is high
Gasification of semi-charcoal
Fig. Weight loss curves of semi-charcoals
obtained by carbonization at Tc, max = 823,
1073, 1273 K and coke at TG = 1173 K in
CO2 gas atmosphere.
0 20 60Reaction time [min]
We
ightloss[%]
0
-20
-60
40
CokeSemi-charcoal c max= 1273 K c max= 1073 K c max= 823 K
-40
-80
-100
Fig. Weight loss curves of semi-charcoals
obtained by carbonization at Tc, max = 823,
1073, 1273 K and coke at TG = 1273 K in
CO2 gas atmosphere.
0 20 60Reaction time [min]
We
ightloss[%]
0
-20
-60
40
-40
-80
-100
Gasification of semi charcoal
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Arrhenius plots of reaction rate of gasification
Tc, max
E[kJ/mol]
823 K1073 K 1273 K Coke
138 162 219139
Gradient Activation energy
Tc, max is low
Activation energy is low
Gasification of semi-charcoal
-100.7 0.8 1.0
1/TG [K-1]
Reactionrate:ln
kC,
CO2
[1/min]
-6
0.9
-4
-2
[10-3]
TG[K]
11001200 100013001400
-8
Semi-charcoal
Tc,max= 823 K Tc,max= 1073 K Tc,max= 1273 K Coke
Fig. Reaction rate per unit mass at TG= 1073,
1173, 1273 K in CO2atmosphere.
This result of activation energy might
be influenced by specific surface area
and crystallizationof these samples.
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Carbonaceous material
Activation energy
(kJ/mol)
Graphite
Bintyo char
Bamboo char
Coke
Glassy carbon
Activated carbon
Semi-charcoalat Tc,max= 823 K
Semi-charcoalat Tc,max
= 1073 K
Semi-charcoal at Tc,max= 1273 K
Semi-coal-char at Tc,max= 1073 K
Coke
217(29)
182(29)
181(29)
200(29)
211(29)
149(29)
138 *
139*
162*
174*
219*
Table 1. Comparison of activation energies for
variouscarbonaceous materials.(27)
* Present work
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2(Cu-K) /degree
Diffraction
intensity/arb.un
it
(b) Semi-charcoala) Semi-coal-char
20 30 40 50 60 7020 30 40 50 60 70
2(Cu-K) /degree
Diffractionintensity/arb.unit : Carbon
TC, max = 1273 K
1073 K
823 K
TC, max = 1273 K
1073 K
973 K
: Carbon: Unknown
The crystal structures of semi-coal-char and semi-charcoal
Semi-charcoalSemi-coal-char
Amorphous
structure
Crystalline
structureFig. 6
R d ti f i h l it i id ll t
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Reduction of semi-charcoal composite iron oxide pellets
Preparation of semi-charcoal composite iron oxide pelletsSemi-charcoal : Fe2O3= 1 : 4Binder Bentonite (1 mass%)Particle size: 2335, 6375, 105150 mPellets size: about 15 mmKeeping at 378 K for 24 h to remove water
Reduction experiment and analysis
Reduction conditionsN2gas atmosphereAnalysisGas chromatography
Reduction behavior of iron oxide in semi-charcoal composite
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TR= 1073 K
Fig. Reduction curves of semi-charcoal
composite pellets using semi-charcoal at
Tc,max= 823, 1073, 1273 K and coke at
TR = 1073 K in N2gas atmosphere.
Fractional reduction
Reduction time [min]
FractionalreductionF
[%]
0 30 60
15
30
Tc,max= 823 K
Tc,max= 1073 K
Tc,max= 1273 K
0
Particle size: 6375 m
Reduction behaviorF of semi-charcoal compositepellet at TC, max= 823Kwas 19 %
for 60 minand higher than any
other pellets by 78 %.When TC, maxwas lower, namelythe pellet had more residual
V.M., the reduction of semi-
charcoal composite pellet was
much enhanced.
Reduction behavior of iron oxide in semi-charcoal composite
pellets at TR= 1073 K in the N2gas atmosphere
Coke
823 K1073 K
1273 K
Tc,max
Coke
Reduction behavior of iron oxide in semi-charcoal composite
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Fig. Reduction curves of semi-charcoal
composite pellets using semi-charcoal at
Tc,max= 823, 1073, 1273 K and coke at
TR =1173 K in N2gas atmosphere.
TR= 1173 K
Reduction time [min]
Fractionalredu
ctionF
[%]
0 30 60
25
50
0
Fractional reduction
Particle size: 6375 m
Reduction behaviorF of semi-charcoal compositepellet at TC, max= 823Kwas 40 %
for 60 minand higher than any
other pellets.When TC, maxwas lower, namelythe pellet had more residual
V.M., the reduction of semi-
charcoal composite pellet was
much enhanced.
TC,max= 823 K
TC,max= 1073 K
TC,max= 1273 K
Coke
823 K1073 K
1273 K
T
c,max
Coke
Reduction behavior of iron oxide in semi-charcoal composite
pellet at TR= 1173 K in N2gas atmosphere
Reduction behavior of iron oxide in semi-charcoal composite
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TR= 1273 K
Fig. Reduction curves of semi-charcoal
composite pellets using semi-charcoal at
Tc,max= 823, 1073, 1273 K and coke at
TR = 1273 K in N2gas atmosphere.
Reduction time [min]
Fractionalredu
ctionF
[%]
Tc,max= 823 K
Tc,max= 1073 K
Tc,max= 1273 K
0 30 600
50
100
Fractional reduction
Reduction behaviorF of semi-charcoal compositepellets at TC, max= 823, 1073 and
1273 K were over 90 % for 60 min
and indicated the same behaviorat TR= 1273 K.These reducibility of semi-charcoalcomposite pellets were high and
were not dependent on residual
V.M. at TR= 1273 K.
Particle size: 6375 m
Coke
823 K1073 K
1273 K
Tc,max
Coke
Reduction behavior of iron oxide in semi-charcoal composite
pellets at TR= 1273 K in N2gas atmosphere
The influence of crystallinity of semi-charcoal on reduction of
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Reduction time [min]
FractionalreductionF
[%]
823
1073
1273
CharCharcoal
0 10 20 30 40 50 600
20
40
60
80
100
Tc,max (K)
Fig. Reduction curves of carbon composite pellets
using semi-charcoal and semi-coal-char at
Tc,max = 823, 1073, 1273 K with time at TR =
1273 K in N2gas atmosphere.
Semi-charcoal composite pellet
Semi-coal-char composite pellet
The influence of crystallinity of semi-charcoal on reduction of
iron oxide in semi-charcoal composite pellet at TR= 1273 K
Fractional reduction
Reduction rateReduction rate of semi-charcoalcomposite pellets are higher
than that of semi-coal-char
composite pellets.
Semi-charcoal Semi-coal-char
Reducibility
Amorphous
structure
Crystalline
structure
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Total gas volume generated by carbonization
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Total gas volume generated by carbonization
Totalgasvolume[m3(s.t.p.)]
Maximum carbonization temperature TC, max (K)
H2
CO
CO2
CH4
C2H4
C2H6
C3H8
Total gas volume generated by carbonizationH2 gas was released more than any other gases at TC, max = 1273 K,but was released less than CO, CO2 and CH4gases at TC, max= 823 K.
The higher TC, maxwas, the more H2gas was released.Semi-charcoal retained much V.M., namely H2gas, at TC, max = 823 K.
823 1073 1273
0.01
0.02
0.03
0.04
0
Japanese
cypress
O/C H/C mole ratio (Van Krevelen diagram)
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moleratio
mole ratio
demethanation
Dehydration, decarboxylation
Calorific power low Semi-coal-charTC, max = 823 KTC, max = 873 KTC, max = 973 KTC, max = 1073 KTC, max = 1173 KTC, max = 1273 KSemi-charcoal
TC, max= 823 KTC, max= 1073 KTC, max= 1273 KCoke
TC, max = 823 K
873 K
973 K
1173 K
1073 K
1273 K
Tc, max = 823 K
1073 K
1273 K
Semi-coal-char
Coke
Semi-charcoal
The higher TC, maxwas,the lower O/C and H/C
values were.
0 0.05 0.10
0.2
0.4
0.6
O/C, H/C mole ratio (Van Krevelen diagram)
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3. OUTLINE OF THE PRESENT STUDY
From the accumulated date mentioned-above on semi-charcoal, in the first step, the
first author is going to study the optimum
conditions for the use of both semi-charcoal
and carbonization gas (biogas) released at
carbonization in ironmaking such as carboncomposite agglomerates by data analyses in
Univ. Federal de Ouro Preto with Prof. Assis;
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we can expect that the lower the
carbonizing temperature Tc,max is, the
better the reactivity of semi-charcoal
becomes but the less the amount of
carbonization gas releases in the
carbonizing step.
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As the carbonizing temperature Tc,max
decreases, the activation energy of semi-
charcoal decreases gradually, while the
amount of carbonization gas release in the
carbonizing step, namely, the amount of
biogas, decreases rather drastically. There
will be some optimum carbonizing
temperature Tc,max in an actual process forboth preparing reactive semi-charcoal and
producing much biogas.
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In the second step, the experimental
program will be proposed to search theoptimum conditions for the use of both
semi-charcoal and carbonization gas
released in the carbonizing step. Of
course, the experimental program has
to be expanded from wood to variouskinds of biomass.
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In addition, literatures on various
kinds of biomass will be collected andanalyzed. Application of semi-
charcoal to another manufacturing
industry will also be searched.
In the third step, the experimental
apparatus will be designed for thenext year research period.
CONCLUDING REMARKS
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CONCLUDING REMARKS
From the previous study on pre-reduction of
iron oxide pellets by coal carbonization gas, we
proposed a novel carbon composite pellets; semi-coal-char was used as carbonaceous material to
enhance the rate of reduction and at the same
time to decrease the starting temperature ofreduction reaction. We expanded these results to
semi-charcoal.
The first author is going to study the optimumconditions for the use of both semi-charcoal and
carbonization gas released at carbonization in
ironmaking by data analyses in Univ. Federal de
Ouro Preto with Prof. Assis.
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Muito obrigado.
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O/C, H/C mole ratio (Van Krevelen diagram)
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moleratio
mole ratio
demethanation
Dehydration, decarboxylation
Calorific power low Semi-coal-charTC, max = 823 KTC, max = 873 KTC, max = 973 KTC, max = 1073 KTC, max = 1173 KTC, max = 1273 KSemi-charcoal
TC, max= 823 KTC, max= 1073 KTC, max= 1273 KCoke
TC, max = 823 K
873 K
973 K
1173 K
1073 K
1273 K
Tc, max = 823 K
1073 K
1273 K
Semi-coal-char
Coke
Semi-charcoal
The higher TC, maxwas,the lower O/C and H/C
values were.
0 0.05 0.10
0.2
0.4
0.6
/ , / ( g )