Title of Invention

A DIRECT REDUCTION PROCESS FOR A METALLIFEROUS MATERIAL

Abstract A direct reduction process for a metalliferous material is disclosed. The process comprises supplying the metalliferous material, a solid carbonaceous material, an oxygen-containing gas, and a fluidising gas into a fluidised bed in a vessel and maintaining the fluidised bed in the vessel, at least partially reducing metalliferous material in the vessel, and discharging a product stream that comprises the at least partially reduced metalliferous material from the vessel, wherein the process comprises the steps of: (a) reducing the metalliferous material in a solid state in a metal-rich zone in the vessel; (b) injecting the oxygen-containing gas above the supply of the metalliferous material into a carbon-rich zone in the vessel with a downward flow in a range of plus or minus 40 degrees to the vertical and generating heat by reactions between oxygen and the metalliferous material, the solid carbonaceous material and other oxidisabie solids and gases in the fluidised bed, and (c) transferring heat from the carbon-rich zone to the metal-rich zone by movement of solids within the vessel.
Full Text The present invention relates to a direct reduction process for a metalliferous feed ma-
terial, particularly, although by no means exclusively, to a direct reduction process for
an iron-containing feed material, such as iron ore.
The present invention also relates to a process for reducing a metalliferous feed mate-
rial that comprises a direct reduction process for partially reducing metalliferous feed
material in the solid state and a smelting process for melting and further reducing the
partially reduced metalliferous feed material to a molten metal.
The present invention was made during the course of an on-going research project car-
ried out by the applicant to develop the so called "CIRCOFER technology" for the direct
reduction of iron ore.
CIRCOFER technology is a direct reduction process that is capable of reducing iron ore
in the solid state to a metallisation of 50% or higher.
CIRCOFER technology is based on the use of fluidised beds. The main feed materials
to the fluidised beds are fluidising gas, metal oxides (typically iron ore fines), solid car-
bonaceous material (typically coal) and oxygen-containing gas (typically oxygen gas).
The main product produced in the fluidised beds is metallised metal oxides, i.e. metal
oxides that have been at least partially reduced.
One of the findings of the applicant in the research project is that it is possible to estab-
lish separate reaction zones within a single fluidised bed and to optimise the reactions
in these zones. One reaction zone is a carbon-rich zone in which solid carbonaceous
material, such as coal, and other oxidisable reactants are oxidised and generate heat.
The other reaction zone is a metal-rich zone in which metalliferous feed material, such
as iron ore, is reduced in the solid state. The two reaction zones are spaced apart
within the fluidised bed, with the metal-rich zone typically being in a lower section and

the carbon-rich zone being spaced above the metal-rich zone. The zones may be con-
tiguous. The fluidised bed comprises upward and downward flows of. solids and this
movement of material facilitates transfer of heat generated in the carbon-rich zone to
the metal-rich zone and maintains the metal-rich zone at a temperature required for
reducing the metalliferous feed material.
According to the present invention there is provided a direct reduction process for a
metalliferous material which comprises supplying the metalliferous material, a solid
carbonaceous material, an oxygen-containing gas, and a fluidising gas into a fluidised
bed in a vessel and maintaining the fluidised bed in the vessel, at least partially redu-
cing metalliferous material in the vessel, and discharging a product stream that compri-
ses the at least partially reduced metalliferous material from the vessel, which process
is characterised by: (a) reducing the metalliferous material in a solid state in a metal-
rich zone in the vessel; (b) injecting the oxygen-containing gas into a carbon-rich zone
in the vessel with a downward flow in a range of plus or minus 40 degrees to the verti-
cal and generating heat by reactions between oxygen and the metalliferous material
(including metallised material), the solid carbonaceous material and other oxidisable
solids and gases in the fluidised bed, and (c) transferring heat from the carbon-rich zo-
ne to the metal-rich zone by movement of solids within the vessel.
Preferably the process comprises injecting the oxygen-containing gas with a downward
flow in a range of plus or minus fifteen degrees to the vertical.
The term "carbon-rich" zone is understood herein to mean a region in the fluidised bed
in which there is a relatively large amount of carbon-containing material in relation to
the amount of metalliferous material than in other regions of the fluidised bed.
The term "metal-rich" zone is understood herein to mean a region in the fluidised bed in
which there is a relatively large amount of metalliferous material in relation to the
amount of carbon-containing material than in other regions of the fluidised bed.
Preferably the process comprises forming the metal-rich zone in a lower section of the
vessel and the carbon-rich zone in an intermediate section of the vessel.

Preferably the intermediate section is intermediate said lower section and an upper
section of the vessel.
Preferably the process comprises injecting the oxygen-containing gas into a central
region in the vessel, i.e. a region that is located inwardly of a side wall of the vessel.
Preferably the process comprises controlling the temperature difference between the
bulk temperature in the fluidised bed and the average temperature of the inwardly fac-
ing surface of a side wall of the vessel to be no more than a 100°C.
The term "bulk temperature" is understood herein to mean the average temperature
throughout the fluidised bed.
More preferably the temperature difference is no more than 50°C.
In the case of reducing metalliferous material in the form of iron ore fines, preferably
the bulk temperature in the fluidised bed is in the range 850°C to 1000°C.
Preferably the bulk temperature in the fluidised bed is at least 900°C, more preferably
at least 950°C.
In addition, preferably the process comprises controlling the temperature variation to be
less than 50°C within the fluidised bed.
The temperature difference may be controlled by controlling a number of factors includ-
ing, by way of example, the amounts of the solids and the gases supplied to the vessel.
Furthermore, in the case of reducing metalliferous material in the form of iron ore fines,
preferably the process comprises controlling the pressure in the vessel to be in the
range of 1-10 bar absolute and preferably 4-8 bar absolute.

Preferably the process comprises injecting the oxygen-containing gas so that there is a
downward flow of the gas in the vessel.
Preferably the process comprises injecting the oxygen-containing gas via at least one
lance having a lance tip with an outlet positioned in the vessel inwardly of the side wall
of the vessel in the central region of the vessel.
Preferably the lance tip is directed downwardly.
More preferably the lance tip is directed vertically downwardly.
The position of the lance and, more particularly, the height of the outlet of the lance tip,
is determined by reference to factors, such as the oxygen-containing gas injection velo-
city, the vessel pressure, the selection and amounts of the other feed materials to the
vessel, and the fluidised bed density.
Preferably the process comprises water-cooling at least the lance tip to minimise the
possibility of accretions forming on the lance tip that could block the injection of the
oxygen-containing gas.
Preferably the process comprises water cooling an outer surface of the lance.
Preferably the process comprises injecting the oxygen-containing gas through a central
pipe of the lance.
Preferably the process comprises injecting the oxygen-containing gas with sufficient
velocity to form a substantially solids-free zone in the region of the lance tip to minimise
the formation of accretions on the lance tip that could block the injection of the oxygen-
containing gas.
Preferably the process comprises injecting nitrogen and/or steam and/or other suitable
shrouding gas and shrouding the region of the outlet of the lance tip to minimise oxida-
tion of metal that could result in accretions forming on the lance tip that could block the
injection of the oxygen-containing gas.

Preferably the process comprises injecting the shrouding gas into the vessel at a velo-
city that is at least 60% of the velocity of the oxygen-containing gas.
Preferably the process comprises supplying the metalliferous feed material, the carbo-
naceous material, the oxygen-containing gas, and the fluidising gas to the fluidised bed
and maintaining the fluidised bed with (a) a downward flow of the oxygen-containing
gas, (b) an upward flow of solids and fluidising gas countercurrent to the downward flow
of the oxygen-containing gas, and (c) a downward flow of solids outwardly of the up-
ward flow of solids and fluidising gas.
In the fluidised bed described in the preceding paragraph, solids in the upward and
downward flows of solids are heated by heat generated by reactions between the oxy-
gen-containing gas, the solid carbonaceous material and other oxidisable materials
(such as CO, volatiles, and H2) in the carbon-rich zone. The solids in the downward
flow of solids transfer heat to the metal-rich zone.
In addition, the upward and downward flows of solids shield the side wall of the vessel
from radiant heat generated by reactions between the oxygen-containing gas and the
solid carbonaceous material and other oxidisable solids and gases in the fluidised bed.
In the case of reducing metalliferous material in the form of iron ore fines, preferably
the fines are sized at minus 6 mm.
Preferably the fines have an average particle size in the range of 0.1 to 0.8 mm.
One of the advantages of the process is that it can accept a substantial amount of met-
alliferous feed material with a particle size of less than 100 microns without a significant
'
amount of this material exiting the process entrained in off-gas. This is believed to be
due to an agglomeration mechanism operating within the fluidised bed that promotes a
desirable level of agglomeration between particles of feed materials, particularly sub-
100 micron particles, without appearing to promote uncontrolled agglomeration capable
of interrupting operation of the fluidised bed. Similarly, friable ores that have a ten-

dency to break down during processing and to thereby increase the proportion of parti-
cles in the fiuidised bed with a size of less than 100 microns may be processed without
significant loss of feed material in process off-gas.
Preferably the carbonaceous material is coal. In such a situation, the process devolati-
lises the coal to char and at least part of the char reacts with oxygen and forms CO in
the fiuidised bed.
Preferably the fluidising gas comprises a reducing gas, such as CO and H2.
Preferably the process comprises selecting the amount of H2 in the fluidising gas to be
at least 15% by volume of the total volume of CO and H2 in the gas.
Preferably the process comprises discharging the product stream comprising at least
partially reduced metalliferous material from the lower section of the vessel.
Preferably the product stream also comprises other solids (for example char).
Preferably the process comprises separating at least a portion of the other solids from
the product stream.
Preferably the process comprises returning the separated solids to the vessel.
Preferably the process comprises discharging an off-gas stream containing entrained
solids from an upper section of the vessel.
Preferably the process comprises separating solids from the off-gas stream.
Preferably the process comprises maintaining a circulating fiuidised bed by separating
entrained solids from the off-gas stream and returning the solids separated from the off-
gas to the vessel.

Preferably the process comprises returning solids separated from the off-gas to the
lower portion of the vessel.
Preferably the process comprises preheating metalliferous feed material with the off-
gas from the vessel.
Preferably the process comprises treating the off-gas after the preheating step and re-
turning at least a portion of the treated off-gas to the vessel as the fluidising gas.
Preferably the off-gas treatment comprises one or more of (a) solids removal, (b) coo-
ling, (c) H20 removal; (d) C02 removal, (e) compression, and (f) reheating.
Preferably the off-gas treatment comprises returning solids to the vessel.
The process may be operated to produce a product stream ranging from low to high
metallisation depending on the downstream requirements for the at least partially redu-
ced metalliferous material. The metallisation may range from 30 to in excess of 80%.
In situations in which metallisation greater than 50% is required, preferably the process
comprises operating with reducing gas in the fluidising gas. One option for the fluidi-
sing gas in this instance is treated off-gas from the vessel. In situations in which metal-
lisation less than 50% is required, it is envisaged that it will not be necessary to operate
with reducing gas in the fluidising gas and sufficient reductant can be obtained via solid
carbonaceous material supplied to the process.
The oxygen-containing gas may be any suitable gas.
Preferably the oxygen-containing gas comprises at least 90% by volume oxygen.
According to the present invention there is also provided a process for reducing a met-
alliferous material that comprises (a) a direct reduction process for partially reducing
metalliferous material in a solid state as described herein and (b) a smelting process for
melting and further reducing the partially reduced metalliferous material to a molten
metal.

The present invention is described further with reference to the accompanying drawings,
of which:
Figure 1 is a diagram of an apparatus for direct reduction of a metalliferous mate-
rial by one embodiment of a process in accordance with the present in-
vention which illustrates the reaction zones formed by the process within
the vessel shown in the Figure; and
Figure 2 is the same basic diagram as that shown in Figure 1 which illustrates the
movement of solids and gases in the vessel caused by the process.
The following description is in the context of direct reduction of a metalliferous material
in the form of iron ore particles in the solid state. The present invention is not so limited
and extends to direct reduction of other iron-containing materials (such as ilmenite) and
more generally to other metalliferous materials.
The following description is also in the context of direct reduction of iron ore with coal
as a solid carbonaceous material, oxygen as an oxygen-containing gas, and a mixture
of at least CO, and H2 as a fluidising gas. The present invention is not so limited and
extends to the use of any other suitable solid carbonaceous material, oxygen-
containing gas, and fluidising gas.
With reference to the Figures, the solid feed materials, namely iron ore fines and coal,
oxygen and fluidising gas are supplied to the vessel 3 shown in the Figures and estab-
lish a fluidised bed in the vessel.
The solid feed materials are supplied to the vessel via a solids delivery device such as
screw feed or solids injection lance 5 that extends through a side wall 7 of the vessel.
The oxygen is injected into the vessel via a lance 9 having an outlet located within a
downwardly extending lance tip 11 that directs the oxygen downwardly in a central re-
gion 31 (Figure 2) of the vessel. The central region extends radially from a central axis

of the vessel toward the vessel wall. The oxygen is injected so as to have a downward
flow directed in the range between vertical and forty degrees to the vertical but is pref-
erably within the range of vertical to fifteen degrees to the vertical. Solids within the
region of the lance outlet may become entrained in the oxygen flow. The interaction
between the substantially downward flow of oxygen and the substantially upward flow
of fluidising gas is believed to significantly reduce the tendency for particles entrained
in the oxygen flow to contact side walls of the vessel and form accretions.
The fluidising gas is injected via a series of tuyeres or nozzles (not shown) in a base 13
of the vessel.
The above-described supply of solids and gases produces an upward flow of fluidising
gas and entrained solids in the central region of the vessel. Increasingly, as the solids
move upwardly, the solids disengage from the upward stream of fluidising gas and flow
downwardly in an annular region between the central region and the side wall of the
vessel. These recirculated solids are either entrained again in the upward stream of
fluidising gas or are discharged from the vessel. This movement of material in the ves-
sel is illustrated in Figure 2.
The above-described supply of solids and gases also produces the following reactions
in the vessel.
Devolatilisation of coal to char and decomposition of coal volatiles to gaseous products
(such as H2 and CO) and reaction of at least part of the char with oxygen to form CO.
Direct reduction of iron ore to at least partially reduced iron ore by gaseous products
CO and H2. These reactions in turn produce C02 and H20.
Reaction of part of the C02 with carbon to form CO (Boudouard reaction).
Oxidation of solids and gases such as char and particles of partially reduced metallifer-
ous feed material, coaf volatiles, CO, and H2 with oxygen, which generates heat and

promotes controlled agglomeration of smaller partially reduced ore particles with other
particles within the fluidised bed.
The relative densities of the solids and the above-described injection of the solids and
the gases, including the locations of the solids/gas injection, results in the formation of
reaction zones within the vessel. The reaction zones may be contiguous.
One reaction zone is a carbon-rich zone 17 in the region of the lance tip 11 of the lance
9. In this zone the predominant reactions are oxidizing reactions involving combustion
of char, coal volatiles, CO, and H2 with oxygen which generate heat.
The other reaction zone is a metal-rich zone 19 in which (a) coal is devolatilised and
forms char and coal volatiles and (b) iron ore fines are at least partially reduced by CO
and H2.
The above-described downward flow of solids in the annular region between the central
region and the side wall facilitates transfer of heat from the carbon-rich zone to the
metal rich zone.
In addition, the downward flow of solids partially shields the side wall from direct expo-
sure to radiant heat from the central region of the vessel.
The above-described process also produces a stream of off-gas and entrained solids
that is discharged from the vessel via an outlet 27 in an upper section of the vessel.
The off-gas stream is processed by separating solids from the off-gas and returning the
separated solids to the vessel via a solids return leg 29. Thereafter, the off-gas is
treated by a series of steps of including (a) solids removal, (b) cooling the off-gas, (c)
H2O removal, (d) CO2 removal, (e) compression, and (f) reheating. The treated off-gas
is thereafter returned to the vessel as part of the fluidising gas.
The above-described process produces a stream of solids, including at least partially
reduced iron ore and char, that is discharged from the vessel via an outlet 25 in the
base of the vessel. The solids stream may be processed by separating the at least

partially reduced iron ore and a portion of the other solids. The other solids, predomi-
nantly char, separated from the product steam may also be returned to the vessel as a
part of the solids feed for the process. The at least partially reduced iron ore is further
processed as required. By way of example, the at least partially reduced iron ore may
be supplied to a molten bath-based smelting vessel and smelted to molten iron, for ex-
ample by a process such as the so called "Hlsmelt process".
As is indicated above, the present invention was made during the course of an on-
going research project carried out by the applicant to develop CIRCOFER technology
for the direct reduction of iron ore. The research project included a series of pilot plant
runs on 350mm diameter and 700mm diameter pilot plant set-ups of the applicant.
The following discussion focuses on research work on the 700 mm diameter vessel
pilot plant.
The pilot plant comprises an apparatus of the type shown in Figure 1 and 2. The pilot
plant was operated as a circulating fluidised bed at atmospheric pressure. The vessel
has a height of 10.7 m. An upper section of the vessel has a height of approximately
8.9 m and an internal diameter of 700 mm. A lower section of the vessel has a height
of approximately 1.8m and an internal diameter of 500 mm. This height of 1.8 m inclu-
des the height of a fluidising grate and a transition section between the 500 mm diame-
ter and the 700 mm diameter sections. The vessel is refractory lined.
Off-gas from the vessel was processed to remove entrained solids by passing the off-
gas successively through 3 cyclones connected in series. The first cyclone (cyclone 1)
received off-gas directly from the vessel. Solids separated in the cyclone were re-
turned to the vessel via a seal pot that provided for pressure sealing. The second cyc-
lone (cyclone 2) received off-gas from cyclone 1. Solids separated in the cyclone were
returned to the vessel via a direct return of solids (i.e. no seal pot). The third cyclone
(cyclone 3) received off-gas from the second 2. Solids separated by cyclone 3 were
not returned to the vessel.

After solids separation by the three cyclones, the off-gas was further treated by a radial
flow scrubber, which further removed solids from the off-gas. These solids were con-
centrated by a thickener and then passed through a drum filter to produce thickener
sludge.
Off-gas leaving the radial flow scrubber was then treated by a tube cooler that operated
to dewater the off-gas by cooling it to within the range 10-30°C. Following treatment by
the tube cooler, the off-gas was combusted.
The fluidised bed was fluidised by air during the initial stages of testing and was later
fluidised by a mixture of nitrogen and hydrogen gas. As there were no provisions for
processing and recycling the process off-gas, e.g. CO2 removal and compression, it
was not possible for it to be returned to the vessel as fluidising gas. In this regard,
hydrogen gas was used to simulate the effect of using processed off-gas as fluidising
gas.
In summary, the research work demonstrated the following:
The concept of a coal based fluidised bed reduction process with oxygen injection, pro-
ducing a reduced product with metallisation levels of up to 78%.
Injecting oxygen into/or close to a fluidised bed with up to 42% metallic iron in the bed
appears to be feasible without the formation of accretions.
The concept of simultaneously reducing iron ore and partially burning coal for energy in
a single bed vessel appears to be feasible, at metallic iron loadings up to 48% in the
product.
The position of the oxygen lance in the vessel is important because of the desirability of
transferring the heat of oxidation back into the bed while minimising the level of iron re-
oxidation. The 4-m position is about right for the conditions tested.

High phosphorus Brockman iron ore was successfully fluidised and reduced without
excessive dust make. (Brockman ore is a friable West Australian iron ore made avail-
able by Hamersley Iron Pty Ltd, Perth, Western Australia.)
Objectives of the experimental program:
The primary objective was to achieve stable operation for a significant amount of time
with high phosphorus Brockman ore (-3mm) and Blair Athol coal.
The plan was to operate with low iron ore feed (up to 20% in product discharge) for two
days with the oxygen lance in a low position (1.9-m above the distributor plate (not
shown in the Figure) of the vessel. The aim was then to operate for three days with
high ore feed (up to 70% in the product) with the oxygen lance in an upper position
(3.8-m above the distributor plate).
Start-up:
The campaign started on the 9th of December 2003 at 0600 hrs with a gradual heat up
of the 700-mm vessel (hereinafter also referred to as a "CFB") using alumina as the
bed material. Once the target temperature was reached, coal and oxygen were intro-
duced into the vessel at 1550 hrs. The oxygen rate was increased up to 105 Nm3/hr
while the coal rate was in the range 300-450 kg/hr.
Operation with coal and oxygen 10/12/03 - 11/12/03
Operation with coal, air and oxygen was conducted on 10/12/03. The operation was
very smooth with the system stabilising fairly quickly and the vessel maintaining its
temperature of 900-930°C without any problems.
The standard operating conditions during this period were as follows.
CFB temperature: 930°C bottom and 900°C top
Fluidising gas flowrate: 140Nm3/hr (N2) and 300Nm3/hr (air)

Pressure drop CFB: 80-140 mbar
Oxygen flowrate: up to 100 Nm3/hr
N2 shield gas flowrate: 30 Nm3/hr
Coal Feed Rate: 340-450 kg/hr
A summary of the results is as follows:
Bed Discharge Rate: 100-160 kg/hr
Cyclone 3 Discharge: 10-14 kg/hr
Offgas Analysis

The discharge product was clean with only some small +2mm pieces which looked like
residual refractory material. The dust make was reasonably low with charge reporting to the final cyclone discharge.
Operation with Iron Ore (10-140 kg/hr), Coal and Oxygen (lance 2-m height) 10/12/03 -
12/12/03
10/12/03 2200 - 11/12/03 0600: Iron Ore at 10 kg/hr
Iron ore ( 10 kg-hr. Hydrogen was also introduced into the fluidising gas at a rate of 20 Nm3/hr to
simulate use of processed off-gas as fluidising gas. The operation was smooth with the
bed AP being maintained at about 100-120 mbar and the temperature profile having a
range of only 10°C between the bottom and the top of the bed.
The product appeared fine without any signs of accretions or agglomerates. However,
on screening the product (at 2mm) some larger scale type material was found but this
was only a very small proportion of the overall product. The scale appeared to be

made up of ash/char and probably formed on the walls of the vessel or distributor plate
in the vessel.
The standard operating conditions and results during this period were as follows.
CFB temperatures: 930°C bottom and 900°C top
Fluidising gas flowrate: 350 Nm3/hr (N2) and 20 Nm3/hr (H2)
Pressure drop CFB: 100-130 mbar
Oxygen flowrate: 100-115 Nm3/hr
N2 shield gas flowrate: 30 Nm3/hr
Coal Feed Rate: 280-360 kg/hr
Iron Ore Feed Rate: 10 kg/hr
A summary of the results is as follows:
Bed Discharge Rate: 125 kg/hr
Cyclone Discharge: 15 kg/hr
Offgas Analysis

The iron ore feed rate was increased up to 20 kg/hr at 0600 on 11/12/03 until 1200
11/12/03 and the hydrogen gas rate was also increased up to 40 Nm3/hr. The operation
continued to be smooth without any disruptions. The vessel bed pressure was being
maintained at about 80-100 mbar and the temperature profile had a range of only 10°C
between the bottom and the top of the bed.

The appearance of the product continued to be good without any signs of accretions or
agglomerates. As before the only exception to this was the odd piece of scale type
material, which appeared to be composed of ash/char.
The standard operating conditions and results during this period were as follows.
CFB temperatures: 952°C bottom and 940°C top
Fluidising gas flowrate: 350 Nm3/hr (N2) and 40 Nm3/hr
Pressure drop CFB: 80-100 mbar
Oxygen flowrate: 112 Nm3/hr
N2 shield gas flowrate: 30 Nm3/hr
Coal Feed Rate: 430 kg/hr
Iron Ore Feed Rate: 20 kg/hr
A summary of the results is as follows:
Bed Discharge Rate: 125 kg/hr
Cyclone 3 Discharge: 15 kg/hr
Offgas Analysis


11/12/03 1200 - 12/12/03 0600: tron Ore at 40 kg/hr
Summary:
The iron ore feed rate was increased up to 40 kg/hr at 1200 on 11/12/03 and operated
with this rate until 0600 12/12/03, while the hydrogen gas rate was maintained at 40
Nm3/hr and the coal rate was around 360-420 kg/hr. The operation continued to be
smooth without any disruptions and the iron product discharge was highly metallised.
Dust make was also low with less than 10% of the total discharge coming from the final
cyclone (i.e. cyclone 3). The vessel bed AP was being maintained at about 90-135
mbar and the temperature profile had a range of less than 10°C between the bottom
and the top of the bed.
Results
The appearance of the product continued to be good without any signs of accretions or
agglomerates.
The standard operating conditions and results during this period were as follows.
CFB temperatures: 953°C bottom and 941 °C top
Fluidising gas flowrate: 370 Nm3/hr (N2) and 40 Nm3/hr (H2)
Pressure drop CFB: 98-130 mbar
Oxygen flowrate: 113 Nm3/hr
N2 shield gas flowrate: 30 Nm3 /hr
Coal Feed Rate: 426 kg/hr
Iron Ore Feed Rate: 40 kg/hr
A summary of the results is as follows:
Bed Discharge Rate: 190-210 kg/hr
Cyclone 3 Discharge: 15-20 kg/hr
Offgas Analysis


The high metallisation achieved (70-77%) indicates that the oxygen lance (even at its
1.9-m position) did not penetrate too far to the bottom of the bed and that there was
good segregation within the bed. The lower part of the bed is iron rich. The higher part
of the bed is carbon rich and this is interacting with the oxygen lance to generate heat
and this heat is then transferred back into the bed by the recirculation of the solids to
the lower parts of the bed. The low CO/CO2 ratio in the off-gas indicates achievement
of high post combustion, with the energy levels being transferred back into the bed,
while maintaining high metallisation levels in the product discharge.

The iron levels in the product and the degree of metallisation indicates that the 700-mm
vessel can be operated in gasification mode with up to 20-25% metallic iron content
without any problems with accretions. This is a significant achievement.
Oxygen Lance Inspection (12/12/03)
The lance was taken out of the 700-mm vessel and inspected on 12/12/03.
In summary, the lance was clean. The water cooled pipe as well as the nozzle tip had
no evidence of any buildup of material.
The lance was repositioned in the vessel at a higher position i.e. 3.8-m above the dis-
tributor plate. The vessel was restarted with coal and oxygen and then once stabilised
iron ore and hydrogen.
Operation with Iron Ore (110-200 kg/hr). Coal and Oxygen (lance 4-m height) 13/12/03
-16/12/03
13/12/03 0600 - 13/12/03 1200: Iron Ore at 110 ko/hr
Summary;
The iron ore feed rate was increased stepwise up to 110 kg/hr at 0625 on 13/12/03 and
operated with this rate until 1200 13/12/03 while the hydrogen gas rate was also in-
creased stepwise up to 110 Nm3/hr over a 2 hr period. The coal rate was around 360-
400 kg/hr. The operation continued to be smooth without any disruptions and the iron
product discharge from the vessel was up to 78% metallised. Dust make was also low
with vessel bed AP was being maintained at about 90-135 mbar and the temperature profile
had a range of less than 5°C between the bottom and the top of the bed.
Increasing the lance height from 1.9m to 3.8m did not seem to impact on the bed tem-
perature profile. In fact, the temperature spread was less than 5°C from top to bottom.

Results:
The appearance of the product continued to be good without any signs of accretions or
agglomerates.
The standard operating conditions and results during this period were as follows.
CFB temperatures: 953°C bottom and 951 °C top
Fluidising gas flowrate CFB 10 Nm3/hr (N2) at 860°C, 110 Nm3/hr (N2) at 740°C, 180
Nm3/hr (N2) at 680°C, and 110 Nm3/hr (H2) at 860°C
Pressure drop CFB: 80-100 mbar
Oxygen flowrate: 110 Nm3 /hr
N2 shield gas flowrate: 30-40 Nm3/hr
Coal Feed Rate: 360-400 kg/hr
Iron Ore Feed Rate: 110 kg/hr
A summary of the results is as follows:
Bed Discharge Rate: 162 kg/hr
Cyclone 3 Discharge: 16 kg/hr
Offgas Analysis


With the higher oxygen lance position the uniform bed temperature profile of the lower
lance was maintained. This indicates that even with the oxygen lance at the 3.8m posi-
tion the solids recirculation profile is such that enough heat is transferred back into the
bottom of the bed.
The temperature profile in the vessel and the cyclones indicated that there was proba-
bly no increase in dust make with the increase in iron ore feed rate up to 110 kg/hr.
The discharge from the final cyclone relative to the vessel also did not change signifi-
cantly. This suggests that either the iron ore is not breaking down as much as predicted
or that any fines generated are re-agglomerated in the high temperature region of the
oxygen lance.
13/12/03 1200 - 16/12/03 0500: Iron Ore at 120 - 230 ka/hr
Summary:
For the first period of this operation from 17:00 13/12/03 to 12:00 15/12/03 the opera-
tion rate was approximately 120 kg/h iron ore feed. This included a period of distur-
bance where there was no feed. The final period operated at approximately 230 kg/h
iron ore feed.
The operation with 230 kg/hr iron ore feed rate was smooth without any disruptions and
the iron product discharge from the CFB ranged from 48% to 78% metallised. Dust
make was also low at bed AP was being maintained at about 80-100 mbar and the temperature profile range
had now increased to about 20°C between the bottom and the top of the bed.
Operating the vessel at the higher iron ore feed rate of 200 kg/hr increased the range of
the CFB temperature profile with the bottom part of the bed now being up to 20°C
colder than the middle of the bed. The metallisation levels were also lower at the
higher iron ore feed rates but they were still in the 60-80% metallisation range.

Results:
The appearance of the product continued to be good without any signs of accretions or
agglomerates.
The standard operating conditions and results during this period were as follows.
CFB temperatures: 947°C bottom and 960°C top
FB gas heater temperature: 740°C and 615°C main heater
Fluidising gas flowrate CFB: 20 Nm3/hr (N2) at 840°C, 100 20 Nm3/hr (N2) at 740°C,
185 20 Nm3/hr (N2) at 615°C, and 140 Nm3/hr (H2) @ 840°C
Pressure drop CFB: 83-96 mbar
Oxygen flowrate: 113 Nm3/hr
N2 shield gas flowrate: 30-40 Nm3/hr
Coal Feed Rate: 380 kg/hr
Iron Ore Feed Rate: 200 kg/hr
A summary of the results is as follows:
Bed Discharge Rate: 227-286 kg/hr
Cyclone 3 Discharge: 18-24 kg/hr
Offgas Analysis (0400 hrs 15/12/03)




At the high iron ore feed rates (200 kg/hr) the discharge from the vessel increased sig-
nificantly while the discharge from the final cyclone only increased slightly. However,
the discharge from the final cyclone relative to the vessel did not seem to change. It
was further observed that the amount of fines the amount of fines breaking down as much as predicted or that any fines generated are re-agglomerated
in the high temperature region of the oxygen lance. The temperature profile through
the cyclones also supports this since there were no significant increases in tempera-
tures through the cyclone system at the higher iron ore feed rates. The product metal-
lisation levels were maintained in the range of 68-78% during the high iron ore feed
rates while the product discharge had up to 48% metallic iron.
Oxygen Lance and Vessel Inspection (16/12/03 and 19/12/03)
The lance was taken out of the 700-mm vessel and inspected on 16/12/03. In sum-
mary, the lance was fairly clean. The water cooled pipe had a thin coating of material
while the nozzle tip was relatively clean. The nature of the build up (flaky and thin)
suggested that this would not lead to any operational problems.
Iron Distribution & Agglomeration
Analysis of the Brockman ore sample used as feed to the fluidised bed indicated a fines
content of approximately 10.6% sub 45 micron. These units were expected to appear
as output from cyclone 3 or as thickener sludge. Due to the friable nature of Brockman
Ore, it was expected that additional fines would be produced during processing. It was
therefore expected that the percentage of iron units exiting the system through cyclone
3 would exceed 10.6%.
It was observed that approximately 7% of the iron units input to the fluidised bed were
discharged through cyclone 3, either as direct output from cyclone 3 (approximately
4%) or as output from the radial flow scrubber (approximately 3%). Analysis of the
main product output from the fluidised bed indicated that an agglomeration mechanism
was present within the process. This mechanism appeared to be primarily smaller par-

tides, typically sub 100 micron particles, agglomerating to each other and larger parti-
cles.
Many modifications may be made to the embodiments of the present invention shown
in Figures 1 and 2 without departing from the spirit and scope of the invention.

WE CLAIM :
1. A direct reduction process for a metalliferous material such as described
herein which comprises supplying the metalliferous material, a solid carbona-
ceous material such as herein described, an oxygen-containing gas such as
herein described, and a fluidising gas such as herein described into a fluidised
bed in a vessel and maintaining the fluidised bed in the vessel, at least par-
tially reducing metalliferous material in the vessel, and discharging a product
stream that comprises the at least partially reduced metalliferous material from
the vessel, wherein the process comprises the following steps:
(a) reducing the metalliferous material in a solid state in a metal-rich
zone in the vessel;
(b) injecting the oxygen-containing gas above the supply of the met-
alliferous material into a carbon-rich zone in the vessel with a downward flow
in a range of plus or minus 40 degrees to the vertical and generating heat by
reactions between oxygen and the metalliferous material, the solid carbona-
ceous material and other oxidisable solids and gases in the fluidised bed, and
(c) transferring heat from the carbon-rich zone to the metal-rich zone
by movement of solids within the vessel.

2. Process as claimed in claim 1, wherein the oxygen-containing gas is
injected with a downward flow in a range of plus or minus fifteen degrees to
the vertical.
3. Process as claimed in claim 1 or 2, wherein the metal-rich zone is
formed in a lower section of the vessel and the carbon-rich zone is formed in
an intermediate section of the vessel.
4. Process as claimed in claim 3, wherein the intermediate section is in-
termediate said lower section and an upper section of the vessel.
5. Process as claimed in any of the preceding claims, wherein the oxygen-
containing gas is injected into a central region in the vessel.

6. Process as claimed in any of the preceding claims wherein the metalli-
ferous material is in the form of iron ore fines, and wherein the bulk tempera-
ture in the fluidised bed is in the range 850°C to 1000°C.
7. Process as claimed in any of the preceding claims wherein the metalli-
ferous material is in the form of iron ore fines, and wherein the pressure in the
vessel is controlled to be in the range of 1-10 bar absolute.
8. Process as claimed in any of the preceding claims, wherein the oxygen-
containing gas is injected so that there is a downward flow of the gas in the
vessel.
9. Process as claimed in any of the preceding claims, wherein the oxygen-
containing gas is injected via at least one lance having a lance tip with an out-
let positioned in the vessel inwardly of the side wall of the vessel in the central
region of the vessel.
10. Process as claimed in claim 9, wherein the lance tip is directed vertically
downwardly.
11. Process as claimed in claim 9 or 10, wherein the position of the lance
and, more particularly, the height of the outlet of the lance tip, is determined by
reference to factors, such as the oxygen-containing gas injection velocity, the
vessel pressure, the selection and amounts of the other feed materials to the
vessel, and the fluidised bed density.
12. Process as claimed in any of claims 9 to 11, wherein at least the lance
tip is water-cooled.
13. Process as claimed in any of claims 9 to 12, wherein an outer surface of
the lance is water-cooled.

14. Process as claimed in any of the preceding claims, wherein the oxygen-
containing gas is injected through a central pipe of the lance.
15. Process as claimed in any of the preceding claims, wherein the oxygen-
containing gas is injected with a velocity to form a substantially solids-free
zone in the region of the lance tip.
16. Process as claimed in any of the preceding claims, wherein nitrogen
and/or steam and/or other suitable shrouding gas such as herein described is
injected and the region of the outlet of the lance tip is shrouded.
17. Process as claimed in any of the preceding claims, wherein the metalli-
ferous feed material, the carbonaceous material, the oxygen-containing gas,
and the fluidising gas is supplied to the fluidised bed and the fluidised bed is
maintained with (a) a downward flow of the oxygen-containing gas, (b) an up-
ward flow of solids and fluidising gas countercurrent to the downward flow of
the oxygen-containing gas, and (c) a downward flow of solids outwardly of the
upward flow of solids and fluidising gas.
18. Process as claimed in claim 17, wherein solids in the upward and down-
ward flows of solids are heated by heat generated by reactions between the
oxygen-containing gas, the solid carbonaceous material and other oxidisable
materials in the carbon-rich zone.
19. Process as claimed in claim 17 or 18, wherein the upward and down-
ward flows of solids shield the side wall of the vessel from radiant heat gener-
ated by reactions between the oxygen-containing gas and the solid carbona-
ceous material and other oxidisable solids and gases in the fluidised bed.
20. Process as claimed in any of the preceding claims wherein the metalli-
ferous material is in the form of iron ore fines, and wherein the fines are sized
at
21. Process as claimed in any of the preceding claims, wherein the fines
have an average particle size in the range of 0.1 to 0.8 mm.
22. Process as claimed in any of the preceding claims, wherein the carbo-
naceous material is coal.
23. Process as claimed in any of the preceding claims, wherein the fluidis-
ing gas comprises a reducing gas, such as CO and H2.
24. Process as claimed in claim 23, wherein the amount of H2 in the fluidis-
ing gas is selected to be at least 15% by volume of the total volume of CO and
H2 in the gas.
25. Process as claimed in any of the preceding claims, wherein the product
stream comprising at least partially reduced metalliferous material is dis-
charged from the lower section of the vessel.
26. Process as claimed in claim 25 wherein the product stream also com-
prises char, and wherein at least a portion of the char is separated from the
product stream.
27. Process as claimed in claim 26, wherein the separated char is returned
to the vessel.
28. Process as claimed in to any of the preceding claims, wherein an off-
gas stream containing entrained solids from an upper section of the vessel is
discharged.
29. Process as claimed in claim 28, wherein solids from the off-gas stream
are separated.

30. Process as claimed in any of the preceding claims, wherein a circulating
fluidised bed is maintained by separating entrained solids from the off-gas
stream and the solids separated from the off-gas are returned to the vessel.
31. Process as claimed in claim 30, wherein solids separated from the off-
gas are returned to the lower portion of the vessel.
32. Process as claimed in any of the preceding claims, wherein metallifer-
ous feed material is preheated with the off-gas from the vessel.
33. Process as claimed in any of the preceding claims, wherein the off-gas
is treated after the preheating step and at least a portion of the treated off-gas
is returned to the vessel as the fluidising gas.
34. Process as claimed in claim 33, wherein the off-gas treatment com-
prises one or more of (a) solids removal, (b) cooling, (c) H2O removal; (d) CO2
removal, (e) compression, and (f) reheating.
35. Process as claimed in claim 33 or 34, wherein the off-gas treatment
comprises returning solids to the vessel.
36. Process as claimed in any of the preceding claims, wherein the oxygen-
containing gas comprises at least 90% by volume oxygen.
37. Process as claimed in any of the preceding claims, wherein the process
comprises an additional smelting process for melting and further reducing the
partially reduced metalliferous material to a molten metal.


A direct reduction process for a metalliferous material is disclosed. The
process comprises supplying the metalliferous material, a solid carbonaceous
material, an oxygen-containing gas, and a fluidising gas into a fluidised bed in
a vessel and maintaining the fluidised bed in the vessel, at least partially reducing
metalliferous material in the vessel, and discharging a product stream
that comprises the at least partially reduced metalliferous material from the
vessel, wherein the process comprises the steps of: (a) reducing the metalliferous
material in a solid state in a metal-rich zone in the vessel; (b) injecting
the oxygen-containing gas above the supply of the metalliferous material into a
carbon-rich zone in the vessel with a downward flow in a range of plus or minus
40 degrees to the vertical and generating heat by reactions between oxygen
and the metalliferous material, the solid carbonaceous material and other
oxidisabie solids and gases in the fluidised bed, and (c) transferring heat from
the carbon-rich zone to the metal-rich zone by movement of solids within the
vessel.

Documents:

03176-kolnp-2006 abstract.pdf

03176-kolnp-2006 claims.pdf

03176-kolnp-2006 correspondence others.pdf

03176-kolnp-2006 description(complete).pdf

03176-kolnp-2006 drawings.pdf

03176-kolnp-2006 form-1.pdf

03176-kolnp-2006 form-3.pdf

03176-kolnp-2006 form-5.pdf

03176-kolnp-2006 international publication.pdf

03176-kolnp-2006 pct other document.pdf

03176-kolnp-2006-assignment.pdf

03176-kolnp-2006-correspondence others-1.1.pdf

03176-kolnp-2006-pct others.pdf

03176-kolnp-2006-priority document.pdf

3176-KOLNP-2006-ABSTRACT 1.1.pdf

3176-KOLNP-2006-ABSTRACT-1.2.pdf

3176-KOLNP-2006-AMANDED CLAIMS-1.1.pdf

3176-KOLNP-2006-AMANDED PAGES OF SPECIFICATION.pdf

3176-kolnp-2006-assignment.pdf

3176-KOLNP-2006-CLAIMS.pdf

3176-KOLNP-2006-CORRESPONDENCE 1.1.pdf

3176-KOLNP-2006-CORRESPONDENCE 1.3.pdf

3176-KOLNP-2006-CORRESPONDENCE-1.2.pdf

3176-kolnp-2006-correspondence.pdf

3176-KOLNP-2006-DESCRIPTION (COMPLETE) 1.1.pdf

3176-KOLNP-2006-DESCRIPTION (COMPLETE)-1.2.pdf

3176-KOLNP-2006-DRAWINGS 1.1.pdf

3176-KOLNP-2006-DRAWINGS-1.2.pdf

3176-KOLNP-2006-EXAMINATION REPORT REPLY RECIEVED.pdf

3176-kolnp-2006-examination report.pdf

3176-KOLNP-2006-FORM 1 1.1.pdf

3176-kolnp-2006-form 18.1.pdf

3176-kolnp-2006-form 18.pdf

3176-KOLNP-2006-FORM 2.pdf

3176-KOLNP-2006-FORM 3 1.1.pdf

3176-kolnp-2006-form 3.pdf

3176-kolnp-2006-form 5.pdf

3176-KOLNP-2006-FORM-27.pdf

3176-KOLNP-2006-FORM-271.1.pdf

3176-kolnp-2006-gpa.pdf

3176-kolnp-2006-granted-abstract.pdf

3176-kolnp-2006-granted-claims.pdf

3176-kolnp-2006-granted-description (complete).pdf

3176-kolnp-2006-granted-drawings.pdf

3176-kolnp-2006-granted-form 1.pdf

3176-kolnp-2006-granted-form 2.pdf

3176-kolnp-2006-granted-specification.pdf

3176-KOLNP-2006-OTHERS-1.1.pdf

3176-KOLNP-2006-OTHERS.pdf

3176-kolnp-2006-others1.2.pdf

3176-KOLNP-2006-PA.pdf

3176-KOLNP-2006-PETITION UNDER RULE 137.pdf

3176-kolnp-2006-reply to examination report.pdf

abstract-03176-kolnp-2006.jpg


Patent Number 249004
Indian Patent Application Number 3176/KOLNP/2006
PG Journal Number 38/2011
Publication Date 23-Sep-2011
Grant Date 20-Sep-2011
Date of Filing 31-Oct-2006
Name of Patentee OUTOKUMPU TECHNOLOGY OYJ
Applicant Address RIIHITONTONTIE 7, F1-02200 ESP00, FINLAND
Inventors:
# Inventor's Name Inventor's Address
1 DRY ROD 326 THE BOULEVARD, CITY BEACH, W.A. AUSTRALIA
2 ORTH ANDREAS OBERE ROMERHOFSTRASSE 132, 61381 FRIEDRICHSDORF, GERMANY
3 PHILP DONALD KEITH (DECEASED) 1 SHERBROOK GARDENS, BIBRA LAKE, W.A.6163, AUSTRALIA
4 EICHBERGER HEINZ AM HAAG 12J, 65812 BAD SODEN , GERMANY
PCT International Classification Number C21B 5/14,C21B 13/00
PCT International Application Number PCT/EP2005/005472
PCT International Filing date 2005-05-20
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 2004902900 2004-05-31 Australia