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Influences on bulk density and its effect on coke quality and internal gas
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Article · January 2013

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 Influences on Bulk Density and Its Effect on Coke Quality and Internal Gas Pressure

Dr. Drazen Gajic

DMT GmbH & Co. KG,
Cokemaking Technology Division,
Am Technologiepark 1,
45307 Essen, Germany
Phone: +49 201 172 1826
Fax: +49 201 172 1328
E-mail: drazen.gajic@dmt.de

Key words: bulk density, carbonization, coke quality, internal gas pressure

INTRODUCTION

The optimum use of alternative raw materials to increase the viability and competitiveness of European coke plants is essential in the
current volatile global economic situation. The increasing of the substitution of expensive premium coking coals through medium and
low caking coals and alternative raw materials have to be developed. Pre-carbonization technologies could be suitable to increase the
charge density in the oven and to maintain coke quality and safe oven operation. Possible useful densifying technologies are pre-
drying, briquetting, stamping, improved crushing or oiling1-24.
The project “Improving the Use of Alternative Raw Materials in Coking Blends through Charge Densification” carried out with a
financial grant of the Research Programme of the Research Fund for Coal and Steel compromises the investigation of all pre-
carbonization technologies. DMT is responsible to investigate the influences on bulk density by water adjustment and oiling.
The oiling with liquid organic additives is common practice in coking plants for densification of coke charges, usually it is
commercial or by-product waste oil provided by refineries for utilization in coke ovens. DMT will investigate systematically the oiling
effect on bulk density, coking behavior and coke quality.
 METHODS

Cold chamber rig

DMT GmbH & Co. KG (DMT) used the cold chamber rig for the bulk density tests. The cold chamber is a box. Above the box is
arranged a vertical pipe. The pipe length is 4 m and the diameter is 300 mm. The coal drops in to the coal chamber from 4 m height.
After filling the coal is uniformly distributed in the box for the reason that the top of the coal cuboids should be in-plane with the top
edge of the cold chamber. The chamber dimensions and the sketch of the cold chamber are shown in Figure 1.

Figure 1: Cold chamber rig

The coal cuboid was released in a hopper by opening the bottom door of the box. Subsequently, the coal is weighted. The calculation
of the bulk density was determined by the coal weight and the volume of the box.

Pilot-scale coke oven (Small-scale coking retort)

The pilot scale carbonization test permits less time consuming investigations with limited quantities of coal (approx. 11 kg charging
weight) in comparison to the semi-industrial scale coke oven. Figure 2 contains the most important data of the carbonization retort.
While the semi-industrial scale oven is always operated as close as possible to the plant conditions, the heating conditions of the
electrically heated retort are always fixed standard conditions. After a coking time of approx. four hours a final coke temperature
between 1,030 and 1,040 °C is attained. Size distribution moisture content and bulk density are adjusted as given by the industrial
scale plant. Despite from the fact that the course of carbonization differs in some details from the industrial scale oven the laboratory
scale carbonization delivers valuable results concerning coke quality with respect to CRI and CSR.
Probes
Final coke
Temperature
temperature:
gas pressure
1030 - 1040 °C
Coking time:
approx. 4 hours

Coal charge
Charging height: 505 mm
Internal diameter: 180 mm
Charge weight: approx. 11 kg

Insulation brick

Figure 2: Pilot-scale coke oven

Semi-industrial coke oven
DMT is operating a movable wall oven with underfired natural gas heating flues. The chamber width is flexible and can be varied in
three dimensions (450, 600 and 750 mm). The capacity of the oven is 450 to 1,500 kg depend on chamber width and bulk density.
The refractory brick work consists of Silica bricks and the heating flues have similar cross cut dimensions as those of the industrial
scale oven. Therefore the heat transfer from the heating walls into the coal charge occurs in a very similar manner compared with the
industrial scale plant. Thus an optimum simulation of the plant conditions is guaranteed.

Figure 3. Semi-industrial carbonization test oven with movable wall

Structure and dimensions of the semi-industrial coke oven used by DMT are shown in Figure 3 and Figure 4. Figure 3 displays a cross
cut of the movable wall oven. The chamber width is the decisive dimension for the heat transfer from the heating walls to the coal
charge and is simulated in the test oven in the scale 1:1. Length and height of the pilot oven chamber are reduced quite significantly:
the distance between the door plugs is approx. 1.3 m and the charging height approx. 1.0 m.

Figure 4: Semi-industrial coke oven – dimensions

The particular feature of the semi-industrial coke oven is its ability to modify chamber width between 450 and 750 mm. Besides from
the possibility to vary the chamber width the movable wall oven has the advantage that the forces exerted to the movable wall during
carbonization by the swelling pressure of the charge can directly be monitored via load cells. Moreover, the internal gas pressure, the
course of temperature in the coal charge center and the coal charge shrinkage are determined by means of adequate probes (see
Figure 4).
The semi-industrial coke oven can be charged either by gravity or by stamp charging. The charge weight ranges between approx. 500
and 1,500 kg (depending on chamber width and coal bulk density). The produced amount of coke is sufficient for the determination of
all the usual coke quality indices.
Under the premises that the operating conditions are exactly simulated concerning size distribution, moisture content, bulk density and
heating flue temperature reliable results for the plant operator can be guaranteed with respect to the swelling behavior of the coal
charge and the resulting coke quality.
RESULTS

Water adjustment
DMT tested four single coals in the cold chamber. The single coals are the American low volatile coal Kepler, the middle volatile
coals Hail Creek (Australia) and Elk Valley Standard (Canada) and the American high volatile coal Carter Roag. The main properties
of the coals are shown in Table 1.
Table 1: Coal Properties
Carter Roag Elk Valley St. Hail Creek Kepler
Ash (db) % 9.8 10.1 10.2 7.2
Volatile (daf) % 32.0 25.5 22.8 21.3
Fe2O3 (Coal ash) % 5.3 7.7 9.8 7.9
CaO (Coal ash) % 3.1 2.3 2.9 1.7
Vitrinite % 76 59 51 80
Inertinite % 13 32 41 14
Rm - 1.05 1.21 1.27 1.39
Contraction % 30 11 20 30
Dilatation % 88 4 -7 68
Max Fluidity DDPM 534 48 31 165
CSN - 8.0 7.0 6.0 9.0
Size / < 2.0 mm % 74.2 72.2 58.3 69.3

For the tests the moisture content was adjusted by 1.5 %, 4 %, 6 %, 8 %, 10 %, 12 % and 14 %. Figure 5 shows the results for the four
single coals.

Figure 5: Bulk density (dry) for the four single coals

The diagram shows the typical curve shapes of bulk density progression when moisture content varied 23. The relation between bulk
density and moisture content is affected by size distribution, interparticle friction and particle deformation. These factors are not
limited for the coal particles, also valid for the agglomerated coal particle during the packing process24. Other very important factor is
the surface property of the coal which depends strongly from the rank of the coal. Figure 6 indicates the influence of the fix carbon
content on the bulk density for different moisture contents.

Figure 6: Effect of fix carbon content and moisture content on the bulk density (dry)
The increasing of the moisture content reduces the influence of coal surface properties on the bulk density. For moisture contents
higher than 6 % the influence of the coal surface is negligible and the level of the bulk densities is very low. The bulk densities rises
with higher moisture content than 10 %, but in a very small range not comparable with the increasing of bulk density with lower
moisture content than 6 %.
The systematically investigation of the impact of water content, different coals and coal blends and grain size on the bulk density
results in a high amount of data that allows to create a formula for the calculation of expected dry bulk density (kg/m³) by following
data input: water content (%), volatile matter daf (%) and grain size average (mm). The obtained calculation formula is
Bulks density (dry) [kg/m³] = 838.18 + 2.98 * moisture² - 61.12 * moisture + 2.01 * volatile matterdaf + 59.73 * grain size average
The Figure 7 shows the high correlation between measured bulk densitiesdry (kg/m³) and calculated data from the formula.

Figure 7: Measured bulk densitiesdry (kg/m³) and calculated data from the formula
Oiling
For the oiling test it was used a standard fuel oil and a used fuel oil. The specification with relevant data for the flow characteristics of
the standard fuel oil is shown in Table 2.
Table 2: Fuel oil specification
Density (15 °C) g/ml 0.86
Cloud point °C <1
Kin. Viscosity (20 °C) mm²/s 5.5

The used oil is residue oil from a machine shop for trucks that its replaced by fresh oil in engines. The oil has higher amount of
cracked long chain hydrocarbons and higher kinematic viscosity (40°C; 51 mm²/s) as the standard fuel oil.
The parameter water content was fixed for all tests at 8 %. The oil content mass weight share was increased from 0 % in 0.25 % steps
up to mass weight sharer when the clear decline of the bulk density is recognized. Figure 8 shows the results of the oiling tests with
standards oil and the four single coals, Carter Roag, Elk Valley Standard, Hail Creek and Kepler.

Figure 8: Bulk density (dry) for the four single coals with fuel oil

All curves indicate the same progression. In the first part of the curve progressions it is to recognize a clear increasing of the bulk
densities. All single coals reach a maximum by an oil content of 0.5 %. A declining is identified after reaching the maximum. The
difference between the coals is in the reached absolute bulk density at 0.5 % oil content. This impact of oiling is also recognized when
the bulk densities at 0.5 oil content are compared with the bulk densities from the cold chamber test at 8 % water content without oil.
Table 3 shows this comparison.
Table 3: Fuel oil – Water - Comparison
8 % moisture 8 % moisture Difference Relative
+ 0.5 % fuel oil
kg/m³ (dry) kg/m³ (dry) kg/m³ (dry) %
Carter Roag 660 705 45 6.8
Elk Valley St. 601 735 134 22.3
Hail Creek 612 768 156 25.5
Kepler 616 749 133 21.6

The results of the oiling test with used oil shows the same progression of the curves, but the positive effect of bulk density increasing
is hear clear lower due to the degradation of the hydrocarbons during the insert in the engine. Figure 9 shows the result of the oiling
test with used oil and the four single coals.
 Figure 9: Bulk density (dry) for the four single coals with used fuel oil
The different impact on the bulk density by same oil content with different coals accords with the experience of DMT. DMT
recognized that different coals need different amount of oil to achieve the desirable bulk density for semi-technical carbonization tests.
The Figure 10 shows the different oil content that needed to achieve a bulk density of 800 kg/m³ in the semi-industrial carbonization
oven. The Figure 10 show that the needed oil content depends from the maceral group distribution of the coal.

Figure 10: DMT oiling experience for the adjustment for semi-technical carbonization tests
The relation between the vitrinite content of the single coals and the achieved bulk densities at 0.5 % oil content is shown in Figure 11.
 Figure 11: Relation between vitrinite content and bulk density at 0.5 % oil content
Figure 11 shows a weak relation between vitrinite and bulk density. The movement of the curve indicates a decline of bulk density
with higher vitrinite content. This fact approved the experience of DMT, which is shown in Figure 10. The weak relation could be
reasoned in the hydrophilic character of vitrinite. The hydrophobic charter of the oil should be better related to the hydrophobic part of
the coal. Figure 12 shows the relation between the inertinite content and the bulk density achievable by 0.5 % oil content. The relation
is better than the relation between vitrinite content and bulk density, but the relation is not strong. The movement of the curve
indicates an increasing bulk density with higher inertinite content, which approves also the experienced behavior by DMT as shown in
Figure 10.

Figure 12: Relation between inertinite content and bulk density at 0.5 % oil content
A possible reason for the insufficient relation between inertinite content and bulk density is most likely the fact that not all inertinite
individual macerals of the inertinite group have a hydrophobic character like semifusinite. Figure 13 shows the relation between the
bulk density and the inertinite content reduced by the semifusinite content.
 Figure 13: Relation between (inertinite – semifusinite) content and bulk density at 0.5 % oil content
Figure 13 indicates the good correlation between share of hydrophobic parts of the coal and the achievable bulk density at 0.5 % oil
content.
Fuel oil as additive indicated that the highest increasing in bulk density was achieved with a light fuel oil content of 0.5 %. DMT have
varied the water content of a Kepler coal to investigate the influence of water content by constant oil content of 0.5 %. Figure 14
shows the high influence on bulk density by lower water content and oil addition.

900

850

Kepler without oil

800
Bulk densitydry [kg/m³]

Kepler with 0.5 % oil

750

700

650

600

550
0 2 4 6 8 10 12 14 16 18
Water content [%]
Fig. 14: Bulk density of Kepler coal by water adjustment and oil addition
The cold chamber rig tests have indicated the clearly enhancement of the coal drying effect on bulk density increasing by fuel oil
addition.

Coke quality and coking behaviour

The pilot scale carbonizations tests are performed in the 10 kg- scale retort. The produced amount of the coke was between 7 and
10 kg. A portion of a five kilogram greater than 20 mm was put into the ISO drum and tested by 100 and 500 revolutions. The
determined values from the drum test were M30, M20, M10, I30, I20 and I10. These values are not directly comparable with drum tests
values according ISO556, but they can give a relative coke quality change for each coal or blend regarding to different bulk densities.
Additionally, the CRI and CSR were determined according to ISO 18894.
Two quality parameters were enhanced by increasing of bulk density. The CSR value increase about 5 % then the bulk density rise
100 kg/m³. The I10 value decrease about 2 % then the bulk density rise 100 kg/m³. Both relations are confirming with the DMT
experiences. The Figure 15 shows the effect of bulk density on the CSR values from all four single coals.

Figure 15: Effect of bulk density on the CSR values

Figure 16 shows the effect of bulk density on the I10 values from all four single coals.

Figure 16: Effect of bulk density on the I10 values

The bulk density increasing has not only positive effects; also, it should be considered the increasing of the maximal internal gas
pressure during the carbonization as shown in Figure 17. The maximal internal gas pressures for all four coals are dangerous increased
with bulk density increasing, in particular for the American and Canadian coals.
 Fig. 17: Effect of bulk density on the maximal internal gas pressure
The internal gas pressure increased exponentially with increasing bulk density due to the increasing of evolved gas and increasing
resistance of gas flow in the plastic layer. The higher bulk density produces a coke with a higher number of small size pores. The
small size pore coke has a coke texture with wider bridges and higher porosity. The wider bridges enable the higher CSR values.
The increasing of bulk density would allow the increasing of poor coking coals or alternative materials in the blend and could reduce
the share of expensive premium coking coals in the blend. This effect of increasing the CSR value through bulk density increasing is
useful for the replacement of expensive premium coking coal by poor coking coal. This matter of fact shows the Table 4 with the
results of the blend tests of 80 % Hail Creek and 20 % Carter Roag.
Table 4: Test results blend test 80 % Hail C. and 20 % Carter R.
100 % Hail 100 % Carter 80 % Hail C 80 % Hail C
Creek Roag 20 % Carter R. 20 % Carter R.
Moisture % 8.0 8.0 8.0 5.6
Bulk density kg/m³ 700 700 700 800
Max. IGP kPa 2.6 9.8 1.0 15.5
CRI % 29.2 30.7 31.2 30.8
CSR % 64.4 52.3 59.6 63.1
Difference to % - - 12.1 - 4.8 - 1.3
100 % Hail C.

The results indicate the decline of the CSR value when 20 % Carter Roag is added at same bulk density. The increasing of the bulk
density through coal drying, also increases the CSR value of the blend, which is near the same as the CSR value from the 100 % Hail
Creek test. Also, the test with the 80 % Elk Valley St. and 20 % Carter Roag blend indicate the possibility through bulk density
increasing to achieve higher CSR value or the same CSR value with a higher portion of poor coking coal.

Semi-industrial tests in the movable coke oven

DMT tested the Kepler coal in the semi-industrial movable coke oven to investigate the effect of coal drying and oiling on coke
quality and coke oven safety. The bulk densities were adjusted in the cold chamber rig tests as shown in Figure 14. Table 5 shows the
coking conditions and the coking behavior in terms of internal gas pressure and wall load for the three tests with Kepler coal.
 Table 5: Coking conditions and coking behavior of the coking tests with Kepler coal
Test Test Test
No.1 No.2 No.3
Coal component
Kepler % 100 100 100
Coking conditions
Moisture % 6.0 8.0 10.0
Fuel oil % 0.5 0.5 0.5
Bulk density (wet) kg/m³ 915 815 810
Bulk density (dry) kg/m³ 860 750 730
Heating flue temp. °C 1,250 1,250 1,250
Chamber width mm 450 450 450
Coking time h 17.6 18.3 17.9
Coking behaviour
Max. Int. Gas pressure mbar 1,010 612 401
Wall load mbar > 500 > 500 398

The reducing of moisture to 6.0 % and the addition of 0.5 % fuel oil increased the dry bulk density clear higher than 800 kg/m³. The
dry bulk density of Kepler with a moisture content of 6.0 % without oil was only 650 kg/m³. The combination of drying and oiling
indicate clear the huge effect on bulk density. But, Table 5 displays also clear that the internal gas pressure and wall load extremely
increase then bulk density increase.
After discharge of the coke from the cooling coffer coke is stabilised by dropping the coke from a height of 4 m via a gravity chute
with an incline of 45° onto to a steel plate. In this way the normal mechanical stress imposed onto cokes at industrial coke plants is
simulated. The grain size distribution of the coke resulting after one drop is comparable to that obtained at an industrial coke plant
prior to coke screening. To evaluate the quality of coke produced in the test oven the following analysis are accomplished after
carbonisation: grain size distribution, CRI/CSR, M40/M10, I40/I10 and other. Table 6 shows clear the improvement of abrasion and
CSR value of the coke from the test no.1. The higher bulk density leads to a better coke quality. As expected the CRI value was not
affected by bulk density variation.
Table 6: Yield and quality from the cokes of the Kepler coal carbonization tests
Test Test Test
No.1 No.2 No.3
Coal component
Kepler % 100 100 100
Coke yield
Coke yield % 80.6 79.8 80.3
Coke quality
M40 (> 40 mm) % 78.5 80.5 80.8
M10 (> 40 mm) % 7.1 7.7 7.9
CRI % 24.8 25.0 25.1
CSR % 69.5 66.3 65.8

CONCLUSIONS

The moisture adjustment tests with single coals indicate that the clearly increasing of the bulk density of single coals is possible under
very dry conditions.
The investigation with fuel oil as additive clearly illustrate the importance of the knowledge of coal surface properties for the wetting
and in the end its influence of the achievable bulk density. The optimum oil mass content in the coal blend should be approx. 0.5 %.
The increasing of bulk density allows the increasing of poor coking coals or alternative materials in the blend and could reduce the
share of expensive premium coking coals in the blend. It is to consider, that the bulk density increasing involves the danger of the
increasing of the maximal internal gas pressure.

ACKNOWLEDGEMENTS
The research leading to these results has received funding from the European Union’s Research Fund for Coal and Steel (RFCS)
research programme under Grant Agreement No. RFCR-CT-2010-00007.
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