Pergamon

&maw and Biocnerg~Vol. 7. Nos. l-6, pp. 237-244, 1994

0961-9534(94)000654
Copyright c1995 Elsevier Science Lid
Printed in Great Britain. All rights reserved
0961-9534194 $7.00 +0.00
UPGRADING OF FLASH PYROLYSIS OIL AND
UTILIZATION IN REFINERIES
W. BALDAUF, U. BALFANZ and M. RUPP
VEBA OEL AG, Pawiker Str. 30, D-45876 Gelsenkirchen, Germany
Abstract-Flash pyrolysis oil from an ENSYN RTP pilot plant was upgraded in a continuous bench scale
unit with commercial CoMo and NiMo catalysts in anticipation of scaling up the process. Large amounts
of product were produced in a pilot plant for use in an extended analytical characterisation programme.
In bench-scale experiments, high deoxygenation rates of 88-99.9% were achieved. Low liquid and high
water yields were obtained. The fractionated products of the production run did not fulfil the requirements
for direct use as gasoline and diesel.
The process is restricted by several operational problems such as rapid catalyst deactivation, coking and
plugging. Due to high feedstock and hydrogen addition costs, pyrolysis upgraded oil by the process tested
is significantly more expensive than petroleum-derived oil at present oil prices.
INTRODUCTION
Pyrolysis oils from biomass are characterized by
their high oxygen content. They are also very
unstable, and properties like viscosity and water
content change during storage and heating. The
evidence for this is water formation and polym-
erisation initiated by side reactions.
The properties and composition of pyrolysis
oils mainly depend on the pyrolysis conditions.
Rapid or fast pyrolysis processe? are charac-
terised by a temperature range of 450-900C
and short residence times (< 1 s). Under these
conditions very low amounts of char are pro-
duced. In the region of 450-6OoC, most of the
products are liquids. These liquids contain high
amounts of water (approx. 30%) and acids and
have low viscosities, especially when compared
with slow pyrolysis oils which have high viscosi-
ties.
Because of their poor quality, the utilisation
of raw pyrolysis oils is difficult. Possible appli-
cations are their use as fuel oil for electricity
production in boilers and gas turbines5 or as
feedstock in petroleum refineries. For both
routes it is necessary to upgrade the oil, e.g. by
hydrotreatment. Recent investigations cover
laboratory experiments on a small scale> while
the target of the reported project is to investi-
gate possible routes for pyrolysis oils from
biomass to be processed in standard petroleum
refineries. Applied technology and experience
from the hydrotreating of conventional coker
distillates are the background to this study.
PETROLEUM REFINERY
A petroleum refinery is a very complex se-
quence of processes, which convert petroleum
crude oils into lighter marketable fuels and
chemical feedstocks. A simplified scheme is
shown in Fig. 1, which shows only the major
processes and major product streams.
The crude oil enters the refinery via the
desalting unit. After desalting the crude oil is
atmospherically distilled and fractionated into
naphtha and middle distillate. The naphtha cut
is either routed to the naphtha pool, reformed
to produce high-octane naphtha components, or
treated in olefin plants to produce ethene and
propene. The middle distillate can be directly
routed to the middle distillate pool, or disul-
phurised prior to this. These pools supply gaso-
line, jet fuel, diesel and fuel oil to the market.
The high boiling residue from the atmos-
pheric distillation tower is further distilled in a
vacuum tower. The resulting distillates are cata-
lytically cracked in hydrocrackers or fluid cat
crackers, respectively. The residues are ther-
mally cracked in visbreaking or coking units, or
in thermal hydrocracking processes. The lighter
products are treated in the same way as the
straight-run distillates.
237
238 W. BALDAUF et al.
Atm.
Disttllatton
v&z.
Diiillatton
Fig. 1. Refinery schematic.
Raw pyrolysis oils are not miscible with con-
ventional petroleum crudes or any fractions
and this leads to the need for a pretreatment
step prior to processing pyrolysis oil in the
refinery.
FEEDSTOCK
Flash pyrolysis oil was provided by ENSYN
(Canada). The oil was produced from mixed
hardwood sawdust (maple/oak). The pyrolysis
plant operated at a temperature of 525C and a
residence time of 0.35 s. The ENSYN oil was
analysed with standard analytical methods.
Results are listed in Table 1.
Depending on the quality of the pyrolysis oil
after pretreatment, it can be routed to either
atmospheric or vacuum distillation, from where
it ends up very diluted in the three distillate
streams. Another possibility is to feed it directly
into the conversion units. If pretreating product
qualities allow, it could also be possible to distil
the hydrotreated oil separately and to feed the
distillates to the corresponding conversion units
or to the corresponding product pools.
The possible feed points for pyrolysis oils are
indicated in Fig. 1.
Table 1. Characterisation of raw pyrolysis oil
Water content % 29.85
Density (30C) g cm- 1.192
HHV MJ kg- 16.23
LHV MJ kg- 14.47
Pourpoint C - 30
Flashpoint C 51
Elemental analysis
(solids free)
C wt% 39.17
H wt% 8.04
S
ppm
5
N wt% 0.05
0 wt% 52.74
Solids
Acetone insolubles wt% 2.2
Pyridine insolubles wt% 2.1
Ash content wt% 0.15
Because the crude pyrolysis oil contained 2%
of char the oil had to be filtered prior to
hydrotreating.
EXPERI MENTAL
The upgrading test runs were performed in
a continuously operating bench-scale catalyst
testing unit. The unit is designed for pressures of
up to 30 mPa, temperatures of up to 500C and
flow rates up to 300 g h-. Especially for pro-
cessing pyrolysis oil the unit was modified for an
optional down- or upflow mode operation. A
simplified flow scheme of this continuous-flow
fixed-bed unit is shown in Fig. 2.
The make-up hydrogen was supplied from a
high-pressure hydrogen supply and the liquid
feedstock was fed by means of a high-pressure
pump. Both feed rates were continuously
measured by flowmeters. After contacting gas
and liquid the reactor was charged in the se-
lected mode.
The reactor (30mm internal diameter and
1130 mm long) had a volume of 7 16 cm3, minus
the volume of a central thermowell which con-
Upgrading of flash pyrolysis oil
239
Reactor
Stab. Gas
Fig. 2. Bench-scale unit for catalyst testing.
tained thermocouples for measuring the
temperatures along the reaction section. The
reactor was externally heated by five
heating zones which were independently con-
trolled and monitored by means of the thermo-
couples.
Preheating was performed in the first part of
the reactor, which was filled with inert SIC. The
centre part of the reactor was filled with cata-
lyst. The feedstock was further heated up to the
reaction temperature in the first third of the
reactor which was isothermal in the remaining
catalyst zone. The catalysts were standard refin-
ery catalysts in their sulphided form. To prevent
desulphiding and thus deactivation of the cata-
lyst small amounts of DMDS (dimethyldisul-
240 W. BALDAUF et a l .
WHSV:0.40
*
,z,
WHSV:0.80
340 350 360 370
Temperature I [Cl
Fig. 3. Influence of temperature on deoxygenation.
380
phide) were added to the feed to ensure a
minimum H, S partial pressure.
The product leaving the reactor was cooled
down at pressure. The offgas was separated
from the liquid phase in the high-pressure sepa-
rator and depressurised by a control valve which
established the operating pressure of the unit.
The liquid phase was depressurised and separ-
ated into a liquid product and stabilisation gas
in the stabiliser.
The production run was performed in a hy-
drotreating pilot plant which was designed for
oil flow rates of up to 10 kg h-. The configur-
ation of the plant is similar to that of the
bench-scale unit described above. A detailed
description of the plant is given in ref. [8].
Material balances were performed by
sampling the liquid and gaseous products. The
observation of mass balance was 48 h after
establishment of stable conditions.
Raw mass balances were corrected by a calcu-
lation procedure which closed elemental bal-
ances of carbon, hydrogen, oxygen, sulphur and
nitrogen. Hydrogen consumption was calcu-
lated as the difference in hydrogen content of
the product streams minus hydrogen content in
the liquid feed. H,S, NH3 and additional H,O
were calculated by balancing S, N and 0 in
liquid product and feed (water in feed oil and
DMDS were taken into account). Finally
flow rates were corrected by closing the carbon
balance. C,-C,, CO, CO*, and C,, were calcu-
lated from corrected flow rates and the compo-
sitions of liquid products, off gases and stripper
gases.
RESULTS
During the experiments the effects of tem-
per at ur e (350-37OC), s pace vel oci t y
(0.154.80 kg (kg h))), up- and downflow
mode, and different catalysts (CoMo, NiMo)
were investigated.
In order to reduce the number of independent
variables (temperature, space velocity) the
severity parameter deoxygenation rate was
introduced for the following interpretation of
the test results. Deoxygenation rate represents
the reduction of concentration of organic oxy-
gen in product oil related to organic oxygen
concentration in the feed. Depending on the
operating conditions, deoxygenation rate in-
creases with increasing severity which is illus-
trated in Fig. 3.
The results of analytical inspection of product
oils are summarised in Table 2. The correspond-
ing balances and product distributions are listed
in Table 3.
Oil yields decrease from 36 to 32% with
increasing deoxygenation. Water shows the
highest yields. In addition to the water in the
feed, 21-25.5 wt% of water was produced. Gas
and water yields increase at higher severities. In
addition to water formation, significant
amounts of oxygen were removed as CO and
c o, . With increasing deoxygenation the
amounts of CO and CO* decrease. This means
that, at higher severity, oxygen removal shifts
more and more to water production instead of
CO, production. Oxygen rejection via water
increases hydrogen consumption. As deoxy-
Upgrading of flash pyrolysis oil
Table 2. Characterisation of product oils
241
Run no. 540
Flow direction downflow
Catalyst type CoMo
Temperature (C) 370
Space velocity (kg(kg h))) 0.25
Deoxygenation 99.92
rate (X)
Elemenial analysis (water .free)
c (wt%) 86.79
H (wt%) 13.17
s (wt%) 0.070
N (wt%) 0.003
0 (wt%) 0.021
Density (g cn-) 0.83
H,O content (ppm) 50
CCR (wt%) 0
arom. C (wt%) 10.0
HHV (MJ kg-) 45.96
LHV (MJ kg-) 43.09
Boiling range
0-200c (wt%)
200-350C (wt%)
350-500C (wt%)
> 5OOC (wt%)
40.8
38.5
20.7
541
downflow
CoMo
370
0.40
98.53
87.22 86.84 86.50 85.94 86.93 86.82 86.47
12.35 11.82 11.23 10.79 11.87 11.52 12.90
0.004 0.004 0.008 0.055 0.055 0.007 0.021
0.033 0.082 0.021 0.152 0.129 0.23 0.009
0.39 1.25 2.14 3.06 1.06 1.20 0.60
0.86 0.896 0.928 0.94 0.90 0.93 I 0.866
210 510 1900 4200 350 351 102
0.09 1.40 3.39 5.52 1.79 1.60 0.28
17.0 18.8 25.9 27.0 18.8 22.7 9.8
45.26 44.46 43.43 41.20 44.38 43.44 44.83
42.60 41.87 40.99 38.87 41.68 40.91 42.00
40.0 30.6 27.6 25.3 29.8 21.4 38.5
36.2 31.4 29.6 29.2 30.2 32.1 36.3
21.2 23.1 23.0 21.6 23.8 27.6 22.3
2.6 14.9 19.8 23.9 16.2 18.9 3.0
542 543 544
downflow downflow downflow
CoMo CoMo CoMo
350 350 370
0.25 0.40 0.80
95.17 91.78 88.32
545 551 557
downflow upflow downflow
CoMo CoMo NiMo
370 370 370
0.40 0.40 0.15
95.88 95.25 97.20
genation increases from 88 to lOO%, hydrogen
consumption increases by about 50%.
Product properties show the following depen-
dencies with decreasing severity:
?? specific gravity increases from 0.83 to
0.94 g ml-;
??water content in product oil increases from 50
to 4200 ppm;
??higher and lower heating value decrease from
46.0 (43.1) to 41.2 (38.9) MJ kg-;
??Conradson Carbon Residue (CCR) content
increases from 0 to 5.5%;
??aromatic carbon content increases from ap-
prox. 10 to 27%;
??naphtha and middle distillate concentrations
in the liquid product decrease from 41 and
39% to 21 and 29%, while vacuum gas oil
remains relatively constant at approx. 20-22%
and residue > 500C increases from 0 to 24%.
In order to get a measure of catalyst stability,
run 541 was repeated at similar operating con-
ditions after approx. 150 h (run 545). A signifi-
cant drop of deoxygenation rate from 98.5 to
95.9% indicates the rapid catalyst deactivation
Table 3. Mass balances and yields
Balance no. 540 541 542 543 544 545 551 557
Flow direction downflow downflow downflow downflow downflow downflow upflow downflow
Catalyst type CoMo CoMo CoMo CoMo CoMo CoMo CoMo NiMo
Temperature (C) 370 370 350 350 370 370 370 370
Space velocity (kg(kg h))) 0.25 0.40 0.25 0.40 0.80 0.40 0.40 0.15
Deoxygenation 99.92 98.53 95.17 91.78 88.32 95.88 95.25 97.20
rate (X)
Gases (total) (wt%) 16.69 18.47 18.53 16.72 15.85 16.76 17.12 16.90
c, (wt%) 3.22 3.32 3.12 2.67 2.57 3.35 3.53 3.68
c, (wt%) 4.06 4.04 4.27 3.69 2.62 3.81 3.61 3.63
c, (wt%) 2.70 2.49 2.20 1.76 1.25 1.81 1.85 2.32
c.$ (wt%) 2.04 1.88 1.66 1.29 0.90 1.31 1.34 0.57
co (wt%) 0.13 0.16 0.11 0.15 0.32 0.15 0.15 0.55
co, (wt%) 4.46 6.53 7.11 7.15 8.20 6.33 6.51 4.70
Water (wt%) 55.51 53.61 52.89 52.45 50.97 53.58 53.14 54.53
Oil (wt%) 32.81 32.28 32.68 34.51 36.34 33.78 33.75 33.58
Total products 105.01 104.42 104.10 103.68 103.16 104.12 104.01 105.01
(wt%)
H, consumption 5.01 4.42 4.10 3.68 3.16 4.12 4.01 5.01
(wt%)
242 W. BALDAUF et al.
Table 4. Characterisation of product oil from the oilot plant production run
Product
Total product Naphtha Diesel VGO Residue
>sooc <18oC I go-350C 350-500C
Elemental analysis
c (wt %)
H (wt%)
S (ppm)
N (ppm)
0 (wt%)
Ca @pm)
Ni (ppm)
V (ppm)
Mo (ppm)
Fe @pm)
Na (ppm)
Density (g cm-)
n-Paraffins (wt%)
iso-Paraffins(wt%)
Naphthenes (wt%)
Polynaphthenes (wt%)
Aromatics (wt%)
Mono aromatics (wt%)
Diaromatics (wt%)
Polycyclic aromatics (wt%)
MOZ/ROZ (-)
Cetane number (-)
Cetane index (-)
Cloudpoint (C)
CCR (wt%)
Stability test (ASTM D 2274)
86.45 85.45 87.08
13.22 14.72 12.88
851 130 109
83 2 51
0.2 0.05 0.07
0.8503 0.7517
20.56
12.52
61.41
I .47
4.03
62162
87.54
12.26
426
162
0.4
<I
<I
< I
<I
<I
<I
0.8739 0.9303 0.9316
29.3
0.6
neg.
0.7
45
39.7
- 34
0.02
which is not acceptable for technical fixed-bed
reactor systems. The result of rapid deactivation
was proved by the fact that the test run was
terminated due to pressure build-up in the reac-
tor caused by plugging.
While the test runs 540 to 545 were performed
with downflow mode and with a CoMo catalyst,
in additional test runs the influences of a differ-
ent catalyst (NiMo, run 557) and of upflow
mode (run 551) were tested. The influences on
liquid product qualities can be interpreted as
follows:
??at similar operating conditions, deoxygenation
rate in the upflow mode is less than in the
downflow mode;
odeoxygenation with the NiMo catalyst is less
than with CoMo catalyst;
@in upflow mode at the same deoxygenation
rate, lower amounts of naphtha and higher
amounts of vacuum gas oil are formed; conse-
quently the liquid product density in the
upflow mode is higher;
??nitrogen removal in the upflow mode is signifi-
cantly less than in the downflow mode; sul-
phur content in the liquid product is
influenced by sulphur injection to the feed and
does not represent the behaviour of the hydro-
treating process;
??the content of aromatic carbon is lower with
NiMo catalyst;
??test runs with CoMo catalyst were terminated
by coking and plugging in the low-tem-
perature catalyst zone, whereas the test
run with NiMo catalyst ended due to plug-
ging of product lines with a gum-like sub-
stance;
??all other properties are only determined by
deoxygenation rate or severity, but are inde-
pendent of flow mode and catalyst.
Despite operational problems during bench-
scale test runs, the potential of upgraded pyrol-
ysis oil as feedstock for petroleum refineries
should be demonstrated. To provide large
amounts of upgraded oil, a production run was
performed in a pilot plant. The bench-scale
experience led to operation in downflow mode
with NiMo catalyst. Operational parameters
were adjusted for a medium deoxygenation rate
of 97.3%. The product from the pilot plant test
run was used for characterisation of total crude
and its related fractions with respect to refinery
requirements.
Results are shown in Table 4. Total
liquid product and fractions can be defined as
follows.
Upgrading of flash pyrolysis oil
WV
243
01
I
0 50 104 150
Pyrolysis Oil I ECU/t
Fig. 4. Economics of upgrading.
Total liquid product
The product oil is a light brown low viscosity
liquid with a boiling range from 35-535C.
Naphtha (boiling range < 180C)
High naphthene content and low octane num-
ber reduce its suitability as a gasoline pool
component. Only small amounts can be blended
as gasoline. Further upgrading in the reformer
plant and conversion to olefins in steam crack-
ers are more promising routes.
Diesel (boiling range 180 -350C)
The diesel fraction is characterised by high
density, low cetane number and high aromatics
content. This fraction does not meet the specifi-
cations of a marketable diesel product. The
oxygen stability test was negative. The need for
further upgrading of this fraction for stabilis-
ation and aromatics reduction prior to use as a
diesel pool component is evident.
Vacuum gasoil{ VGO (boiling range 350 -500C)
CCR and metals content of VGO are at the
limits recommended for feedstocks for hydro-
cracking (HC) and fluid cat cracking (FCC)
plants. Alternatively, the fraction might be used
without further upgrading as heavy fuel oil.
Residue ( > 500 C)
The residue fraction represents only a very
small amount with a final boiling point of
535C. Commercial vacuum distillation units
will not separate this fraction because VGO cut
points usually are > 535C. That means that the
residue will be part of the VGO fraction and is
treated as described above. Restrictions might
occur if CCR and metal contents of vacuum gas
oil are significantly changed by the shift of the
cut point.
Results of yield structure and fraction qual-
ities indicate that the total liquid product cannot
be fed to a single further upgrading process.
Separate fractionation or feeding to the pet-
roleum crude oil distillation unit (which is more
economic in an existing refinery) is necessary to
split the oil into the main fractions.
The reported possible suitability routes are to
be evaluated on the basis of the major analytical
properties of the fractions. The final decision for
suitability has to be confirmed by experimental
test programmes.
ECONOMICS OF UPGRADING
Low yields and high hydrogen costs are re-
sponsible for the high cost of upgraded pyrolysis
oil. In Fig. 4 the costs for highly upgraded oil
are shown as a function of raw pyrolysis oil
price. Product costs are calculated as the sum of
the feedstock cost, upgrading cost and hydrogen
cost, minus a credit for the hydrocarbon gases
on the following basis:
??raw pyrolysis price is varied between 50 and
15OECU t-;
??upgrading costs are 15 ECU t- feedstock at a
hydrotreating plant capacity of
0.8 x lo6 t year-;
??hydrogen costs are 0.09 ECU Nmd3 for steam
reforming of natural gas;
??hydrocarbon product gases are credited at a
price proportional to their heating value which
leads to approx. 30-50 ECU t- of gas.
The result is that upgraded pyrolysis oil is
more expensive by a factor of 1.5-3 than equiv-
alent petroleum oil products. At typical feed-
stock costs of 100 ECU t- for raw pyrolysis oil,
1 t of upgraded oil costs about 450 ECU t-l,
compared with 18&220 ECU t- for petroleum-
244 W. BALDAUF et al.
derived naphtha and middle distillate and
SO-100 ECU t- for fuel oil. The major contri-
bution to this cost is the feedstock price (3 t of
feedstock are necessary to produce 1 t of up-
graded pyrolysis oil); about 150 ECU t- of
product has to be expended for hydrogen.
Credits for the hydrocarbon product gases and
the upgrading costs offset each other.
The situation is similar for partially upgraded
oil, compared to prices of conventional fuel oils.
The value of extenuities such as CO, tax or a
credit for zero sulphur content can improve the
price relations for biomass resources. These
benefits are reduced if the hydrogen and process
energy production by fossil resources are taken
into account.
CONCLUSIONS
Catalytic upgrading of flash pyrolysis oil in a
fixed-bed reactor system was realised for short
run times. High deoxygenation rates were ob-
tained. Water is the major product and the oil
yield is only 30-35%. The products are light
liquids with low oxygen and water content and
high heating values. At lower severity of lower
deoxygenation rate the solubility of product oil
in water is increased and the separation of
aqueous and organic phases is increasingly
difficult.
The catalyst deactivated very rapidly and
steady-state conditions could only be obtained
for a short period. Several operational problems
caused by the instability and coking potential of
the pyrolysis oil made processing difficult.
Tubes and valves were plugged or covered with
gum-like deposits. Operating and control sys-
tems such as flow meters and level controllers
were disturbed by adhesive deposits. With
CoMo catalysts the catalyst bed plugged and
coked in the preheater, whereas with a NiMo
catalyst the reactor outlet was plugged by gum-
like substances.
Although the products are already hydrogen-
ated, some fractions did not fulfil the required
product specifications.
The naphtha fraction is unsuitable for direct
use as gasoline. Only very small amounts could
be routed to the gasoline pool. An additional
upgrading (e.g. in a reformer) or the use of the
naphtha fraction as a feedstock for olefin pro-
duction should be more promising.
Low cetane number (45) high density
(0.873 g ml-), and oxygen instability illustrate
the poor potential of the diesel fraction for
direct use as a pool component. Further upgrad-
ing is necessary.
Total liquid product from the pretreatment
step is recommended to be routed to the crude
distillation tower, where the fractions end up
diluted in the naphtha, diesel and VGO cut and
are further upgraded in subsequent conversion
units together with petroleum-derived products.
A fixed-bed reactor system is not recom-
mended, since the rapid catalyst deactivation
must be compensated by continuous regener-
ation. An ebullated bed or liquid-phase reactor
system with homogenous or without catalysts
might be more promising.
Acknowledgements-The work was performed with the
financial support of the European Union, DG XII in the
framework of the JOULE programme. We thank ENSYN,
Canada and Energy and Mines Resources, Canada for
providing the pyrolysis oil.
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