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A continuous fluidized-bed plant (PDU-scale) for fast pyrolysis of lingnocellulosic biomass gives rise to bio-oil yields of
65 wt.-%. The average reactor gas residence time was 1.2 s only. The gas and charcoal yields were 15±20 wt.-%, respectively. The
bio oils were chemically characterized. The main monomeric products of the thermal degradation of carbohydrates are acetic
acid, hydroxyacetaldehyde, hydroxypropanone, and levoglucosan. The process described in this paper can also be used for
disposal of inorganic-, metal-organic-, and chlorine-organic contaminated waste-wood. Inorganic compounds of wood
preservatives are concentrated in the charcoal fraction and can be separated easily. Chlorine-organic wood preservatives are
mostly degraded. The process has been positively tested as a technique for disposal, recycling, and exploitation of industrial
biomass waste (wood waste, grinding grit, fibre sludge, cocoa shell and modern composites like HPL). Bio oil from fast pyrolysis
can be used for the production of energy and chemical feedstock. Research for these purposes is ongoing.
±
[*] C. Gerdes, Dr. C. M. Simon, Prof. Dr. W. Kaminsky, Universität Hamburg,
Institut für Technische und Makromolekulare Chemie, Bundesstraûe 45, Figure 1. Flow scheme of BFH-pyrolysis plant; (1) Silo, (2) vibration conveyor,
D-20146 Hamburg; T. Ollesch, Dr. D. Meier, Bundesforschungsanstalt für (3) screw feeder, (4) fluidized-bed reactor, (5) cyclone, (6) heat exchanger,
Forst- und Holzwirtschaft, Institut für Holzchemie und chemische (7) intensive cooler, (8) electrostatic precipitator, (9) flare, (10) compressor,
Technologie des Holzes, Leuschnerstraûe 91, D-21031 Hamburg. (11) gas preheater 1, (12) gas preheater 2, (13) overflow container.
Eng. Life Sci. 2 (2002) 6, Ó WILEY-VCH Verlag GmbH, D-69469 Weinheim, 2002 1618-0240/02/0606-0167$$17.50+.50/0
0930-7516/02/0606-0167 17.50+.50/0 167
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back into the reactor. The remaining gas volume is burned in a The heating zone of the reactor heating half-shells is
flare (9). For the purpose of analysis, samples can be taken from designed for a standard fluidized-bed height of 330 mm. This
the gas flow [12]. height is caused by experiences with other plants [11,16,17].
The resulting freeboard height of 220 mm does not fit to
standard designs of fluid bed plants. A retail of solids (small
3 Design of the Plant charcoal/coke particles) is intentional to separate pyrolyzed
charcoal particles of small size and low density from the
fluidized bed with the gas stream and help of the cyclone
3.1 Reactor and Heating of Fluidizing Gas
system (blow-through design).
All components of the plant, where biomass is pyrolyzed
with gas recycling, are built compactly in a rack made of steel
tube frames. 3.2 Feeding System
The reactor itself is relatively small and consists of stainless
steel (material: 1.4841), likewise the fluidizing gas preheater The common practice for feedstock transport is to use two
that is suitable for high temperature use up to 1200 C. The combined feeding screws. This could not be exerted to feed
reactor measures result from the given reactor residence time fibrous, longish wood-splints [12,13]. Wood processing indus-
(fluidized bed and freeboard) for pyrolysis gas. Reactor tries are using drag-bottom plants, special rambling-screws
residence time should not be longer than a second, with a total and/or discharge-rotor systems [18,19]. These systems are
gas flow (standard conditions) of 15 m3 maximum (due to the relatively complicated for small-scale application. Hence, the
maximum power of the compressor). Before going into the first dosing-screw has been replaced through a vibration-
fluidizing bed, the fluidizing gas can be preheated up to 900 C channel. Wood-splints trend to bridge formation. Therefore,
temperature. the silo was constructed with a longish, quadrate discharge
The plant heating system is run electrically. Due to the opening. The connected vibration channel was extended.
characteristic of pyrolysis processes, the energy input should Additionally, the silo with a volume of 130 L, was provided
be quick to achieve high heating rates in the feedstock and to with a magnet vibrator.
avoid thermal stress of the pyrolysis products. Burners are The feedstock, transported by the vibration channel, is
more effective than electrical heating but they are more falling on the high speed feeding screw (60 rpm), and fed into
difficult to run. All parts of the plant are made of stainless steel the fluidized bed. The flow of cold pyrolysis- or inert gas
1.4571. All flanges and connections are built according the assures, that hot pyrolysis gas from the reactor is not able to
German industry norms (DIN). As seal material 2 mm penetrate the feed system. The silo and vibration channel are
graphite-sheet metal is used. connected via a quadrate compensator made of silicone.
The first fluidizing gas preheater consists of a tube with The stainless steel feeding screw (material 1.4571) is
three heating rods; with 900 W power each, inside. The rotating in a water- or air-cooled screw jacket. The screw has
fluidizing gas is passing the heating rods and is heated to a a diameter of 35 mm, a kernel cross-section dimension of
temperature of 350 C. The gas preheater is isolated and 15.5 mm and a feed-length of 295 mm. Cooling prevents the
covered with sheet steel. The second gas heater is directly screw of coking respectively smelting of feedstock (e.g.,
connected with the reactor to minimize temperature loss. The possible when using plastics) in the feeding system.
reactor is indirectly heated by two Kanthal-heating half-shells The screw pivoted with three ball bearings and the screw-
from outside through the reactor wall. The Kanthal heating shaft lead-trough is packed by a stuffing bushing. As sealing
half-shells are made of ceramic-isolation material including material, a gasket made of graphite/silk/teflon is used.
electric heating wires with 2.5 kW power each half. With the
heating half-shells, suitable for temperatures of 1150 C
maximum, it is possible to heat the fluidizing gas above the 3.3 Separation of Solids
reaction temperature in question.
Other plant concepts showed, that heat input by overheated Solids, leaving the reactor with the pyrolysis gas flow can
gas is optimal for biomass pyrolysis. As a result of the accrue from different sources. To the one hand the small-size
composition of overheated fluidizing gas, undesired coke may particles from the fluidized bed material is blown out the
develop, so that overheating of fluidizing gas is not wise for fluidized bed, on the other hand pyrolysis coke is forming and
every plant concept. Therefore plastic pyrolysis is performed blown out of the reactor in terms of small-size particles. Lastly,
at fluidizing temperatures between 400±500 C, when using a number of feedstock itself contains inorganic percentage
recycled pyrolysis gas for fluidizing [13±15]. that is leaving the reactor as coked small-size dust. Addition-
Between Reactor and fluidizing gas preheater, a fluidizing ally, pyrolyzed particles of lower weight and smaller size are
disk is inlayed. The disk consists of a 5 mm stainless steel sheet carried away by the gas flow.
with 81 holes and bend tubes welt on, through which the For solid separation from the gas flow, aero-cyclone systems
fluidizing gas is flowing and being distributed over the whole are used. These systems are well known in technical processes
reactor cross-section. of other pyrolysis plants. To achieve high separation rates, in-
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line multi-cyclone systems are necessary. This affects ad- The fluidizing gas is adjusted with a needle valve on the
versely a higher pressure drop and therewith a higher energy suction side of the compressor. The maximum gas flow is
consumption of the compressor. For solid separation, the 16 m3/h at 1 bar backpressure. A variable area flowmeter
introduced plant uses a dual in-line cyclone system. The design displays the flow of fluidizing gas. A bellow gas meter registers
calculations are including a lot of empiric numerical propor- the fluidizing gas amount, which is necessary for the gas
tions. Generally the separation output and the particle of balance. Another variable area flowmeter allows conduction
critical size are increasing with gas velocity of circulation. of a cold stirring gas flow through the feeding system to
Hence, the perimeter of cyclone has to be chosen as small as prevent it from reflow of hot pyrolysis gas. Choosing standard
possible although a small perimeter causes higher pressure configuration, a third variable area flowmeter is used to flush
drop. For heating the cyclones, the feed line and branching off the overflow container.
up to 450 to 500 C, filaments where installed. Discharging of surplus gas (pyrolysis gas) is performed with
To separate small-size particles from the pyrolysis gas flow an unidirectional restrictor valve with 20 mbar response
after a cyclone, other working groups developed hot gas pressure. It works self-controlled on the suction side of the
filtration systems. Thereby, problems relating high tempera- compressor. A bellow gas meter (maximal gas flow 6 m3/h)
tures (450 to 500 C), choice of materials, cleaning of the filter quantifies the gas flow drained to the flare.
and high pressure drop are coming up [20,21]. All electric heating are run via thyristors AC controllers
(e.g., combined with current limiting). A thermocouple in the
middle of the fluidized bed is used for controlling the rector
temperature.
3.4 Condensation of Liquids
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modification was made to refrain from the original blow- 5 Short Description of the Modified Pyrolysis
through design, where too much charcoal flew through the Plant
liquid collection system and contaminated the pyrolysis oil.
Primary, the overflow pipe connected to the overflow The main principle of the plant has been fully described in
container is separating the charcoal particles. The dual Sect. 2. Here, the most important changes in the design (Fig. 2)
cyclone system remains in operation in order to separate the are discussed. After separation of small scale particles with the
small-size particles. dual cyclone system (5), pyrolysis products are condensed in a
Important for the quality of pyrolysis liquid, beside the gas scrubber (9). The scrubber is cooling hot pyrolysis gas
already mentioned parameters reactor residence time and directly with a quench liquid from a reservoir (7). The quench
temperature, is the choice of the condensation method. liquid is pre-cooled to 15 C with an heat exchanger (8) before
Stepwise, fractionated condensation via in-line heat exchan- entering the scrubber. The quench liquid is recirculated
gers is not optimal. Pyrolysis products resist too long on a high permanently with a mono pump without any loss of liquid. The
temperature level. Condensation is too slow and promotes quench medium is immiscible with pyrolysis oil and separates
unwanted secondary reactions. A further disadvantage is the quickly from product oil. Non-condensable gases and resisting
need for reunion of the obtained oil fractions to whole oil; here aerosols are passing the electrostatic precipitators with 20±
the oil may separate into two ore more phases. This leads to the 35 C (10). There, a complete separation of small-scale
necessity of using solubilizer. According to this, fractionated charcoal particles and liquids is taking place. A gas fraction is
condensation is disadvantageous for application of the process resisting, which is passing an intensive cooler (0 C) (11) and is
in process demonstration- or industrial scale. fed back into the reactor as circulating gas through preheaters
(14), (15) by using a compressor.
gas
14
7 Material and Methods
oil 7 13
circulating gas The company J. Rettenmaier & Söhne GmbH & Co, JRS
Figure 2. Modified pyrolysis plant for biomass; (1) Silo, (2) vibration conveyor, Faserstoff-Werk, has supplied the feedstock used in the first
(3) screw feeder, (4) fluidized-bed reactor, (5) cyclones, (6) pump, (7) quench experiments. Its specifications can be taken from Tab. 1. The
liquid reservoir, (8) heat exchanger, (9) gas scrubber, (10) electrostatic
precipitator, (11) intensive cooler, (12) flare, (13) compressor, (14) gas
most important experimental parameters of the temperature
preheater 1, (15) gas preheater 2, (16) overflow pipe, (17) overflow container. series TP16 to TP 24 are scheduled in Tab. 2. Quartz sand of
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0.5±0.6 mm particle size has been used as fluidizing bed As internal standard, fluorantene has been added to
material and has been replaced by clean, new sand after each pyrolysis oil samples of each condensed fraction. The
experiment. compounds of each oil sample were separated by gas
chromatography technique (GC/MS), detected, and identi-
fied via MS. Additionally, oil components were quantified by
GC/FID technique. With each peak-area, retention time, and
response factor the main compounds of oil could be
7.1 Analysis quantified. The response factors where determined by GC/
FID-analysis of prepared standard solutions of single com-
The qualitative and quantitative analysis of pyrolysis gas pounds. A sample chromatogram that is demonstrating the
and oil has been performed by gas chromatography. For complexity of the chemical composition is shown in Fig. 4.
identification of pyrolysis products a mass-selective detector
and a specific spectra library with selected pyrolysis products
has been available. Determination of water content has been
performed by Karl-Fischer-Titration. A complete analysis of
bio oil is difficult, since the oil contains higher molecular
weight ratios of degradation products of hydrocarbons
(pentoses, hexoses), and lignin beside the chromatographi-
cally detectable share. In addition, the oil contains polar, non-
volatile components that are only accessible to HPLC (Fig. 3).
10.00 15.00 20.00 25.00 30.00 35.00 40.00 45.00 50.00 55.00 60.00 65.00 [min)
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The mass of each fraction, except the mass of gases, had pyrolysis, whereby degradation is depending on pyrolysis
been obtained by weighing wood (feed) and the product oil temperature. At 587 C ratios of 0 to 16.66 wt.-% of 10 studied
and char. The mass of gases are determined by calculating the additives, which where added in ªworst caseº amounts, could
difference of total in- and output. The mass balances could be be recovered. DDT was not found in any of the analyzed oils.
closed to 100 % and are comparable to each other. The in- and The most stable substances proved to be propioconazole and
output is rounded t ± 1 g. Using the original experimental tebuconazole.
setup without the gas scrubber; four oil fractions accrued: The additives where utilised in high concentration, pyrolysis
1. heat exchanger 1; 2. Heat exchanger 2; 3. intensive cooler, of real contingent would lead to reduction of additive
4. electrostatic precipitator. concentration. Temperatures over 600 C are necessary for
Fig. 5 shows the yields of three obtained pyrolysis fractions: complete thermal degradation of the most stabile preserva-
oil, gas and char subjecting to pyrolysis temperature. As already tives., whereby the yield of pyrolysis oil would be reduced and
demonstrated with a laboratory scale plant, a maximum oil the gas yield would increase inevitably [2]. For a technical
application, it should be considered whether a complete
destruction of preservatives is necessary or whether mixing of
oils from non-contaminated oils could reduce resisting
contamination.
Using chloro-organic additives, formation of chlorinated
dioxins and furans could occur. Within the scope of studies
different contingents from a wood sorting site where
investigated. For this purpose cable drums, trelliswork fence,
particleboards, railway sleepers, and window frames where
used for pyrolysis. Non of the obtained oils contained organic
preservatives. Only sleepers had been an exception, here a
broad spectrum of polycyclic aromatics could be found. The
results are correlating, with reference to non-contaminated
wood, to data published before. Beyond it, the plant is useful
to reduce contaminations with organic wood preservatives
and to separate heavy metals.
The next logical step has been the use of industrial biomass
waste in the process described above. It should be determined,
whether biomass other than wood could be converted. Within
the scope of a PhD thesis and with the collaboration of
Figure 5. Pyrolysis product yields (wt.-%) of beech wood pyrolysis experi-
different companies, diverse biomass waste had been pyr-
mental series described in Tab. 2 (calculated on dry feed basis).
olyzed. So far, fast pyrolysis processes all over the world are
merely using well-defined, non-contaminated wood and bark.
yield can be observed at a pyrolysis temperature between 470
Beside traditional waste-wood recycling companies, wood
and 500 C. The product distribution shows the typical spectra
processing industries, like furniture, panel boards, or charcoal
of fast pyrolysis of wood. 50±70 wt.-% oil yield can be expected,
producers are interested in suggestive and new recycling and
char and gas ratio rest with 15±25 wt.-%. Reactor residence
disposal processes. Therefore, beech wood waste of a charcoal
time had been sub-optimal with 1.38 s average [23].
producer has been pyrolyzed.
Processing the experimental series TP25±38, pyrolysis of
Today, paper recycling is a common practice in paper
well-defined, contaminated wood had been performed to
business. With each cycle, the paper fibers become shorter.
calculate better mass balances. Target of these experiments
After several cycles the fibers are too short to make paper of
had been to obtain reproducible and meaningful results.
acceptable quality. This is also valid for the production of new
Hence, inorganic (on CKB-basis), metal-organic (Cu-HDO
paper. Ultimately, there were at least 1.9 million tons of sludge
and Al-HDO), and 10 different chloro-organic wood pre-
from paper recycling in 1997. A German paper mill supplied
servatives had been utilised. Terminal, waste wood from a
the fiber sludge used for pyrolysis [24,25].
wood-sorting-site of a commercial disposal company has been
Producers of modern composite materials, e.g., high
included in the study 1).
pressure laminates (HPL), are searching for recycling
Relating to wood treated with CKB, Cu-HDO and Al-
processes for their used-up products and production residues.
HDO, heavy metals are fully remaining in pyrolysis char.
These processes permit recycling of both the macromolecular
Pyrolysis oil is not contaminated and therefore unrestrictedly
polymers and the biomass so that monomers can be recovered
usable. Analysis of experiments with organic wood preserva-
as well. For example, HPL is produced with an amount of
tives showed that they are predominantly degraded during
30 wt.-% phenol-formaldehyde resole resins. It could be
± demonstrated that 50±60 wt.-% of phenolic compounds could
1) List of abbreviations at the end of the paper. be recovered via pyrolysis.
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Feedstock like grinding grit from a panel board producer or fraction that is already used commercially as liquid smoke in
cocoa shell of a German cocoa roasting company could be food industry in the USA and Canada. Also in Europe, liquid
converted with a much smaller (200 g/h feed) laboratory scale smoke is coming to the market. Phenolic compounds of
pyrolysis plant of similar design. The results where promising. thermal lignin degradation can be used in formulation of
The plant runs without problems and leads to good oil yields. resins for woody materials. Further investigations for a
Detailed results of the experiments presented in this paper are complete commercial use of pyrolysis oil from biomass would
already open to public [7,11,23,26,27]. be desirable [33].
The product fraction pyrolysis oil consists of condensable Technology of fast pyrolysis via fluidized-bed reactors is
product gases and separated aerosols. Contrary to mineral oil, considered to as fully developed. Now, pilot- and industrial
a distillation of pyrolysis oil is not possible because of its scale plants are required to bring the described process on the
thermal instability. market.
The oil fractions from three heat exchangers, respectively Received: February 27, 2002 [F 005]
from the scrubber and the electrostatic precipitators, are
analyzed quantitatively and qualitatively and are summed in
the mass balance. A comparison of a separation capacity of Abbreviations
each heat exchanger is not useful because of the missing
regulation and control of cooling capacity. Condensation PDU process demonstration unit
ranges could not be fixed. TP Technicum scale pyrolysis
It is difficult to define quality characteristics for pyrolysis oil. Al-HDO synonym for: Xyligen-Al, salt of:
There are a few working groups who are dealing with n-nitroso-n-cyclohexylhydroxylamin,-
application of physical and chemical analysis techniques on tris-(n-cyclohexyldiazenium-dioxy)-Al
pyrolysis oil. An important criterion for the quality of the HPL high-pressure-laminate
process and the pyrolysis oil is the ratio of reaction water, which
is the total water amount minus wood moisture. Too much
reaction water (40 wt.-% and more) is an indicator for unwanted References
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