Note: Descriptions are shown in the official language in which they were submitted.
K 977
Hsb/Sb
CONVERTING A STREAM CONTAINING HEAVY HYDRVCARBONS
INTO A STREAM CONTAINING HYDROCARBONS
HAVING A LOWER BOILING RANGE
The present invention relates to a process for
converting a stream containing heavy hydrocarbons
having a high boiling range into a stream containing
hydrocarbons having a lower boiling range.
It is an object of the present invention to
provide a process for converting in a first stage a
substantially liquid stream and in a second stage a
: substantially gaseous stream.
To this end the process for converting a stream
containing heavy hydrocarbons having a high boiling
; range into a stream containing hydrocarbons having a
lower boiling range according to the invPntion
comprises the steps of
~ a) passing through a first conversion zone
:~ 15 containing a conversion catalyst in the presence of
- hydrogen the stream containing heavy hydrocarbons
:~ having a high boiling range at a temperature between
325 and 600 C, a pressure between l and 30 MPa and at
an hourly space veIccity between 0.05 and 5 kg~l/hour
to produce a primary converted stream;
~ : b) passing the primary converted stream ~o a first
:: separation zone and removing from the first separation
zone a gaseous stream and a liquid stream;
:~ c) passing at least a part of the gaseous stream
to a second conversion zone; and :
d) passing through the second conversion one
containing a conversion catalyst in the presence of
hydrogen the gaseous stream at a temperature between
325 and 600 oc, a pressure between l and 30 MPa and at
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an hourly space velocity between 0.1 and 10.0 kg/l/hour
to produce a further converted stream having a lower
boiling range.
An advantage o~ the process according to the
invention is that no fractional distillation is carried
out between the first conversion zone and the second
conversion zone. A further advantage i5 that the
gaseous stream is maintained at a high pressure and at
a high temperature.
Known is a process for hydrotreating pyrolysis
gasoline, which is a hydrocarbon-containing stream
having a boiling range between 180 and 205 C,
comprising treating the stream in a ~irst reactor at a
temperature between 80 and 130 C and a pxessure o~
about 6 MPa, separating the effluent from the first
reactor into a gaseous stream and a liquid stream of
which a part is returned to the first reactor, treating
the gaseous stream and the remaining part of the liquid
stream combined in a second reactor at a temperature
between 230 and 280 C and a pressure between 4.5 and
6.5 MPa, and separating the e~fluent from the second
reactor into a gaseous stream which is recycled to the
second reactor and a liquid product stream.
; In the specification and in the claims the
expression "heavy hydrocarbons having a high boiling
range" is used to refer to hydrocarbons containing more
than 70% by weight of hydrocarbons having a boiling
range above 370 C. These hydrocarbons ~urther may
con~ain sulphur~ for example between 0.05 and 8~ by
weight, and heavy metals such as vanadium, for example
between 0.5 and 2 000 ppm (parts per million). The
~` expression "hydrocarbons having a lower boiling range"
is used to refer to hydrocarbons which are liquid at
normal conditions containing more than 40% by weight
hydrocarbons having a boiling range below 370 C.
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In the speci~ication and in the claims the hourly
space velocity is expressed as kg hydrocarbon-
containing stream per liter of catalyst per hour
(kg/l/hour).
The first conversion zone contains a ~irst
conversion catalyst suitable l`or hydrocarbon
conversion, for removal of asphaltenes, for producing
hydrocarbons having a decreased amount of carbon
residue left after evaporation and pyrolysis, and/or
for demetallization. Examples of suitable catalysts are
catalysts comprising an inorganic oxidic carrier, for
example silica and/or alumina, containing one or more
compounds of nickel, vanadium, molybdenum and tungsten.
The second conversion zone contains a second
conversion catalyst suitable for desulphurization,
hydrogenation and/or denitrogenation of a gaseous
hydrocarbon stream. Examples of suitable catalysts are
catalysts comprising an inorganic oxidic carrier, for
example alumina and/or silica, containing either nickel
and/or cobalt, or molybdenum and~or tungsten.
Heavy metals from the hydrocarbons having a high
boiling range are deposited on the catalyst in the
first conversion zone. Furthermore, in the separation
zone heavy highly aromatic molecules, which are still
present in the product from the first conversion zone,
are separated from the gaseous stream. Therefore a
stream substantially free of heavy metal~ and of heavy
aromatic molecules is contacted with ths catalyst in
the second conversion zone. This has a beneficial
effect on the life of the catalyst in the second
conversion zone.
The invention will now be described by way of
example in more detail with reference to the drawings,
wherein
Figure 1 shows schematically a first embodiment of
the invention:
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Figure 2 shows schematically a second embodiment
o~ the invention;
Figure 3 shows schematically a third embodiment of
the invention; and
Figure 4 shows schematically a fourth embodiment
of the invention.
Re~erence is made to Figure 1 showing an apparatus
~or carrying out the process according to the
invention. The apparatus comprises a ~irst conversion
zone in the ~orm of first reactor 1, a ~irst separation
zone in the form of ~irst gas/liquid separator 4 and a
second conversion zone in the form o~ second reactor 7.
To the first reactor 1 a hydrogen supply conduit 8 and
a feed supply conduit 9 are connected. The first
gas/liquid separator 4 is connected to the first
reactor 1 by means of conduit 10. The upper zone of the
first gas/liquid separator 4 is connPcted to the second
reactor 7 by means of conduit 12, and a li~uid conduit
15 is connected to the lowar
zone of the ~irst gas/liquid separator 4. To the second
reactor 7 a second hydrogen supply conduit 17 is
connected, and to the upper end of the second reactor 7
: an effluent removal conduit 18 is connected.
During normal operationt a preheated, ~ubstantially
liquid stream containing hea~y hydrocarbons having a
high boiling range is supplied to the first reactor 1
through the feed supply conduit 9, and hydrogen is
supplied to the first reactor 1 through the hydrogen
supply conduit 8. The temperature of the hydrocarbon-
containing stream is between 325 and 600 C and
suitably between 350 and 500 C, the pressure between 1
and 30 MPa and suitably between 2 and 25 MPa, and the
rate at which the hydrocarbon-containing stream i~
supplied is selected such that in the first reactor 1
the hourly space velocity is between 0.05 and 5
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kg/1/hour and suitably between 0.1 and 2.5 kg/l/hour.
The amount of hydrogen is suitab]y between 250 and 2
ooO Nm3 per 1 000 kg hydrocarbon-containing stream. A
primary converted stream is removed from the first
reactor 1 and is passed via conduit 10 to the first
gas/liquid separator 4. From the first gas/liquid
separator 4 a gaseous stream and a liquid stream are
removed. Since the gas/liquid separation is carried out
substantially at the same pr~ssures and temperatures as
the conversions in the ~irst reactor and second reactor
the gaseous stream, which contains hydrogen, is passed
to the second reactor without substantially heating
and/or pressurizing.
The gaseous stream is supp]ied via conduit 12 to
the second reactor 7 at a temperature between 325 and
600 C and suitably between 350 and 500 C, a pressure
between 1 and 30 MPa and suitably between 2 and 25 MPa.
The amount of catalyst in the second reactor 7 is such
that at the rate at which the hydrocarbon~containing
stream is supplied the hourly space velocity is between
0.1 and 10.0 kg/l/hour and suitably between 0.25 and
5.0 kg/l/hour. In addition hydrogen can be supplied to
the second reactor 7, the amount of hydrogen being
suitably up to 2 000 Nm3 per kg hydrocarbon-containing
stream. A further converted stream containing hydro-
carbons having a lower boiling range is withdrawn from
the second reactor 7 through effluent removal conduit
18.
To control the pressurs in the first gas/li~uid
separator 4 and in the second reactor 7, the conduits
10 and/or 12 may be provided with pressure control
means (not shown)O
EXAMPLE 1
A liquid hydrocarbon-containing stream containing
93.5% by weight of hydrocarbons having a boiling range
above 370 C`, 4~7~ by weight sulphur, and 84 ppm
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vanadium is supplied to the first reactor l at an
hourly space velocity of l kg/l/hour, a temperature of
440 oc and a pressure of 15 MPa. Hydrogen is supplied
to the first reactor l at a rate of l 000 Nm3/l 000 kg
S of liquid hydrocarbon-contain:ing stream. The ~irst
reactor l is filled with a ca1:alyst comprising a
silica-containing carrier and compounds of nickel and
vanadium. The primary converted stream produced in the
~irst reactor 1 is passed to t:he first gas/liquid
separator 4 and from the first: gas/liquid separator 4 a
gaseous stream and a liquid st:ream are removed.
The liquid stream is removed from the first
gas/liquid separator 4 through liquid conduit 15, and
the amount of the liquid stream is 39% by weight of the
liquid hydrocarbon-containing stream supplied to the
first reactor. The liguid stream contains 53.47% by
weight of hydrocarbons having a boiling range between
370 and
520 C and 46.53% by weight o~ hydrocarbons having a
boiling range above 520 oc, and contains further 3.2%
by weight of sulphur and 4 ppm vanadium.
The gaseous stream removed from the first
gas/liquid separator 4 through conduit 12 comprises
hydrocarbons and hydrogen, the hydrocarbon content of
this stream is 6~% by weight of the liquid hydrocarbon-
containing stream supplied to the first reactor lo The
hydrocarbon part o~ the gaseous stream comprises 83% by
weight hydrocarbons having a boiling range below 370 C
and 0.8% by weight sulphur.
This gaseous stream is suppIied to the second
reactor 7 at a temperature of 410 C and a pressure of
13 MPa. ~o extra hydrogen is supplied to the second
reactor 7. The second reactor 7 is filled with a
catalyst comprising an alumina-containing carrier and
compounds of nickel and molybdenum. The volume of the
reactor filled with catalyst is such that at the rate
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at which the stream to be treated is supplied the
hourly space velocity is 0.5 kg/l/hour.
The further converted stream produced in the
second reactor 7 contains hydrocarbons, hydrogen and
gaseous contaminants such as H2S and NH3. The hydro-
carbon content of the further converted stream e~lals
61% by weight of the licluid hydrocarbon-containing
stream supplied to the first reactor 1, and it
comprises 9.64~ by weight of hydrocarbons having l to 4
carbon atoms, 32.7B% by weight of hydrocarbons having
more than 5 carbon atoms and a boiling range below 250
C, 49.61% by weight of hydrocarbons ha~ing a boiling
range between 250 and 370 C, 7.98% by weight of
hydrocarbons having a boiling range between 370 and 520
C, and 0.014% by weight o~ sulphur. It will be
appreciated that hydrogen sulphide and hydrogen can be
removed from the further converted stream in a
conventional manner which is not described here, and
that the separated hydrogen can be compressed and
reused in the first or second conversion zone.
In the embodiment of the invention shown in Figure
2 liquid conduit 15 is connected by means of conduit 20
to the feed supply conduit 9. The parts of the
apparatus shown in Figura 2 which are similar to the
parts shown in Figure 1 have the same referenc~
numerals. This embodiment allows passing to the first
reactor l a part of or substantially all lic~id
separated from the primary converted stream tQ the
first r~actor 1, so that the liquid stream can be
further converted with the catalyst in the first
reactor 1.
EXAMPLE 2
The hydrocarbon-containing stream of Example 1 is
supplied uncler the same conditions to the first reactor
1 together with a recycle stream to be described
hereinafter.
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The amount of liquid stream removed ~rom the first
gas/liquid separator 4 is 106~ by weight of the liquid
hydrocarbon-containing stream supplied to the first
reactor 1. The liquid stream contains 61.03~ by weight
of hydrocarbons having a boiling range between 370 and
520 C and 38.97~ by weight of hydrocarbons ha~ing a
boiling range above 520 C, and contains further 2% by
weight of sulphur and 2 ppm vanadium. From the liquid
removed from the first gas/lic~id separator 4 an amount
equal to ~0% by weight of the liquid hydrocarbon-
containing stream supplied to the first reactor 1 is
passed as the recycle stream to the first reactor 1
through conduit 20.
The amount of liquid stream removed from liquid
conduit 15 downstream to the point where conduit Z0 is
connected to conduit 15 is 46% by weight of the
hydrocarbon-containing stream supplied to the first
reactor 1, and this stream is removed as a bottom
product.
The gaseous stream removed fxom the gas/liquid
separator 4 through conduit 12 contains hydrocarbons
and hydrogen, the hydrocarbon cont~nt of the gaseous
stream is 54% by weight of the hydrocarbon-containing
stream supplied to the first reactor 1. The hydrocarbon
part of the gaseous stream comprises 73% by weight of
hydrocarbons having a boiling range below 370 C and
0.9~ by weight sulphur. This gaseous stream is supplied
to the second reactor 7 at a temperature of 410 C and
a pressure of 13 MPa. No extra hydrogen is supplied to
the second reactor 7. The second reactor 7 is filled
with the same catalyst as in Example l. The volume of
the reactor filled with catalyst is such that at the
rate at which the stream ~o be treated is upplied the
hourly space velocity is 0.5 kg/l/hour.
The further converted stream produced in the
second reactor 7 contains hydrocarbons, hydrogen and
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contaminants such as H2S and NH3. The hydrocarbon part
of the further converted stream comprises 7.33~ by
weight of hydrocarbons having 1 to 4 carbon atoms,
28.86% by weight of hydrocarbons having more than 5
carbon atoms and a boiling range below 250 C, 50.73
by weight of hydrocarbons having a boiling range
between 250 and 370 C, and 13.08% by weight of
hydrocarbons having a boiling range between 370 and
520 C and 0.021% by weight of sulphur. The amount of
hydrocarbons in the range C1-C~ in the ~urther
converted stream per unit of converted heavy
hydrocarbon is less than in the further converted
stream produced in h'xample l.
For some kinds of heavy hydrocarbons to be
converted it would be more profitable to increase the
upper limit of the boiling range of the gaseous skream
supplied to the second reactor in order to improve the
overall conversion of the hydrocarbons having a boiling
range above 370 C.
To increase the upper limit of the boiling range
of the gaseous stream liquid outlet 15 is connected to
a second separation zone in the ~orm of second gas/-
liquid separator 24 (see Figure 3). The gaseous
hydrocarbons are removed from the second gas/liquid
separator 24 and passed through conduit 25 to conduit
12 and into the second conversion reactor 7.
The liquid hydrocarbons are removed from the
second gas/liquid separator 24 through conduit 26. If
required a part of the liquid hydrocarbons may be added
through conduit 27 to the stream containing heavy
hydrocarbons having a high boiling range before this
stream i.s passed through the first reactor 1.
EXAMPLE 3
A hydrocarbon-containing stream containing 90.5%
by weight o~ hydrocarbons having a boiling range above
370 C, 4.7% by weight sulphur, and 84 ppm vanadium is
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supplied to the first reactor 1 at an hourly space
velocity of 1 kg/l/hour, a temperature of 440C and a
pressure of 15 MPa, together with a recycle stream to
be described hereinafter. Hydrogen is supplied to the
first reactor 1 at a rate of 1 000 Nm3/1 000 kg of
hydrocarbon-containing stream. The first reactor 1 is
filled with a catalyst comprising a silica-containing
carrier and compounds of nickel and vanadium. The
primary converted stream produced in the first reactor
1 is passed to the first gas/liquid separator 4 and
from the first separation zonle a gaseous stream and a
liquid stream are removed.
The liquid stream is removed from the gas/liquid
separator 4 through liquid conduit 15. The amount of
this liquid stream is 77% by weight of the hydrocarbon-
containing stream supplied to the first reactor 1, and
the liquid stream does not contain hydrocarbons having
a boiling range below 410 C, and contains 1.9~ by
weight of sulphur and 4 ppm vanadium. The liquid stream
is supplied to the second gas/liquid separator 24. In
the second gas/liquid separator 24, operating at a
pressure of 30 mm Hg, the stream is separated into a
gaseous stream, corresponding to 28.4 % by weight of
the hydrocarbon-containing stream supplied to the first
reactor ~, and a liquid stream. The gaseous stream is
supplied to the second reactor 7. The liquid stream
contains 4.03% by weight of hydrocarbons having a
boiling range between 370 and 520 C and 95.97% by
weight of hydrocarbons having a boiling range above
520 CO A fraction of the liquid stream, corresponding
to 30 % by weight of the hydrocarbon-containing stream
supplied, is supplied as the recycle stream to the
`~ first reactor 1 through conduit 27 to the first reactor
1, and the remaining part of the liquid stream,
correspondin~ to 19 % by weight of the hydrocarbon-
containing stream supplied to the flrst reactor 1, is
,
removed through conduit 26 downstream conduit 27 as a
bottom product.
The gaseous stream removed from the gas/liquid
separator 4 through conduit 12 contains hydrocarbons
and hydrogen, the hydrocarbon content of the gaseous
stream is 54~ by weight of the hydrocarbon-containing
stream supplied to the first :reactor 1. The hydrocarbon
part of the gaseous stream comprises 73% by weight o~
hydrocarbons having a boiling range below 370 C and
0.9% ~y weight of sulphur. Th.i~ gaseous stream is
supplied to the second reactor 7.
The gaseous streams from the separators 4 and 24
are supplied to the second reactor 7 at a temperature
o~ 410 oc and a pressure of 13 MPa. The total amount of
the gaseous streams is 81% by weight o~ the hydro-
carbon-containing stream supplied to the first reactor
1. No extra hydrogen is supplied to the second reactor
7. The second reactor 7 is Pilled with a catalyst
comprising an alumina cont ining carrier and compounds
of nickel and molybdenum. The volume of the reactor
~illed with catalyst is such that at the rate ak which
the streams to be treated are supplied the hourly space
velocity is 0.5 kg/l/hour.
The hydrocarbon content o~ the further converted
: 25 stream produced in the second reactor 7 is 81% by
weight o~ the hydrocarbon-containing stream supplied to
the first reactor 1, and the further converted stream
comprises 5.75% by weight of hydrocarbons having 1 to 4
carbon atoms, 25.90% by weight of hydrocarbons having
more than 5 carbon atoms and a boiling range below 250
C, 42.34% by weight of hydrocarbons having a boiling
range between 250 and 370 C, 25.74% by weight of
hydrocarbons having a boiling range between 370 and 520
C, 0.26% by weight of hydrocarbons having a boiling
range above 520 DC, and 0.032% by weight o~ sulphur~
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Reference is now ~ade to Figure 4, showing an
embodimant of the invention wherein the liquid stream
removed from the first gas/liquid separator 4 is passed
through conduit 15 for further conversion to a third
conversion zone in the form of third reactor 30. In the
third reactor 30 the liquid stream is contacted in the
presence of hydrogen with a conversion catalyst of the
kind which is present in the second reactor 7 to
produce a secondary converted stream.
This conversion catalyst is suitable for
desulphurization, hydrogenation and/or denitrogenation
o~ a gaseous hydrocarbon stream. Examples of suitable
catalysts are catalysts comprising a carrier containing
alumina or silica and alumina, and either nickel and/or
cobalt, or molybdenum and/or tungsten.
The temperature of the liquid stream is between
325 and 600 C and suitably between 350 and 500 C, the
; pressure in the third reactor 30 is between 1 and 30
MPa and suitably between 2 and 25 MPa, and the volume
o~ catalyst in the third reactor 30 i~ such that at the
rate at which the liquid stream is supplied the hourly
space velocity in the third reactor 30 is between 0.05
and
10 kg/l/hour and suitably between Ool and 5 kg/l/hour.
~ 25 If required hydrogen can be supplied to the third
; reactor through hydro~en supply conduit 31. The
secondary converted stream is removed ~rom the third
reactor 30 through outlet conduit 32.
To remove the gaseous components from the
secondary converted stream this stream can be passed
directly to the first gas/liquid separator (not shown),
or the secondary converted stream can be passed to a
third sep~ration zone in the form of third gas/liquid
separator 35.
From the third gasJliquid separator 35 a gaseous
straam is passed through conduit 36 to the second
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reactor 7. A liquid stream is removed from the third
gas/liquid separator 35 through conduit 37. Xf required
a part or all of the liquid stream can be passed
through conduit 3g to the first reactor 1.
EXAMPLE 4
The hydrocarbon-containing stream of Example 1 is
supplied under the same conditions to the first reactor
1 together with a recycle stream as hereinafter
described.
The gaseous stream removed fxom the gas/liquid
separator 4 through conduit 12 contains hydrocarbons
and hydrogen, and the hydrocarbon content of the
gaseous stream is 54% by weight of the hydrocarbon-
containing stream supplied to the first reactor 1. The
hydrocarbon part of the gaseous stream comprises 73% by
: weight of hydrocarbons having a boiling range below 370
C, 0.9% by weight of sulphur. This gaseous stream is
supplied to the second reactor 7 at a temperature o~
410 C and a pressure of 13 MPa.
The liquid stream is removed from liguid conduit
15. The amount of the liquid stream is 76% by weight of
the hydrocarbon-containing stream supplied to the first
reactor 1, and comprises 63% by weight having a boiling
range above 52~ C and does not contain hydrocarbons
25 having a boiling range below 410 C, and 1.9% by weight
of sulphur.
The liquid stream is passed to the third reactor
~ 30 which is filled with a catalyst comprising an
: alumina-containing carxier and compounds of nickel and
molybdenum. The volume of the reactor filled with
catalyst is such that at the rate at which the stream
to be treated i5 supplied the hourly space velocity is
2.7 kg/l/hour. The secondary converted stream produced
in the third reactor 30 comprises 97~ by weight of
hydrocarbons having a boiling range above 370 C and
58% by weight of hydrocarbons having a boiling range
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above 520 ~C, and 0.4% by weight of sulphur. This
stream is passed through conduit 32 to the third
gas/liquid separator 35, operating at 30 mm Hg.
The amount of liquid stream obtained in the third
gas/liquid separator 35 is 45% by weight of the
hydrocarbon-containing stream supplied to khe first
reactor 1. The liquid stream contains 3.97% by weight
of hydrocarbons having a boiling range between 370 and
520 C and 96.03% by weight O:e hydrocarbons having a
boiling range above 520 C. A part of the liquid
stream, corresponding to 15~ by weight of the
hydrocarbon-containing stream as supplied to the first
reactor 1, is removed through conduit 37 as a bottom
product.
The remaining part of the liquid stream is passed
through conduit 38 ~s the recycle stream to the first
reactor 1, the amount of this stream is 30% by weight
of the hydrocarbon-containing stream supplied to the
first reactor 1.
The amount of the gaseous stream obtained in the
third gas/liquid separator 35 equals 31% by weight of
the hydrocarbon-containing stream supplied to the first
reactor 1. The gaseous stream is passed through conduit
36 to the second reactor 7, where it is converted
together with the gaseous stream from the first
gas/liquid separator 4. No extra hydrogen is supplied
to the second reactor. The second reactor 7 is ~illed
with a catalyst comprising an alumina-containing
carrier and compounds of nickel and molybdenum. The
volume of the reactor filled with catalyst is such that
at the rate at which the stream to be treated is
supplied the hourly space velocity is 0.5 kg/l/hour.
The hydrocaxbon content of the further converted
stream produced in the second reactor 7 is 84.90% by
weight of the hydrocarbon-containing stream supplied to
the first reactor 1, the further converted stream
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comprises 6.15% by weight of hydrocarbons having 1 to 4
carbon atoms, 24.50% by weight o~ hydrocarbons having
more than 5 carbon atoms and a boiling range below 250
oc, 41.41% by weight of hydrocarbons having a boiling
ranye between 250 and 370 C, 27.59% by weight of
hydrocarbons having a boiling range between 370 and 520
C, 0.33% by weight of hydrocarbons having a boiling
range above 520 C, and 0.020% by weight of sulphur.
A reactor as referred to in the Figures with
reference numeral 1, 7 or 31 may be a packed bed
reactor wherein the catalyst is arranged in a
stationary bed, or a moving bed reactor wherein spent
catalyst is continuously removed from the reactor at a
predetermined rate and fresh catalyst is supplied to
the reactor to replace spent catalyst, or a fluidized
bed reactor wherein catalyst is fluidized by upwardly
flowing fluid to be converted.
Each conversion zone may comprise a single reactor
~ or more than one, fox example three or four.
: 20 Hydrogen may be introduced as a separate stream
into the reactor, or it may be mixed with the fluid to
be converted before the fluid enters into the reactor.
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