Specification
METHOD FOR FILLING A CHAMBER WITH A VARIABLE-DENSITY
PARTICLE BED
The present invention relates to a method for filling a
chamber with a particulate solid, allowing the density
of the deposited particle bed to be adjusted.
The invention relates more particularly to the loading
of chemical or electrochemical, petroleum or
petrochemical fixed bed reactors, with solid particles
in the divided state, which may be in the form of
beads, grains, cylinders, pellets, rods, or any other
shape, but having relatively small dimensions. The
particles may in particular be molecular sieves or
catalysts in bead or pellet form or most often in the
form of extrudates, of single- or multilobe type, the
dimensions of which vary, according to each case, from
a few tenths of millimeters to a few centimeters.
This is the application to which reference is made more
particularly in the rest of the present description,
but the method in accordance with the invention applies
to the loading of any other type of solid particles
into a chamber, in which it is necessary to adjust, on
demand, the density of the loaded particle bed.
In the field of charging fixed bed chemical reactors
with solid catalyst particles, two filling techniques
are mainly singled out, namely:
• the conventional technique, generally denoted
by the term "sock loading", which consists in
introducing, at the top of the reactor, the catalyst
particles into the upper end of a generally flexible
sock in order to deposit them by gravity, via the other
end of the same sock, at the bottom of the reactor,
then onto the fixed bed that is in the process of being
formed; and
• the dense loading technique that consists in
introducing the catalyst particles also via the top of
the reactor, then in dispersing them during their fall
via a generally movable device containing suitable
deflectors, located in the upper part of the chamber,
so as to make them drop individually by a "rain effect"
onto the loading front where they are positioned
freely.
The catalyst beds thus obtained are loaded in a nondense
and inhomogeneous manner with the sock loading
type filling technique whereas the loading is dense and
homogeneous when the filling method is the rain-effect
method.
The devices and methods enabling rain-effect loading of
fixed bed chemical reactors are described for example,
in applications EP 007 854, EP 116 246, EP 769 462,
EP 482 991, FR 2 766 386 and FR 2 721 900.
The various rain-effect loading techniques commonly
used have the advantage of using as much as possible of
the space available inside the chamber, while allowing
a quantity of catalyst, which may possibly range up to
20% more than with the conventional "sock loading"
technique, to be introduced into a given reactor
volume.
The high homogeneity of fixed catalyst beds loaded in a
dense manner is obtained by a highly regular
distribution of the catalyst particles, promoting
homogeneous flow and reaction kinetics over the whole
of the catalyst bed volume, whereas the conventional
technique of loading using a sock (sock loading) often
leads to the formation of preferential pathways for the
reaction medium that are the cause of a reduction in
the yield of the reactor. The dense catalyst beds have,
in addition, the advantage of not settling very much
throughout their whole operating period, this settling
- 3 -
generally not exceeding 1 to 2% of the height of the
catalyst bed, whereas it may reach 8 to 10% for a
conventional loading, that is to say of sock loading
type.
Although the dense loading techniques currently
represent a large part of the market, bringing them
into general use has been held back up till now by the
fact that high-density beds have a relatively higher
pressure drop (AP) than non-dense fixed beds of
equivalent height. As a result, in such a high-density
bed, the reaction medium flow rate for a given pressure
is lower than in a non-dense bed or, conversely, in
order to obtain an identical reaction flow rate, it is
then necessary to apply a higher pressure. In addition,
one of the features of the dense loading techniques is
that the density obtained in due to luck, for the most
part depending only on the geometric features and the
state of the surface of the catalyst particles, that is
to say without control being possible by adjustment of
the devices and methods used.
Until now, a person skilled in the art therefore had to
choose between, on the one hand, non-dense catalyst
beds affected by a lack of homogeneity and a
significant settling of the bed over time, and
homogeneous dense catalyst beds, admittedly allowing
excellent reaction yields, but having a significantly
higher pressure drop (AP).
FR 2 812 824 proposes a method of rain-effect loading
into a liquid contained in the chamber to be loaded,
making it possible to thus obtain a homogeneous and
non-dense loading. Unfortunately, said liquid, which
must be inert with respect to the particles to be
loaded, is not always available on the loading site or
the specific physicochemical properties of said
particles do not allow their immersion in a liquid.
There is therefore a demand for a method for filling
catalytic fixed bed reactors that allows catalyst beds
to be obtained that are both homogeneous and relatively
low dense.
Within the scope of their research aiming to improve
the known methods for loading reactors, the Applicant
has developed a novel filling method that makes it
possible to obtain homogeneous catalyst beds having a
density between that of dense beds and that of nondense
beds (obtained by sock loading). This novel
method is a loading method using a "solid diluent",
namely a granular solid material introduced into the
reactor at the same time as the catalyst and which will
be removed before or during start-up of the reactor, by
simply dissolving it with a suitable solvent, said
solvent possibly being formed directly by the reactive
load. The higher the quantity of solid diluent, removed
before or during start-up of the reactor, the lower the
final density of the catalyst bed. Therefore, this
final density of the bed may be adjusted by modifying
the proportion of solid diluent introduced with the
catalyst.
Consequently, one subject of the present invention is a
method for filling a chamber, especially a chemical
reactor, with a granular solid material at an
adjustable loading density, comprising the following
steps consisting in:
(a) filling said chamber with a mixture of a
first granular solid material (A) and a solid diluent
(B) , which is a second granular solid material, having
different solubility properties from the first granular
solid material (A); and
(b) removing all of the solid diluent (B) and
leaving only the first granular solid material (A) in
the chamber, by passing through the fixed bed deposited
in step (a), a solvent having a zero ability to
dissolve the first granular solid material (A) and a
strong ability to dissolve the second granular solid
material (B).
The method for filling the chamber with the mixture of
the two solid materials (A and B) may use the
conventional technique of loading with a sock (sock
loading), but preferably will use the technique known
as the "rain-effect" technique, consisting in
depositing the material grains over the entire surface
of the bottom of the chamber, then over the surface of
the catalyst bed during its formation. The rain-effect
loading technique may use a device consisting of a
rotating, solid or hollow, central shaft, onto which
flexible strips, for example made from rubber, are
placed and also distributed at various levels, which
diverge from said shaft according to its rotation
speed.
As explained above, this loading method allows the
density of the final catalyst bed to be freely adjusted
within a given range of densities. The higher the
volume proportion of the solid diluent (B) in the
granular solid catalyst (A) + solid diluent (B)
mixture, the lower the final loading density. A person
skilled in the art will however easily understand that
this proportion of solid diluent (B) must not exceed a
certain upper limit that depends, in particular, on the
shape of the catalyst particles and on the size ratio
of the catalyst particles to the solid diluent. Indeed,
beyond a certain solid diluent (B) portion limit, the
catalyst bed will become mechanically unstable after
dissolving the solid diluent, and will settle as a
whole under the effect of gravity or of the flow of the
reaction medium, thus creating preferential flow paths
that are undesirable.
The Applicant has observed during their research that
the volume proportion of solid diluent (B) in the
granular solid (A) + solid diluent (B) mixture should
generally not exceed 20 to 30%. The terra "volume
proportion" is understood to mean here the ratio of the
bulk volume of the solid diluent (B) to the sum of the
bulk volumes of the granular solid (A) and the solid
diluent (B) . This upper limit is close to 20% when the
granular solid (A) and the solid diluent (B) have
approximately the same dimensions and when almost all
the solid diluent particles are used to separate the
catalyst particles. On the other hand, when the solid
diluent has dimensions that are markedly below those of
the granular solid material, and when a certain
fraction of the solid diluent particles are located
either in the pores or cavities of the catalyst, or in
the interstices between the catalyst particles without
separating these particles, the volume proportion limit
may be greater than 30%.
Consequently, in the method of the present invention,
the degree of dilution of the first granular solid
material (A) by the solid diluent (B) , that is to say
the V(A)/(V(A)+V(B) ) volume ratio (with V(A) = bulk
volume of the granular solid (A) and V
Documents
Application Documents
| # |
Name |
Date |
| 1 |
1309-DELNP-2007_EXAMREPORT.pdf |
2016-06-30 |
| 1 |
abstract.jpg |
2011-08-21 |
| 2 |
1309-delnp-2007-pct-304.pdf |
2011-08-21 |
| 2 |
1309-delnp-2007-abstract.pdf |
2011-08-21 |
| 3 |
1309-delnp-2007-pct-210.pdf |
2011-08-21 |
| 3 |
1309-delnp-2007-claims.pdf |
2011-08-21 |
| 4 |
1309-DELNP-2007-Correspondence-Others.pdf |
2011-08-21 |
| 4 |
1309-delnp-2007-gpa.pdf |
2011-08-21 |
| 5 |
1309-delnp-2007-form-5.pdf |
2011-08-21 |
| 5 |
1309-delnp-2007-description (complete).pdf |
2011-08-21 |
| 6 |
1309-DELNP-2007-Form-3.pdf |
2011-08-21 |
| 6 |
1309-delnp-2007-drawings.pdf |
2011-08-21 |
| 7 |
1309-delnp-2007-form-2.pdf |
2011-08-21 |
| 7 |
1309-delnp-2007-form-1.pdf |
2011-08-21 |
| 8 |
1309-delnp-2007-form-2.pdf |
2011-08-21 |
| 8 |
1309-delnp-2007-form-1.pdf |
2011-08-21 |
| 9 |
1309-DELNP-2007-Form-3.pdf |
2011-08-21 |
| 9 |
1309-delnp-2007-drawings.pdf |
2011-08-21 |
| 10 |
1309-delnp-2007-description (complete).pdf |
2011-08-21 |
| 10 |
1309-delnp-2007-form-5.pdf |
2011-08-21 |
| 11 |
1309-DELNP-2007-Correspondence-Others.pdf |
2011-08-21 |
| 11 |
1309-delnp-2007-gpa.pdf |
2011-08-21 |
| 12 |
1309-delnp-2007-pct-210.pdf |
2011-08-21 |
| 12 |
1309-delnp-2007-claims.pdf |
2011-08-21 |
| 13 |
1309-delnp-2007-pct-304.pdf |
2011-08-21 |
| 13 |
1309-delnp-2007-abstract.pdf |
2011-08-21 |
| 14 |
abstract.jpg |
2011-08-21 |
| 14 |
1309-DELNP-2007_EXAMREPORT.pdf |
2016-06-30 |