Note: Descriptions are shown in the official language in which they were submitted.
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Reaction Vessel Holdina Device fi ~~AN~~.,~~'10N
The present invention relates to a reaction
vessel holding device, as defined in the preamble of
the independent Claim 1, and a reaction block with a
reaction vessel holding device of this type.
In chemical research in the pharmaceutical
industry and universities, it is becoming more and more
important to discover as fast as possible a large
number of potential active ingredients and then to test
them. Some of the chemical research, therefore,
currently deals with combinatory chemistry, parallel
synthesis and high-speed chemistry. In this work, the
possibility of being able to employ known or new types
of chemical reactions with the least possible amount of
adaptation and to the greatest extent is of central
importance.
In consequence, the most varied types of devi-
ces have been created for carrying out a multiplicity
of chemical, biochemical or physical processes in
parallel. All of these processes, however, are either
only suitable for special applications or are too
complicated in construction, too large or are not user-
friendly and/or do not permit the individual process
steps to be sufficiently automated.
Such a device is marketed by Advanced Chemtech,
Europe SA under the designation 496 MBS. This compri-
ses a reaction block with a plurality of included
depressions within which the reactions can be carried
out. The complete block is moved by a vibration devi-
ce, which is attached below it and this leads to a not
very efficient mixing of the reactants in the depres-
CA 02294941 1999-12-15
1
sions. Liquids can be supplied to and/or extracted
from the depressions by means of hollow needles,
sealing of the individual depressions relative to the
outside being realized by means of septa/septum plates.
This device also has the disadvantage that it
is necessary to move the full weight in order to shake
the reaction block. This is one reason why shaking (or
vibration) is only carried out with small amplitudes.
Shaking during the supply or extraction of fluid, which
is often necessary or even essential, is impossible for
technical reasons (needles would, for example, be moved
along with the septum) . In addition, operation with a
gas is only possible to a very limited extent (septa) .
Theoretically, operation under vacuum would only be
possible to a very limited extent. The septa are no
longer leak-tight, at the latest after each penetration
by the needles usually employed. In addition, a part
of the evaporated medium, for example, condenses on the
cold septa which, on the one hand, makes contamination
of the reaction mixture probable due, for example, to
softeners in the plastic of the septum (this also
applies to all the other applications of septa in the
chemical or biological reaction procedure described
here). In addition, however, particularly in associa-
tion with the sealing argument quoted above, very many
applications demand evaporation of high-boiling-point
solvents, for example dimethyl formamide or dimethyl
sulphoxide, in a relatively short time and/or at
relatively low temperatures (due, for example, to the
usually limited stability of chemical compounds in che-
mical or biological processes). The reaction vessels
cannot be fully opened and closed automatically.
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A reaction vessel holding device is known from
US-A-5 503 805 which has a fixed part and a multiplici-
ty of reaction vessels fastened to it by means of
flexible hoses. The supply of liquid into the reaction
vessels takes place from a starting vessel via a
further hose, a multiple valve and the flexible hoses
mentioned or otherwise from below. One disadvantage of
this device consists in the fact that powder cannot be
supplied to the reaction vessels, that it is not possi-
ble to dose precisely in this way and that the supply
of different liquids in different reaction vessels is
relatively complicated because the supply takes place
in each case via the starting vessel or otherwise from
below.
In view of the disadvantages of the previously
known devices, as described above, the invention is
based on the following object. A reaction vessel
holding device of the type mentioned at the beginning
is to be created which permits a movement of reaction
vessels fastened to it, without this movement being
transmitted to the fixed part, and which permits a
supply of liquid, solids and gas into the reaction
vessels and an extraction from the reaction vessels in
a simple manner.
This object is achieved by means of the reac-
tion vessel holding device according to the invention,
as defined in the independent Claim 1. A reaction
block according to the invention with such a reaction
vessel holding device is defined in Claim 12. Prefer-
red embodiment variants are given by the dependent
claims.
The essential feature of the invention consists
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in the fact that in a reaction vessel holding device
having a fixed part and a plurality of connectors,
which are connected to it and to which reaction vessels
can be fastened, at least one part of each connector
being flexible, at least one of the connectors and the
fixed part have an opening through which a supply
and/or extraction tool can be introduced into a
reaction vessel fastened to the connector.
Because the reaction vessels are fastened by
means of movable, and advantageously removable, connec
tors on the fixed part, which fixed part can be
configured, for example, as a switching block or other
block with or without clamped, screwed or inserted
septa, the reaction vessels can be shaken without the
relevant fixed part moving with them. By means of ad-
ditional axial flexibility of the flexible connectors,
it is even possible for at least two reaction vessels
which are rigidly connected together to be shaken. In
addition, the full weight of the reaction vessels,
including content, is not laid on the shaking device so
that relatively weak shaking devices are sufficient to
generate the vibrations, which are relatively small
despite relatively large shaking amplitudes. Only this
arrangement makes it at all possible to use vibration-
sensitive peripheral units, such for example as samp-
lers, robots or other automation devices for the supply
and/or extraction of liquids and/or solids. Furthermo-
re, such relatively weak shaking devices have favoura-
ble costs and the reaction vessels can be shaken with a
relatively large amplitude at very high frequencies.
An essential and decisive advantage lies in the
fact that, even during the shaking, it is possible to
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supply and/or extract a liquid, a gas or a solid to or
from a reaction vessel without difficulty by means of a
supply and/or extraction tool, such for example as hol-
low needles, grippers or spoons. This is not the case
with the previously known devices but is frequently
demanded, particularly for chemical reactions.
Such connectors advantageously have a bellows
between a rigid fastening part at the reaction vessel
end and a part at the fixed part end. Alternatives to
the bellows are, for example, a flexible tube, a sphe-
rical joint or a twin-axis or multiple-axis linkage.
Liquids, gases and/or solids can preferably be
supplied and/or extracted to or from the reaction ves
sels through the fixed part. If the fixed part is con
figured as a switching block, it advantageously compri
ses a gas duct plate, a gas duct and, advantageously,
an adjacent functional plate, one of these plates being
advantageously arranged so that it can be displaced
relative to the other. The gas duct plate or plates
and the functional plate or plates have through-holes,
through-slots and/or depressions and/or horizontal
through-cavities, which are located opposite one
another, in each case in at least one plate position,
in such a way that
a) gases and/or liquids can be supplied to or
extracted from at least one reaction vessel via the gas
duct or via at least one gas duct, and
b) gases, liquids and/or solids can be supplied to or
extracted from at least one reaction vessel both
through the gas duct plate or through at least one gas
duct plate and through the functional plate or through
at least one functional plate.
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By means of this switching block, it is possi-
ble - depending on the plate position - to supply or
extract liquids or gases to or from all or individual
reaction vessels via the gas duct or ducts and/or to
generate a vacuum or a positive pressure in the reac-
tion vessels and/or to supply or extract gases, liquids
and/or solids to or from the reaction vessels with or
without pressure balance through mutually opposite
through-holes or through-slots with holes and/or
depressions with holes and/or through-cavities with
holes in the gas duct plate or plates and in the
functional plate or plates. The sealing of the reac-
tion vessels takes place by means of the functional
plate or by means of at least one functional plate in
certain plate positions so that septa are not absolute-
ly necessary. It is therefore possible to dispense
with the use of a septum or it can, if necessary, be
arranged in such a way that it is only used as a seal
for the reaction vessels in certain plate positions.
If, instead of being attached to a switching
block, the flexible connectors are attached to a simple
block as the fixed part, the same advantages as descri-
bed above exist, with the exception of those which are
specifically associated with the functional plate.
Because of the flexible connectors and the
functional plate or plates, various process steps can
be carried out without the relevant switching block
having to be displaced or modified. The functional
plate or plates also permit a compact design of the
switching blocks.
For operating the switching blocks or blocks
with or without clamped, screwed or inserted septa and
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the reaction vessels, a commercially obtainable sampler
combined with a dilutor, for example the Gilson
Aspec XL of the Gilson company, France, or another
robot or another automatic unit can be employed, which
units may possibly be adapted to the switching blocks
according to the invention or to blocks with or without
clamped, screwed or inserted septa and reaction ves-
sels. As mentioned above, the flexible connectors can
also, however, be attached - with all the advantages
described above - to a simpler block provided with
little switching or none at all. Thus, for example,
the dosing described here is likewise possible during
the shaking and, in fact, as well if septa are employed
as if the reaction vessels are left open. Pressure
balance is, for example, ensured by means of the needle
(commercially obtainable) during the supply of liquid
or by means of a central pipe with a permanent or a
(for example by means of a valve) switchable connection
to, for example, an argon source and, for example,
permanent connections of the central gas duct to the
through-holes, i.e. to the reaction vessels.
For certain applications, a removable reflux
cooler is preferably arranged between at least one of
the reaction vessels and the fixed part. This reflux
cooler has a cooling tube which extends sufficiently
far into the reaction vessel for cooling to take place
in the reaction vessel in the connection region between
the reaction vessel and the reflux cooler or below this
region. It is then advantageous for the cooling tube
to be arranged in one half only of the opening cross
section of the reaction vessel, so that the supply and
extraction instrument can be centrally immersed deep
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into the reaction vessel.
In this way, it is possible - with simultaneous
reflux cooling - to supply a liquid to the reaction
vessel, for example by means of a supply tool or via
the or a gas duct, to add and/or extract a protective
gas, gaseous reactant, gaseous catalyst or a solid,
and/or a pressure balance can be achieved and/or the
reaction vessels can be shaken at high frequency. All
these interventions in the reaction vessel take place
through the same opening, which contributes to the fact
that the device according to the invention can be
constructed in a relatively compact and low-cost manner
and be maintenance-friendly and operator-friendly.
For further applications, special reaction ves
sels are necessary which permit the reaction vessel, or
its contents, to be tempered over a temperature range
which is as wide as possible. The reaction vessels
produced for this purpose advantageously have a second
chamber, which is fitted in a fixed or removable manner
at the lower end of the reaction vessel and through
which a tempering medium can be pumped. Units for
delivering tempered media are obtainable on the market
- a Unistat of Huber GmbH, which can be employed over a
very wide temperature range, can, for example, be used.
This unit, together with a special medium (for example
polydimethyl siloxane, No. 85413 from Fluka AG) permits
tempering of the reaction vessel in the range from
approximately -80°C to approximately +200°C. So that
these reaction vessels can be shaken in the manner
described above (i.e. while using flexible connectors,
i.e. with simultaneous dosing of a material, for
example), a decisive feature is that the second cham-
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ber, which is firmly connected to the reaction vessel,
should be directly or indirectly flexibly connected to
the tempering unit and/or to the further reaction
vessels (connected, for example, in parallel) and/or to
another medium-conveying unit. An example of an indi-
rect connection between two reaction vessels is shown
in Fig. 26. In this arrangement, a second chamber of
one reaction vessel is connected via a helical, medium-
carrying line to a second chamber of another reaction
vessel. The simplest arrangement is for flexible hoses
composed of plastic to be employed for connecting the
tempering chambers to one another and to the tempering
unit. Since, particularly in the case of applications
which demand a very large temperature range (-80 to
+300°C), plastics either have too little flexibility
(particularly at low temperatures) and/or are excessi-
vely unstable (particularly at high temperatures),
specially produced and arranged helical connectors in
form of hollow metal wires (for example aluminium,
copper, steel, spring steel) or Teflon hoses (most of
the commercially available fluorinated hydrocarbon
polymers are suitable) are advantageously employed as
the connections between the tempering chambers and the
tempering unit, particularly in the case of dense
packings of reaction vessels with, therefore, small
distances between the tempering chambers. As an alter-
native to this system, flexible chambers with connect-
ing sleeves for the reaction vessels have been
specially produced. These chambers are produced in
enriched form, for example, from silicone of various
hardness, thermoplastic elastomers, such as, for exam-
ple, polyethylene or polypropylene, copolymers of, for
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example, styrene, ethylene or butylene with silicone
oil. These flexible chambers satisfy the same condi-
tions as the chambers composed of a stiff material
described above, which are flexibly connected together
or to the tempering unit by means of medium-carrying
lines. In this case, the flexibility is achieved by
means of the flexible material from which the chambers
are manufactured instead of by means of hoses composed
of a flexible material or by means of the sprung heli-
ces composed of a relatively stiff material. In prin-
ciple, the chambers correspond to a "hot-water bottle",
with the reaction vessels advantageously let into them
in such a way that the latter are in direct contact
with the heat carrier and are sealed toward the outside
so that the heat carrier remains in the circuit.
Reaction vessels, which permit, for example,
a mixture of an insoluble and a soluble material to be
separated by filtration, are useful and often necessary
for further applications. This advantageously takes
place, by means of the arrangement according to the
invention, in such a way that the filtrate is transfer-
red without manual intervention for further processing
into a second reaction vessel, so that it is available
for further processing (for example distilling off the
solvent ) on the same access plane of , for example, the
sampler employed. The same advantages appear in the
case of the filter cake present in the reaction vessel
before the frit. This is achieved by means of the
reaction vessels described in Fig. 20, together with a
special function in the fixed part, or with analogous
valve controls, in such a way that the reaction vessel,
which contains the frit, is closed in a vacuum-tight
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manner and, at the same time, the reaction vessel,
which catches the filtrate, is placed under vacuum.
The same can be achieved by pressure instead of vacuum
so that - expressing the matter generally - a relative
positive pressure has to be generated in the reaction
vessel with the frit. The switching block described
above automatically makes this necessary pressure dif-
ference possible, controlled by means of a PC, because
the displaceable plate takes up the corresponding
asymmetrical position. All the twin filtration vessels
connected, or the mixtures located in them, are then
filtered in parallel.
All the possible combinations can also be
employed with all the reaction vessels mentioned above
for the special and further applications quoted. As an
example, the reflux coolers can be placed on the twin
filtration vessels, which are in turn provided with the
second chambers, described above, for tempering the
contents of the reaction vessels. One or a plurality
of these combinations can then, for example, be placed
on a switching block or a simple block with flexible
connectors which are attached in a fixed or removable
manner. By means of embodiment examples of flexible
connectors, which are also axially flexible, it is also
possible for each two rigidly connected reaction ves-
sels to be shaken with the advantages described, i.e.
with simultaneous supply, for example, of a material by
means of a dosing device.
The reaction vessel holding device according to
the invention and the reaction block according to the
invention are now described in more detail with
reference to the attached drawings. In these:
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Fig. 1 shows a perspective view, obliquely
from above, of an embodiment example
of a device for carrying out a multi-
plicity of chemical, biochemical, biolo-
gical or physical processes in parallel;
Fig. 2 shows a perspective view, obliquely
from below, of an embodiment example
of a device for carrying out a multi-
plicity of chemical, biochemical, biolo-
gical or physical processes in parallel,
a flexible connector being also shown;
Fig. 3 shows a side view of a connector;
Fig. 4 shows a section through the connector
of Fig. 3 along the line A-A;
Fig. 5 shows a simple block with a gas duct,
with septum plate omitted and cover
plate omitted, so that the connections
of the reaction vessels via depres-
sions in the block and the connections
to the gas duct are visible, with two
embodiment examples of flexible con-
nectors;
Fig. 6 shows a perspective view of an embodi-
ment example of a simple block with
individual septa screwed on and two
rows of three reaction vessels each
with indicated shaking device and con-
nection of the reaction vessels to the
same;
Fig. 7 shows a switching block with an embo-
diment example of a flexible connector
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and an embodiment example of a reac-
tion vessel attached to it;
Fig. 8 shows the switching block of Fig. 7
with two different embodiment examples
of a flexible connector broken down
into its individual parts;
Fig. 9 shows an embodiment example of the
botto m of the functional plate of the
switc hing block of Fig. 7;
Fig. 10 shows an embodiment example of the top
of the functional plate of the
switc hing block of Fig. 7;
Fig. 11 shows a segment of an embodiment va-
riant of a slide plate of the switch-
ing block of Fig. 7, the necessary
conne ctions between the reaction ves-
sels and the gas duct of the gas duct
plate being configured as through-
cavit ies;
Figures 12 to 15 show sections through the segment of
Fig. 11, which show the construction
of th e through-cavities;
Fig. 16 shows a perspective view of the gas
duct plate of the switching block of
Fig. 7;
Fig. 17 shows a side view of the gas duct
plate of the switching block of
Fig. 7, parts which are not visible
being shown dotted;
Fig. 18 shows a plan view of the gas duct
plate of the switching block of
Fig. 7, parts which are not visible
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being shown dotted;
Fig. 19 shows a flexible connector with a
simple reaction vessel fastened to it
and an embodiment example of a reflux
cooler;
Fig. 20 shows an embodiment example of two
reaction vessels connected flexibly or
rigidly to a tube, with a frit in one
of the two reaction vessels in order
to permit filtration, for example, of
a mixture into the second reaction
vessel, which is located at the same
level;
Figures 21, 22 show an embodiment example of a reac-
tion vessel with a second attached
chamber, with connections for a supply
line and a drain line, in order to
permit a series or parallel connection
of the reaction vessels arranged in
parallel to one another or to a
tempering unit, in order to permit
tempering of the reaction mixture;
Fig. 23 shows a section through the reaction
vessel of Fig. 22 along the line B-B;
Fig. 24 shows a section through the reaction
vessel of Fig. 22 along the line C-C;
Fig. 25 shows a section through the reaction
vessel of Fig. 22 along the line D-D;
Fig. 26 shows an embodiment example of two
reaction vessels flexibly connected to
one another in the most constricted
space below the flexible part of the
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connector;
Fig. 27a shows a flexible chamber composed of a
material which is stable and flexible
over a large temperature range and in
which the reaction vessels are immer-
sed, so that a lower part of the
latter is directly in contact with the
tempering medium and an emergence of
tempering medium from the chamber is
prevented by sealing lips;
Fig. 27b shows a section through the flexible
chamber of Fig. 27a;
Fig. 28 shows a flexible chamber in accordance
with Fig. 27a, which includes a cen-
tral part of the reaction vessel; and
Fig. 29 shows a diagrammatic circuit diagram
of a device according to the invention
for carrying out a multiplicity of
chemical, biochemical, biological or
physical processes in parallel.
The embodiment example shown, of a device for
carrying out a multiplicity of chemical, biochemical,
biological or physical processes in parallel, comprises
a support frame 24, into which two switching blocks 1
are inserted and between which there is still space for
three further switching blocks 1. The switching blocks
1 are fastened by means of screws, for which the
support frame 24 has screw holes 241. An educt vessel
frame 25, which is used for holding educt vessels 250,
is also arranged on the support frame 24. The educt
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vessel frame 25 is configured in such a way that the
educt vessels 250 can be arranged on two planes. This
serves the better utilization of the space available
and therefore serves to increase the number of educt
vessels 250. Two holding blocks or capture plates 27
are provided for holding additional educt vessels 250
or sample extraction vessels. Solvent extraction
points 28 permit the extraction of solvents from
solvent tanks.
An arm 26 of a sampler is used to support a
hollow needle for the handling of starting materials or
products. The corners of the access surface for the
hollow needles 261 are indicated by needles 261.
A shaking device 7, a vacuum pump 2, a
plurality of gas supply devices, valves for the gas
supply devices and the vacuum pump, tempering units, a
plurality of control units, a dilutor and a plurality
of reaction vessels 5 are also part of the device, and
are shown further below in Figure 29.
The following statement applies to the further
description overall. If reference numbers are con-
tained in a figure for the purpose of drawing clarity
but are not mentioned in the directly associated
descriptive text, reference is to be made to their
mention in the previous description of figures.
Ficr2
An embodiment variant of the device for
carrying out a multiplicity of chemical, biochemical,
biological or physical processes in parallel, from
Fig. 1, has two flexible connectors 4 and another frame
25 for holding educts.
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Figures 3 and 4
The connector 4 shown comprises a part 41 at
the block end and a part 42 at the reaction vessel end,
between which is arranged a bellows 43 which satisfies
the function that the part 42 at the reaction vessel
end should be movable relative to the part 41 at the
block end and, in fact, both laterally and also in the
x-, y- and z-direction. The part 41 at the block end
is provided with a thread 411 so that the connector 4
can be screwed into a hole 111 of the switching block,
which hole 111 is shown in Fig. 16 and is provided with
an internal thread. The part 42 at the reaction vessel
end additionally comprises a fixing region 421 for
applying fastening clamps and a standard ground joint
422 for the releasable fastening of a reaction vessel 5
or other parts used, such as, for example, reflux
cooler 6. The connector 4 has a central opening 433.
Ficr5
A simple block 1' comprises a gas duct plate
11' and two embodiment examples of flexible connectors
4, 4' - one with a flexible bellows 43, the other with
a flexible tube 43' - as the flexible part of the
connector. A rigid fastening part 42 or 42',
respectively, is attached to the flexible part for
fastening a reaction vessel 5.
The connector 4, which is described in more
detail below, is screwed by means of a thread 411 into
the bottom of the block shown, into an internal thread
of the block. The opposite end is used for the
removable fastening of reaction vessels 5. In
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addition, the reaction vessels can be sealed by means
of a septum plate, which is not visible here.
The connector 4 can, for example, consist of
the materials which are described further below in
association with Fig. 7.
Gas duct holes are indicated by 113, through-
holes by 114, screw holes by 161, a hole for a pin by
162 and depressions by 119 (see also Fig. 8 and 16-18).
Fig-6
A section through an embodiment example of a
block 1 with a row consisting of three reaction
vessels, which are each firmly sealed on the block 1 by
a septum 73 (fixing by means of plastic screw caps 74).
The reaction vessels 5 are respectively connected to
the switching block 1 by means of a flexible connector
4. The reaction vessels 5 are guided by a drive 71
which is firmly connected to the diagrammatically shown
shaker 7. The shaking motion takes place in the
direction of the arrow. The co-ordinate axes 58
indicate that the end 59 of the reaction vessels facing
away from the connector and the end 57 of the reaction
vessels at the connector side can be moved in three
degrees of freedom.
Fig. 7
The flexible connectors 4, 4' described in
Fig. 5 are used for the removable fastening of reaction
vessels 5 on the switching block 1. Each through-hole
111 of the gas duct plate can be associated with a
reaction vessel 5 or a plurality of holes 75 can be
associated with a reaction vessel 5.
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A switching block 1 used in the device of
Fig. 1 has a gas duct plate 11, a functional plate 12
in the form of a slide plate, a backing plate 13 and a
support plate 14, which are located one above the
other . The support plate 14 , the backing plate 13 and
the gas duct plate 11 are held together by screws,
which are arranged in screw holes 10. An end plate 16
with holes for pins and screw holes 161 additionally
connects these three plates by means of pins and screws
(not shown). The functional plate 12 is arranged so
that it can be displaced between the gas duct plate 11
and the backing plate 13. It is driven by a stepper
motor 15 via a pinion 151 and a rack 152. Fastening,
distance and positioning elements are indicated by the
reference number 18.
The support plate 14 also has two rows of
through-holes 131, which permit a needle 261, described
in Fig. 1, or some other solid object to pass through
the plate. This plate is mainly used for stabiliza-
tion, for protection and for holding the drive device
for the functional plate 12. A panel 135 is used as a
collecting point for the light barrier signals. As an
alternative to this arrangement, a standard interface
can be used for controlling the functions listed above.
The backing plate 13 has screw holes 10' and
through-holes 10, which are located opposite the screw
holes 10' and through-holes 10 of the support plate 14.
It preferably consists of a high-quality material and,
in particular, its side facing toward the functional
plate 12 is made more exactly than the support plate
14.
The functional plate 14 is narrower than the
CA 02294941 1999-12-15
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backing plate 13 and the gas duct plate 11, so that it
fits exactly between the connecting screws of these two
plates and is also even guided by these connecting
screws. It includes through-holes 10, whose rims are
slightly raised relative to the plate surface and thus
ensure a good seal. On the bottom, furthermore, it
also has depressions which are explained in more detail
further below.
Fig-8
In addition to the screw holes 114 and the
through-holes 10, the gas duct plate 11 has gas duct
holes 113, which end in a central gas duct 112. An
appropriate number of vacuum pumps and gas supply
devices can be connected to the open end of the gas
duct 112 by means of a valve, preferably a multiple
valve. These vacuum pumps and gas supply devices
supply the reaction vessels 5 via the flexible
connectors 4'.
Between the backing plate 13 and the support
plate 14, it is also possible to arrange a septum
composed of a material which can be penetrated by a
needle, which septum acts as an additional, optional
seal for the reaction vessel openings when the through-
holes of the backing plate 13, the gas duct plate 11
and the functional plate 12 are located opposite one
another.
The individual parts of the switching block
can, for example, consist of metal (in particular
stainless steel, brass or titanium alloys), glass (in
particular Si02 glass), plastic (in particular Teflon,
polypropylene or polyethylene), natural stone (in
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particular granite or gneis), or ceramic (in particular
A103 or MACOR~). The connectors can, for example,
consist of plastic or a metal, in particular of Teflon,
polypropylene, polyethylene or steel sheet.
The bottom of the functional plate 12 has, in
this case, a pattern which is repeated eight times. An
individual pattern comprises four different arrange-
ments of through-holes 121, depressions 122 and sealing
surfaces 123 which, depending on the plate position,
are located opposite the through-holes 121 and the gas
duct holes 113 of the gas duct plate 11 and/or of the
support plate 13 and, in this way, define four
different functional plate functions.
The first arrangement has two through-holes 121
and, between the latter, a depression 122. The first
functional plate function therefore leaves both
associated reaction vessels 5 completely open, i.e.
both for supply and/or extraction tools and relative to
the gas duct. A single long depression 12 is present
in the case of the second arrangement.
The third arrangement comprises a depression
and two sealing surfaces 123. The third functional
plate function completely closes off an associated
reaction vessel, whereas it leaves the other associated
reaction vessel 5 open relative to the gas duct 112
only, so that a pressure difference can be generated in
rows of reaction vessels connected in parallel.
In the fourth arrangement, two through-holes
121 and two depressions 123 are present. The fourth
functional plate function leaves the two associated
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reaction vessels 5 open for supply and/or extraction
tools but closes them off relative to the gas duct 112.
The rims of the through-holes 121, the
depressions 122 and the sealing surfaces 123 are all
slightly raised above the plate surface and therefore
ensure a good seal, with the possibility of a complete
sealing of the reaction vessels 5 or the possibility of
applying a vacuum.
Other arrangements of the through-holes 121,
the depressions 122 and the sealing surfaces 123, and
consequently other functional plate functions or other
patterns, are of course also conceivable.
Fig. 10
This functional plate 12' differs from the
functional plate 12 in that, on the top, it is not just
the rims of the through-holes 121 which are raised
above the plate surface but also the regions between
the through-holes 121.
An alternative embodiment variant of the func-
tional plate 12 described in Fig. 7, only one segment
of the pattern, which is repeated eight times, of a
complete functional plate 12 being represented. The
slots shown in Fig. 7 are configured as through-
cavities 129 in this embodiment example, the individual
positions of the functional plate being represented in
the sequence of Fig. 12 to Fig. 15. Otherwise, the
same functionality is provided.
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Figures 12 to 15
Sections which represent the individual posi-
tions of the functional plate in the sequence Fig. 12
to Fig. 15.
Figures 16,. 17 and 18
In order to ensure sufficient drainage of
possibly condensed solvents as far as the closed end,
the gas duct plate 11 shown has a central gas duct
which rises slightly from the open end and from which
gas-duct holes 114 extend to the plate surface facing
toward the functional plate. The through-holes 113 are
arranged in two parallel rows corresponding to the
through-holes 132 of the backing plate 13 and the
through-holes of the support plate 14 and the screw
holes 141 are arranged to correspond respectively to
the screw holes 131 or those of these plates. Screw
holes for fastening the end plate are indicated by 161.
A multiple valve, to which an appropriate number of
vacuum pumps and/or devices for the supply of one or a
plurality of gases is connected, is advantageously
attached, for example screwed in, at the open end of
the gas duct 11. A vacuum or a positive pressure can
then be generated in the reaction vessels 5 and/or the
most varied gases can be supplied to the reaction
vessels 5. In this way, the atmospheres and conditions
achievable by means of the functional plate functions
can be multiplied, with simultaneous shaking, in the
reaction vessels 5.
In its upper region, the reflux cooler 6 shown
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has a standard ground joint inner surface 62 for the
releasable fastening of the reflux cooler 6 to the
standard ground joint 63 of a connector 4 or a reaction
vessel 5 and, in its lower region, it has a standard
ground joint external surface 63 for the releasable
fastening of a reaction vessel 5. It also includes a
cooling tube 61, which extends sufficiently far into
the reaction vessel 5 for cooling to take place in the
reaction vessel 5 below the connection region 51 of the
l0 reaction vessel 5 and the reflux cooler 6. This achie-
ves the effect that the gas phase condenses relatively
far down in the reaction vessel; the condensate there-
fore remains in the reaction vessel 5 and condenses
before the standard ground joint connection 62.
The cooling tube 61 is arranged asymmetrically
in the opening cross section of the reaction vessel 5,
i.e. it is displaced toward the outside relative to the
centre of the reflux cooler in order to create space
for the introduction into the reaction vessel 5 of a
supply and/or extraction tool or the addition of, for
example, a protective gas, gaseous reactant, gaseous
catalyst or a solid, etc. The supply and removal of
the cooling medium, for example water, takes place as
shown by the arrows B and C by means of flexible supply
and removal lines, which are arranged and are
connected, for example, to the supply and removal lines
of the reflux cooler of further reaction vessels in
such a way that their space requirement is minimized.
Fig. 20
In the device according to the invention, many
different types of reaction vessels can, in principle,
CA 02294941 1999-12-15
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be used; they all, however, have a connection possibi-
lity, such as a standard ground joint 62 for example,
for the releasable or firm fastening of the reaction
vessel to, for example, a reflux cooler 6 or a
connector 4. The shape and the acceptable volumes of
the reaction vessels can be varied over a wide range as
a function of the available space and the desired
number of reaction vessels to be used adjacent to one
another. As an example, cylindrical reaction vessels
with round or flat bottoms, round beakers, pointed
beakers, etc, in particular with acceptable volumes
between 0.3 ml - 200 ml, can be considered.
Two reaction vessels 5" and 5"', which can be
used for filtration, and which are connected by a
flexible or a rigid line 52, are shown here. The first
end of the tube protrudes into the upper region of the
reaction vessel 5", whereas the second end is melted
into a frit 53, for example glass frit, in the bottom
region of the reaction vessel 5"'. Filtration can be
carried out through the frit 53 by the generation of
pressure in the reaction vessel 5"', as shown by the
arrow, and/or by the generation of vacuum in the
reaction vessel 5", as shown by the arrow, and this can
take place with simultaneous and/or previous shaking
and, in fact, in such a way that both the filter cake
remaining in front of the frit 53 and the filtrate are
available at the same level for access by the supply
device for further processing.
Figures 21 to 25
It is also possible to use reaction vessels 5'
onto which an additional chamber 8 with an inlet and an
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outlet 81, 81', 81" and 81"' is melted. These chambers
can be used as cooling or heating chambers and are
preferably connected to one another in a space-saving
manner. The reaction vessels 5 described in Fig. 12
can also be provided with additional cooling or heating
chambers and/or can be combined with reflux coolers 6.
Fundamentally, the most widely varying combinations of
these elements are conceivable with all possible types
of reaction vessels 5.
Fig. 26
An alternative reaction vessel 5" with a second
additional chamber 8 with connections for the supply
and removal lines 81, 81' and, attached to them, lines
82, 82', 82" for media, which lines - in order to build
up, in the most restricted space, mechanical flexibili-
ty between the two reaction vessels 5" adjacent to one
another - are wound in the form of helices around a rod
84 or 84' attached to the two chambers 8.
On the left-hand reaction vessel, a reflux
cooler 6 with the reflux cooler tube 61 is attached by
means of the standard ground joint 63 to the reaction
vessel 5", which is in turn connected by means of the
standard ground joint 62 to the flexible connector 4.
Figures 27a and 27b
An embodiment example of a flexible chamber 9
composed of a flexible material which is stable over a
large temperature range (plastics such as silicone,
relatively thin-walled Teflon, polypropylene, etc), in
which the reaction vessels 5 are immersed in such a way
that a lower part of the reaction vessel 5 is in direct
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contact with the tempering medium. The outlet of
tempering medium from the chamber is achieved by means
of the upwardly extended cylindrical walls 91 and the
sealing rings 92. The supply of the heat carrier takes
place by means of the connections 93.
Ficr. 28
An alternative variant of a flexible chamber 9
differs from that described in Figures 27a and 27b in
that the reaction vessel not only enters the flexible
chamber but passes through the latter so that the
tempering medium is in direct contact with a central
region of the reaction vessel 5. In consequence,
upwardly extended cylindrical walls 91 and sealing
rings 92 are fitted both at the inlet point and at the
outlet point. The connections 93 for the supply lines
are fitted at the end surface.
The present embodiment example of a device has
five switching blocks 1, below which a shaking device 7
is arranged. The access to the gas duct 112 of the
respective gas duct plate 11 is controlled by multiple
valves 3, by means of which a vacuum can be generated
by a vacuum pump 23 or else gas can be supplied or ex-
tracted by means of a device for the supply or ex-
traction of gas . In the embodiment example shown, the
gas supply and extraction device includes a tank for a
gaseous material, for example argon, hydrogen, etc.
At least one cryostatic temperature regulator
is provided to supply each of the cooling tubes 61 of
the reflux cooler 6 and each of the melted-on, second
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additional chambers 8 or the flexible chambers 9 of the
reaction vessels 5 with a heat carrier. The handling
of the starting materials or products takes place by
means of a device for the supply and extraction of
liquids and/or solids, which device comprises one or a
plurality of hollow needles 261 or other supply and/or
extraction tools. The starting materials or products
are stored, in part, in vessels 250 which are arranged
in the vessel frame 25. Solvent or solution extraction
points 28 permit the extraction of solvents or
solutions from tanks.
A control unit 88, for example a PC, is used
for controlling the supply and extraction of liquids,
gases and/or solids, i.e. for controlling a device 261
for the supply and extraction of liquids and/or solids,
for controlling the device for the supply and
extraction of gases, for controlling the vacuum pump
23, for controlling the multiple valves 3 and for
controlling the functional plates 9 and their motors
15, and for controlling the shaking device 7 and the
cryostatic temperature regulators 29, 89.
In addition to the previously described device
for carrying out a multiplicity of chemical, biochemi-
cal, biological or physical processes in parallel,
further design variations can be realized.
It is expressly mentioned at this point that
the connections between the connectors 4, the reflux
coolers 6 and the reaction vessels 5 do not necessarily
have to take place by means of standard ground joints
63 but, for example, threads, face grinding, etc can
also be provided. Similarly, the connection 411
between the block and the flexible connector 4 does not
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necessarily have to be screwed but can be a fixed
connection, a ground face or a bayonet fixing.
