EP2342017A1

EP2342017A1 - Reactor array for producing and analyzing products

Info

Publication number: EP2342017A1
Application number: EP09760476A
Authority: EP
Inventors: Michael Gruss; Matthias Ridder
Original assignee: Gruenenthal GmbH
Current assignee: Gruenenthal GmbH
Priority date: 2008-10-28
Filing date: 2009-10-26
Publication date: 2011-07-13
Also published as: US20110257048A1; US9339816B2; WO2010049108A1

Abstract

The present invention relates to a reactor array for producing and/or analyzing products, comprising a plurality of vessels in which products can be produced on a preparative or analytical scale.

Description

Reactor array for the production and analysis of products

The present invention relates to a reactor array for the production and / or analysis of products with a plurality of vessels in which products can be prepared and / or analyzed on a preparative or analytical scale.

Investigations of substances in the medium or high-throughput process make it necessary to carry out reactions and / or analytical measurements in arrays which have a multiplicity of vessels in or on which the respective product is located. An analysis method is the X-ray powder diffractometry, which is a standard method, for example, in the determination of the polymorphism of substances. In this measurement, an X-ray beam is successively directed to a product to be analyzed on the sample carrier and the portion of the radiation diffracted therefrom is evaluated. This method can be used in transmission or reflection geometry. At present, no reactors are known in the prior art, for example EP 1972 377 A2 and US Pat. No. 6,507,636 B1, which simultaneously optimally meet the requirements of chemical synthesis and / or crystallization and those of an optimal sample carrier, for example the X-ray analysis is sufficient.

It was therefore an object of the present invention to provide a reactor array that meets the above requirements.

The object is achieved with a reactor array for the production and / or investigation of products with a variety of vessels in which products can be prepared and / or analyzed on a preparative or analytical scale, each vessel has at least temporarily a gas-tight lid and at least the bottom of each Vessel has a low X-ray absorption.

According to the invention, the reactor array has a multiplicity of vessels for the production and / or examination of products. In these vessels, products are prepared on a preparative or analytical scale or the vessels are filled with products for their analysis. Preparative or analytical scale in the context of the invention relates to vessels with up to 50 ml filling volume and / or 5 g filling weight, preferably up to 2 ml filling volume and / or 500 mg filling weight, particularly preferably up to 0.5 ml filling volume and / or 50 mg filling weight of the substance to be synthesized and / or to be analyzed. According to the invention, each of these vessels now at least temporarily has a gas-tight lid, which in particular retains vapors of organic solvents at temperatures of preferably 0-120 ° C. Preferably, the loss of solvent or gas by leakage is at most 20% of the filling volume in 24 hours, more preferably at most 10% of the filling volume in 24 hours, most preferably at most 1% of the filling volume in 24 hours, at a temperature of 30 ⁰ C below , preferably 15 ° C below, most preferably at the boiling point of the solvent or gas relative to the pressure surrounding the vessels. In particular, during the manufacture and / or prior to the analysis of the products, the lid is located on the vessels. For analysis, the lid is preferably removed.

Preferably, the vessel and / or its lid consists of a chemically inert material and / or is coated with a chemically inert material. Chemically inert materials include glass, ceramics, stainless steels and some plastics. Preferably, the vessel and / or its lid is designed or dimensioned such that it is dimensionally stable both against overpressure and underpressure. Further preferably, the vessel is made of a thermally conductive material, so that the production and / or analysis of the product can be carried out with heat and / or heat dissipation. Further preferably, the vessel is easy to fill and easy to empty. For example, it has no undercuts and no sharp corners. Preferably, the vessel has means for mixing the vessel during manufacture of the product and / or during the analysis. This mixing is preferably carried out by shaking and / or stirring. Preferably, the lid and / or the vessel by deep drawing, casting, tips or injection molding of a plastic produced. Further preferred production methods are cutting processes or rapid prototyping (solidification of a plastic powder or granulate). In this case, a variety of lids or vessels can be produced simultaneously. Their separation, if desired, takes place before or after the joining of lid and vessel. According to the invention, in particular the bottom of the vessel is designed so that it has the highest possible transmission with respect to X-rays, preferably in a wavelength range of 0.45 - 2.5 A. For this purpose, the bottom of the vessel preferably has a thickness of less than or equal to 5 mm, particularly preferably less than or equal to 100 μm, and is particularly preferably produced from a X-ray amorphous material.

Preferably, the filling level and the filling density of the products in the vessels are each as identical as possible in order to obtain the best possible comparability of the measurements in both the X-ray reflection and the X-ray transmission analysis.

Preferably, the lids of the individual vessels are interconnected, so that they can be applied to all vessels in one operation or removed from all vessels.

Preferably, the vessels are stored on a plate in bearings provided therefor. A plate according to the invention need not be a continuous plate, but may have recesses. A plate according to the invention is also a structure in which the storage of the individual vessels are connected by webs. The plate according to the invention will generally not be flat, but have elevations and / or indentations, for example for storage of the vessels or for removing the lid from the vessels.

Preferably, the storage of the vessels in each case one or more bearings and / or a common heat exchange means, with which the respective vessel can be heated or cooled. Preferably, the temperature in each vessel is individually adjustable.

Preferably, in the region of the storage of the vessels, the plate in each case has a lid opener with which the lid can be removed from the vessel, preferably automatically. This is preferred, especially immediately, prior to analysis of the products. This is particularly advantageous in the case of X-ray analysis because the lid then does not impede the transmission of X-rays represents. Preferably, all lids are removed simultaneously from the respective vessels. In a preferred embodiment, the removal of the lid is carried out by their particularly preferred reversible deformation. By the deformation of a positive and / or positive connection between the lid and vessel is repealed and the lid can be removed from the respective vessel. Preferably, the removal of the lid is carried out by a lowering movement of the vessel and the lid.

Preferably, each lid has means for attaching, for example, process engineering apparatuses, metering devices and / or measuring devices to the lid.

In a preferred embodiment, the vessel is rotatably disposed in the storage. This preferred embodiment of the present invention has the advantage that the vessel can be rotated, for example, during analysis of the product therein. As a result, measurement errors are at least reduced, for example due to different filling levels, varying filling density and a specific orientation of crystals or preferred orientation of the crystals.

Preferably, the vessels for each have a drive means. This drive means can act positively and / or non-positively, for example with a drive belt or a drive wheel together. However, the vessels may also have non-contact drive means, for example means which are flowed by a gas or liquid flow or by electromagnetic action, the respective vessel set in rotation.

Preferably, the drive is contactless by a temperature-controlled gas or liquid flow, which allows the setting of different temperatures. This is for example advantageous in the investigation of substances whose properties are temperature-dependent (for example, polymorphs or solvates). In a preferred embodiment, the respective vessel is arranged in a separately provided from the plate storage, which storage is then preferably set in rotation.

Another object of the present invention is a lid array having a plurality of individual lids, which are arranged in a grid. The cover array according to the invention is particularly suitable as a retrofit kit for existing reactor arrays.

Preferably, the lid array is made of a flexible material. Flexible in the context of the invention means that the material of the lid array is sufficiently flexible that it can be removed by bending successively from the reactor array without, for example, a peel aid is needed and without the lid is damaged and the reactor array then closed again can be.

Preferably, each lid has a seal. This seal can be made of the same or different material as the lid.

The invention will be explained below with reference to FIGS. 1-13. These explanations are merely exemplary and do not limit the general inventive concept.

FIG. 1 shows the reactor array.

Figure 2 shows the lid in three views.

FIG. 3 shows a first embodiment of the vessel with lid.

FIG. 4 shows a second embodiment of the vessel with lid.

Figure 5 shows procedural and metering in the

Cover.

Figure 6 shows an ejector.

FIG. 7 shows a further embodiment of the ejector.

FIG. 8 shows interconnected vessels. FIG. 9 shows a particularly flat embodiment of the vessel

FIG. 10 shows a first embodiment of rotatably arranged

Vessels.

FIG. 11 shows drive means for the vessel

FIG. 12 shows the assembly of the arrangement according to FIG. 11.

Figure 13 shows another example of the assembly of the device

according to FIG. 11.

FIG. 1 shows the reaction array 1 according to the invention, which has a multiplicity of vessels 3, here in an arrangement 8 × 12, which are arranged, for example, on a plate 5. The arrangement of the vessels 3 is preferably equidistant from a uniform pattern.

Figure 2 shows schematically the associated lid in three views. Each vessel has a lid with gas-tight seals 13, which is mounted on a respective vessel. In the present case, the lids are arranged contiguously. However, this need not be the case and / or is only temporary. For example, it is possible to provide all the lids in a one-piece component, to mount them on the vessels and then to separate them so that each lid is present individually thereafter. But it is also possible to connect the cover by webs or the like with each other. These webs can then be cut later, if necessary. Preferably, however, the lids remain connected to each other. They remain during the production of the respective product and / or until the vessels are placed on the plate on the vessels and are then preferably removed for analysis and then optionally re-attached to the vessels. The individual vessels can be held together by interconnected lids.

FIG. 3 shows a first embodiment of the vessel 3, which is provided with a cover 2. There is a seal 13 between the lid and the vessel. In the present case, but not necessarily, the vessel is of two made of different materials, wherein the bottom has a low absorption with respect to X-rays. On the lid 2 means for the arrangement of a process engineering apparatus, such as a reflux cooling, and / or a dosing means are arranged. At its lower edge, the cover has two positive locking means 2.1, which cooperate with positive locking means 5.2 of the underlying plate and thus fix the vessel together with the holder in a very specific position, which is advantageous for the heat transfer and the mixing process. The underlying plate 5 further comprises heat exchange surfaces 5.1, with which it is possible to heat or cool the vessel 3, wherein the shape of the heat exchange surface is preferably adapted to the shape of the bottom of the vessel. In the present case, the cover 2 are shown without connection to each other, but this need not be the case or only temporarily the case.

FIG. 4 essentially shows the vessel 3 together with the lid 2, wherein, in the present case, the lid has no means 9 for the arrangement of process engineering apparatuses and / or metering devices.

FIG. 5 shows, in addition to the example according to FIG. 3, the arrangement of a process engineering apparatus 14, in this case a reflux condenser, on the cover 2. Furthermore, it can be seen that the cover 2 has a recess through which a metering unit, here a syringe, is feasible, with which a solid, a liquid or a gas can be injected into the vessel.

In the embodiment according to FIG. 6, the plate 5 has ejectors 8, the upper end of which when lowering the vessels 3 together with the cover 2 interact with the positive locking means 2.1 of the cover and thereby spread the cover outwards. Thereby, a positive and / or non-positive connection 21, which secures the lid 2 to the vessel 3, dissolved and the lid 2 can be removed. Furthermore, the plate 5 in the present case, a spring means 16, with which the downward movement of the vessel 3 can be cushioned. As can be seen from FIG. 7, an ejector 8 is arranged in each case between four covers 2, each cover having a plurality of, here four, clamps 2.1, with which a releasable positive and / or non-positive connection with the vessel 3 can be produced in each case.

FIG. 8 shows that the vessels 3 can also be connected to one another by webs 3.1. As a result, for example, all vessels 3 can be positioned simultaneously on a plate 5 and / or a heat exchange between the vessels via the webs 3.1 can take place. The compound 3.1 can optionally be solved by cutting.

FIG. 9 shows a particularly flat embodiment of the vessel 3. This vessel is particularly suitable for X-ray powder diffractometry. Otherwise, reference is made to the execution of Figure 3.

FIG. 10 shows an embodiment of the present invention in which the vessel 3 and / or its lid 2 and / or its holder are provided with drive means 11. In the present case, the drive means 11 are blades, which are arranged at a uniform distance along the circumference of the vessel or the lid or along the holder and which, if necessary, can be flowed through by an air flow 17, the vessel 3 and / or lid 2 and / or whose holder rotates drives. Furthermore, it can be seen in FIG. 10 that an air flow can also be directed laterally and / or from below against the vessel and / or its storage, for example, the frictional resistance between the vessel 3 and its holder and / or between the holder and the reduce underlying plate and / or drive the vessel.

FIG. 11 shows an insert 19 provided with air blades 11, which is arranged in a bearing 6 of the plate 5. The vessel 3 is arranged in the insert 19. Again, the blades 11 are driven by air. The person skilled in the art recognizes that the drive means 11 can also be belts or toothed wheels or any other means with which a force and / or a torque for rotary drive of the vessel 3 can be impressed. FIG. 12 essentially shows the illustration according to FIG. 11, it being possible to see how the bearing 6, the insert 19 and the vessel 3 interact.

FIG. 13 essentially shows the illustration according to FIGS. 11 and 12, wherein here the inserts 19 are arranged on a plate 20 and are lowered into the bearing 6 by means of the plate 20.

LIST OF REFERENCE NUMBERS

1 reactor array

2 Lid, cover array 2.1 Positive locking means

3 vessel, crucible

3.1 Connecting bridge between two vessels

4 bottom of the vessel

5 plate

5.1 heat exchange surfaces

5.2 Positive locking means

6 Storage of the vessels

7 heat exchange medium

8 lid opener, ejector

9 means for arranging attachments

10 fasteners, brackets

11 drive means

12 Drivable holder

13 seal

14 Process engineering apparatus

15 dosing agent

16 spring means, damping

17 gas flow or liquid flow

18 x-ray beam

18.1 diffracted x-ray

19 Insert 0 Plate 1 positive and / or non-positive connection

Claims

claims:

1. reactor array (1) for the production and / or examination of products with a plurality of vessels (3) in which products can be prepared and / or analyzed on a preparative and / or analytical scale, each vessel (3) at least temporarily a gas-tight Lid (2), characterized in that at least the bottom (4) of each vessel (3) has a low X-ray absorption.

2. reactor array according to claim 1, characterized in that the cover (2) are interconnected.

3. Reactor array according to one of the preceding claims, characterized in that the vessels are mounted on a plate (5).

4. reactor array according to claim 3, characterized in that the plate in the region of the storage (6) of the vessels (3) each having a heat exchange means (7).

5. Reactor array according to one of claims 3 or 4, characterized in that the plate in the region of the storage (6) of the vessels (3) each having a lid opener (8).

6. reactor array according to claim 5, characterized in that the lid opener (8) when lowering the vessels (3) on the plate (5), the cover (2) away from the vessels.

7. Reactor array according to one of the preceding claims, characterized in that each cover (2) has means (9) for arranging attachments.

8. Reactor array according to one of the preceding claims, characterized in that the vessels (3) are each arranged rotatably in the bearing (6).

9. reactor array according to claim 8, characterized in that the vessels (3) each have a drive means (11).

10. Reactor vessel according to one of claims 8 or 9, characterized in that between the vessel (3) and bearing (6) each have a drivable mount (12) is provided.

11. reactor array according to any one of claims 8, 9 or 10, characterized in that the drive of the vessel (3) or the holder (12) takes place without contact.

12. reactor array according to claim 11, characterized in that the drive is effected without contact via a tempered gas or fluid.

13. cover array (2), characterized in that it comprises a plurality of individual lids (2) which are arranged in a grid.

14. cover array, characterized in that it is made of a flexible material.

15. cover array according to one of the preceding claims, characterized in that each cover has a seal.