DE10225931A1 - Reactor system for carrying out chemical reactions in parallel, in particular polymerization reactions - Google Patents

Abstract

An automatic synthesizer is formed from one or more reactor modules (2), each with a reactor (3), one or more feed vessels (4) for a liquid educt or educt mixture, and with one or more metering and conveying devices (5) for the Conveying and metering of liquid educt or educt mixture from the feed vessel (s) (4) into the reactor (3), proposed, each dosing and conveying device (5) comprising the following components: A) a flexible delivery line (6), which is formed from two sections (7, 8) and with a metering finger (11) is provided on at least one end of the flexible delivery line (6), B) a pump (10) and C) a two-position valve (9) which is between the Parts (7, 8) is arranged and via which the parts (7, 8) can be connected alternately to the pump (10).

Description

The invention relates to an automatic synthesizer with one or more dosing and Funding facilities and a method for carrying out parallel reactions in the Reactors of a synthesis machine.

The growing need for synthetic products with increased quality requirements has led to the development of automatic synthesizers, in which chemical syntheses program-controlled, without manual intervention.

Here, automatic synthesizers with several reactor modules are often used to to allow the reactor modules to run parallel reactions.

Frequently, reactions with continuous metering of one or more liquid educts or educt mixtures are carried out. This can cause problems with regard to the dosing accuracy of the inlets due to the dead volumes in the Inlet lines occur. Dead volumes can occur due to volatile compounds the inlets, due to the cleaning required after operation and / or possible deposits occur. This is particularly important for very small inlet volumes Dead volumes of the delivery lines represent a significant potential source of errors.

It was therefore an object of the invention to provide an automatic synthesizer with one or more To provide dosing and conveying devices that are continuous and uniform metering of liquid educt or educt mixture and thus a high Ensure reproducibility of the synthesis results.

• A) eine flexible Förderleitung, die aus zwei Teilstücken gebildet ist und wobei an mindestens einem Ende der flexiblen Förderleitung ein Dosierfinger vorgesehen ist,
• B) eine Pumpe sowie
• C) ein Zweistellungsventil, das zwischen den Teilstücken angeordnet ist und über das die Teilstücke alternierend mit der Pumpe verbunden werden können.

The object is achieved by an automatic synthesizer, formed from one or more reactor modules, each with a reactor, one or more feed vessels for each a liquid educt or educt mixture, and with one or more metering and conveying devices for metering in liquid educt or educt mixture from the feed vessel (the feed vessels) into the reactor, which is characterized in that each metering and conveying device comprises the following components:

• A) a flexible delivery line which is formed from two sections and wherein a metering finger is provided on at least one end of the flexible delivery line,
• B) a pump as well
• C) a two-position valve which is arranged between the sections and via which the sections can be connected alternately to the pump.

The automatic synthesizer according to the invention consists of one or more reactor modules educated. Each reactor module comprises one or more reactors Inlet vessels for receiving a liquid educt or educt mixture as well as one or more dosing and conveying devices for the dosing of liquid Educt or educt mixture from the feed vessel or the feed vessels into the reactor.

The invention is not restricted in terms of volume, geometry or Reactor materials. However, preference is given to automatic synthesizers with reactors whose Volumes in the range from 1 ml to 100 ml, in particular in the range from 10 to 50 ml lie. With regard to the reactor geometry, cylindrical reactors are often used, however, rectangular reactors can also be used, for example.

The number of reactor modules is basically not restricted. One is preferred Number of reactor modules in the range from 10 to 50, preferably in the range from 20 to 35th

The number of inlet vessels within each reactor module depends on the number of the liquid educt or educt mixture streams to be metered in, which are due to possible Reactions must be metered in separately from each other. This can often be the case be sufficient to a starting material presented in a reactor or Starting material mixture a single liquid educt stream or educt mixture stream to meter. However, preferably several, in particular two, liquid ones Educt streams or educt mixture streams are metered in. The number of inlet vessels is according to the number of liquid required for the respective reaction To provide educt streams or educt mixture streams.

According to the invention, each of the liquid educt streams is used for conveying and metering or educt mixture flows from the feed vessel or the feed vessels into the reactor one metering and conveying device each used, one of two sections formed flexible delivery line, a pump and a two-position valve, the is arranged between the sections of the flexible conveyor line and the Alternatively, sections can be connected to the pump. In order to be automatic Carrying out the dosing requires flexible at least one end Delivery line to provide a dosing finger operated by a robot arm.

In the present case, a flexible delivery line is generally understood to be a hose preferably made of a plastic material, for example Teflon. It is possible that Form hose from a transparent material.

The flexible delivery line is formed from two sections, between which one Two-position valve is arranged, via which the sections alternate with the pump can be connected. According to the invention, a valve is thus used, which in a first position the connection of a first section of the flexible delivery line with the Pump allows, while connecting the second section of the flexible Delivery line with the pump is interrupted and that in a second position Connection of the second section of the flexible delivery line to the pump guaranteed, according to the connection between the first section of the flexible delivery line and the pump is interrupted.

The invention is not restricted with regard to the promotion and dosage of liquid educts or educt mixtures of usable pumps. The selection regarding Material and funding volume will be based on the specific synthesis task. It is for example possible to use a piston pump.

Each reactor module is preferably designed as a unit which can be moved in a uniform manner, the The reactor and the inlet vessel (the inlet vessels) are arranged on a base plate. This makes it possible to flexibly match the number of reactor modules in the automatic synthesizer adapt specific synthesis task.

A preferred embodiment relates to automatic synthesizers, which are particularly suitable for Conduct chemical reactions under reflux.

Accordingly, synthesis machines are made available, with reactors that each have a lid which is designed as a hollow body and a cavity encloses with a supply line and a discharge line for a heat exchange medium in or from the cavity and with one or more feed-through lines for each liquid educt or educt mixture in the reactor.

Due to this design, the reflux condenser is in the reactor cover integrated. This provides a miniaturized system that is simpler Way can be operated by a robot arm. In particular, the can now as Simply remove the reflux cooler designed for cleaning purposes. and be installed.

In a preferred embodiment variant, the cover is flat, in particular as a flat disc. This geometric configuration is advantageous with regard to Manufacturability, assembly, sealing and cleaning.

In particular, the formation of deposits, so-called Fouling, reduced on the lid, with a correspondingly reduced cleaning effort.

In order to improve the heat dissipation, the best possible flow through the Lid cavity through the heat exchange medium desirable. For this, the is preferred Supply line for the heat exchange medium designed such that it in the cavity of the cover protrudes and / or the discharge line for the heat exchange medium in the way that they are flush with the inner wall surrounding the cavity the lid ends.

In a preferred embodiment, the feed-through lines are for the or liquid educts or educt mixtures designed such that they over the lower Project the edge of the lid into the interior of the reactor. This will make one Uniformity of the reflux is achieved because the condensate on the lower Edge of the lid protruding into the interior of the reactor Feed-through lines drip off and are not distributed on the underside of the lid.

In a further preferred embodiment, the lid has on its lower and Top of each a cross-sectional expansion. This will make Assembly and cleaning made easier.

The invention also relates to a method for carrying out reactions in the Reactor (in the reactors) of a synthesis machine described above, formed from one or more reactor modules, each with one reactor, one or more Inflow vessels for a liquid educt or educt mixture as well as with one or several dosing and conveying devices for the conveying and dosing of liquid educt or educt mixture from the feed vessel (s) into the Reactor.

• - in einem ersten Verfahrensschritt mit dem Zulaufgefäß verbunden wird,
• - in einem zweiten Verfahrensschritt bei geöffneter Stellung des Zweistellungsventils zwischen dem ersten Teilstück der flexiblen Förderleitung und der Pumpe das erste Teilstück der flexiblen Förderleitung mit flüssigem Edukt oder Eduktgemisch gefüllt wird,
• - in einem dritten Verfahrensschritt bei geschlossener Stellung des Zweistellungsventils zwischen dem ersten Teilstück und der Pumpe und geöffneter Stellung des Zweistellungsventils zwischen dem zweiten Teilstück und der Pumpe das zweite Teilstück mit flüssigem Edukt oder Eduktgemisch aus der Pumpe gefüllt wird,
• - die Verfahrensschritte zwei und drei so lange wiederholt werden, bis das Edukt oder Eduktgemisch blasenfrei aus dem zweiten Teilstück austritt, und anschließend Verfahrensschritt zwei wiederholt wird,
• - in einem vierten Verfahrensschritt das zweite Teilstück über den Dosierfinger mit dem Reaktor verbunden wird,
• - in einem fünften Verfahrensschritt bei geschlossener Stellung des Zweistellungsventils zwischen dem ersten Teilstück und der Pumpe und geöffneter Stellung des Zweistellungsventils zwischem dem zweiten Teilstück und der Pumpe das zweite Teilstück mit flüssigem Edukt oder Eduktgemisch aus der Pumpe gefüllt wird und anschließend das Edukt oder Eduktgemisch aus dem zweiten Teilstück in den Reaktor abgegeben wird, und wobei
• - die Verfahrensschritte zwei und fünf programmgesteuert solange wiederholt werden, bis das Edukt oder Eduktgemisch in der vorgegebenen Menge im Reaktor vorliegt.

The method is characterized in that the free end of the first section of the flexible feed line is always connected to the inlet vessel and the free end of the second section, on which the dosing finger is provided,

• is connected to the inlet vessel in a first process step,
• in a second process step with the two-position valve open between the first section of the flexible delivery line and the pump, the first section of the flexible delivery line is filled with liquid starting material or starting material mixture,
• in a third process step with the closed position of the two-position valve between the first section and the pump and the open position of the two-position valve between the second section and the pump, the second section is filled with liquid starting material or starting material mixture from the pump,
• process steps two and three are repeated until the educt or educt mixture emerges from the second section without bubbles, and process step two is then repeated,
• in a fourth process step, the second section is connected to the reactor via the metering finger,
• - In a fifth process step with the closed position of the two-position valve between the first section and the pump and the open position of the two-position valve between the second section and the pump, the second section is filled with liquid educt or educt mixture from the pump and then the educt or educt mixture from the second section is discharged into the reactor, and wherein
• - The process steps two and five are repeated under program control until the starting material or starting material mixture is present in the reactor in the predetermined amount.

In process steps one to three, the free ends of each of the two sections are thus connected to the feed vessel. By switching the two-position valve between the second and third process step, the first and the second section of the flexible delivery line are alternatively filled with the liquid starting material or starting material mixture by means of the pump. Process steps 2 and 3 are repeated according to the invention until the educt or educt mixture emerges bubble-free from the section on which the metering finger is provided. This is monitored in a suitable manner and transmitted to the computer controlling the process. This ensures that the section connected to the dosing finger is completely filled with liquid educt or educt mixture. Since the liquid educt or educt mixture runs back into the feed vessel in this process section, there is no loss of educt and no chemical waste.

In the next, fourth section of the method, the free end of the second section becomes which the dosing finger is provided, no longer with the feed vessel, but now connected to the reactor. Process step two is then repeated, i. H. at open position of the two-position valve between the first section of the flexible Delivery line and the pump becomes the section of the flexible delivery line with liquid Educt or educt mixture filled; in a fifth step, closed position of the two-position valve between the first section and the Pump and open position of the two-position valve between the second section and the pump filled the second section with liquid educt or educt mixture and then the starting material or starting material mixture from the second section into the reactor issued. Process steps two and five are program-controlled as long repeated until the starting material or starting material mixture in the specified amount in the reactor is present.

The invention is based on drawings and one Embodiment explained in more detail.

The individual shows:

Fig. 1 is a schematic representation of a synthesizer 1 of example 20 reactor modules 2,

Fig. 2 is a schematic representation of one embodiment of a reactor module 2 with metering and conveying means 5,

Fig. 3 is a schematic representation of a lid 13 for a reactor 3 with a sectional view A / A in Fig. 3A and

Fig. 4 shows the schematic representation of the measurement results (weight gain over the dosing period).

The synthesizer 1 shown schematically in Fig. 1 is an example equipped with 20 reactor modules 2, which are respectively uniformly movable. Each reactor module 2 has two inlet vessels 4 and one reactor 3 each. A metering and conveying device 5 is provided for each inlet vessel 4 , of which only the pumps 10 and the metering fingers 11 movable by means of a robot arm are shown in FIG. 1. The delivery line between pump 10 , dosing finger 11 and feed vessels 4 or reactor 3 is not shown .

FIG. 2 shows the schematic representation of an exemplary embodiment of a reactor module 2 for an automatic synthesizer 1 according to the invention in the position corresponding to the second method step. For reasons of simplicity of illustration, the figure shows a single feed vessel 4 and correspondingly a single metering and conveying device 5 . Inlet vessel 4 and reactor 3 are arranged, for example, on a base plate 12 . The metering and conveying device 5 comprises the flexible conveying line 6 , which is formed from the two sections 7 and 8 and a metering finger 11 is arranged at the end of the section 8 . Between the sections 7 and 8 of the flexible delivery line 6 , the two-position valve 9 is arranged, which is shown by way of example in the position that corresponds to the second method step, that is, according to which the section 7 of the flexible delivery line 6 is connected to the pump 10 , and the section 8 of the flexible delivery line 6 is separated from the pump 10 accordingly. The free ends of both sections 7 and 8 of the flexible delivery line 6 are shown connected to the feed vessel 4 , according to their position in the second process step.

Fig. 3 shows the schematic representation of an embodiment of a lid 13 with an integrated reflux condenser for a reactor. In the cross-sectional view in FIG. 3, four feed lines 17 are shown for a liquid educt or educt mixture into the reactor. The bushing shown as a central double circle, which has no reference number, is intended to accommodate a stirrer.

Fig. 3 illustrates that in the particular embodiment shown, the feed line 15 for the heat exchange medium protrudes into the cavity of the cover 13 and that the discharge line 16 for the heat exchange medium ends flush on the inner wall surrounding the cavity of the cover 13 .

The sectional view A / A in FIG. 3a clarifies the shape of the cover 13 as a hollow body which encloses a cavity 14 . In Fig. 3a can also be seen the feed-through lines 17 , which are extended beyond the lower edge of the lid, as well as feed line 15 and discharge line 16 for the heat exchange medium. In Fig. 3a can also be seen that the cover has a cross-sectional widening on its bottom and top.

embodiment

A dosing and conveying device according to the invention was then tested whether Liquids are evenly dispensed into a target vessel over a long period of time can be.

Using a computer-controlled piston pump with a piston volume of 1 ml, water was formed at room temperature (21 ° C) via a flexible delivery line made of Teflon with an inner diameter of 0.8 mm, consisting of two sections that were alternately connected to the piston pump via a two-position valve dosed into a beaker with a capacity of 0.1 l as a target vessel, which was placed on a Sartorius RC 250 S balance with 0.1 mg measuring accuracy. The metered amount was recorded at 30-second intervals via the change in weight in the target vessel and recorded. The test results are shown in FIG. 4 and show that the weight gain over the metering period and thus the metering process were linear. The step effect in the graphic representation is due to the drop formation at the end of the delivery line that is not immersed in the liquid.

The experiment was repeated for liquids with water-like viscosity, whereby the same results were obtained in each case.

Claims (11)

1. Automatic synthesizer ( 1 ), formed from one or more reactor modules ( 2 ), each with a reactor ( 3 ), one or more feed vessels ( 4 ), each for a liquid starting material or starting material mixture, and with one or more metering and conveying devices ( 5 ) for the conveyance and metering of liquid educt or educt mixture from the inlet vessel (s) ( 4 ) into the reactor ( 3 ), characterized in that each metering and conveying device ( 5 ) comprises the following components: A) a flexible delivery line ( 6 ), which is formed from two sections ( 7 , 8 ) and a metering finger ( 11 ) is provided on at least one end of the flexible delivery line ( 6 ), B) a pump ( 10 ) and C) a two-position valve ( 9 ) which is arranged between the sections ( 7 , 8 ) and via which the sections ( 7 , 8 ) can be alternately connected to the pump ( 10 ). 2. Automatic synthesizer ( 1 ) according to claim 1, characterized in that the number of reactor modules ( 2 ) is in the range from 10 to 50, preferably in the range from 20 to 35. 3. Automatic synthesizer ( 1 ) according to claim 1 or 2, characterized in that the volume of each reactor ( 3 ) is in the range from 1 ml to 100 ml, preferably in the range from 10 to 50 ml. 4. Automatic synthesizer ( 1 ) according to one of claims 1 to 3, characterized in that the pump (s) ( 10 ) is (are) a piston pump. 5. Automatic synthesizer ( 1 ) according to one of claims 1 to 4, characterized in that each reactor module ( 2 ) is designed as a uniformly movable unit, the reactor ( 3 ) and the inlet vessel (the inlet vessels) ( 4 ) on a base plate ( 12 ) are arranged. 6. Automatic synthesizer ( 1 ) according to one of claims 1 to 5, characterized in that each reactor ( 3 ) each has a cover ( 13 ) which is designed as a hollow body which encloses a cavity ( 14 ) with a feed line ( 15 ) and a discharge line ( 16 ) for a heat exchange medium in or out of the cavity ( 14 ) and with one or more feed lines ( 17 ) for each liquid educt or educt mixture into the reactor ( 3 ). 7. Automatic synthesizer ( 1 ) according to claim 6, characterized in that the cover ( 13 ) is flat, preferably as a flat disc. 8. Automatic synthesizer ( 1 ) according to claim 6 or 7, characterized in that the feed line ( 15 ) for the heat exchange medium protrudes into the cavity ( 14 ) of the cover ( 13 ) and / or that the discharge line ( 16 ) for the heat exchange medium is flush the inner wall of the cover ( 13 ) surrounding the cavity ( 14 ) ends. 9. Automatic synthesizer ( 1 ) according to one of claims 6 to 8, characterized in that the feed-through line (s) ( 16 ) projects into the interior of the reactor ( 3 ) via the lower edge of the cover ( 13 ). 10. Automatic synthesizer ( 1 ) according to one of claims 6 to 9, characterized in that the cover ( 13 ) has a cross-sectional widening on its top and bottom. 11. The method for automatically carrying out reactions in the reactor (in the reactors) ( 3 ) of an automatic synthesizer ( 1 ) according to one of claims 1 to 10, wherein the free end of the first section ( 7 ) of the flexible delivery line ( 6 ) always with Inlet vessel ( 4 ) is connected and the free end of the second section ( 8 ) of the flexible feed line ( 6 ) on which the dosing finger ( 11 ) is provided, - is connected to the feed vessel ( 4 ) in a first process step, - In a second process step with the two-position valve ( 9 ) open between the first section ( 7 ) of the flexible delivery line ( 6 ) and the pump ( 10 ), the first section ( 7 ) of the flexible delivery line ( 6 ) is filled with liquid starting material or starting material mixture becomes, - In a third process step with the closed position of the two-position valve ( 9 ) between the first section ( 7 ) and the pump ( 10 ) and the open position of the two-position valve ( 9 ) between the second section ( 8 ) and the pump ( 10 ), the second section ( 8 ) is filled with liquid starting material or starting material mixture from the pump ( 10 ), process steps two and three are repeated until the educt or educt mixture emerges from the second section ( 8 ) without bubbles, and process step two is then repeated, - In a fourth process step, the second section ( 8 ) is connected to the reactor ( 3 ) via the metering finger ( 14 ), - In a fifth process step with the closed position of the two-position valve ( 9 ) between the first section ( 7 ) and the pump ( 10 ) and the open position of the two-position valve ( 9 ) between the second section ( 8 ) and the pump ( 10 ), the second section ( 8 ) is filled with liquid educt or educt mixture from the pump ( 10 ) and then the educt or educt mixture from the second section ( 8 ) is released into the reactor ( 3 ), and wherein - The process steps two and five are repeated under program control until the starting material or starting material mixture is present in the reactor ( 3 ) in the predetermined amount.