Field of the Invention
The invention relates to a method for carrying out a chemical reaction by reacting two or more substances in a container, a container for carrying out the reaction, a set of such containers, and the use of such a container for stopping a chemical reaction.
Description of Related Art
A method for carrying out a chemical reaction by reacting two or more substances in a reactor is described in WO 02/13969 A1 (and the corresponding document US 2004/0235046 A1), in which at least one of the substances required for the reaction is present in a container that is closed in a gas-tight manner, is introduced in or with said container into the reactor, and is released from the container by breaking open the container either before the reaction or during the reaction. Here, the containers are broken open within the reactor by untargeted application of a chemical, physical or mechanical influence, typically for example by the impact effect of a stirrer provided in the reactor. Furthermore, the pressure prevailing in the reactor may also cause the substance containers to break open. In the case of the method in WO 02/13969 A1, a set of substance containers are used, which each contain substance quantities graduated based on mole equivalents. The use of such containers pre-filled with substance quantities graduated based on mole equivalents facilitates for the laboratory chemist the correct metered addition of the substances necessary for the respective reaction, and/or makes it possible with pre-filled substance quantities to “handle” a necessary substance quantity. This is of great significance, in particular when carrying out parallel reactions.
With many chemical reactions, relatively small and minimal substance quantities often have to be introduced during the course of the reaction into the reaction mass located in the reactor at precisely determined moments in time or once a precisely defined physical state, for example pressure, is reached. If there is a relatively high pressure in the reactor at this moment in time, the introduction of the substance requires extremely complex and accordingly cost-intensive equipment. A further frequent problem is also that the substances to be introduced are often very sensitive and for example must not come into contact with air or moisture. On the other hand, certain catalysts in polyolefin synthesis for example can only be added once a precisely determined pressure (for example ethylene gas pressure) of the reaction mixture is reached. This again significantly increases the complexity of the equipment required for the metered addition of such substances. In the field of polyolefin synthesis, a very small quantity for example, typically 0.6 mg for example, of a highly sensitive catalyst in a suspension has to be pumped by means of a high-pressure pump with absolute air and moisture exclusion into a reactor typically having a volume of 100-1000 ml or even greater, typically against 30 bar of pressure. A further even more serious problem is that, with the very active catalysts available nowadays, for example in the case of heterogeneous catalysis, it is virtually impossible to meter extremely small catalyst quantities in a suspension into a reactor against a high pressure, for example of 60 bar, without the few suspended catalyst particles becoming lost or destroyed as a result of the practically unavoidable residual moisture or residual air in the complex, generally confusing lines before they have reached the reactor. If in addition, as is conventional, sensitive co-catalysts and if necessary further reagents are added, the metered addition under pressure is even more problematic.
Many chemical reactions require the addition of specific substances during a specific phase of the course of the reaction. In practice, this means that the reactor has to be made accessible for the substance feed, which, with a pressurised reactor, of course necessitates specific technically complex dosing equipment that is difficult to clean of residual air or residual water (pressure pumps, hoses, etc.). Even with a high level of technical complexity, it is practically impossible to add the substances in pure, for example solid, form. This alone would open up new possibilities however and would therefore be particularly desirable.
A further problem exists when carrying out what are known as parallel reactions using a plurality of reactors. If the reactions require the metered addition of minimal quantities of highly sensitive substances, in particular against high reactor pressures, the complexity of the equipment required increases enormously. A further problem generally exists when carrying out any parallel experiments, in particular with short and medium reaction times. It is precisely this however that is the most interesting part for parallel synthesis for example. In practice, such reactions can then only be carried out in a pseudo-parallel manner, that is to say the substances are metered sequentially, such that the complexity of the equipment required remains within reasonable limits. For example, if the reaction time is 10 minutes and the metered addition of a substance requires one minute, the first reactor has to be treated further, that is to say supplied with a further substance, at the latest as the substance is metered into the tenth reactor. Here, there is often the difficulty that the reaction taking place in a reactor already requires the metered addition of a substance whilst the piece of equipment provided for this purpose is still blocked by another reactor. For a pipetting robot for example, this is practically impossible to solve without enormous technical effort. This problem can indeed be mitigated in part by what is known as “scheduling” with the aid of highly complex software algorithms, but in practice cannot be solved satisfactorily.
It is therefore desirable to have a simple solution, with which, with the simplest software and the simplest hardware, all reactions could be handled at the same time, particularly for example so as to be able to add a desired substance to any reaction for example at any desired moment in time, for example even at the same moment in time in all reactions. This would provide a technical breakthrough, not only for parallel synthesis, but also for experiments carried out conventionally. Document WO 02/13969 A1, as cited in the introduction, primarily concerns the provision of substance containers, which each contain substance quantities graduated based on mole equivalents, as already mentioned. The above-explained problem when metering particularly delicate substances is not addressed in any way in this document. Furthermore, no solution approach for this problem can be found either explicitly or inexplicitly in this document. In addition, this document does not disclose a solution for the problem of “scheduling”. In addition, this document also does not describe that a reaction could be completely prepared such that it (or possibly also merely parts thereof) could be carried out in a “remote-controlled” manner so to speak.
A method and a device suitable therefor for producing mixtures formed of at least three components are described in DE 10 2005 059 000 A1. The device comprises a flask-shaped mixing vessel, in which one of the mixing components is located. A two-chamber inner container is inserted and fixed in an opening neck of the mixing vessel. The two chambers of the inner container are separated by a separating diaphragm that can be broken open and each contains one of the two other mixing components. A rotatable closure cap sits on the opening neck of the mixing vessel. The inner container is closed at the bottom, that is to say toward the interior of the mixing vessel, by a rupture disc. Toward the top, the inner container is closed only indirectly via the closure cap of the mixing vessel. The closure cap is coupled mechanically and/or kinematically to a rod protruding into the inner container and standing up on the diaphragm. By rotating the closure cap, the rod is pressed inwardly and the separating diaphragm is thus broken open, wherein the two mixing components located in the inner container are mixed and react with one another. During the mixing and/or reaction of the two components, an increased pressure is produced in the inner container as a result of gas development and breaks open the rupture disc at the lower end of the inner container, such that the contents of the substance container pour out into the mixing vessel and mix with the mixing component located there. With the device disclosed in this document and/or the mixing method disclosed therein, the mixing process is triggered by a manual, mechanical force effect on and the resultant breaking open of the separating diaphragm between the two chambers of the inner container. The inner container is fixed against movement in the mixing vessel and is not closed in a gas-tight manner on its own.