APPARATUS AND METHOD FOR ANALYZING REACTIONS

Abstract

The invention proceeds from an apparatus for analyzing reactions, comprising a starting material distributor (7) and at least two reactors (3) which are connected in parallel and are each connected via a connecting conduit (5) to an outlet of the starting material distributor (7). To set the inflow, a pressure regulator (33) and a restrictor (19) are installed in each connecting conduit (5) between the starting material distributor (7) and the reactors (3) or an outlet conduit (13) in which a restrictor (19) and a pressure regulator (33) are installed branches off from each connecting conduit (5).

The invention further relates to a method for analyzing reactions in such an apparatus.

Claims

1. An apparatus for analyzing reactions, comprising a starting material distributor (7) and at least two reactors (3) which are connected in parallel and are each connected via a connecting conduit (5) to an outlet of the starting material distributor (7), wherein a pressure regulator (33) and a restrictor (19) are installed in each connecting conduit (5) between the starting material distributor (7) and the reactors (3) in order to set the inflow or an outlet conduit (13) in which a restrictor (19) and a pressure regulator (33) are installed branches off from each connecting conduit (5).

2. The apparatus according to claim 1, wherein the pressure regulator (33) is an exit pressure regulator and is installed between the starting material distributor (7) and the restrictor (19).

3. The apparatus according to claim 1, wherein the pressure regulator (33) is an admission pressure regulator and is installed between the restrictor (19) and the reactor (3).

4. The apparatus according to claim 1, wherein the restrictor (19) is a capillary, a microstructured component, an orifice plate or a nozzle.

5. The apparatus according to claim 1, wherein the reactors (3) are connected to a further distributor (9).

6. The apparatus according to claim 1, wherein a restrictor (19) is positioned between the further distributor (9) and each reactor (3).

7. The apparatus according to claim 5, wherein a pressure regulator (33) is installed between the further distributor (9) and each restrictor (19) or between each restrictor (19) located downstream of the further distributor (9) and the following reactor (3).

8. The apparatus according to claim 5, wherein the starting material distributor (7) and the further distributor (9) are each connected by means of a connecting conduit (5; 11) to the reactor (3), where the connecting conduits (5, 11) are brought together as a connecting point (35) and a joint feed conduit (39) which opens into the reactor (3) branches off from the connecting point (35) and the pressure regulator (33) is installed in the joint feed conduit (39).

9. The apparatus according to claim 8, wherein a restrictor is installed in the connecting conduit (5; 11).

10. A method for analyzing reactions in an apparatus according to claim 1, in which starting materials are fed into each reactor (3) via the starting material distributor (7), wherein the flow of the starting materials is regulated by means of the pressure regulators (33) and evaluation of the reaction product from each reactor (3) is carried out in the analysis unit.

11. The method according to claim 10, wherein at least one starting material is fed in via the starting material distributor (7) and at least one further starting material is fed in via the further distributor (9).

12. The method according to claim 10, wherein starting materials are fed in via the starting material distributor (7) and diluent gases or gases comprising moderators are fed in via the further distributor (9).

13. The method according to claim 10, wherein each reactor (3) is charged with a catalyst to be examined.

14. The method according to claim 10, wherein the reactors (3) are supplied with different volume flows of starting material and/or different partial pressures and/or different compositions and/or different pressures.

15. The method according to claim 10, wherein the reactors (3) are all supplied with the same volume flow and subjected to the same pressure.

Description

[0037] Embodiments of the invention are depicted in the figures and are explained in more detail in the following description. The figures show:

[0038] FIG. 1 a schematic depiction of an apparatus for analyzing reactions,

[0039] FIG. 2 a reactor of an apparatus for analyzing reactions with an exit pressure regulator for setting the flow,

[0040] FIG. 3 a reactor of an apparatus for analyzing reactions with an admission pressure regulator for setting the flow,

[0041] FIG. 4 a reactor of an apparatus for analyzing reactions with two starting material feed conduits,

[0042] FIG. 5 a reactor of an apparatus for analyzing reactions with a pressure regulator in the outlet conduit,

[0043] FIG. 6 a reactor of an apparatus for analyzing reactions with two starting material feed conduits in a further embodiment,

[0044] FIG. 7 a reactor of an apparatus for analyzing reactions with two starting material feed conduits in a further embodiment.

[0045] FIG. 1 shows a schematic depiction of an apparatus for analyzing reactions.

[0046] An apparatus for analyzing reactions 1 comprises at least two reactors 3 which are connected in parallel and are each connected via a connecting conduit 5 to a starting material distributor 7. When it is not possible to mix the starting materials to be fed into the reactor or when a variable starting material composition is to be obtained, a further distributor 9 via which further starting materials can be introduced is, as depicted here, provided. For this purpose, the further distributor 9 is connected via a further connecting conduit 11 to the reactor 3. The further connecting conduit 11 can, as shown here, open into the connecting conduit 5 by means of which the starting material distributor 7 is connected to the reactor 3 before entry into the reactor 3. As an alternative, it is also possible for both connecting conduits 5, 11 to open into the reactor 3 and the starting materials fed in via the connecting conduits 5, 11 to come into contact with one another only in the reactor 3. This is particularly useful when a reaction is triggered immediately on contact of the starting materials with one another.

[0047] The starting materials fed into the reactors 3 are preferably gaseous. However, it is also possible to introduce liquid starting materials.

[0048] In the embodiment depicted in FIG. 1, an outlet conduit 13 which branches off from the connecting conduit 5 is additionally provided. The outlet conduit 13 serves, in particular, for discharging part of the starting material, so that the flow can be regulated by discharge of part of the starting material from the process as a result of the starting material being added in an excess and such an amount of starting material that the desired amount is fed into the reactor 3 always being taken off via the outlet conduit 13. When introduction regulation is effected via the connecting conduit 5 or the further connecting conduit 11, the outlet conduit 13 can also be omitted.

[0049] The starting materials introduced via the connecting conduit 5 and optionally the further connecting conduit 11 are fed into the reactor 3 in which a chemical reaction occurs. The reactor 3 is preferably a continuously operated reactor, for example a tube reactor. When the apparatus is to be used for examining catalysts or for examining reactions which are catalytically activated, the reactor 3 is charged with a catalyst. In the case of a tube reactor, a catalyst bed 15 is usually introduced into the reactor 3 for this purpose. The starting materials fed into the reactor 3 then flow through the catalyst bed 15 and form a reaction mixture which comprises the reaction product, optionally by-products and optionally unreacted starting materials. When an inert gas is introduced into the reactor in order to dilute the reaction mixture, for example via the further distributor 9 or a third distributor (not shown here), the reaction mixture also comprises the inert gas since this does not react with the starting materials fed in. When a moderator-comprising gas is introduced into the reactor, the reactivity

of the catalyst changes and the reaction mixture comprises both unreacted or desorbed moderator and also reaction products of the moderator.

[0050] After flowing through the reactor 3, the reaction mixture leaves the reactor 3 through an offtake conduit 17. The offtake conduit 17 can either open into a vessel in which the reaction mixture is collected in order then to be passed to analysis at a later point in time or it is conducted directly to an analysis unit 37 so that an “on-line measurement”, by means of which even short-term fluctuations in the course of the reaction can be detected, is carried out. For the analysis, use is made of an analysis unit in which the reaction mixture can be analyzed qualitatively and/or quantitatively, for example by chromatographic methods such as gas chromatography or high performance liquid chromatography or else by spectroscopic methods such as infrared spectroscopy, with combinations of different methods also being possible. The reaction mixture is usually fed to the analysis unit by means of a selection valve in order to be able to utilize the analysis unit for a number of reactors.

[0051] In order to feed the same starting materials to all reactors, the starting material distributor 7 is connected to a central starting material feed conduit 25 through which the starting materials are fed to the starting material distributor and, when a further distributor 11 is present, this is connected to a further central feed conduit 27 through which either further starting materials or else an inert gas are fed in and then, as described above, distributed in the further distributor 11 to the reactors 3. When an outlet conduit 13 is provided on each reactor 3, these preferably open into a collector 29. From the collector 29, the streams of material which have been collected and combined in the collector 29 are then removed from the process via a central outlet channel 31.

[0052] In the apparatus, it is possible either to carry out a number of reactions simultaneously under the same conditions, in which case it is necessary, in particular, to supply all reactors with the same starting material volume flows at the same pressure, or under different conditions, for example in order to examine the influence of pressure and/or volume flow of a starting material of the reaction. In order to be able to set exactly the same volume flows at the same pressure or to be able to set different volume flows in a targeted manner, a restrictor and a pressure regulator are, in one embodiment, installed in the connecting conduit 5 between starting material distributor 7 and reactor 3. FIG. 2 here shows an embodiment having an exit pressure regulator and FIG. 3 shows an embodiment having an admission pressure regulator.

[0053] To simplify the depiction, only one reactor 3 is shown in each of the FIGS. 2 and 3. In the total apparatus having a plurality of reactors, each reactor 3 is connected in the same way to the starting material distributor 7. In contrast to the embodiment depicted in FIG. 1, the embodiments depicted in FIGS. 2 and 3 only have the starting material distributor 7. In this case, all the components fed to the reactor are introduced via the starting material distributor 7 into the reactors 3. For this purpose, the individual components are mixed upstream of the starting material distributor and then fed via the starting material feed conduit 25 to the starting material distributor 7. The mixing of the components can be carried out by means of any mixing device known to those skilled in the art, as have now already been used for apparatuses for the analysis of reactions having a plurality of reactors connected in parallel.

[0054] In the embodiment depicted in FIG. 2, a restrictor 19 and an exit pressure regulator 21 as pressure regulator are installed in each connecting conduit 5 between the reactor 3 and the starting material distributor 7. An essentially equal volume flow from the starting material distributor 7 to the reactors 3 is produced by the restrictor 19. For this purpose, a pressure drop which is greater than the pressure drop in the pipes and the other plant parts located upstream of the restrictor 19 in the flow direction of the starting materials starting from the distributor 7 and downstream as far as the pressure maintenance is produced in the restrictor 19. The pressure of the stream of material fed via the starting material distributor 7 through the connecting conduit 5 is set individually by means of the exit pressure regulator 21 before entry into the restrictor 19. For this purpose, the exit pressure regulator 21 is located between the starting material distributor 7 and the restrictor 19. The setting of the pressure in the stream of material before entry into the restrictor 19 enables the exact volume flow of the stream of material to be set on the basis of the known flow resistance in the restrictor 19. For this purpose, a pressure measurement is carried out between the pressure regulator 33 of the exit pressure regulator 21 and the restrictor 19 and if the measured pressure differs from a prescribed intended value, the pressure regulator 33, preferably a valve, is open further or closed in order to adjust the pressure. When the pressure measured between the restrictor 19 and the pressure regulator 33 is lower than the desired intended value, the pressure regulator is closed further in order to reduce the pressure and correspondingly is opened in the case of a measured pressure which

is higher than the desired intended value in order to lower the pressure in the connecting conduit 5 upstream of the restrictor 19. In this way, it is possible always to feed the stream of material into the restrictor 19 with essentially the same pressure, so that the volume flow which is supplied to the reactor 3 remains constant. As an alternative, it is of course also possible, if this is desirable for the reaction to be examined, to vary the volume flow, in which case the prescribed intended value for the pressure in the stream of material before entry into the restrictor 19 is varied in accordance with the desired volume flow.

[0055] In the alternative embodiment depicted in FIG. 3, the pressure regulator 33 is positioned between the restrictor 19 and the reactor 3. In this case, the use is made of an admission pressure regulator 23 in which the pressure of the stream of material leaving the restrictor 19 is measured. On the basis of the pressure measured at the exit from the restrictor 19, the pressure regulator 33 is then set in order to obtain a prescribed pressure on the outlet side of the restrictor 19. In this way, the volume flow of the stream of material fed to the reactor 3 can then likewise be set.

[0056] FIG. 4 shows an embodiment having a starting material distributor and a further distributor for introduction of starting materials or inert gases.

[0057] In contrast to the embodiments depicted in FIGS. 2 and 3, the embodiment depicted in FIG. 4 additionally comprises a further distributor 9 which is connected by means of a further connecting conduit 11 to the reactor 3, with the further connecting conduit 11 opening into the connecting conduit 5 at a connecting point 35 in the embodiment illustrated here.

[0058] The further distributor 9 can be connected without a restrictor or pressure regulator. However, a preferred alternative is also to provide a restrictor in the further connecting conduit 11. In addition, it is also possible to provide a pressure regulator, in which case both the volume flow of the stream of material fed in via the starting material distributor 7 and the volume flow of the stream of material fed in via the further distributor 9 can be set exactly. When no starting material but instead an inert gas as diluent gas is introduced via the further distributor 9, it is generally sufficient to provide a restrictor 19.

[0059] For precise setting of the volume flow, a restrictor 19 and a pressure regulator 33 are installed in the connecting conduit 5. Here, the pressure regulator can, as shown here, be arranged between the starting material distributor 7 and the restrictor 19. However, it is also possible as an alternative for the pressure regulator 33 to be arranged, as shown in FIG. 3, between the restrictor 19 and the reactor 3, in which case the pressure regulator 33 is preferably an admission pressure regulator.

[0060] When a pressure regulator is additionally provided in the further connecting conduit 11, this can likewise be positioned, as shown in FIGS. 2 and 3, either upstream of the restrictor or downstream of the restrictor; here too, an exit pressure regulator is used in the case of arrangement upstream of the restrictor and an admission pressure regulator is used in the case of positioning downstream of the restrictor.

[0061] When a pressure regulator 33 is provided only between the starting material distributor 7 and the reactor 3 and no pressure regulator is positioned in the further connecting conduit 11 between the further distributor 9 and the reactor 3, it is also possible to feed in the starting materials not via the starting material distributor 7 but instead via the further distributor 9 and, for example, introduce a diluent gas via the starting material distributor 7. However, the starting materials are usually conveyed via the distributor 7 and/or 9, in which case the flow of material can be set exactly. Introducing the starting materials via the further distributor 9 and a gas containing a moderator via the distributor 7 is preferred when the influence of the amount of moderator on the reaction is to be examined.

[0062] When starting materials are fed in both via the starting material distributor 7 and also the further distributor 9, particular preference is given to a restrictor 19 and a pressure regulator 33 being installed in each case in the connecting conduit 5 between starting material distributor 7 and reactor 3 and in the further connecting conduit 11 between further distributor 9 and reactor 3.

[0063] In the embodiments depicted in FIGS. 2, 3 and 4, there is no outlet conduit for branching off part of the starting material provided. However, depending on the reaction to be carried out, an outlet conduit as shown in FIG. 1 can also be provided. When the apparatus is to be used for examining different reactions, it is also possible to provide an additional valve in the outlet conduit 13 so that the conduit can be closed by means of this valve when no starting material is to be discharged from the apparatus via the outlet conduit 13.

[0064] A further alternative embodiment is depicted in FIG. 5. In contrast to the embodiments depicted in FIGS. 2, 3 and 4, the stream of material fed into the reactor 3 is set by setting the stream of material taken off via the outlet conduit 13 in the embodiment depicted in FIG. 5. For this purpose, the restrictor 19 and the pressure regulator 33 are installed in the outlet conduit 13. Preference is given to there being a restrictor and no pressure regulator in the connecting conduits 5, 11 between the starting material distributor 7 and the reactor 3 and, if present, between the further distributor 9 and the reactor 3, as shown here.

[0065] In this embodiment, the setting of the stream fed to the reactor 3 is carried out not directly but instead indirectly by setting of the stream of material which is taken off through the outlet conduit 13. For this purpose, the pressure regulator 33 is positioned in the outlet conduit 13 between the reactor 3 and the restrictor 19, with the pressure regulator 33 here being an exit pressure regulator. The stream of material which has not been fed to the reactor 3 can be determined from the pressure measured in the outlet conduit 13 before entry into the restrictor 19, so that the stream of material fed to the reactor 3 can in this way be set with the aid of the pressure in the outlet conduit 13. As an alternative to the embodiment depicted in FIG. 5, it is also possible to use an admission pressure regulator for setting the stream of material, in which case this is positioned downstream of the restrictor 19 in the flow direction.

[0066] FIG. 6 shows a further embodiment of a reactor of an apparatus for analyzing reactions having two starting material feed conduits. In contrast to the embodiments shown in FIGS. 4 and 5, the pressure regulator 33 here is not installed in the connecting conduit 5 or 11 but instead in a joint feed conduit 39 upstream of the reactor 3 and, in the flow direction of the fluids, downstream of the connecting point 35 at which the connecting conduit 5 and the further connecting conduit 11 are brought together. As in FIG. 5, an outlet conduit 13 is also possible here, but depending on the experiments to be carried out and the streams of material fed in is not always necessary. In the case of more than two starting material streams, it is also possible for further starting material distributors and connecting conduits from the starting material distributors to the reactor or to the connecting point 35 to be present, but these are not shown here. In the embodiment depicted in FIG. 6, too, an inert gas can be introduced instead of a further starting material via one of the connecting conduits 5, 11. Particularly when changes in the partial pressure do not have any influence on the reaction carried out in the reactor, it is possible to dispense with a restrictor, at least in the connecting conduit through which the inert gas is fed in.

[0067] FIG. 7 shows a further embodiment of a reactor of an apparatus for analyzing reactions having two starting material feed conduits. In contrast to the embodiment depicted in FIG. 4, the restrictor 19 is positioned in the joint feed conduit 39 in the embodiment depicted in FIG. 7. This embodiment requires a smaller volume flow to be fed in via the further connecting conduit 11 than the maximum amount that can flow through the joint feed conduit 39, so that no backflow into the connecting conduit 5 occurs. An advantage of this embodiment is that the total flow remains essentially constant at the same or comparable viscosity of the streams from the distributor 7 and the further distributor 9 through the feed conduit 39 and only the composition of the total stream changes when the amount introduced via the further connecting conduit 11 is altered.

Examples

[0068] In a test setup having three parallel individual introduction trains analogous to that depicted in FIG. 3, an individual flow regulator was examined. By means of an exit pressure regulator upstream of the starting material distributor, the pressure p.sub.1 was produced in the starting material distributor by introducing appropriate amounts of nitrogen from the exit pressure regulator upstream of the starting material distributor. The installation of actual reactors was omitted and the respective outflow from the partial system was measured as a function of time using a mass flow meter. A capillary having a length L and an internal diameter ID was in each case installed as restrictor in the individual introduction train (analogous to connecting conduits 5 to the reactor in FIG. 3) and an admission pressure regulator (manufacturer: “Pressure Control Solutions”; model: LF1SNN12B-NSMP1000T150G10VVB/Equilibar LF Series Precision Back Pressure Regulator) was installed downstream in the flow direction. The individual pressure downstream of the restrictor produced by this admission pressure regulator will hereinafter be referred to as p.sub.2. For individual experiments, a further admission pressure regulator (same Equilibar from Pressure Control Solutions) was installed at the outlet of the introduction train in order to examine the effect of a nonatmospheric reactor pressure. This pressure will hereinafter be referred to as p.sub.3 and will be given as 0 bar g for experiments without this additional admission pressure regulator.

[0069] For experiments on individual gas introduction, the corresponding pressure p1 was generated by means of nitrogen. The following experiments were carried out using capillaries having a length of 1 m and a nominal internal diameter of 80 μm as restrictor at room temperature (23-24° C.). p.sub.0 is ambient pressure. p-term designates the term: (p.sub.1.sup.2−p.sub.2.sup.2)/p.sub.0.

TABLE-US-00001 TABLE 1 Study on individual flow metering of nitrogen Capillary/ introduction Volume flow of Volume flow/ train p.sub.1 p.sub.2 p.sub.3 p.sub.0 p-term nitrogen p-term Re # [bar(g)] [bar(g)] [bar(g)] [bar a] [bar] [mln/h] [mln/bar/h] [—] 1 8.97 0.00 0.00 1.01 97.70 53.36 0.55 977 1 11.01 0.00 0.00 1.01 141.98 70.83 0.50 1297 1 12.97 0.00 0.00 1.01 192.48 88.33 0.46 1617 1 25.04 24.72 0.00 1.01 16.08 10.20 0.63 187 1 25.06 23.06 0.00 1.00 100.35 52.34 0.52 958 1 25.05 21.01 0.00 1.00 193.53 87.87 0.45 1609 1 25.02 24.70 15.00 1.01 16.67 11.37 0.68 208 1 24.99 23.14 0.00 1.01 91.82 51.04 0.56 934 1 24.99 23.24 15.00 1.01 87.03 49.43 0.57 905 1 24.92 20.68 0.00 1.01 199.43 90.85 0.46 1663 1 24.92 20.64 15.00 1.01 200.99 91.03 0.45 1666 2 25.02 24.72 15.00 1.01 15.37 10.18 0.66 186 2 24.99 23.19 0.00 1.01 89.30 51.22 0.57 938 2 24.99 23.23 15.00 1.01 87.59 51.59 0.59 944 2 24.92 20.74 0.00 1.01 196.93 92.03 0.47 1685 2 24.92 20.70 15.00 1.01 198.37 91.49 0.46 1675 2 8.96 0.00 0.00 1.01 97.48 54.63 0.56 1000 2 10.98 0.00 0.00 1.01 141.58 72.31 0.51 1324 2 13.01 0.00 0.00 1.01 193.80 90.63 0.47 1659 2 25.04 24.76 0.00 1.01 13.97 9.39 0.67 172 2 25.06 23.10 0.00 1.00 98.41 51.31 0.52 939 2 25.05 21.05 0.00 1.00 192.10 89.55 0.47 1639 3 8.94 0.00 0.00 1.01 97.15 53.99 0.56 988 3 11.02 0.00 0.00 1.01 142.20 72.12 0.51 1320 3 13.02 0.00 0.00 1.01 194.02 90.04 0.46 1648 3 25.04 24.75 0.00 1.01 14.87 9.70 0.65 178 3 25.06 23.11 0.00 1.00 97.98 50.66 0.52 927 3 25.05 21.02 0.00 1.00 193.16 89.14 0.46 1632

[0070] The deviation of the flow regulation was 0.1% of the respective flow. Only at large pressure differences of the admission pressure regulator for p.sub.2, i.e. large pressure difference p.sub.2 and p.sub.3, could deviations in the flow regulation of max. 1% be observed.

[0071] For experiments on n-hexadecane flow regulation, a 100 ml vessel which was filled with n-hexadecane was integrated into the inflow conduit of the starting material distributor. For the duration of the experiment, this filled vessel was pressurized with nitrogen, with regulation being effected by means of the existing exit pressure regulator. The liquid streams from the individual introduction trains were conveyed into sample containers which were weighed before and after the experiment. The corresponding mass flow conveyed was determined by measuring the introduction time and converted into a volume flow with the aid of the density.

[0072] The following experiments were carried out using capillaries having a length of 3 m and a nominal internal diameter of 127 μm at room temperature (23-24° C.).

TABLE-US-00002 TABLE 2 Study on individual flow metering of n-hexadecane Capillary/ introduction Volume flow of Volume flow/ train p.sub.1 p.sub.2 p.sub.3 Delta p n-hexadecane Delta p # [bar(g)] [bar(g)] [bar(g)] [bar] [ml/h] [ml/bar/h] 1 12.02 5.76 0 6.26 0.051 8.09E−03 1 12.05 8.86 0 3.19 0.025 7.88E−03 1 30.06 17.97 0 12.09 0.089 7.32E−03 1 30.12 18.10 0 12.02 0.088 7.28E−03 1 29.96 17.88 0 12.08 0.090 7.47E−03 1 30.07 24.02 0 6.05 0.049 8.07E−03 1 30.01 24.12 0 5.895 0.048 8.10E−03 1 30.60 21.04 0 9.56 0.071 7.45E−03 1 30.02 17.81 0 12.205 0.090 7.35E−03 1 30.00 18.00 0 12 0.088 7.35E−03 1 30.00 18.22 0 11.78 0.087 7.36E−03 2 12.02 5.76 0 6.26 0.050 7.94E−03 2 12.05 8.73 0 3.315 0.026 7.81E−03 2 30.06 17.99 0 12.07 0.088 7.31E−03 2 30.12 18.12 0 12 0.087 7.25E−03 2 29.96 17.87 0 12.09 0.090 7.42E−03 2 30.07 24.04 0 6.035 0.048 7.99E−03 2 30.01 24.09 0 5.925 0.047 7.94E−03 2 30.60 21.00 0 9.595 0.071 7.36E−03 2 30.02 17.83 0 12.185 0.089 7.32E−03 2 30.00 18.01 0 11.985 0.087 7.30E−03 2 30.00 18.19 0 11.805 0.086 7.27E−03 3 12.02 5.99 0 6.035 0.048 7.97E−03 3 12.05 8.82 0 3.225 0.024 7.58E−03 3 30.06 17.93 0 12.125 0.086 7.08E−03 3 30.12 18.10 0 12.025 0.085 7.03E−03 3 29.96 17.87 0 12.09 0.087 7.17E−03 3 30.07 24.04 0 6.035 0.048 7.92E−03 3 30.01 24.10 0 5.91 0.046 7.85E−03 3 30.60 21.06 0 9.535 0.069 7.28E−03 3 30.02 17.82 0 12.2 0.088 7.24E−03 3 30.00 18.06 0 11.94 0.085 7.15E−03 3 30.00 18.24 0 11.76 0.084 7.11E−03

[0073] It is clear from the experimental examples that the flow dependence on the admission and exit pressure for a capillary (here length=3 m and internal diameter=125 μm, or 1 m and 80 μm) as restrictor element can surprisingly be described very well by the known physical relationships for compressible media (ideal gases; here nitrogen) and incompressible media (ideal liquids; here n-hexadecane) for flows in the laminar flow regime. A consequence of this is that, proceeding from an initial value, it is possible to predict the required admission and exit pressures for a desired flow directly, without substance-specific or mixture-specific properties such as temperature dependence of the viscosity having to be known. A further advantage is that the regulation qualities given by the pressure regulation and measurement, so that in the case of the regulation quality being too low, an improved regulation quality can be achieved by increasing the flow resistance of the restrictor (for example lengthening of a capillary) and correspondingly increasing the difference between admission pressure and exit pressure.

[0074] Since the individual regulation of the flow occurs by control of the admission or exit pressure at the restrictor by means of the pneumatic conduits and no electronic components have to be present, for example for flow measurement, the setup can be operated at very high temperatures, so that individual flow regulation is also possible for mixtures having very high dew points (for example hydrocarbon mixtures having an intermediate boiling range (for example up to 200° C.) which have been vaporized under high pressures or mixtures comprising vaporized water and having high water vapor partial pressures).

[0075] Likewise, the experimental examples have surprisingly shown that not only large flow changes by a factor of 10 but also small changes in the flow by 1% are possible in a pilot plant setup.

[0076] A further aspect is that pressure changes can occur effectively ad hoc over time, while temperature changes are limited in time by the thermal mass of the respective setup and heat removal and introduction.

LIST OF REFERENCE NUMERALS

[0077] 1 Apparatus for analyzing reactions [0078] 3 Reactor [0079] 5 Connecting conduit [0080] 7 Starting material distributor [0081] 9 Further distributor [0082] 11 Further connecting conduit [0083] 13 Outlet conduit [0084] 15 Catalyst bed [0085] 17 Offtake conduit [0086] 19 Restrictor [0087] 21 Exit pressure regulator [0088] 23 Admission pressure regulator [0089] 25 Starting material feed stream [0090] 27 Further feed stream [0091] 29 Collector [0092] 31 Outlet channel [0093] 33 Pressure regulator [0094] 35 Connecting point [0095] 37 Analysis unit [0096] 39 Joint feed conduit