Apparatus for investigating chemical processes in an entrained-flow reactor

Abstract

The present invention relates to an apparatus for investigating chemical processes, wherein the apparatus comprises a hopper (11), an entrained-flow reactor (13) and a reactant feed (19), and further comprises a measuring and control device. The chemical processes relate to the investigating of FCC or other fluid catalysts, or processes relating hereto. The hopper (11) and the entrained-flow reactor (13) are linked by a connection (9). Particulate material coming from the hopper (11) is transferred through the together with a reactant flow through the entrained-flow reactor (13) into a separator (17), where the particulate material is separated from a reaction product, wherein the apparatus is characterised in that the connection (9) of the hopper (11) to the entrained-flow reactor (13) comprises a compensation gas feed (21) with a difference flow controller (25) which is coupled to the measuring and control device of the apparatus in the manner wherein the current flows of the fed and discharged gas flows are detected by the one measuring and control device and can be compensated by the compensation gas feed (21).

Description

[0001] Device for investigating chemical processes in an entrained flow reactor

[0002] The present invention relates to the further development of a device and a method for investigating FCC or other fluid catalysts and chemical processes in the entrained stream in the range between laboratory and pilot plant scale.

[0003] Fluid catalytic cracking (FCC) has been one of the key technologies in the industrial processing of crude oil and petroleum components for many decades. The improvement and further development of such processes is of great interest in order to reduce the carbon dioxide emissions of established processes. Further goals include the processing of residual products from the petroleum industry or the processing of waste products into valuable products in a future circular economy, as well as the adaptation and optimization of the processes to ensure that the target components required in the process chains of the various local operating sites are produced with high yields during product composition.For example, the transformation in the automotive industry from combustion engines to new drive systems will lead to a decrease in the importance of fuel production and, at the same time, an increase in the importance of basic chemical production.

[0004] Large-scale FCC plants have catalyst capacities ranging from approximately 30 to 1200 l. In an FCC plant, the catalyst is in a recirculating process, with the functional elements of the FCC plant comprising a regenerator, an upwardly transporting entrained-flow reactor (hereinafter also referred to as a riser reactor or riser), and a stripper. The functional elements are connected to process components in such a way that catalyst is continuously transported from the regenerator to the inlet of the riser reactor, where feed is simultaneously injected into the riser reactor along with steam. Due to the process conditions, a high gas flow velocity is formed, which transports the mixture of catalyst and feed upstream through the riser reactor within a few seconds, where the chemical components are reacted.Over the course of process development over the past decades, the contact times between catalyst and chemical components in the riser reactor during FCC plant operation have been continually shortened. In today's FCC plants, the residence time of an FCC catalyst in the riser reactor is in the range of 2 to 3 seconds. The cracking reactions taking place in the reactor are endothermic, so the temperature at the inlet of the riser reactor is 100 to 200 K higher than the temperature at the outlet. For example, if the inlet temperature in the riser is 670 °C, the outlet temperature can be 530 °C.

[0005] A large number of different apparatuses for testing FCC catalysts already exist on a laboratory and pilot plant scale. The different apparatuses are characterized by different types of reactors and the quantities of catalyst used for the test. Descriptions of these devices and methods are published in the specialist literature, for example, in WO 2019 / 020655 A1 or in Catal. Today 218-219 (2013), pp. 107-114.

[0006] An apparatus for testing FCC catalysts that had become established on the market over the past two decades was sold by John Kayser under the brand name ACE™ (the abbreviation stands for Advanced Cracking Evaluation). The reactor used in the ACE apparatus, described in US patent US 6,069,012, enables catalytic tests to be conducted in a statically fluidized catalyst bed.

[0007] Both US 7,378,059 B1 and WO 2019 / 020655 A1 disclose devices with downstream transporting reactors through which an FCC catalyst is passed from a hopper to a separator, wherein a feed is added to the reactors and reacted with the introduced catalyst.

[0008] WO 2021 / 213974 A1 discloses a device and a method for investigating heterogeneously catalyzed reactions. The device comprises a reactor through which particulate catalyst flows. Downstream of the reactor, a separation device is arranged for separating the particulate catalyst from a reaction product containing condensable gases. Downstream of the separation device, a liquid separator is arranged for separating liquid components from the reaction product. The liquid separator comprises a metal tube and a deflection body connected to the liquid separator. Furthermore, the liquid separator has a gas outlet connected to at least one sample vessel.

[0009] One of the objects underlying the invention is to provide an apparatus and method for investigating FCC or other fluid catalysts and processes that enable improved investigations compared to the prior art. A further object was to provide a method that is robust and allows for the control of various process parameters. At the same time, the method according to the invention should also run automatically, if possible.

[0010] The object stated according to the invention and further objects not mentioned are achieved by providing a device and a method for investigating chemical processes, wherein the device comprises a hopper 11, an entrained-flow reactor 13, linked by a connection 9 to the hopper 11 and through which particulate material coming from the hopper 11 can flow, and a reactant feed 19 as well as a measuring and control device, wherein downstream of the entrained-flow reactor 13 there is arranged a separator 17 for separating the particulate material from a reaction product containing condensable vapors and downstream of the separator 17 there is arranged a sample vessel 63 for receiving reaction product, wherein the device is characterized in that the connection 9 from the hopper 11 to the entrained-flow reactor 13 comprises a compensation gas feed 21 with a differential flow regulator 25,which is coupled to the measuring and control device of the device in such a way that the flow rates of the supplied and discharged gas streams can be detected by the measuring and control device and compensated by the compensation gas supply 21.

[0011] In a preferred embodiment of the device, a liquid separator for separating liquid components is arranged downstream of the separator 17, and the sample vessel 63 is arranged downstream of the liquid separator 27. Using this preferred embodiment, the condensable vapors can be collected in the liquid separator.

[0012] In a further preferred embodiment of the device, the compensation gas supply is connected to a pressure sensor 35, wherein a pressure control valve 31 is arranged downstream of the liquid separator 27 or downstream of the separator 17, if the device does not have a liquid separator 27. More preferably, the pressure control valve 31 is connected to the pressure sensor 35, wherein it is preferred that the measured value of the pressure sensor 35 serves to control the pressure control valve 31. By means of the pressure control valve 31 and the said arrangement, the device can be operated at different pressures or pressure levels, wherein the pressures can be adjusted during operation of the device. The adjustment of the pressure control valve has the advantage that it can absorb pressure changes that arise, for example, in processes associated with changes in the amount of substance, which are accompanied by changes in volume.In the device according to the invention, which comprises an entrained-flow reactor 13, the flow and control parameters are recorded and correlated by a program controller. Disturbances caused by system-related or process-related fluctuations are recorded by the program controller and compensated for by feeding in a compensating gas via a compensation gas supply 21. The flow rates are recorded and adjusted by the compensation gas supply 21 in real time. Real time means that the time period for data acquisition and adjustment by feeding in compensation gas is <2 seconds; more preferably, the time period contributes <1.5 seconds, further preferably <1.0 seconds, and most preferably <0.75 seconds.A suitable test duration is preferably 30 to 300 seconds, more preferably a suitable test duration is 30 to 180 seconds, furthermore preferably 30 to 90 seconds, very preferably 30 to 60 seconds. The adjustment of the compensation gas supply in real time means that the metered flow rate of compensation gas is regulated several times over the test duration, namely every second or every fraction of a second. In a preferred embodiment, this results in the partial pressure of the feed to be metered being able to be set to a target value and thus kept almost constant over time. In a preferred embodiment of the method according to the invention, the partial pressure of the reactant fluid to be metered is calculated on the basis of different material flows, wherein the different material flows are at least partially detected by the measuring sensors. To determine the partial pressure of the feed to be metered p.Feed the physical relationship can be used, which is given by equation 1. The molar fraction of the feed y Feed is calculated and the total pressure p is measured. It is preferred that the molar fraction of the sum of all molar reactor input flows 2 n corresponds to the feed mass flow m Feed and the average molar mass of the feed M Feed determined or calculated. These can be known values ​​preset by the user or measured values ​​determined based on the invention. This means the measured quantities determined by using the device according to the invention and by performing the method according to the invention.

[0013] PFeed = ypeed ' P = P 'mFeed / MFeedEquation 1 ri i

[0014] The partial pressure is characterized by the amplitude of fluctuations in pressure and mole fraction, as well as by the frequency or duration of such fluctuations. Keeping the partial pressure virtually constant over time means that the fluctuations in pressure and mole fraction are in the range < 500 mbar or < 10%, preferably in the range < 250 mbar or < 5%, furthermore preferably in the range < 150 mbar or < 3%, particularly preferably in the range < 100 mbar or < 2%. Further preferably, the duration of the fluctuations in pressure and concentration is < 15 s, particularly preferably the duration of the fluctuations is < 10 s, and even more preferably the duration of the fluctuations is < 5 s.

[0015] The device and method according to the invention enable improved replication of the process conditions that exist in large-scale processes with entrained-flow reactors, and in particular FCC plants, compared to the devices and methods known from the prior art. The invention offers the advantage that process development is simplified by refineries and the chemical industry, as time and costs can be saved when scaling up the process development. This allows energy to be saved and the CCh emissions that occur during process development can be reduced. It is completely unexpected and therefore surprising that the performance characteristics of the device and method as described here could be further improved compared to the devices known from the prior art.The device and method according to the invention are highly complex with regard to control and regulation. The advantage is that the measurement data obtained using the device and method are in better agreement with the measurement data that can be obtained using pilot plants. It should be noted that pilot plants usually comprise riser reactors and require a much larger amount of catalyst for operation than is necessary for operation of the device and method according to the invention. For example, a catalyst quantity in the range of 5 kilograms is necessary for operation of a pilot plant with a small riser reactor. When operating the device according to the invention, catalyst quantities in the range of 50 to 150 g are necessary.Thus, the device according to the invention makes it possible to conduct the measurements using only one-fiftieth of the catalyst quantity required for the study using a pilot plant. At the same time, the duration of the experiment can be significantly shortened compared to operating a pilot plant. Operating a pilot plant requires significantly greater operating and energy expenditure, as well as a much greater use of materials in terms of solid catalyst and feeds, compared to operating the device according to the invention.

[0016] With regard to the entrained-flow reactor 13, it should be noted that this is preferably a tubular reactor. The entrained-flow reactor 13 is preferably arranged vertically, with the longitudinal axis of the reaction tube being perpendicular to the horizontal plane. The vertical arrangement means that the feasibility of the invention is in no way restricted by the longitudinal axis of the reactor deviating from the vertical orientation at a certain angle. It is conceivable that the longitudinal axis of the entrained-flow reactor 13 can have deviations from the vertical orientation of up to 45 degrees. However, the deviation is preferably less than 30 degrees, more preferably less than 10 degrees, and in particular less than 5 degrees. The entrained-flow reactor 13 is preferably a cylindrical tubular reactor having a length in the range of 0.3 - 3 m, more preferably 0.5 - 2.5 m.The diameter of the reactor is preferably in the range of 0.3-10 cm, more preferably in the range of 0.5-5 cm, and most preferably in the range of 0.6-2 cm. In further embodiments, a helically descending wound design of the reaction tube is also mentioned.

[0017] The hopper 11 used for storage and dosing preferably has a catalyst capacity in the range of 0.1 to 5 liters, more preferably the catalyst capacity is in the range of 0.2 to 3.5 liters. In the case of FCC catalyst, the bulk density is in the range of approximately 0.9 g / cm 3Therefore, depending on the design of the container, approximately 0.1–4.5 kg can be accommodated by the hopper 11. The catalyst feed time is in the range of approximately 60 seconds, with the catalyst dosing rate preferably in the range of 30–150 g / min. Using a hopper with a larger capacity offers the advantage that a larger number of repetitions of the process can be performed without having to refill the hopper. This allows the process to be operated without interruption if the influence of different process conditions is to be investigated.

[0018] The terms "hopper" and "catalyst storage container" are used synonymously. In a preferred embodiment of the device according to the invention, the hopper is equipped so that the particulate material contained in the hopper is stored in a fluidized state. Due to the fluidized state, the catalyst bed is in motion, whereby a homogeneous heat distribution at the temperature of the catalyst bed can be achieved. In a preferred embodiment, the lower part of the hopper 11 has a funnel-shaped element 12. More preferably, the funnel-shaped element 12 comprises a porous region through which gas can be introduced into the hopper, causing fluidization of the particulate material contained in the hopper 11. More preferably, the hopper 11 has an internal volume in the range of 0.5 to 10 L; more preferably, the volume is in the range of 0.5 to 5 L.Fluidization is advantageous for achieving uniform temperature control of the catalyst or the particulate material. Mixing the catalyst or the particulate material in the hopper is useful for minimizing temperature fluctuations that can be caused by the introduction of catalyst material with non-uniform temperature control during the process. It should also be noted that the hopper, in combination with the catalyst fluidization device within the hopper, leads to a further improvement of the device and the process according to the invention.

[0019] For metering the particulate material, a preferred embodiment of the device is one in which the particulate material is transferred from the hopper to the hopper outlet to the transport gas stream 23 by a positive differential pressure. A preferred embodiment of the device is one in which the hopper 11 and the separator have an operative connection 42 that controls a continuously acting pressure control valve 41, via which a differential pressure between the hopper and the separator is adjusted. Regarding the use of differential pressure control and pressure-controlled catalyst metering, it should be noted that this is particularly advantageous.

[0020] Another possibility for dosing the particulate material would be an embodiment in which a conveyor screw is arranged at the outlet of the hopper, which feeds the particulate material into the transport gas stream. Yet another possibility for dosing the particulate material would be an embodiment in which catalyst is transferred from the hopper into the transport gas stream by means of a vibration drive. A vibration drive is used in various powder dosing processes. However, this has the disadvantage that it can lead to a certain segregation of the particulate material according to particle size, whereby the agglomeration of larger particles can easily lead to clogging problems at the outlet of the hopper. Furthermore, a vibration drive is also preferred in conjunction with a hopper in which the particulate material is not in a fluidized state.To ensure a homogeneous temperature distribution in the bed of particulate material, the hopper must be small, with an internal volume in the range of 100 to 200 mL. This is disadvantageous for automated operation, since the hopper must be refilled after only one or two runs of the process. Frequent refilling of the hopper is disadvantageous for the automatic operation of the device according to the invention. However, embodiments of the devices according to the invention in which the device is equipped with several smaller hoppers are also conceivable. Configuring the device with several hoppers is advantageous if, when carrying out the process, it is intended to carry out the process several times in succession using different catalyst materials.In a preferred embodiment, the process is carried out such that the catalyst-to-oil ratio (cat / oil ratio) is in the range of 1-100, more preferably the cat / oil ratio is in the range of 3-50, and further preferably the cat / oil ratio is in the range of 4-25. It is preferred that a series of experiments can be carried out, each with a filling of the hopper and a filling of the storage container for liquid feeds, all of which are carried out according to the process according to the invention. The technical basis is provided by the fact that the liquid dosage is carried out via the program control and the amount of dosed liquid is recorded simultaneously. The amount of catalyst fed in can be determined by calibrating the solids dosing device or by weighing out the collected catalyst.The wide range of different catalyst / oil ratios that can be specified when carrying out the process is advantageous because it allows the process conditions to be investigated in a very large parameter field.

[0021] Regarding the feed injector, it should be noted that a spray nozzle that produces very fine-particle spray is preferably used for injecting liquid feeds. Examples of suitable injectors are described in EP 3 283 209 B1.

[0022] Furthermore, an embodiment of the device according to the invention is preferred, which is characterized in that the separator 17 has a gas supply 47. Preferably, a porous base plate that is permeable to gas is arranged in the lower interior of the separator. Preferably, the gas supply to the separator is arranged below the porous base plate, whereby the particulate material collected in the hopper is stored in the separator in a fluidized state. By fluidizing the collected particulate material, a better homogeneity of the temperature distribution can be achieved compared to non-fluidized storage. Furthermore, the device is preferred which is equipped with a differential pressure dosing device, which additionally has a vibration drive in the region of the lower outlet line of the hopper.In this arrangement, the vibration drive has the advantage that the susceptibility to line blockage can be further reduced, which is very advantageous for the automatic operation of the device.

[0023] In a further embodiment of the device, which is equally preferred, hopper 11 and entrained-flow reactor 13 are equipped with heating devices, and the connection 9 between hopper and entrained-flow reactor is equipped with a preheating section 71. More preferably, the elements from the group of separator 17, liquid separator 27, and sample vessel (63) are equipped with temperature control devices. Regarding the advantageous use of connection 9 with a preheating section 71, reference is also made to the description disclosed in PCT application WO 2021 / 074407 A1, wherein the process is carried out at a reactor temperature in the range from 400 to 850°C, more preferably in the range from 500 to 800°C, and furthermore preferably in the range from 650 to 750°C. It is preferred that the temperature of the preheating section be in a range from 400 to 1200°C.Temperature control of the catalyst in the preheating section is necessary to ensure the energy input necessary for the process to be carried out at high temperatures in the entrained-flow reactor. Due to the short residence times in the entrained-flow reactor, temperature control of the entrained-flow reactor is not sufficient to ensure the high reaction temperatures.

[0024] In a further preferred embodiment, the separator is equipped with a stripping gas supply 47. More preferably, the separator is equipped with a collection system for particulate material, specifically in the form of one or more sample collection vessels. The collection system preferably has two to ten sample collection vessels 72, 72'. The stripping gas supply 47 makes it possible to continue to pass purge gas through the separator after chemical processes have been carried out in the entrained-flow reactor in order to prevent undesired subsequent reactions and to at least partially remove product components adhering to the surface of the particulate material. Furthermore, the stripping gas supply 47 offers the possibility of transferring the particulate material collected in the separator to a sample collection vessel after the stripping process has been completed. The particulate material is transferred by means of compressed air bursts.Performing stripping using a stripping gas supply has the advantage that the process conditions can be adjusted to match the refinery process. During the stripping process, valuable products are removed from the catalyst surface and collected in the liquid separator 27.

[0025] In a preferred embodiment, the device is characterized in that the pressure regulator 31 downstream of the liquid separator 27 has a control dynamics in the range of 1:100, preferably in the range of 1:1,000, more preferably in the range of 1:10,000. The control dynamics result from the ratio of the smallest and largest conductance of the valve.

[0026] In particular, an embodiment of the device according to the invention is characterized in that the pressure regulator downstream of the liquid separator has a control quality whose deviation from the setpoint is <10%, preferably the deviation from the setpoint is <5%, and more preferably the deviation from the setpoint is <1%, and / or the settling time of the regulator is in the range of 0.1 - 30 seconds, preferably the settling time is <10 seconds, more preferably <5 seconds, and especially preferably <2 seconds. Overall, in a preferred embodiment, the device has at least two different pressure control lines connected to the pressure regulator 41 and the pressure regulator 31. In addition, there is the differential flow control, which is made possible by the compensation gas supply 21 being coupled to the outflowing streams and then compensating them.Thus, the device according to the invention requires a high level of control engineering effort.

[0027] By means of the device and the method according to the invention, conditions can be created that correspond with a high degree of accuracy to the process conditions prevailing in large-scale processes with entrained-flow reactors, and in particular FCC plants, with regard to residence times, partial pressures, and flow characteristics. In contrast to the operation of a large-scale FCC plant, the process according to the invention is carried out in a batch mode. In batch mode, the process has the advantage that a large number of tests can be carried out under different process conditions within a given time, thereby accelerating a development process compared to other methods. Compared to a pilot plant with a circulating catalyst, the process according to the invention is very resource-efficient and rapid.In a preferred embodiment, the device according to the invention has a plurality of automation elements with which the discontinuous operation can be carried out at least partially in an automated operation, which leads to an increase in throughput.

[0028] Thus, synergy effects arise here through the combination of the device according to the invention and the method according to the invention, which result in the data accuracy being increased and, at the same time, the examination being able to be carried out at least partially automatically at a high speed, so that results with a higher accuracy can be generated in a shorter time compared to those methods known from the prior art.

[0029] In a preferred embodiment, the method is carried out several times in succession, wherein it is further preferred that no intervention by a user of the device or the method is necessary during the implementation of the method and the repetitions, which is advantageous since the device according to the invention and the method according to the invention can be carried out in a laboratory or pilot plant for 24 hours a day without shift work being required for the user of the device according to the invention. Furthermore, it should be noted that the partial or even complete automation of the device and the method is advantageous since it reduces the sources of error that can be caused by manual work steps.

[0030] The invention relates to a method for investigating chemical processes in a device having one of the embodiments mentioned here in the description and the claims, wherein the method comprises the following steps: i) particulate material coming from the hopper 11 is passed with transport gas through the connection to the inlet of an entrained-flow reactor 13; ii) reactant stream is passed to the inlet of the entrained-flow reactor, wherein the reactant stream is brought into contact with the particle-containing gas stream and mixed; iii) the mixture of particle-containing gas stream and reactant stream is passed through the entrained-flow reactor into a separator 17; iv) the particulate material is separated in the separator and the gaseous components are led to an outlet line, wherein condensable components are collected in a separator 27 and non-condensable components are collected in a sample vessel 63 and fed for analytical characterization;When carrying out steps i) to iii) of the process, the particle-containing gas stream and the reactant stream each have a predetermined mass flow; wherein the implementation of steps i) to iii) of the process at the predetermined mass flows is in the time range from 10 to 500 seconds and the implementation of step iv) of the process is in the time range from 150 to 1200 seconds, preferably the duration of step iv) is in the time range from 200 to 600 seconds, furthermore preferably in the time range from 250 to 500 seconds.

[0031] In a preferred embodiment of the method according to the invention, the steps are carried out as follows:

[0032] - the particulate material stored in the hopper 11 is transferred from the hopper 11 into the connecting line 9 by means of positive differential pressure and, when carrying out step i), the flow rate of the transport gas, the flow rate of the hopper gas supply and the flow rate of the overpressure discharge from the hopper are recorded;

[0033] - when carrying out step ii), the flow rate of the reactant stream is recorded;

[0034] - The flow rates recorded in process steps i) and ii) are correlated, and deviations from specified target values ​​are compensated by supplying compensation gas. Process steps i), ii), and iii) can be approximately classified as process steps, and process step iv) as a processing step or separation step. The duration of process steps i), ii), and iii) is shorter than the duration of process step iv) (thus the processing step).

[0035] In a preferred embodiment, the duration of the process steps, or process steps i), ii), and iii), is in the range of 15 to 120 seconds, more preferably in the range of 30 to 90 seconds. The average residence time of a catalyst particle in the entrained-flow reactor is, depending on the selected process conditions, in the range of 0.5 to 4 seconds. Another advantageous property of the device according to the invention is that the process parameters can be selected to simulate the process conditions of selected large-scale FCC or other entrained-flow plants.

[0036] Table with a summary of dosing parameters.

[0037] In a preferred embodiment, the process according to the invention is carried out at a pressure in the range from 0.5 to 10 bara, preferably at a pressure in the range from 1.0 to 7.5 bara, particularly preferably at a pressure in the range from 1.0 to 6 bara.

[0038] Furthermore, it is also preferred to carry out the process, wherein the entrained flow reactor 13 is tempered at a temperature in the range of 100 to 950 °C when carrying out the process, preferably the entrained flow reactor 13 is tempered at a temperature in the range of 250 to 750 °C when carrying out the process.

[0039] In a preferred embodiment, the particulate material comprises a fluid or FCC catalyst, the process being carried out with at least one liquid feed, and the ratio of catalyst to liquid feed, also referred to as catalyst / feed ratio, being in a range from 1 / 1 to 100 / 1, preferably the catalyst / feed ratio being in a range from 3 / 1 to 50 / 1, and more preferably the catalyst / feed ratio being in a range from 4 / 1 to 25 / 1. The catalyst-to-feed ratio is given here as a mass ratio. In a further embodiment, which is also a preferred embodiment, the process is carried out in conjunction with a gaseous fluid, the gaseous feed being supplied as an auxiliary feed or being supplied as the sole feed.If the gaseous feed is supplied as the sole feed, the catalyst-to-feed mass ratio is in the range from 1 / 1 to 100 / 1, preferably in the range from 3 / 1 to 50 / 1, and more preferably in the range from 4 / 1 to 25 / 1. If both gaseous fluid and liquid fluid are used as starting material, the mass ratio mentioned here refers to the sum of gaseous and liquid fluid. The terms fluid and feed are used synonymously in the present description.

[0040] Examples of gaseous feeds are hydrogen, which is added as feed in hydrogenation reactions, and also ethane or propane, which can be converted into ethene or propene by dehydrogenation.

[0041] When carrying out the process, it is particularly preferred that the process steps are carried out multiple times, wherein during the repetitions of the process at least one process parameter selected from the group consisting of catalyst / feed ratio, temperature, pressure, feed, composition of the feed, partial pressure of the feed (if this is vaporizable), or the concentration of the feed in the inlet region of the entrained flow reactor, catalyst, additive is changed, whereby a process parameter set is generated; preferably the process is carried out at least three times in series, whereby the catalyst / feed ratio is changed in the process parameter set. When evaluating the experimental data thus obtained as a function of the catalyst / feed ratio, regression curves can be fitted to the measured data.Based on the different regression curves, different catalysts and feeds, or other of the above-mentioned process parameters, can be better compared with each other. The comparisons can be based on values ​​at constant conversion, constant catalyst-to-feed ratio, or constant coke deposition. A minimum amount of coke deposition on the catalyst is important in large-scale FCC processes for catalyst regeneration and for providing the heat required for the endothermic cracking reactions. Excessive coke deposition can lead to thermal damage to plant components in large-scale FCC plants during regeneration.

[0042] Furthermore, it is preferred that one or more reactant components selected from the group consisting of petroleum, oils, heavy oils, gas oils, vacuum gas oils, residual oils, vegetable oils, fats, fatty acids, triglycerides, lipids, bio-oils, pyrolysis condensates, hydrothermal oils, pyrolysis oils, peat oil, tall oil, lignin, gasoline, diesel, naphtha, polymer melts, paraffin oils, wax melts, sugar solutions, carbohydrate solutions, liquid organic extracts, turpentine, resins, tar oils, and pitch are used in the process. The exploratory use of the device and the process results in synergistic effects, as the process is resource-efficient and rapid compared to processes in pilot plants and, more precisely, compared to other state-of-the-art laboratory processes. In particular, new approaches for the refinery of the future can be investigated, which involve using biomass, residues, or waste streams as feed sources or at least admixing them.

[0043] The processing step, or separation step, involves stripping gases and condensable vapors from the particulate material in the separator. After stripping the product components, the catalyst collected in the separator is removed.

[0044] In a preferred embodiment of the device and method according to the invention, the catalyst is removed from the separator 17 by blowing it out, preferably by means of pneumatic transport, into one or more collection containers 72 using a carrier gas stream. The catalyst collected in the collection container is subjected to carbon analysis to determine the carbon content on the catalyst. Analyzers and methods known from the prior art are used to perform the carbon analysis (for example, an RC612 device from Leco Instrumente GmbH can be used as the carbon analyzer).

[0045] The components condensed in the liquid separator 27 are subjected to qualitative and quantitative analysis. The gases collected in the sample vessel 63 are also subjected to qualitative and quantitative analysis. In a preferred embodiment, the qualitative and quantitative analysis is performed using an online analyzer known from the prior art, for example, an online FTIR or an online GC.

[0046] In a further embodiment, the device according to the invention is equipped without a liquid separator, so that all gaseous components, including the condensable components, are transferred into one or more sample vessels. In this embodiment of the device, the sample vessel or vessels are stored at a temperature that prevents condensation of the condensable components. In a preferred embodiment, one or more sample vessels are used, which are disclosed in PCT application WO 2020 / 078952 A1. The sample vessels disclosed in PCT application WO 2020 / 078952 A1 are gas cylinders, which are preferably operated by means of a pneumatic piston. Compared to gas traps, which are based on the principle of water displacement, the gas cylinders have the advantage that they are also suitable for collecting polar components.Since polar components are often water-soluble or can react with water, they can be removed from the sample chamber in an uncontrolled manner in gas separators with water displacement.

[0047] In a further embodiment, the device according to the invention is equipped with two or more feed dosing units for liquid feeds 91, 92. The use of two or more feed dosing units for liquid feeds is particularly advantageous when the feeds to be dosed are immiscible. For this purpose, it is also advantageous to use the device in an embodiment equipped with multiple feed inlets, preferably a first feed inlet and a second feed inlet. The advantage here is that immiscible feeds can be processed or injected together.

[0048] The invention also relates to a computer program for controlling a device for investigating chemical processes by means of an entrained flow reactor 13, wherein the device has one of the embodiments shown here.

[0049] The invention also relates to a computer program for carrying out the method according to the invention by means of an entrained flow reactor 13, which is presented in the context of the present disclosure.

[0050] Short description of the characters

[0051] Fig. 1 shows a schematic representation of a device for investigating chemical processes with an entrained-flow reactor 13, in which the hopper 11 and the separator 17 have an operative connection 42, via which a differential pressure is set by means of a pressure control valve 41, wherein the flow regulator that controls the gas flow to the hopper U is connected to the flow regulator of the compensation gas supply 21 via the differential flow regulator 25. The device has a reactant supply 19, which is designed for the supply of gaseous components; Fig. 2 shows a schematic representation of the device shown in Fig. 1; the reactant supply 19 has a feed supply for liquids, which is provided with a feed container 18 and a pump 15, and an evaporation gas supply 14; downstream of the liquid separator and the pressure control valve 31, a selection valve 61 and a sample container 63 are arranged.

[0052] Fig. 3 shows a schematic representation of a device for investigating chemical processes with an entrained-flow reactor 13 in an embodiment in which the connection 9 between the hopper 11 and the entrained-flow reactor 13 is equipped with a preheating section 71. Furthermore, the hopper 11 has a porous inner element 12.

[0053] Fig. 4 shows a schematic representation of an apparatus for investigating chemical processes with an entrained-flow reactor 13 in an embodiment equipped with an electronic differential pressure controller 46 (DPIC) between the hopper 11 and the separator 17. An electronic differential pressure controller 46 means that the measured values ​​of pressure in the separator 17 and hopper 11 are recorded by pressure sensors. The differential pressure controller controls the flow and pressure controllers and ensures that the hopper 11 is pressurized to transfer the catalyst into line 9.

[0054] Fig. 5 shows a schematic representation of an apparatus for investigating chemical processes with an entrained-flow reactor 13 in one embodiment equipped with a first feed inlet and a second feed inlet. The apparatus is also equipped with an electronic differential pressure control 46. The feeds from the first and second feed inlets are first mixed and, after mixing, subjected to vaporization gas.

[0055] Fig. 6 shows a schematic representation of a device for investigating chemical processes with an entrained flow reactor 13 in an embodiment which is equipped with a first structural unit of a feed inlet 91 and a second structural unit of a feed inlet 92, the device further being equipped with collecting containers for receiving particulate material, in the present case with six collecting containers 72, 72'"; downstream of the collecting containers is a carbon analyzer 74; downstream of the separator is a group with three liquid separators 30, ... 30"; downstream of the liquid separator is a sample vessel for receiving gases, downstream of the sample vessel is an online analyzer 79;

[0056] Fig. 7 shows a schematic representation of the device according to the invention in a simplified representation with an identification of the individual mass flow streams, which are identified as Str. A to Str. E or as Str. A to Str. E, wherein the meaning of the abbreviation “Str.” means “stream” or “stream”, wherein Str. A represents the compensation gas stream, Str. B the transport gas stream, Str. D the hopper gas feed stream, Str. E the hopper gas outlet stream and Str. C the difference between Str. D and Str. E.

[0057] Fig. 8 shows several diagrams with experimental examples in which the temporal progression of the flow rate of compensation gas was recorded within comparative example measurements and several example measurements. Diagram I shows comparative examples (VB1 to VB6) from the prior art in which the feed gas has a constant progression and thus no adjustment of the compensation gas supply takes place. Diagram II shows examples B1 to B5, which were carried out according to the method according to the invention. The examples shown in diagrams III (Examples B6 to B8), IV (Examples B9 to B11), and V (Examples B12 to B15) were also carried out according to the method according to the invention.

[0058] Fig. 9 shows the representations from Fig. 8, wherein, instead of the compensation gas, the total amount of gas supplied to the entrained-flow reactor during the various experimental examples is shown. Illustration I in Fig. 9 shows the six comparative examples VB1 to VB6. Illustrations II, III, IV, and V show the total gas quantities supplied to the entrained-flow reactor as a function of time in the device system according to the invention in examples B1 to B5 (in II, B6 to B8 (III), B9 to B11 (IV), and B12 to B15 (V).

[0059] Fig. 10 shows the pressure curves—specifically, the partial pressure of the hydrocarbon feed calculated at the inlet of the entrained-flow reactor during the tests shown in Fig. 8 and Fig. 9. Diagram I in Fig. 10 shows pressure fluctuations recorded in the various comparative examples (VB1 to VB5) for the prior art process. Diagrams II, III, IV, and V show the process according to the invention, with the pressure assuming a constant value after a sudden increase in an induction phase at the beginning of the process.

[0060] Fig. 11. a shows a graphical representation of the partial pressure values ​​at the inlet of the entrained flow reactor as a function of the cat / oil ratio (C / O) at three different pressure levels (600 mbar, about 1130 mbar and about 1300 mbar) in connection with an implementation of the method according to the present invention;

[0061] Fig. 11.b shows a graphical representation of the partial pressure values ​​at the inlet of the entrained flow reactor as a function of the cat / oil ratio (C / O) when carrying out a method according to the prior art, whereby a pressure change can be seen which has a relationship to the cat / oil ratio;

[0062] Fig. 12 shows a graphical representation of analytical data in the form of yields of different product components or product fractions or product classes, as well as conversion and mass balance, with the analytical data plotted against the catalyst-to-oil ratios used in the process (see Figures I to XII and Table 3). The results are based on the examples shown in Fig. 11a. The partial pressure was varied in different runs of the process. The variation of the partial pressure was carried out by setting the partial pressure of the hydrocarbon feed at the inlet of the entrained-flow reactor to a defined pressure level. Four series of experiments were carried out, with the selected pressure levels being 600 mbar, approximately 1130 mbar, and approximately 1300 mbar.

[0063] The representations of the device shown in the figures depict illustrative embodiments of the device, which are shown only as examples. Other combinations of individual structural elements are also possible, which differ from the figures shown here. For example, Fig. 5 shows a liquid supply for two different liquids, which is equipped with two pumps and a common diluent gas supply. In another embodiment, which is also preferred, each of the two liquid supply lines can be equipped with its own diluent gas supply.

[0064] Fig. 7 shows the fluid flows that are monitored and controlled during the process according to the invention. The device is equipped with a hopper into which the fluidization gas (stream D) is fed. Powdered material exits the lower part of the hopper together with the fluid flow, namely stream C. Pressure peaks in the hopper are diverted through the outlet line via valve 51 (see stream E). Since stream D and stream E are determined by the measuring and control device, stream C, which results from the difference between stream D and stream E, is also known. Stream B is used to transfer the powdered material from the hopper outlet to the entrained-flow reactor. A constant stream B, also called the transport gas stream, is selected during the process.In the lower part of the transfer line from the hopper to the entrained-flow reactor, the reactant fluid is fed into the transfer line or into the inlet area of ​​the entrained-flow reactor. The reactant fluid can be a gas or a gas into which a liquid is injected. This means that the reactant fluid is an inflowing gas or a gas-containing fluid stream that is fed into the entrained-flow reactor at a constant flow rate during the process. Contact between the gas-containing fluid stream and the fluid stream containing powdered material can cause reactive processes to occur that lead to a change in volume and a change in the flow conditions in the feed to the entrained-flow reactor. By means of the device according to the invention, changing flow conditions are recorded in real time and compensated for by the compensation gas supply, wherein the compensation gas supply is shown in Fig.7 was labeled with stream A. This means that in Fig. 7 it is unclear whether the reactant gas feed is a gas feed or a liquid feed with evaporation gas, as shown, for example, in Figs. 1 to 5. Figure 6 shows a device with two structural units for the supply of different feeds. Here too, it should be noted that the structural units for the supply of multiple feeds can be designed very differently. What is characteristic, however, is that these device variants have one or more structural units for the supply of an evaporation gas line which is not the compensation gas line (stream A in Fig. 7). The compensation gas line (stream A) is coupled to stream B, stream D and stream E and enables real-time compensation according to the invention and as explained in more detail above with regard to real time.

[0065] The fact that the collected product fluids and the catalyst contained in the separator are subjected to analytical characterization is known to those skilled in the art from the prior art and therefore requires no further elaboration. Since the process offers a certain degree of flexibility regarding the selection of the process, adjustments can be made. If only highly volatile product fluids are produced in the process, the product fluids can be collected in the gas cylinder, avoiding the collection of product fluid in the liquid separator.

[0066] Examples

[0067] To illustrate the device and method according to the invention in more detail, several example tests were carried out using a device shown in Fig. 4, which also had several elements of process automation, like the device shown in Fig. 6. The device used for the tests was equipped with an entrained flow reactor that was 1.0 m long and had an internal diameter of 0.9 cm. The upper end of the entrained flow reactor was connected to the outlet side of a hopper by a connecting line designed as a preheating section. The hopper for holding the particulate solid catalyst had an internal volume of 1.7 liters and was equipped with a differential pressure dosing device and additional vibration drive. During the tests, the tubular reactor was stored at a temperature of 529 °C by means of a heating device.The hopper and preheating section were stored at a temperature of 700 °C using temperature control elements. The comparative tests according to the state of the art were carried out using a device corresponding to the device shown in WO 2019 / 020655 A1 in Figures 2.a and 2.d, thus without the use of differential flow controller 25.

[0068] All reactions shown in the examples in the entrained-flow reactor were carried out using catalyst material from the same batch and with the same feed oil. The experiments were conducted using an equilibrium catalyst (Equlibrium Catalyst or E-Cat) provided by a refinery. The E-Cat had a particle size distribution in the range of 20–150 pm and a BET surface area of ​​220 m². 2 / g. A vacuum gas oil with a boiling point distribution in the range of 210 - 600 °C, a coke residue of 0.2 wt.%, and an API gravity of 25 was used as feed. First, the injection unit was calibrated to inject the oil used as feed into the reactor at a constant dosing rate of 7 g / min. The process was repeated several times, varying the catalyst-to-oil ratio or the partial pressure at the inlet of the entrained-flow reactor. The catalyst-to-oil ratio was adjusted by specifying and varying the dosing rate of added catalyst by setting the hopper's differential pressure doser to different values, while the total pressure in the entrained-flow reactor and separator was maintained at a constant level of 3 bar via the backpressure regulator 31 and 33 in all experiments described here.The process was carried out using a device designed according to the invention, and for comparison purposes, experiments were carried out according to the prior art. The back pressure regulator 31 and 33 mentioned here consists of the pressure control valve 31 and the pressure regulator 33, with measurement and control taking place at the pressure regulator 33 (see, for example, Fig. 2), and the back pressure regulator 31 and 33 exhibiting the high control quality described above. In all of the examples presented here (i.e., the comparative examples and the examples according to the invention), the process was carried out such that the time for passing the catalyst and feed through the entrained flow reactor was 60 seconds. The residence time of the catalyst and the oil in the entrained flow reactor was in the range of approximately 1 to 2.5 seconds.The catalyst collected in the separator was then treated with stripping gas for at least 300 seconds to remove any products adhering to the catalyst, which were then transferred to the liquid separator or gas collection vessel. The separator was stored at a temperature of 480 °C, and the liquid separator was stored at a temperature of -2 °C. After the catalytic conversion in the entrained-flow reactor was terminated and the components were stripped in the stripping phase, the collected gases and liquids were subjected to quantitative and qualitative analysis. N2 was used as the stripping gas. The catalyst collected in the separator was transferred to a sample collection vessel and then subjected to carbon analysis to quantify coke deposition on the catalyst.An advantage of the method was that the device used was equipped with a series of collection vessels (liquid separators, gas collection vessels, and sample vessels for solids), allowing several sample tests to be carried out automatically in a series, and the device according to the invention could be operated fully automatically over a period of several hours. After each series of sample tests, both the respective masses of the liquids collected in the liquid separators and the respective masses of the catalyst material collected in the sample vessels were determined by weighing. In addition, the gas volumes collected in the gas collection vessels were determined.

[0069] Fig. 8, Fig. 9, and Fig. 10 show the experimental parameters recorded by the measuring and control system during the process. The process data demonstrate the advantage of the invention, which is that, by supplying compensation gas, a more stable steady state can be achieved during the process according to the invention compared to the prior art. This more stable steady state leads to higher data quality and thus also to greater accuracy of the process according to the invention. Furthermore, the partial pressure of the hydrocarbon feed at the inlet of the entrained-flow reactor can be adjusted to a specific target value.It is noteworthy that the contribution of the compensation gas at the beginning of the experiment, from the first seconds up to the fifth and tenth seconds of the process, causes a sudden change in the partial pressure of the hydrocarbon feed at the inlet of the entrained-flow reactor, which is subsequently regulated to a constant value, which, in contrast to the comparative examples from the state of the art, is independent of the respective catalyst / oil ratio. Completely unexpectedly, the extremely complex control mechanism leads to a significant increase in accuracy, as can be seen from the data shown in Fig. 11 and Fig. 12.

[0070] First, reference is made to the results shown in Fig. 10. When the process according to the invention is carried out and the catalyst / oil ratio is varied, the partial pressure values ​​measured at the inlet of the entrained-flow reactor - after a sudden increase in the first few seconds, which is related to the initiation of the catalyst mass flow from the hopper - exhibit a curve with low amplitudes and small temporal fluctuations, as can be seen in Figures II to V. When the process is carried out with a device according to the prior art, the measured partial pressures in Figure I. exhibit much more pronounced amplitudes and larger temporal fluctuations, which show a decrease in the partial pressures with increasing catalyst / oil ratio, as can be seen in Fig. 11.b.The reduction in fluctuations using the device and method according to the invention clearly demonstrates that the experimental process conditions can be controlled with greater precision over a specific range of different catalyst / oil ratios. Thus, disruptive effects and fluctuations associated with varying catalyst-to-oil ratios are more effectively suppressed or completely eliminated. This can be seen from the fact that the plot of the experiments at a constant pressure value in Fig. 11.a shows a horizontal curve along the pressure values ​​at different catalyst-to-oil ratios.

[0071] The individual measurement points are used to generate or display the conversion and yield curves, which represent the yield structure in relation to the process parameters, which also include the feed and catalyst properties. To ensure comparability of different data sets, it is interesting to visually display or calculate the yield structure in relation to different process variables. In addition to determining or displaying the yield structure as a function of the catalyst-to-oil ratio, it is important to display the yield structure as a function of conversion and to display the yield structure as a function of coke deposition on the catalyst. The inventive improvement of the entrained flow reactor in the laboratory results in the achieved data quality showing even better agreement with FCC plants operated on a large scale.In addition, different feeds with different properties, such as different average molecular weights, can be investigated under conditions that are more comparable with each other, for example, at a constant partial pressure at the reactor inlet. Furthermore, the investigations can be conducted in an experimental parameter space that goes beyond the operating parameters of commercially operated FCC plants, thus also providing a means of simulating FCC plants and processes that have not yet been used in this way in commercial operation. The expansion and improved controllability of the experimental parameter space is provided by the fact that the device and the method according to the invention are coupled to the backpressure control or can be coupled to the backpressure control.

[0072] The catalysts and feeds are fed into the reactors of large-scale FCC plants in a continuous process. It is also noteworthy that this large-scale process can be replicated in a very short time frame, as in the present experiments, a duration of just 60 seconds is sufficient to reach a steady state. Times below 60 seconds are also possible, although the duration depends on the properties of the catalyst and feed as well as on the process parameters.

[0073] Agilent GC instruments were used for the gas and liquid analyses. The analytical method is well-known and has been described in other publications. A simulated distillation according to ASTM D 2887 was used to analyze the liquid product samples. A CS744 carbon analyzer from Leco Instrumente GmbH was used to quantify coke deposits on the catalyst material.

[0074] Table 2 with an overview of the experimental examples shown in Fig. 11.a and Fig.H .b, namely in Fig. 11.a according to the invention and in Fig. 11.b according to the prior art.

[0075] Table 2 with a summary of the examples carried out, which are given in Fig. 11.a and Fig. 11.b.

[0076] Figure 12 shows the results obtained from the analytical characterization of the various product fluid streams and catalysts after the process was carried out. A summary of the individual graphical representations is provided in Table 3.

[0077] Table 3 provides a summary of the results of the analytical characterization obtained in different implementations of the method according to the invention.

[0078] The results shown in Fig. 12 and Table 3 correspond to the test procedures shown in Fig. 11a. Regarding the legend in the figures in Fig. 12, the triangle and square symbols are shown either on the vertex or on the side. The data from the SN1 series (at 600 mbar absolute partial pressure at the entrained-flow reactor inlet) are given by the points showing the triangle on its vertex, and the data from the SN2 series (at approximately 1130 mbar absolute partial pressure at the entrained-flow reactor inlet) are represented by the points showing the square on its vertex. The square and the triangle on its side show the results from the SN3 and SN4 series (at approximately 1300 mbar absolute partial pressure at the entrained-flow reactor inlet).

[0079] The results in Fig. 12 show a very clear ranking in the individual graphs with respect to propene (Fig. 12, V.), dry gas (Fig. 12, IV.), ethylene (Fig. 12, III.), C3+C4 (Fig. 12, VI.), and naphtha (Fig. 12, VII.). The data for the SN1 series are also clearly differentiated from the SN2, SN3, and SN4 series for methane (Fig. 12, II.), light cycle oil (Fig. 12, VIII.), slurry (Fig. 12, IX.), coke (Fig. 12, X.), and conversion (Fig. 12, XI.). The gradation found is related to the inlet partial pressure, which is subject to improved control by the process according to the invention compared to the prior art. This differentiation was previously not possible in the prior art. Dry gas is the sum of hydrogen, methane and ethane.

[0080] List of reference symbols:

[0081] 7 Gas supply to the hopper / hopper gas supply

[0082] 8 switching valve

[0083] 9 Connection

[0084] 11 Hoppers

[0085] 12 Hopper bottom with gas-permeable conical element

[0086] 13 entrained flow reactor

[0087] 14 Evaporation gas supply

[0088] 15 Liquid pump, preferably high-pressure pump

[0089] 16 Connecting line from feed tank to pump

[0090] 17 Separator

[0091] 18 feed containers

[0092] 19 Educt supply

[0093] 21 Compensation gas supply

[0094] 23 Transport gas supply

[0095] 24 flow regulators (FIC)

[0096] 25 Differential Flow Controller (DFC)

[0097] 26 Multi-way valve

[0098] 27 Liquid separator 29 Temperature control device, preferably cooler

[0099] 30 liquid separators with cooling device

[0100] 31 Pressure control valve

[0101] 33 Pressure regulator (PIC)

[0102] 35 Pressure sensor (PI)

[0103] 41 Pressure control valve

[0104] 42 Connecting line from the separator to the differential pressure regulator

[0105] 43 Pressure regulator (PIC)

[0106] 45 Differential Pressure Gauges (DPI)

[0107] 46 Differential Pressure Controllers (DPIC)

[0108] 47 Se pa rato rg aszuf uhr

[0109] 48 Flow Regulator Separator (FIC)

[0110] 51 switching valve

[0111] 53 Overpressure discharge

[0112] 55 Flow sensor

[0113] 61 Multi-way valve

[0114] 63 Sample vessel

[0115] 71 Preheating section for heating the connection

[0116] 72 Solids intake

[0117] 73 Transfer line in solids intake

[0118] 74 Carbon Analyzer

[0119] 78 Liquid Sample Analyzer

[0120] 79 Gas analyzer

[0121] 91 Assembly unit with first feed

[0122] 92 Unit with second feed

Claims

Patent claims 1. A device for investigating chemical processes, comprising a hopper (11), an entrained-flow reactor (13), linked by a connection (9) to the hopper (11) and through which particulate material coming from the hopper (11) can flow, and a reactant feed (19) as well as a measuring and control device, wherein downstream of the entrained-flow reactor (13) there is a separator (17) for separating the particulate material from a reaction product containing condensable vapors, and downstream of the separator (17) there is a sample vessel (63) for receiving reaction product, the device being characterized in that the connection (9) between the hopper (11) and the entrained-flow reactor (13) comprises a compensation gas feed (21) with a differential flow regulator (25) which is coupled to the measuring and control device of the device in such a way thatthat the flow rates of the supplied and discharged gas streams can be detected by the measuring and control device and compensated by the compensation gas supply (21).

2. Device for investigating chemical processes according to claim 1, wherein a liquid separator for separating liquid components is arranged downstream of the separator (17) and the sample vessel (63) is arranged downstream of the liquid separator (27).

3. Device for investigating chemical processes according to claim 1 or claim 2, wherein the compensation gas supply is connected to a pressure sensor (35), downstream of the liquid separator (27) or downstream of the separator (17), if the device does not have a liquid separator (27), a pressure control valve (31) is arranged, further preferably the pressure control valve (31) is connected to the pressure sensor (35), wherein it is preferred that the measured value of the pressure sensor (35) serves to control the pressure control valve (31).

4. Device according to one of claims 1 to 3, wherein the hopper and the separator have an operative connection (42) which controls a continuously acting pressure control valve (41) via which a differential pressure between the hopper and the separator is set.

5. Device according to one of claims 1 to 4, characterized in that the entrained flow reactor (13) is tubular, the tube having a length in the range of 0.3 to 3 m and a diameter in the range of 3 to 100 mm.

6. Device according to one of claims 1 to 5, characterized in that the lower part of the hopper (11) has a funnel-shaped element (12), more preferably the funnel-shaped element (12) comprises a porous region through which gas can be introduced into the hopper, which causes fluidization of the particulate material contained in the hopper (11), more preferably the hopper (11) has an internal volume which is in the range of 0.5 to 10 L, more preferably the volume is in the range of 0.5 to 5 L.

7. Device according to one of claims 1 to 6, characterized in that the hopper (11) and the entrained flow reactor (13) are equipped with heating devices and the connection (9) of the hopper with the entrained flow reactor is equipped with a preheating section (71), further preferably the elements from the group separator (17), liquid separator (27) and sample vessel (63) are equipped with temperature control devices.

8. Device according to one of claims 1 to 7, characterized in that the separator is equipped with a stripping gas supply (47), further preferably the separator is equipped with a collection system for particulate material, preferably the collection system has two to ten sample collection vessels (72, 72').

9. A method for investigating chemical processes in a device constructed according to one of the preceding claims 1 to 8, the method comprising the following steps: i) particulate material coming from the hopper (11) is passed with transport gas through the connection to the inlet of an entrained-flow reactor (13); ii) reactant stream is passed to the inlet of the entrained-flow reactor (13), wherein the reactant stream is brought into contact with the particle-containing gas stream and mixed; iii) the mixture of particle-containing gas stream and reactant stream is passed through the entrained-flow reactor (13) into a separator (17); iv) the particulate material is separated in the separator and the gaseous components are led to an outlet line, wherein condensable components are collected in a liquid separator (27) and non-condensable components are collected in a sample vessel (63) and fed for analytical characterization; When carrying out steps i) to iii) of the process, the particle-containing gas stream and the reactant stream each have a predetermined mass flow; wherein the implementation of steps i) to iii) of the process at the predetermined mass flows is in the time range from 10 to 500 seconds and the implementation of step iv) of the process is in the time range from 150 to 1200 seconds, preferably the duration of step iv) is in the time range from 200 to 600 seconds, furthermore preferably in the time range from 250 to 500 seconds.

10. A method for investigating chemical processes using an entrained flow reactor according to claim 9, wherein the steps are carried out as follows: - the particulate material stored in the hopper (11) is transferred from the hopper (11) into the connecting line (9) by means of positive differential pressure and, when carrying out step i), the flow rate of the transport gas, the flow rate of the hopper gas supply and the flow rate of the overpressure discharge from the hopper are recorded; - when carrying out step ii), the flow rate of the reactant stream is recorded; - the flow rates recorded in process steps i) and ii) are related and the deviations from specified target values are compensated by supplying compensation gas.

11. A method for investigating chemical processes with an entrained flow reactor (13) according to claim 9 or claim 10, wherein the method is carried out at a pressure in the range of 0.5 to 10 bara, preferably at a pressure in the range of 1.0 to 7.5 bara, particularly preferably at a pressure in the range of 1.0 to 6 bara, or wherein the entrained flow reactor 13 is tempered at a temperature in the range of 100 to 950 °C or wherein the method is carried out at a pressure in the range of 0.5 to 10 bara and a temperature of the entrained flow reactor in the range of 100 to 950 °C.

12. A method for investigating chemical processes with an entrained flow reactor (13) according to one of claims 9 to 11, wherein the particulate material comprises a fluid or FCC catalyst and wherein the method is carried out with at least one liquid feed, wherein the ratio of catalyst to liquid feed, the so-called catalyst / feed ratio, is in a range from 1 / 1 to 100 / 1, preferably the catalyst / feed ratio is in a range from 3 / 1 to 50 / 1, furthermore preferably the catalyst / feed ratio is in a range from 4 / 1 to 25 / 1.

13. A method for investigating chemical processes using an entrained-flow reactor (13) according to claim 12, wherein the method steps are carried out multiple times, wherein during the repetitions of the method at least one process parameter selected from the group consisting of catalyst / feed ratio, temperature, pressure, feed, composition of the feed, partial pressure of the feed, if vaporizable, or the concentration of the feed in the inlet region of the entrained-flow reactor, catalyst, additive is changed, wherein a process parameter set is generated; preferably the method is carried out at least three times in series, wherein the catalyst / feed ratio is changed in the process parameter set.

14. A method for investigating chemical processes with an entrained flow reactor (13) according to one of claims 9 to 13, wherein one or more reactant components selected from the group consisting of petroleums, oils, heavy oils, gas oils, vacuum gas oils, residual oils, vegetable oils, fats, fatty acids, triglycerides, lipids, bio-oils, pyrolysis condensates, hydrothermal oils, pyrolysis oils, peat oil, tall oil, lignin, gasoline, diesel, naphtha, polymer melts, paraffin oils, wax melts, sugar solutions, carbohydrate solutions, liquid organic extracts, turpentine, resins, tar oils, pitch are used in carrying out the method.

15. A computer program for controlling a device for investigating chemical processes by means of an entrained-flow reactor (13), which has the features according to one of claims 1 to 8, or a computer program for carrying out a method in conjunction with a device comprising an entrained-flow reactor (13) according to one of claims 9 to 14.

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