Improvements in or relating to the monitoring of Fischer-Tropsch chemical reactors

Abstract

1. A chemical reactor system comprising: a) a primary reactor (10) comprising: i) a reaction chamber containing a catalyst; ii) an inlet (11) for supplying a feed gas from a feed source (1) to the reaction chamber to contact the catalyst; and iii) an outlet (12) for reaction products produced in the reaction chamber from the reaction of the feed gas in the presence of the catalyst; and a reaction test module (20) comprising: b) i) an inlet (21) configured to receive a feed gas from the same feed source (1) that supplies the feed gas to the primary reactor; and ii) at least one test reactor (23) in fluid communication with the inlet (21), each test reactor (23) comprising a reaction chamber containing a catalyst; wherein the primary reactor is a Fischer-Tropsch reactor containing a Fischer-Tropsch catalyst.

Description

[Technical Field]

[0001] The present disclosure relates to improvements in monitoring Fischer-Tropsch chemical reactors. In particular, the disclosure relates to a chemical reactor system, a method for detecting catalyst poisoning in a reaction chamber, a reaction test module configured to connect to a feed source of a main reactor, and a microreactor configured to be removably inserted into the reaction test module.

[0002] This disclosure applies to the Fischer-Tropsch process. [Background technology]

[0003] The Fischer-Tropsch process is a series of chemical reactions that convert a mixture of carbon monoxide and hydrogen into liquid hydrocarbons. These reactions take place in a reaction chamber in the presence of a metal catalyst, typically at temperatures between 150 and 300 °C and pressures ranging from one to several tens of atmospheres. Ideally, the Fischer-Tropsch process involves the reaction of the following compounds: n H 2n+2 The more useful reactions produce alkanes as follows: (2n+1)H2+nCO→C n H 2n+2 +nH2O where n is typically 1 to 100 or greater. Formation of methane (n=1) is undesirable. The majority of alkanes produced tend to be linear and are suitable for upgrading to produce middle distillate fuels such as diesel and jet fuel. In addition to alkane formation, competing reactions produce small amounts of alkenes, as well as alcohols and other oxygenated hydrocarbons. The Fischer-Tropsch reaction is highly exothermic due to the standard enthalpy of reaction (ΔH) of CO2, which is -165 kJ / mol.

[0004] The raw gas feed to a Fischer-Tropsch reactor, e.g., synthesis gas (syngas) feed, can be derived from many sources, e.g., natural gas via steam reforming and / or autothermal reforming, municipal solid waste and biomass via high-temperature gasification, or carbon dioxide and hydrogen via reverse water gas shift. The syngas produced by these processes typically contains parts per million (ppm) levels of poisons or impurities, such as hydrogen cyanide and ammonia, which can damage the Fischer-Tropsch catalyst in the reactor if allowed to reach it. For example, relatively high levels of hydrogen cyanide or ammonia can cause acute poisoning of the catalyst in a short period of time. Alternatively, relatively low levels of hydrogen cyanide or ammonia may not poison the catalyst in the short term but may gradually deactivate it over time. Catalyst poisoning and deactivation can lead to reduced operating efficiency and may require the reactor to be taken offline to allow for catalyst replacement and / or regeneration. This, in turn, leads to increased operating costs, further adversely affecting the economic viability of the process.

[0005] Therefore, ideally, hydrogen cyanide and ammonia (as well as any other related poisons or impurities that may be present) are removed to single-digit ppb levels before the syngas reaches the Fischer-Tropsch reactor. A purification unit may be installed upstream of the reactor to remove these species from the syngas. For example, the purification unit may include one or more purification beds that process the syngas. In some examples, purification may involve converting hydrogen cyanide to ammonia by hydrolysis, followed by the removal of the ammonia using a wet scrubber.

[0006] However, despite the use of upstream purification, there remains a risk of contamination of the catalyst in the reactor by poisons and impurities in the feed gas, e.g., syngas. For example, purification beds in the purification equipment may malfunction or become saturated. For example, there may be unexpected poisons or impurities that the purification equipment is not configured to remove.

[0007] The present disclosure seeks to address at least some of the problems associated with the prior art or at least provide commercially acceptable alternative solutions thereto. Summary of the Invention

[0008] In a first aspect of the present disclosure, there is provided a chemical reactor system comprising: a) a primary reactor, i) a reaction chamber containing a catalyst; ii) an inlet for supplying a feed gas from a feed source to the reaction chamber for contact with the catalyst; and iii) the output of reaction products produced in the reaction chamber from the reaction of the feed gas in the presence of the catalyst; a primary reactor comprising: b) a reaction test module, i) an inlet configured to receive a feed gas from the same source that supplies the feed gas to the primary reactor; and ii) at least one test reactor in fluid communication with the inlet, each reactor comprising a reaction chamber containing a catalyst; a reaction test module comprising: Equipped with A chemical reactor system is provided in which the primary reactor is a Fischer-Tropsch reactor containing a Fischer-Tropsch catalyst.

[0009] In some preferred examples, the reaction test module comprises: iii) an analyzer configured to determine the level of catalytic activity of the catalyst in the at least one test reactor by analysis of gases exiting or derived from the reaction chamber of the at least one test reactor.

[0010] For example, the analyzer can determine the level of catalyst activity by analyzing the syngas components of the gas. Such analysis can include measuring the value and / or rate of change of one or more parameters, which can include, for example, CO conversion, methane selectivity, and C5+ productivity.

[0011] In some examples, the analyzer includes a mass spectrometer or a gas chromatograph.

[0012] In some preferred examples, the analyzer is configured to issue an alert indicating poisoning of the catalyst in the at least one test reactor upon detecting a decrease in the level of catalytic activity of the catalyst in the at least one test reactor.

[0013] In some examples, the chemical reactor system further comprises a controller configured to take corrective action when an alert is issued by the analyzer.

[0014] Preferably, the corrective action includes changing the composition of the feed gas, reducing the flow rate of the feed gas to the reaction chamber of the main reactor, or blocking the supply of the feed gas to the reaction chamber of the main reactor.

[0015] In some examples, the reaction test module further comprises a separator for separating gases exiting the reaction chamber of the at least one test reactor into one or more wax and / or liquid and / or gas fractions.

[0016] In some examples, the wax and liquid fraction are separated into a first product stream comprising waxy products and a second product stream comprising light hydrocarbon products and water.

[0017] In some instances, the catalyst in the reaction chamber of the at least one test reactor is the same catalyst as that present in the reaction chamber of the main reactor.

[0018] In some other instances, the catalyst in the reaction chamber of at least one test reactor is one or more catalysts that are different from the catalyst present in the reaction chamber of the main reactor.

[0019] In some preferred examples, the at least one test reactor comprises multiple test reactors arranged in parallel.

[0020] Preferably, one or more, and more preferably each, of the plurality of test reactors is removable from the reaction test module while the remainder of the plurality of test reactors remains in operation.

[0021] In some examples, the at least one test reactor includes three, four, five, six, or more test reactors.

[0022] In some examples, each of the at least one test reactor is a microreactor, i) 250cm 3 Less than 200cm optional 3 Less than 150cm (optional) 3 Less than, optionally 100cm 3 Less than 50cm optional 3 a reaction chamber volume of less than ii) a reaction chamber containing less than 25 grams of catalyst, optionally less than 20 grams of catalyst, optionally less than 15 grams of catalyst, optionally less than 10 grams of catalyst, optionally less than 5 grams of catalyst; and / or iii) a reaction chamber length of 30 to 120 cm and / or a reaction chamber diameter of 5 to 20 mm; The microreactor includes a microreactor having:

[0023] In some examples, the reaction test module further comprises a heating chamber housing at least one test reactor. Advantageously, this may allow the operating conditions of the catalyst in the at least one test reactor to closely match those of the catalyst in the main reactor. In some examples, one or more, and more preferably each, test reactor is independently controlled via an electric heating block, and the temperature profile of the or each test reactor is measured. For example, the catalyst bed temperature profile can be measured using multi-point thermocouples housed in a central thermowell. Alternatively, the temperature can be measured by thermocouples housed in the walls of the test reactor.

[0024] Preferably, the reaction test module is configured as a sidestream unit positioned parallel to the gas flow path through the main reactor.

[0025] In some examples, the chemical reactor system further comprises a flow divider downstream of the feedstock source and upstream of the main reactor, the flow divider receiving a feedstock gas from the feedstock source, the flow divider comprising a first outlet for supplying to the reaction chamber of the main reactor and a second outlet for supplying to at least one test reactor of the reaction test module.

[0026] In some preferred examples, the reaction test module is configured to combine gas exiting the reaction test module with gas exiting the main reactor at a point downstream of the reaction chamber of the main reactor so that gas passing through the reaction test module bypasses at least the reaction chamber of the main reactor.

[0027] In a preferred example, the piping of the chemical reactor system exposed to the source gas is internally coated with a protective coating to prevent the retention of toxic components on the surfaces of the piping. The protective coating may be applied to the piping upstream of the reaction test module and to the internal piping of the reaction test module.

[0028] According to this specification, the primary reactor is a Fischer-Tropsch reactor containing a Fischer-Tropsch catalyst.

[0029] In a second aspect of the present disclosure, there is provided a method for detecting poisoning of a catalyst in a reaction chamber, comprising: a) operating a primary reactor having a reaction chamber containing a catalyst by passing a feed gas through the reaction chamber and contacting the feed gas with the catalyst to produce a reaction product from the reaction of the feed gas in the presence of the catalyst; b) simultaneously operating the reaction test modules by passing a feed gas through at least one test reactor of the reaction test modules, each test reactor comprising a reaction chamber containing the same catalyst or a suitable equivalent thereof as present in the reaction chamber of the primary reactor; c) determining the level of catalytic activity of the catalyst in the at least one test reactor by analyzing gases exiting the reaction chamber of the at least one test reactor and / or analyzing the catalyst in the at least one test reactor using an analyzer; Including, A method is provided wherein the primary reactor is a Fischer-Tropsch reactor containing a Fischer-Tropsch catalyst.

[0030] Preferably, the feed gas supplied to the reaction chamber of the main reactor and the feed gas supplied to the at least one test reactor of the reaction test module are from the same source.

[0031] In some preferred examples, a gas stream from a feedstock source is split into a first stream that feeds the reaction chamber of the primary reactor and a second stream that feeds at least one test reactor in the reaction test module.

[0032] In some preferred examples, analysis of gases exiting the reaction chamber of the at least one test reactor is performed in real time while the main reactor is in operation.

[0033] In some examples, analysis of the gases exiting the reaction chamber of the at least one test reactor is performed by a mass spectrometer or a gas chromatograph.

[0034] In some instances, gases exiting the reaction chamber of at least one test reactor are dried and / or cooled before passing through a mass spectrometer or gas chromatograph.

[0035] In some preferred examples, the method further includes issuing an alert indicating poisoning of the catalyst in the at least one test reactor upon detecting a decrease in the level of catalytic activity of the catalyst in the at least one test reactor.

[0036] In some preferred examples, the method further comprises taking corrective action when an alert is issued by the analyzer.

[0037] Preferably, the corrective action includes changing the composition of the feed gas, reducing the flow rate of the feed gas to the reaction chamber of the main reactor, or blocking the supply of the feed gas to the reaction chamber of the main reactor.

[0038] In some instances, the catalyst in the reaction chamber of the at least one test reactor is the same catalyst as that present in the reaction chamber of the main reactor.

[0039] In some other instances, the catalyst in the reaction chamber of at least one test reactor is one or more catalysts that are different from the catalyst present in the reaction chamber of the main reactor.

[0040] In some preferred examples, the at least one test reactor comprises multiple test reactors arranged in parallel.

[0041] In some preferred examples, analysis of the catalyst in at least one test reactor is performed at a remote location by removing the test reactor from the reaction test module.

[0042] The reaction testing module may be configured to allow analysis of gases exiting the reaction chamber of at least one test reactor in real time during operation of the main reactor, and to allow post-hoc analysis of the catalyst by removing the test reactor from the reaction testing module.

[0043] In some instances, analysis of the catalyst includes elemental analysis of the catalyst to identify poison buildup in the catalyst.

[0044] In some preferred examples, the at least one test reactor comprises a plurality of test reactors arranged in parallel, and analysis of the catalyst comprises periodically removing successive test reactors to allow for identification of trends in poison accumulation in the catalyst.

[0045] In some examples, the method further includes heating the at least one test reactor in a heating chamber.

[0046] According to this specification, the primary reactor is a Fischer-Tropsch reactor containing a Fischer-Tropsch catalyst.

[0047] The present disclosure also provides a reaction test module configured for connection to a feed source of a primary reactor, comprising: i) an inlet configured to receive a feed gas from a feed source; and ii) a plurality of parallel-arranged test reactors in fluid communication with the inlet, each reactor comprising a reaction chamber containing a catalyst; A reaction test module is provided, comprising:

[0048] In some preferred examples, the reaction testing module further comprises an analyzer configured to determine a level of catalytic activity of the catalyst in the plurality of test reactors by analysis of gases exiting the reaction chambers of the plurality of test reactors.

[0049] In some examples, the reaction test module further comprises a heating chamber housing at least one test reactor.

[0050] The catalyst in each reaction chamber is a Fischer-Tropsch catalyst.

[0051] The present disclosure also provides a microreactor configured to be removably inserted into a reaction testing module, comprising: i) 250cm 3 Less than 200cm optional 3 Less than 150cm (optional) 3 Less than, optionally 100cm 3 Less than 50cm optional 3 a reaction chamber volume of less than ii) a reaction chamber containing less than 25 grams of catalyst, optionally less than 20 grams of catalyst, optionally less than 15 grams of catalyst, optionally less than 10 grams of catalyst, optionally less than 5 grams of catalyst; A microreactor is provided, comprising:

[0052] In some examples, the reaction chamber has a length of 30 to 120 cm and / or a diameter of 5 to 20 mm.

[0053] The catalyst in the reaction chamber is a Fischer-Tropsch catalyst.

[0054] In some instances, the catalyst is pre-charged into the reaction chamber of the microreactor and sealed prior to insertion of the reaction test module. If the catalyst has an oxidized form that requires activation by reduction, the catalyst is preferably activated prior to pre-charging. This allows for easier operation of the sidestream unit and eliminates the need for in-situ catalyst activation, saving time and reducing equipment complexity.

[0055] Beneficially, these aspects of the present disclosure can enable detection and / or analysis of catalyst contamination by poisons and impurities in the feed gas.

[0056] When the system is configured for the detection and / or analysis of catalyst contamination by poisons and impurities, it is most preferred if the catalyst in the reaction chamber of the at least one test reactor is the same catalyst as that present in the reaction chamber of the main reactor. In this way, a good correspondence can be ensured between the effects on the catalyst of the main reactor exposed to the feed gas and the effects on the catalyst in the reaction test module.

[0057] A sudden drop in activity of the catalyst within at least one test reactor can be used, for example, as an indication of higher than expected levels of poisons or other contaminants in the feed gas.

[0058] Advantageously, each of the test reactors may contain a much smaller weight / volume of catalyst than is present in the main reactor, making it possible to detect a poisoning event of a decline in catalyst activity much more quickly compared to monitoring the activity of the catalyst in the main reactor. For example, in the main reactor, a poisoning event may initially preferentially affect the catalyst closest to the feed gas inlet. However, the overall catalytic activity of the reactor may initially mask this poisoning, and the gas output from the main reactor may initially appear largely unaffected due to the large amount of catalyst remaining unpoisoned. By the time a decline in the total catalytic activity of the main reactor is detected, a significant amount of catalyst toward the inlet end may be poisoned and require replacement or regeneration.

[0059] The fast response time of the catalyst in the at least one test reactor may also enable detection of poisoning transients. During a transient event, the feed gas to the primary reactor may be diverted to a flare or shut off while still being fed to the reaction test module so that it can be assessed when the transient poisoning event has ended.

[0060] The reaction test module can act as a warning sensor for the presence of poisons or other contaminants in the feed gas. Advantageously, the use of the reaction test module allows for rapid intervention, thus protecting the larger amount of catalyst present in the reaction chamber of the primary reactor.

[0061] Preferably, initiation of corrective action may be automatic or semi-automatic and may be initiated without human intervention, or may involve presenting an alert to a human operator of the reactor (e.g., via an audible and / or visual alert) to prompt the operator to take corrective action.

[0062] The use of the reaction test module can be beneficial during all phases of operation of the primary reactor. For example, catalyst activity can be monitored over part, or preferably the entire, of the primary reactor's operating period. The reaction test module can also be advantageously used during commissioning, e.g., during start-up of the primary reactor. For example, during start-up, the feed gas may only be routed to the reaction test module for a period before the feed gas is routed to the primary reactor. Thus, the reaction test module can be used to ensure that the feed gas is within specifications before exposing the catalyst in the primary reactor to the feed gas. For example, verifying the expected performance of the catalyst in the test reactor avoids damage to the catalyst in the primary reactor at the beginning of its life.

[0063] Additionally, the reaction testing module can be used to enable the evaluation of new catalyst formulations under conditions that closely match those in the main reactor, but advantageously requiring only small amounts of catalyst and no modifications to the main reactor.

[0064] For example, the system may be configured such that the catalyst in the reaction chamber of at least one test reactor is one or more catalysts different from the catalyst present in the reaction chamber of the main reactor. In this manner, the test reactor may be used to evaluate or screen one or more new catalyst candidates for the process and / or to monitor and evaluate the vulnerability of one or more new catalyst candidates to potential poisoning events during "real-world" conditions, which can yield more accurate and informative results compared to small-scale laboratory-based testing. Advantageously, using the reaction testing module as a screening / testing aid avoids the need to reconfigure the main reactor with new catalysts, a process that is very expensive in both time and materials and can only evaluate one catalyst at a time.

[0065] In one mode of operation, the gas output from each of the at least one test reactor may be combined before passing it through the analyzer. However, in a preferred mode of operation, the gas output from each of the at least one test reactor is analyzed separately. For example, the output from a first test reactor can be analyzed over a first period of time, followed by the output from a second test reactor over a second period of time, etc.

[0066] Advantageously, providing multiple test reactors may allow the test reactor to be removed periodically over the duration of the main reactor's operation. By analyzing the catalyst in the test reactor over time, a better understanding of the poison buildup in the catalyst in the test reactor and the main reactor may be obtained. Because catalyst poisoning can sometimes be a slow process, by periodically removing and analyzing catalyst from the reaction test module, poisoning trends may be ascertainable. Advantageously, the use of the reaction test module means that the main reactor can be left in place and does not need to be shut down to draw samples of catalyst from within the main reactor.

[0067] Additionally, the use and analysis of multiple test reactors may allow for increased statistical confidence that a catalyst poisoning event is occurring or has already occurred.

[0068] The analysis may be carried out in the vicinity of the main reactor, or a test reactor may be sent to a separate location for analysis.

[0069] The types of poisons and contaminants accumulated on the catalyst can be identified, for example, by elemental analysis of the catalyst. Advantageously, analyzing the catalyst itself can overcome the difficulties of directly analyzing ppb-level poisons and contaminants in the feed gas. In addition, analyzing the catalyst may enable the detection of previously unanalyzed poisons and contaminants in the feed gas.

[0070] A parallel arrangement of test reactors can be used to ensure that all test reactors present in a reaction test module are exposed to the same feed gas for the same duration (or at least until the test reactor is optionally selectively removed for post-mortem analysis). Additionally, the parallel arrangement may also allow for the removal of one test reactor while the other test reactors remain operational.

[0071] In the present disclosure, the primary reactor is a Fischer-Tropsch reactor containing a Fischer-Tropsch catalyst. Accordingly, the present disclosure will be described below with reference to a Fischer-Tropsch process and reactor, by way of example. However, it will be understood that the systems, methods, and apparatus of the present disclosure are applicable to other processes and reactors. In other examples, the primary reactor may be configured for methanol synthesis, water-gas shift, etc.

[0072] The catalyst for the primary reactor may be provided in different forms known in the art. For example, the catalyst may be provided as one or more catalyst beds. The beds may be fluidized beds or fixed beds, or a combination thereof. For example, the primary reactor may be a fluidized bed reactor or a fixed bed reactor. Alternatively, the catalyst may be housed on multiple catalyst supports received within the reactor tubes of the primary reactor. For example, the primary reactor may be a tubular reactor. WO 2011 / 048361, WO 2012 / 136971, WO 2016 / 050520, and WO 2022064214(A1), the contents of which are incorporated herein by reference in their entireties, describe several examples of catalyst supports configured for use in tubular reactors. [Brief explanation of the drawings]

[0073] Embodiments of the present disclosure will now be described, by way of example only, with reference to the accompanying drawings, in which: [Figure 1] FIG. 1 illustrates a first example of a chemical reactor system according to the present disclosure. [Figure 2] FIG. 1 illustrates a second example of a chemical reactor system according to the present disclosure. [Figure 3] FIG. 10 illustrates a third example of a chemical reactor system according to the present disclosure. [Figure 4] FIG. 10 is a schematic diagram of a third example reaction test module. DETAILED DESCRIPTION OF THE INVENTION

[0074] 1 shows a schematic diagram of a first example of a chemical reactor system according to the present disclosure, comprising a primary reactor 10 and a reaction testing module 20, both of which are supplied with feed gas from a common feed source 1.

[0075] The primary reactor 10 comprises a reaction chamber containing a catalyst, an inlet 11 for supplying a feed gas from a feed source 1 to the reaction chamber to contact the catalyst, and an outlet 12 for reaction products produced in the reaction chamber from the reaction of the feed gas in the presence of the catalyst.

[0076] Output 12 from the primary reactor 10 can be fed to one or more downstream modules (not shown) configured for further processing, recycle, or use. For example, the reaction product may include or consist of a liquid and a gas phase upon exiting the primary reactor 10 and then be cooled downstream and separated into wax, liquid, and gas phases. The wax phase may include heavier hydrocarbons, e.g., having chain lengths of C10 to C100 or higher. The liquid phase may include lighter hydrocarbons and / or a water fraction. The gas phase may be dry or may have some residual water content.

[0077] The reaction test module 20 comprises an inlet 21 configured to receive a feed gas from the same feed source 1 that supplies the feed gas to the main reactor 10, and at least one test reactor in fluid communication with the inlet 21, each test reactor comprising a reaction chamber containing a catalyst. The catalyst may be the same catalyst as present in the reaction chamber of the main reactor 10, or it may be a different catalyst.

[0078] The reaction test module 20 may have an output 22 for reaction products produced in the reaction chamber of at least one test reactor.

[0079] 2 shows a schematic diagram of a second example of a chemical reactor system according to the present disclosure. This example is the same as the first example, except that the output 22 of the reaction testing module 20 is fed back to join the feed from the output 12 of the main reactor at point 13. This can beneficially improve system efficiency by allowing for simplified downstream processing of the reaction products using a single set of modules, e.g., coolers, separators, etc.

[0080] 3 shows a schematic diagram of a third example of a chemical reactor system according to the present disclosure. This example is similar to the previous examples. At least one test reactor, designated by reference numeral 23, receives a feed gas from input 21. Reaction test module 20 further includes separator 25 and analyzer 26. Analyzer 26 may include a mass spectrometer or a gas chromatograph.

[0081] Separator 25 may be configured to obtain a gas fraction from the reaction products output from one or more test reactors 23 and send it to analyzer 26. Separator 25 may include means for cooling the reaction products and / or separating them into wax and / or liquid and / or gas fractions. For example, separator 25 may include one or more knock-out pots. A first knock-out pot may be provided for removing the wax fraction and heavier HC fraction. A subsequent second knock-out pot may be provided for removing lighter HC fractions and / or water. Preferably, the gas fraction sent to analyzer 26 comprises dry gas.

[0082] The analyzer 26 may be configured to determine the level of catalytic activity of the catalyst in the at least one test reactor 23 by analyzing the gas received from the separator 25. For example, the analyzer may determine CO conversion, methane selectivity, product selectivity, e.g., Cn, preferably C5+ selectivity, paraffin and olefin selectivity, and productivity, e.g., C5+ It may be configured to determine catalyst activity by calculating performance parameters such as productivity.

[0083] The system may further include a controller 40 configured to take corrective action when an alert is issued by the reaction test module 20, for example, by the analyzer 26. Corrective action may include changing the composition of the feed gas, reducing the flow rate of the feed gas to the reaction chamber of the primary reactor 10, or preventing the feed gas supply to the reaction chamber of the primary reactor 10, for example, by diverting it to a flare or shutting off the supply entirely. The controller 40 may also be configured to increase the temperature of one or more of the test reactors to maintain target performance parameters so that the catalyst deactivation rate can be quantified. For example, the deactivation rate can be quantified in terms of the excess temperature required to maintain carbon monoxide conversion at a target level.

[0084] As shown schematically in FIG. 4, the reaction test module 20 of the third example (or any of the other examples) may include multiple test reactors 23 arranged in parallel.

[0085] The illustrated example shows six test reactors 23 in parallel.

[0086] The test reactors 23 may be fed by a common inlet manifold 27. Isolation valves (not shown), e.g., solenoid valves, may be provided upstream of each test reactor 23 to selectively shut off gas flow to each test reactor 23 to allow purging, maintenance, and / or removal of the test reactor 23.

[0087] The outlet from each test reactor 23 may be fed to a common outlet manifold 28. A tee-off valve 24 may be interposed between each of the test reactors 23 and the common outlet manifold 28. The tee-off valve 24 may function to selectively direct gas exiting each test reactor 23 to either the common outlet manifold 28 or the output 22 of the reaction test module 20.

[0088] The common outlet manifold 28 may feed the separator 25 of the reaction test module 20 .

[0089] Each of the test reactors 23 may be removable from the reaction test module 20 while the remainder of the test reactors 23 remain in operation.

[0090] Each test reactor 23 is a microreactor, i) 250cm 3 Less than 200cm optional 3 Less than 150cm (optional) 3 Less than, optionally 100cm 3 Less than 50cm optional 3 a reaction chamber volume of less than ii) A microreactor having a reaction chamber containing less than 25 grams of catalyst, optionally less than 20 grams of catalyst, optionally less than 15 grams of catalyst, optionally less than 10 grams of catalyst, optionally less than 5 grams of catalyst.

[0091] The reaction test module 20 may further include a heating chamber that houses the test reactor 23. For example, an oven or other heating chamber may be provided to maintain the test reactor 23 at a suitable elevated temperature.

[0092] Piping in the chemical reactor system exposed to the feed gas may be internally coated with a protective coating to prevent retention of toxic components on the surfaces of the piping. Protective coatings may be applied to piping upstream of the reaction test module 20 and to the internal piping of the reaction test module 20. In some examples, a silicone coating may be applied where needed, particularly to any stainless steel piping present. In one non-limiting example, SilCoNert® coating from SilcoTek® of Bellefonte, Pennsylvania, USA, may be used.

[0093] In use, the reaction test module 20 may enable a method for detecting poisoning of the catalyst in the reaction chamber of the primary reactor 10. The method comprises: a) operating a primary reactor 10 comprising a reaction chamber containing a catalyst by passing a feed gas through the reaction chamber and contacting the catalyst to produce a reaction product from the reaction of the feed gas in the presence of the catalyst; b) simultaneously operating the reaction test modules 20 by passing a feed gas through the test reactors 23, each test reactor 23 comprising a reaction chamber containing a catalyst; c) using the analyzer 26 to determine the level of catalytic activity of the catalyst in the test reactor 23 by analyzing gases exiting or derived from the reaction chamber of the test reactor 23 and / or by analyzing the catalyst of the test reactor 23.

[0094] Analysis of gases exiting or originating from the reaction chamber of the test reactor 23 may be performed in real time while the main reactor 10 is in operation.

[0095] Gases exiting or originating from the reaction chamber of test reactor 23 may be dried and / or cooled by separator 25 before passing to an analyzer 26, such as a mass spectrometer or gas chromatograph.

[0096] The controller 40 can issue an alert indicating poisoning of the catalyst in the test reactor 23 upon detecting a decrease in the level of catalytic activity of the catalyst in the test reactor 23. This can be used as an analogy to detecting poisoning of the catalyst in the main reactor 10.

[0097] Detection or generation of an alert can result in corrective action being taken, such as changing the composition of the feed gas, reducing the flow rate of the feed gas to the reaction chamber of the main reactor 10, or blocking the supply of the feed gas to the reaction chamber of the main reactor 10.

[0098] The reaction test module 20 may additionally or alternatively allow analysis of the catalyst in the test reactor 23 to be performed at a remote location by removing the test reactor 23 from the reaction test module 20 .

[0099] Analysis of the catalyst may include elemental analysis of the catalyst to identify poison buildup in the catalyst.

[0100] The test reactors 23 can be arranged in parallel, and selected test reactors 23 can be periodically removed to identify trends in catalyst poison accumulation. For example, a test reactor 23 can be removed, for example, once a month to analyze trends over a six-month period. The period between removals can be selected as desired. A replacement test reactor 23 can be inserted into the reaction test module 20 to replace one that has been removed.

[0101] Further aspects of the present disclosure are described in the following clauses. Clause 1. A chemical reactor system comprising: a) a primary reactor, i) a reaction chamber containing a catalyst; ii) an inlet for supplying a feed gas from a feed source to the reaction chamber for contact with the catalyst; and iii) an output of reaction products produced in the reaction chamber from the reaction of the feed gas in the presence of a catalyst; and b) a reaction test module, i) an inlet configured to receive a feed gas from the same source that supplies the feed gas to the primary reactor; and ii) at least one test reactor in fluid communication with the inlet, each reactor comprising a reaction chamber containing a catalyst; a reaction testing module comprising:

[0102] Clause 2. The reaction test module iii) an analyzer configured to determine a level of catalytic activity of a catalyst in the at least one test reactor by analysis of gases exiting or derived from a reaction chamber of the at least one test reactor.

[0103] Clause 3. The chemical reactor system of clause 2, wherein the analyzer comprises a mass spectrometer or a gas chromatograph.

[0104] Clause 4. The chemical reactor system of clause 2 or clause 3, wherein the analyzer is configured to issue an alert indicating poisoning of the catalyst in the at least one test reactor upon detecting a decrease in the level of catalytic activity of the catalyst in the at least one test reactor.

[0105] Clause 5. The chemical reactor system of clause 4, further comprising a controller configured to take corrective action when an alert is issued by the analyzer.

[0106] Clause 6. The chemical reaction system of clause 5, wherein the corrective action includes changing the composition of the feed gas, reducing the flow rate of the feed gas to the reaction chamber of the primary reactor, or blocking the supply of the feed gas to the reaction chamber of the primary reactor.

[0107] Clause 7. A chemical reactor system according to any one of clauses 1 to 6, wherein the reaction test module further comprises a separator for separating the liquids and gases exiting the reaction chamber of at least one test reactor into one or more wax and / or liquid and / or gas fractions.

[0108] Clause 8. The chemical reactor system of clause 7, wherein the wax and liquid fraction are separated into a first product stream comprising a waxy product and a second product stream comprising a light hydrocarbon product and water.

[0109] Clause 9. The chemical reactor system of any of clauses 1 to 8, wherein the catalyst in the reaction chamber of at least one test reactor is the same catalyst as the catalyst present in the reaction chamber of the main reactor.

[0110] Clause 10. The chemical reactor system of any one of clauses 1 to 8, wherein the catalyst in the reaction chamber of at least one test reactor is one or more catalysts different from the catalyst present in the reaction chamber of the main reactor.

[0111] Clause 11. The chemical reactor system of any of clauses 1 to 10, wherein the at least one test reactor comprises a plurality of test reactors arranged in parallel.

[0112] Clause 12. The chemical reactor system of clause 11, wherein each of the plurality of test reactors is removable from the reaction test module, while the remainder of the plurality of test reactors remains in operation.

[0113] Clause 13. The chemical reactor system of clause 11 or clause 12, wherein the at least one test reactor comprises three, four, five, six, or more test reactors.

[0114] Clause 14. Each of the at least one test reactor is a microreactor, i) 250cm 3 Less than 200cm optional 3 Less than 150cm (optional) 3 Less than, optionally 100cm 3 Less than 50cm optional 3 a reaction chamber volume of less than ii) a reaction chamber containing less than 25 grams of catalyst, optionally less than 20 grams of catalyst, optionally less than 15 grams of catalyst, optionally less than 10 grams of catalyst, optionally less than 5 grams of catalyst; 14. The chemical reactor system of any one of clauses 1 to 13, comprising a microreactor having:

[0115] Clause 15. The chemical reactor system of any of clauses 1 to 14, wherein the reaction test module further comprises a heating chamber housing at least one test reactor.

[0116] Clause 16. A chemical reactor system according to any one of clauses 1 to 15, wherein the reaction test module is configured as a side stream unit arranged parallel to the gas flow path through the main reactor.

[0117] Clause 17. The chemical reactor system of any of clauses 1 to 16, further comprising a flow divider downstream of the raw material source and upstream of the main reactor, the flow divider receiving raw material gas from the raw material source, the flow divider having a first outlet for supplying to the reaction chamber of the main reactor and a second outlet for supplying to at least one test reactor of the reaction test module.

[0118] Clause 18. A chemical reactor system according to any of clauses 1 to 17, wherein the reaction testing module is configured to combine gas exiting the reaction testing module with gas exiting the main reactor at a point downstream of the reaction chamber of the main reactor such that gas passing through the reaction testing module bypasses at least the reaction chamber of the main reactor.

[0119] Clause 19. The chemical reactor system of any of clauses 1 to 18, wherein the primary reactor is a Fischer-Tropsch reactor containing a Fischer-Tropsch catalyst.

[0120] Clause 20. A method for detecting poisoning of a catalyst in a reaction chamber, comprising: a) operating a primary reactor having a reaction chamber containing a catalyst by passing a feed gas through the reaction chamber and contacting the feed gas with the catalyst to produce a reaction product from the reaction of the feed gas in the presence of the catalyst; b) simultaneously operating the reaction test modules by passing a feed gas through at least one test reactor of the reaction test modules, each test reactor comprising a reaction chamber containing a catalyst; c) using an analyzer to determine the level of catalytic activity of the catalyst in the at least one test reactor by analyzing gases exiting or derived from the reaction chamber of the at least one test reactor and / or analyzing the catalyst of the at least one test reactor.

[0121] Clause 21. The method of clause 20, wherein the feed gas supplied to the reaction chamber of the primary reactor and the feed gas supplied to at least one test reactor of the reaction test module are from the same feed source.

[0122] Clause 22. The method of clause 21, wherein a gas stream from a feed source is split into a first stream that feeds a reaction chamber of a primary reactor and a second stream that feeds at least one test reactor of a reaction test module.

[0123] Clause 23. The method of any one of clauses 20 to 22, wherein the analysis of gases exiting or originating from the reaction chamber of at least one test reactor is performed in real time during operation of the main reactor.

[0124] Clause 24. The method of any one of clauses 20 to 23, wherein the analysis of gases exiting or originating from the reaction chamber of the at least one test reactor is carried out by a mass spectrometer or a gas chromatograph.

[0125] Clause 25. The method of any one of clauses 20 to 24, wherein gases exiting or derived from the reaction chamber of at least one test reactor are dried and / or cooled before passing to a mass spectrometer or gas chromatograph.

[0126] Clause 26. The method of any one of clauses 20-25, further comprising issuing an alert indicating poisoning of the catalyst in the at least one test reactor upon detecting a decrease in the level of catalytic activity of the catalyst in the at least one test reactor.

[0127] Clause 27. The method of clause 26, further comprising taking corrective action when an alert is issued by the analyzer.

[0128] Clause 28. The method of clause 27, wherein the corrective action includes altering the composition of the feed gas, reducing the flow rate of the feed gas to the reaction chamber of the primary reactor, or blocking the supply of the feed gas to the reaction chamber of the primary reactor.

[0129] Clause 29. The method of any one of clauses 20 to 28, wherein the catalyst in the reaction chamber of at least one test reactor is the same catalyst as the catalyst present in the reaction chamber of the main reactor.

[0130] Clause 30. The method of any one of clauses 20 to 28, wherein the catalyst in the reaction chamber of at least one test reactor is one or more catalysts different from the catalyst present in the reaction chamber of the main reactor.

[0131] Clause 31. The method of any one of clauses 20 to 30, wherein the at least one test reactor comprises a plurality of test reactors arranged in parallel.

[0132] Clause 32. The method of any one of clauses 20 to 31, wherein analysis of the catalyst of at least one test reactor is performed at a remote location by removing the test reactor from the reaction test module.

[0133] Clause 33. The method of clause 32, wherein the analysis of the catalyst includes elemental analysis of the catalyst to identify accumulation of poisons on the catalyst.

[0134] Clause 34. The method of any one of clauses 20 to 33, wherein the at least one test reactor comprises a plurality of test reactors arranged in parallel, and wherein analysis of the catalyst comprises periodically removing successive test reactors to enable identification of trends in poison accumulation in the catalyst.

[0135] Clause 35. The method of any one of clauses 20 to 34, further comprising heating at least one test reactor in a heating chamber.

[0136] Clause 36. The method of any one of clauses 20 to 35, wherein the primary reactor is a Fischer-Tropsch reactor containing a Fischer-Tropsch catalyst.

[0137] Clause 37. A reaction test module configured to connect to a feed source of a primary reactor, i) an inlet configured to receive a feed gas from a feed source; and ii) a plurality of parallel-arranged test reactors in fluid communication with the inlet, each reactor comprising a reaction chamber containing a catalyst; A reaction test module comprising:

[0138] Clause 38. The reaction testing module of clause 37, further comprising an analyzer configured to determine a level of catalytic activity of the catalyst in the plurality of test reactors by analyzing gases exiting the reaction chambers of the plurality of test reactors.

[0139] Clause 39. A reaction test module according to clause 37 or 38, further comprising a heating chamber housing at least one test reactor.

[0140] Clause 40. The reaction test module of any one of clauses 37 to 39, wherein the catalyst in each reaction chamber is a Fischer-Tropsch catalyst.

[0141] Clause 41. A microreactor configured to be removably inserted into a reaction testing module, comprising: i) 250cm 3 Less than 200cm optional 3 Less than 150cm (optional) 3 Less than, optionally 100cm 3 Less than 50cm optional 3 a reaction chamber volume of less than ii) a reaction chamber containing less than 25 grams of catalyst, optionally less than 20 grams of catalyst, optionally less than 15 grams of catalyst, optionally less than 10 grams of catalyst, optionally less than 5 grams of catalyst; A microreactor comprising:

[0142] Clause 42. A microreactor according to clause 41, wherein the reaction chamber has a length of 30 to 120 cm and / or a diameter of 5 to 20 mm.

[0143] Clause 43. The microreactor of clause 41 or 42, wherein the catalyst in the reaction chamber is a Fischer-Tropsch catalyst.

[0144] Clause 44. A microreactor according to any one of clauses 41 to 43, wherein the reaction chamber of the microreactor is pre-charged with a catalyst and sealed prior to insertion of the reaction testing module.

Claims

1. 1. A chemical reactor system comprising: a) a primary reactor, i) a reaction chamber containing a catalyst; ii) an inlet for supplying a feed gas from a feed source to the reaction chamber for contact with the catalyst; and iii) an output of reaction products produced in the reaction chamber from the reaction of the feed gas in the presence of the catalyst; and b) a reaction test module, i) an inlet configured to receive a feed gas from the same source that supplies the feed gas to the primary reactor; and ii) a reaction test module in fluid communication with the inlet, the reaction test module comprising at least one test reactor, each reactor having a reaction chamber containing a catalyst; 1. A chemical reactor system wherein the primary reactor is a Fischer-Tropsch reactor containing a Fischer-Tropsch catalyst.

2. The reaction test module iii) an analyzer configured to determine a level of catalytic activity of said catalyst in said at least one test reactor by analysis of gases exiting or derived from said reaction chamber of said at least one test reactor.

3. 3. The chemical reactor system of claim 2, wherein the analyzer is configured to issue an alert indicating poisoning of the catalyst in the at least one test reactor upon detecting a decrease in the level of catalytic activity of the catalyst in the at least one test reactor.

4. a controller configured to take corrective action when the alert is issued by the analyzer; 4. The chemical reactor system of claim 3, wherein optionally, the corrective action comprises changing the composition of the feed gas, reducing the flow rate of the feed gas to the reaction chamber of the main reactor, or blocking the supply of the feed gas to the reaction chamber of the main reactor.

5. 5. The chemical reactor system according to claim 1, wherein the catalyst in the reaction chamber of the at least one test reactor is the same catalyst as that present in the reaction chamber of the main reactor.

6. 5. The chemical reactor system of claim 1, wherein the catalyst in the reaction chamber of the at least one test reactor is one or more catalysts different from the catalyst present in the reaction chamber of the main reactor.

7. 7. The chemical reactor system of claim 1, wherein the at least one test reactor comprises a plurality of test reactors arranged in parallel.

8. 8. The chemical reactor system of claim 7, wherein each of said plurality of test reactors is removable from said reaction test module while the remainder of said plurality of test reactors remains in operation.

9. each of the at least one test reactor is a microreactor; i) 250 cm ３ Less than, optionally 200 cm ３ Less than, optionally 150 cm ３ Less than, optionally 100 cm ３ Less than, optionally 50 cm ３ a reaction chamber volume of less than ii) a reaction chamber containing less than 25 grams of catalyst, optionally less than 20 g of catalyst, optionally less than 15 g of catalyst, optionally less than 10 g of catalyst, optionally less than 5 g of catalyst; and / or 9. The chemical reactor system according to any one of claims 1 to 8, comprising a microreactor having iii) a reaction chamber length of 30 to 120 cm and / or a reaction chamber diameter of 5 to 20 mm.

10. The chemical reactor system according to any one of claims 1 to 9, wherein the reaction test module further comprises a heating chamber housing the at least one test reactor.

11. 1. A method for detecting catalyst poisoning in a reaction chamber, comprising: a) operating a primary reactor comprising the reaction chamber containing the catalyst by passing a feed gas through the reaction chamber and contacting the catalyst to produce a reaction product from the reaction of the feed gas in the presence of the catalyst; b) simultaneously operating the reaction test modules by passing a feed gas through at least one test reactor of the reaction test modules, each test reactor comprising a reaction chamber containing a catalyst; c) using an analyzer to determine the level of catalytic activity of the catalyst in the at least one test reactor by analyzing gases exiting or derived from the reaction chamber of the at least one test reactor and / or by analyzing the catalyst of the at least one test reactor; The process wherein the primary reactor is a Fischer-Tropsch reactor containing a Fischer-Tropsch catalyst.

12. 12. The method of claim 11, wherein the feed gas supplied to the reaction chamber of the main reactor and the feed gas supplied to the at least one test reactor of the reaction test module are from the same source.

13. 13. The method of claim 11 or 12, wherein the analysis of the gases exiting or originating from the reaction chamber of the at least one test reactor is performed in real time during operation of the main reactor.

14. 14. The method of any one of claims 11 to 13, further comprising issuing an alert indicating poisoning of the catalyst in the at least one test reactor upon detecting a decrease in the level of catalytic activity of the catalyst in the at least one test reactor.

15. taking corrective action when the alert is issued by the analyzer; 15. The method of claim 14, wherein optionally, the corrective action comprises changing the composition of the feed gas, reducing the flow rate of the feed gas to the reaction chamber of the main reactor, or blocking the supply of the feed gas to the reaction chamber of the main reactor.

16. 16. The method of any one of claims 11 to 15, wherein the at least one test reactor comprises a plurality of test reactors arranged in parallel.

17. 17. The method of any one of claims 11 to 16, wherein analysis of the catalyst in the at least one test reactor is performed at a remote location by removing the test reactor from the reaction test module.

18. 18. The method of claim 17, wherein analyzing the catalyst comprises elemental analysis of the catalyst to identify poison accumulation in the catalyst.

19. 19. The method of any one of claims 11 to 18, wherein the at least one test reactor comprises a plurality of test reactors arranged in parallel, and wherein the analysis of the catalyst comprises periodically removing sequential test reactors to allow for identifying trends in poison accumulation in the catalyst.

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