Improvements in or relating to fischer-tropsch chemical reactor monitoring

Abstract

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

Description

Technical Field

[0001] The present disclosure relates to improvements in monitoring of Fischer-Tropsch chemical reactors. Specifically, the present disclosure relates to chemical reactor systems, methods for detecting catalyst poisoning in a reaction chamber, reaction test modules configured to be connected to a source of raw materials of a main reactor, and microreactors configured to be removably inserted into the reaction test modules.

[0002] The present disclosure is applicable to the Fischer-Tropsch process. Background Art

[0003] The Fischer–Tropsch process is a collection of chemical reactions that convert a mixture of carbon monoxide and hydrogen into liquid hydrocarbons. These reactions occur in a reaction chamber in the presence of a metal catalyst, typically at temperatures between 150°C and 300°C and pressures between one and several tens of atmospheres. The Fischer–Tropsch process involves a series of chemical reactions that produce various hydrocarbons, ideally having the formula (C n H 2n+2 ). A more useful reaction to produce alkanes is as follows:

[0004] (2n+1)H2+nCO→C n H 2n+2 +n H2O

[0005] wherein n is typically 1-100 or higher. The formation of methane (n=1) is undesirable. Most of the alkanes produced tend to be straight chain and are suitable for upgrading to produce middle distillate fuels such as diesel and jet fuel. In addition to the formation of alkanes, competing reactions also produce small amounts of olefins as well as alcohols and other oxygenated hydrocarbons. The Fischer-Tropsch reaction is a highly exothermic reaction with a standard reaction enthalpy (ΔH) of -165 kJ / mol combined CO.

[0006] The raw gas feed, such as synthesis gas (syngas) feed, sent to the Fischer-Tropsch reactor can be derived from a variety of raw material sources; for example, 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 synthesis gas produced by these processes typically contains ppm levels of poisons or impurities, such as hydrogen cyanide and ammonia, which may damage the catalyst if allowed to reach the Fischer-Tropsch catalyst in the reactor. 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, although not poisoning the catalyst in the short term, can cause the catalyst to gradually deactivate over time. The poisoning and deactivation of the catalyst result in reduced operating efficiency and may require the reactor to be taken offline to allow replacement and / or regeneration of the catalyst. This in turn leads to increased operating costs, further negatively affecting the economic viability of the process.

[0007] Therefore, it is desirable to remove hydrogen cyanide and ammonia (and any other relevant poisons or impurities that may be present) to single-digit ppb levels before the syngas reaches the Fischer-Tropsch reactor. In order to remove these substances from the syngas, a purification train may be established upstream of the reactor. For example, the purification train may include one or more purification beds that process the syngas. In some examples, purification may include converting hydrogen cyanide to ammonia by hydrolysis and then removing the ammonia using a wet scrubber.

[0008] However, despite the use of upstream purification, there is still a risk that the catalyst in the reactor may be contaminated by poisons and impurities in the feed gas (e.g., syngas). For example, a purification bed in the purification train may fail or become saturated. For example, an unexpected poison or impurity may be present, and the purification train is not configured to remove the poison or impurity.

[0009] The present disclosure attempts to address at least some of the problems associated with the prior art or at least provide a commercially acceptable alternative solution thereto. Summary of the invention

[0010] In a first aspect of the present disclosure, a chemical reactor system is provided, the chemical reactor system comprising:

[0011] a) a main reactor, the main reactor comprising:

[0012] i) a reaction chamber containing a catalyst,

[0013] ii) an inlet for feeding a feed gas from a feed source into the reaction chamber to contact the catalyst, and

[0014] iii) an output portion for a reaction product produced by a reaction of a raw material gas in the presence of a catalyst in the reaction chamber;

[0015] and

[0016] b) a reaction test module, the reaction test module comprising:

[0017] i) an inlet configured to receive a feed gas from the same feed source that supplies the feed gas to the main reactor, and

[0018] ii) at least one test reactor in fluid communication with the inlet and each comprising a reaction chamber containing a catalyst,

[0019] The main reactor is a Fischer-Tropsch reactor containing a Fischer-Tropsch catalyst.

[0020] In some preferred examples, the reaction test module further includes:

[0021] iii) an analyzer configured to determine a catalytic activity level of a catalyst within the at least one test reactor by analyzing gases exiting or originating from a reaction chamber of the at least one test reactor.

[0022] For example, the analyzer can determine the level of catalytic activity by analyzing the syngas component of the gas. Such analysis may include, for example, measuring the value and / or rate of change of one or more parameters, which may include, for example, CO conversion, methane selectivity, and C5+ production rate.

[0023] In some examples, the analyzer includes a mass spectrometer or a gas chromatograph.

[0024] In some preferred examples, the analyzer is configured to generate an alarm upon detecting a decrease in the catalytic activity level of the catalyst within the at least one test reactor, the alarm indicating poisoning of the catalyst within the at least one test reactor.

[0025] In some examples, the chemical reactor system also includes a controller configured to take corrective action when the analyzer generates an alarm.

[0026] Preferably, the corrective action comprises changing the composition of the feed gas, reducing the flow rate of the feed gas into the reaction chamber of the primary reactor, or preventing the feed gas from being fed into the reaction chamber of the primary reactor.

[0027] In some examples, the reaction testing module further includes a separator for separating gas exiting the reaction chamber of the at least one test reactor into one or more wax and / or liquid and / or gas fractions.

[0028] In some examples, the wax and liquid fractions are separated into a first product stream comprising a wax product and a second product stream comprising a light hydrocarbon product and water.

[0029] In some examples, 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.

[0030] In some other examples, the catalyst in the reaction chamber of the 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.

[0031] In some preferred examples, the at least one test reactor includes a plurality of test reactors arranged in parallel.

[0032] Preferably, one or more, more preferably each, of the plurality of test reactors can be removed from the reaction testing module while the remaining test reactors of the plurality of test reactors remain in operation.

[0033] In some examples, the at least one test reactor includes three, four, five, six, or more test reactors.

[0034] In some examples, each of the at least one test reactor comprises a microreactor having:

[0035] i) Less than 250cm 3 , optionally less than 200 cm 3 , optionally less than 150 cm 3 , optionally less than 100 cm 3 , optionally less than 50 cm 3 The reaction chamber volume; and / or

[0036] 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

[0037] iii) a reaction chamber length of 30 cm to 120 cm and / or a reaction chamber diameter of 5 mm to 20 mm.

[0038] In some examples, the reaction test module also includes a heating chamber for accommodating the at least one test reactor. Advantageously, this can allow the operating conditions of the catalyst in the at least one test reactor to be closely matched with the operating conditions of the catalyst in the main reactor. In some examples, one or more, more preferably each test reactor is independently controlled via an electric heating block, and the temperature distribution of the test reactor or each test reactor is measured. For example, a multi-point thermocouple contained in a central thermowell can be used to measure the catalyst bed temperature distribution. Alternatively, the temperature can be measured by a thermocouple mounted on the wall of the test reactor.

[0039] Preferably, the reaction testing module is configured as a side stream unit arranged in parallel with the gas flow path through the main reactor.

[0040] In some examples, the chemical reactor system also includes a splitter downstream of the raw material source and upstream of the main reactor, the splitter receiving the raw material gas from the raw material source; the splitter includes a first outlet for feeding the reaction chamber of the main reactor and a second outlet for feeding the at least one test reactor of the reaction test module.

[0041] In some preferred examples, the reaction testing module is configured to combine gas leaving the reaction testing module with gas leaving the main reactor at a point downstream of the reaction chamber of the main reactor so that the gas passing through the reaction testing module at least bypasses the reaction chamber of the main reactor.

[0042] In a preferred example, the interior of the pipes of the chemical reactor system exposed to the raw gas is coated with a protective coating to prevent toxic components from remaining on the surface of the pipes. The protective coating can be applied to the pipes upstream of the reaction test module and the internal pipes of the reaction test module.

[0043] According to the present description, the main reactor is a Fischer-Tropsch reactor containing a Fischer-Tropsch catalyst.

[0044] In a second aspect of the present disclosure, there is provided a method for detecting catalyst poisoning in a reaction chamber, the method comprising:

[0045] a) operating a main reactor comprising said reaction chamber containing said catalyst by passing a feed gas through the reaction chamber to contact said catalyst so as to produce a reaction product by reaction of the feed gas in the presence of the catalyst;

[0046] b) simultaneously operating the reaction test module by passing the feed gas through at least one test reactor of the reaction test module, each test reactor comprising a reaction chamber containing the same catalyst as that present in the reaction chamber of the main reactor or a suitable equivalent thereof; and

[0047] c) using an analyzer to determine the catalytic activity level of the catalyst within the at least one test reactor by analyzing the gases leaving the reaction chamber of the at least one test reactor and / or analyzing the catalyst of the at least one test reactor,

[0048] The main reactor is a Fischer-Tropsch reactor containing a Fischer-Tropsch catalyst.

[0049] Preferably, the raw material gas fed to the reaction chamber of the main reactor and the raw material gas fed to the at least one test reactor of the reaction test module come from the same raw material source.

[0050] In some preferred examples, the gas flow from the raw material source is separated into a first flow that is fed to the reaction chamber of the main reactor and a second flow that is fed to the at least one test reactor of the reaction test module.

[0051] In some preferred examples, during operation of the main reactor, the gas leaving the reaction chamber of the at least one test reactor is analyzed in real time.

[0052] In some examples, gases exiting the reaction chamber of the at least one test reactor are analyzed by a mass spectrometer or a gas chromatograph.

[0053] In some examples, gases exiting the reaction chamber of the at least one test reactor are dried and / or cooled before being passed to a mass spectrometer or a gas chromatograph.

[0054] In some preferred examples, the method further includes generating an alarm upon detecting a decrease in the catalytic activity level of the catalyst within the at least one test reactor, the alarm indicating that the catalyst within the at least one test reactor is poisoned.

[0055] In some preferred examples, the method further includes taking corrective action when the analyzer generates an alarm.

[0056] Preferably, the corrective action comprises changing the composition of the feed gas, reducing the flow rate of the feed gas into the reaction chamber of the primary reactor, or preventing the feed gas from being fed into the reaction chamber of the primary reactor.

[0057] In some examples, 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 primary reactor.

[0058] In some other examples, the catalyst in the reaction chamber of the 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.

[0059] In some preferred examples, the at least one test reactor includes a plurality of test reactors arranged in parallel.

[0060] In some preferred examples, the analysis of the catalyst of the at least one test reactor is performed at a remote location by removing the test reactor from the reaction test module.

[0061] The reaction test module may be configured to allow real-time analysis of gases exiting the reaction chamber of the at least one test reactor during operation of the main reactor, and also to allow post-analysis of the catalyst by removing the test reactor from the reaction test module.

[0062] In some examples, analysis of the catalyst includes elemental analysis of the catalyst to identify accumulation of poisons on the catalyst.

[0063] In some preferred examples, the at least one test reactor includes a plurality of test reactors arranged in parallel, and analysis of the catalyst includes periodically removing successive test reactors to enable identification of trends in poison accumulation on the catalyst.

[0064] In some examples, the method also includes heating the at least one test reactor in a heating chamber.

[0065] According to the present description, the main reactor is a Fischer-Tropsch reactor containing a Fischer-Tropsch catalyst.

[0066] The present disclosure also provides a reaction test module, which is configured to be connected to a raw material source of a main reactor, and the reaction test module comprises:

[0067] i) an inlet configured to receive a feedstock gas from a feedstock source; and

[0068] ii) a plurality of test reactors in fluid communication with the inlet and arranged in parallel, each test reactor comprising a reaction chamber containing a catalyst.

[0069] In some preferred examples, the reaction testing module further includes an analyzer configured to determine catalytic activity levels of catalysts within the plurality of test reactors by analyzing gases exiting reaction chambers of the plurality of test reactors.

[0070] In some examples, the reaction testing module further includes a heating chamber housing the at least one test reactor.

[0071] The catalyst in each reaction chamber is a Fischer-Tropsch catalyst.

[0072] The present disclosure also provides a microreactor, which is configured to be removably inserted into a reaction test module, and has:

[0073] i) Less than 250cm 3 , optionally less than 200 cm 3 , optionally less than 150 cm 3 , optionally less than 100 cm 3 , optionally less than 50 cm 3 The reaction chamber volume; and / or

[0074] 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.

[0075] In some examples, the reaction chamber has a length of 30 cm to 120 cm and / or a diameter of 5 mm to 20 mm.

[0076] The catalyst in the reaction chamber is a Fischer-Tropsch catalyst.

[0077] In some examples, the reaction chamber of the microreactor is pre-loaded with catalyst and sealed before inserting the reaction test module. When the catalyst has an oxidized form that needs to be activated by reduction, it is preferred to activate the catalyst before pre-loading. This can make the side flow unit easier to operate, without the need to activate the catalyst on site, saving time and reducing equipment complexity.

[0078] Advantageously, these aspects of the present disclosure may allow for detection and / or analysis of catalyst contamination by poisons and impurities in the feed gas.

[0079] Where the system is configured to detect and / or analyse catalyst contamination by poisons and impurities, it is most preferred that the catalyst in the reaction chamber of the at least one test reactor is identical to the catalyst present in the reaction chamber of the main reactor, so as to ensure that there is an appropriate correspondence between the effect of the feed gas on the catalyst in the main reactor and the effect on the catalyst in the reaction test module.

[0080] A sudden decrease in catalyst activity within the at least one test reactor may, for example, be used as an indication of higher than expected levels of poisons or other contaminants in the feed gas.

[0081] Advantageously, since each of the test reactors may contain a much smaller weight / volume of catalyst than that present in the main reactor, a reduction in catalytic activity of a poisoning event may be detected more quickly than 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 such poisoning, and since an initial large volume of catalyst remains unpoisoned, the gas output from the main reactor may appear to be largely unaffected. When a reduction in the overall catalytic activity of the main reactor is detected, it may occur that a large amount of catalyst toward the inlet end will be poisoned and require replacement or regeneration.

[0082] The rapid response time of the catalyst in the at least one test reactor can also enable detection of transient periods of poisoning. During a transient event, the feed gas entering the main reactor can be diverted to a flare or shut down while still feeding the reactive test module so that it can be evaluated when the transient poisoning event has passed.

[0083] The reaction test module may be used as a warning sensor for the presence of poisons or other contaminants in the feed gas. Advantageously, the use of the reaction test module may allow for rapid intervention and thereby protect the larger volume of catalyst present in the reaction chamber of the main reactor.

[0084] Preferably, the initiation of corrective action may be automatic or semi-automatic, and may be initiated without human interaction. Alternatively, an alarm may be presented to an operator of the reactor (eg, via an audible and / or visual alarm), prompting them to initiate corrective action.

[0085] The use of the reaction test module can provide benefits during all operating stages of the main reactor. For example, monitoring of catalytic activity can be carried out in some or preferably all operating periods of the main reactor. The reaction test module can also be advantageously used during the trial operation phase, such as during the startup of the main reactor. For example, during startup, before the raw gas is sent to the main reactor, the raw gas can only be sent to the reaction test module for a period of time. Therefore, the reaction test module can be used to ensure that the raw gas is within the specification before the catalyst in the main reactor is exposed to the raw gas. For example, by confirming the expected performance of the catalyst in the test reactor, the catalyst in the main reactor is prevented from being damaged at the beginning of its life.

[0086] Additionally, a reaction testing module may be used to enable evaluation of new catalyst formulations under conditions that closely match those in the main reactor, but advantageously requiring only small volumes of catalyst and without requiring any changes to the main reactor.

[0087] For example, the system can be configured such that the catalyst in the reaction chamber of the 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. In this way, the test reactor can be used to evaluate or screen one or more new candidate catalysts for use in the method, and / or monitor and evaluate the vulnerability of one or more new candidate catalysts to potential poisoning events during "real world" conditions, which can produce more accurate and informative results compared to small-scale laboratory-based testing. Advantageously, using a reaction test module as a screening / testing aid can avoid the need to reconfigure the main reactor with a new catalyst, a process that is very expensive in terms of time and materials and only allows evaluation of one catalyst at a time.

[0088] In one mode of operation, the gas output from each of the at least one test reactor may be combined before being transmitted to 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 may be analyzed in a first time period, followed by the output from a second test reactor in a second time period, and so on.

[0089] Advantageously, providing a plurality of test reactors can enable the test reactors to be removed periodically during the operating duration of the main reactor. Analyzing the catalyst in the test reactors over time can allow a better understanding of the poison accumulation on the catalyst in the test reactors and the main reactor. Since the poisoning of the catalyst can be a slow process in some cases, the regular removal and analysis of the catalyst from the reaction test module can allow the trend of the poisoning to be established. Advantageously, the use of the reaction test module means that the main reactor can remain undisturbed and prevents the need to shut down the main reactor to remove a catalyst sample from the main reactor.

[0090] Additionally, the use and analysis of multiple test reactors may allow for increased statistical confidence that a catalyst poisoning event is occurring or has occurred.

[0091] The analysis may be performed near the main reactor, or the test reactor may be transported to another location for analysis.

[0092] For example, the types of poisons and pollutants accumulated on the catalyst can be identified by elemental analysis of the catalyst. Advantageously, analysis of the catalyst itself can overcome the difficulty of directly analyzing the poisons and pollutants at ppb levels in the raw gas. In addition, analysis of the catalyst can allow detection of poisons and pollutants in the raw gas that are not traditionally analyzed.

[0093] The parallel arrangement of the test reactors can be used to ensure that all test reactors present in a reaction test module are exposed to the same feed gas and for the same duration (or at least until the test reactors are optionally selectively removed for post-analysis). In addition, the parallel arrangement can allow one test reactor to be removed while the other test reactors remain operational.

[0094] In the present disclosure, the main reactor is a Fischer-Tropsch reactor containing a Fischer-Tropsch catalyst. Therefore, hereinafter, the present disclosure will be described by way of example with respect to a Fischer-Tropsch process and reactor. However, it should be understood that the systems, methods and apparatus of the present disclosure may be applied to other processes and reactors. In other examples, the main reactor may be configured for methanol synthesis, water-gas shift, etc.

[0095] The catalyst of the main reactor can be provided in different forms known in the art. For example, the catalyst can be provided as one or more catalyst beds. The bed can be a fluidized bed or a fixed bed or a combination thereof. For example, the main reactor can be a fluidized bed reactor or a fixed bed reactor. Alternatively, the catalyst can be contained in a plurality of catalyst carriers, which are received in the reactor tube of the main reactor. For example, the main reactor can be a tubular reactor. WO2011 / 048361, WO2012 / 136971, WO2016 / 050520 and WO2022064214A1 describe some examples of catalyst carriers configured for use in tubular reactors, which are incorporated herein by reference in their entirety. BRIEF DESCRIPTION OF THE DRAWINGS

[0096] Embodiments of the present disclosure will now be described, by way of example only, with reference to the accompanying drawings, in which:

[0097] Figure 1 is a diagram showing a first example of a chemical reactor system according to the present disclosure;

[0098] Figure 2is a diagram showing a second example of a chemical reactor system according to the present disclosure;

[0099] Figure 3 is a diagram showing a third example of a chemical reactor system according to the present disclosure; and

[0100] Figure 4 is a schematic diagram of a reaction test module of a third example. DETAILED DESCRIPTION

[0101] Figure 1 A schematic diagram of a first example of a chemical reactor system according to the present disclosure is shown. The system comprises a main reactor 10 and a reaction test module 20, both of which are supplied with raw material gas from a common raw material source 1.

[0102] The main reactor 10 includes a reaction chamber containing a catalyst, an inlet 11 for feeding a raw material gas from a raw material source 1 into the reaction chamber to contact the catalyst, and an output 12 for a reaction product produced by a reaction of the raw material gas in the presence of the catalyst in the reaction chamber.

[0103] Output 12 from main reactor 10 can be fed to one or more downstream modules (not shown), which are configured for further processing, recycling or use. For example, when reaction product leaves main reactor 10, it can include liquid phase and gas phase or be composed of liquid phase and gas phase, then cooled and separated into wax phase, liquid phase and gas phase in downstream. Wax phase can include heavier hydrocarbons, for example, with C10-C100 or larger chain length or higher hydrocarbons. Liquid phase can include lighter hydrocarbons and / or water fractions. Gas phase can be dry or have some residual moisture content.

[0104] The reaction test module 20 includes an inlet 21 configured to receive a raw material gas from the same raw material source 1 that supplies the raw material gas to the main reactor 10, and at least one test reactor in fluid communication with the inlet 21 and each including a reaction chamber containing a catalyst. The catalyst may be the same catalyst as that present in the reaction chamber of the main reactor 10 or a different catalyst.

[0105] The reaction test module 20 may have an output 22 for reaction products produced in the reaction chamber of the at least one test reactor.

[0106] Figure 2 A schematic diagram of a second example of a chemical reactor system according to the present disclosure is shown. This example is the same as the first example, except that the output 22 of the reaction test module 20 is fed back to merge with the feed from the output 12 of the main reactor at point 13. This can advantageously improve system efficiency by allowing a single set of modules (e.g., coolers, separators, etc.) to simplify downstream processing of the reaction products.

[0107] Figure 3 A schematic diagram of a third example of a chemical reactor system according to the present disclosure is shown. This example is similar to the previous example. The at least one test reactor is represented by reference numeral 23 and receives a feed gas from input 21. The reaction test module 20 also includes a separator 25 and an analyzer 26. The analyzer 26 may include a mass spectrometer or a gas chromatograph.

[0108] The separator 25 may be configured to obtain a gas fraction from the reactant products output from one or more test reactors 23 and transmit it to the analyzer 26. The separator 25 may include a device for cooling the reactant products and / or separating them into wax and / or liquid and / or gas fractions. For example, the separator 25 may include one or more knock-out pots. A first knock-out pot may be provided to remove the wax fraction and the heavier HC fraction. A subsequent second knock-out pot may be provided to remove the lighter HC fraction and / or water. Preferably, the gas fraction transmitted to the analyzer 26 includes dry gas.

[0109] The analyzer 26 may be configured to determine the catalytic activity level of the catalyst within the at least one test reactor 23 by analyzing the gas received from the separator 25. For example, the analyzer may be configured to determine the catalytic activity by calculating performance parameters such as CO conversion, methane selectivity, product selectivity, such as Cn, suitably C5+ selectivity, paraffin and olefin selectivity, and productivity, such as C 5+ productivity.

[0110] The system may also include a controller 40 configured to take corrective action when an alarm is generated by the reaction test module 20 (e.g., analyzer 26). Corrective action may include changing the composition of the raw gas, reducing the flow rate of the raw gas into the reaction chamber of the main reactor 10, or preventing the raw gas from being fed to the reaction chamber of the main reactor 10, such as by diverting to a flare or shutting off the feed completely. The controller 40 may also be configured to increase the temperature of one or more of the test reactors to maintain a target performance parameter so that the deactivation rate of the catalyst can be quantified. For example, the deactivation rate may be quantified based on the additional temperature required to maintain the carbon monoxide conversion at a target level.

[0111] like Figure 4 As schematically shown, the reaction test module 20 of the third example (or any of the other examples) may include a plurality of test reactors 23 arranged in parallel.

[0112] The example shown shows six test reactors 23 in parallel.

[0113] The test reactors 23 may be fed through a common inlet manifold 27. Isolation valves (not shown), such as solenoid valves, may be provided upstream of each test reactor 23 to allow the gas flow to each test reactor 23 to be selectively shut off, thereby allowing the test reactors 23 to be purged, maintained, and / or removed.

[0114] The output from each of the test reactors 23 may be fed into a common outlet manifold 28. A three-way valve 24 may be inserted between each of the test reactors 23 and the common outlet manifold 28. The three-way valve 24 may be used to selectively direct the gas exiting each test reactor 23 to either the common outlet manifold 28 or the output 22 of the reaction test module 20.

[0115] The common outlet manifold 28 may feed the separators 25 of the reaction testing modules 20 .

[0116] It may be possible to remove each of the test reactors 23 from the reaction testing module 20 while the remaining test reactors 23 remain in operation.

[0117] Each test reactor 23 may include a microreactor having:

[0118] i) Less than 250cm 3 , optionally less than 200 cm 3 , optionally less than 150 cm 3 , optionally less than 100 cm 3 , optionally less than 50 cm 3 The reaction chamber volume; and / or

[0119] 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.

[0120] The reaction testing module 20 may also 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.

[0121] The interior of the pipes of the chemical reactor system that are exposed to the feed gas may be coated with a protective coating to prevent toxic components from remaining on the surface of the pipes. The protective coating may be applied to the pipes upstream of the reaction test module 20 and to the internal pipes of the reaction test module 20. In some examples, a silicon coating may be applied where needed, particularly to any stainless steel pipes present. In one non-limiting example, a silicone coating from Bellefonte, PA, USA may be used. of coating.

[0122] In use, the reaction test module 20 can implement a method for detecting catalyst poisoning in the reaction chamber of the main reactor 10. The method includes:

[0123] a) operating a main reactor 10, which includes a reaction chamber containing a catalyst, by passing a raw material gas through the reaction chamber to contact the catalyst so as to produce a reaction product by a reaction of the raw material gas in the presence of the catalyst;

[0124] b) simultaneously operating the reaction test modules 20 by: passing the feed gas through the test reactors 23, each test reactor 23 including a reaction chamber containing a catalyst; and

[0125] c) using analyzer 26 to determine the catalytic activity level of the catalyst within test reactor 23 by analyzing the gases leaving or originating from the reaction chamber of test reactor 23 and / or analyzing the catalyst of test reactor 23 .

[0126] Analysis of the gases exiting or originating from the reaction chamber of the test reactor 23 may be performed in real time during operation of the main reactor 10 .

[0127] Gases exiting or originating from the reaction chamber of the test reactor 23 may be dried and / or cooled by a separator 25 before being passed to an analyzer 26 (eg, a mass spectrometer or a gas chromatograph).

[0128] The controller 40 may generate an alarm upon detecting a decrease in the catalytic activity level of the catalyst within the test reactor 23, which indicates poisoning of the catalyst within the test reactor 23. This may be used as an analog for detecting poisoning of the catalyst of the main reactor 10.

[0129] Detecting or generating an alarm may prompt corrective action, such as changing the composition of the feed gas, reducing the flow rate of the feed gas into the reaction chamber of the main reactor 10, or preventing the feed gas from being fed into the reaction chamber of the main reactor 10.

[0130] Additionally or alternatively, the reaction testing module 20 may enable analysis of the catalyst of the test reactor 23 to be performed at a remote location by removing the test reactor 23 from the reaction testing module 20 .

[0131] Analysis of the catalyst may include elemental analysis of the catalyst to identify accumulation of poisons on the catalyst.

[0132] The test reactors 23 can be arranged in parallel, and selected test reactors 23 can be removed periodically to enable identification of trends in poison accumulation on the catalyst. For example, the test reactors 23 can be removed, for example, once a month to allow analysis of trends over a 6 month period. The time period between removals can be selected as desired. Replacement test reactors 23 can be inserted into the reaction test module 20 to replace those that were removed.

[0133] Other aspects of the disclosure are set out in the following clauses:

[0134] Clause 1. A chemical reactor system comprising:

[0135] a) a main reactor, the main reactor comprising:

[0136] i) a reaction chamber, said reaction chamber containing a catalyst,

[0137] ii) an inlet for feeding a feedstock gas from a feedstock source into the reaction chamber to contact the catalyst, and

[0138] iii) an output portion for a reaction product produced by a reaction of the raw material gas in the presence of the catalyst in the reaction chamber;

[0139] and

[0140] b) a reaction test module, the reaction test module comprising:

[0141] i) an inlet configured to receive a feed gas from the same feed source that supplies the feed gas to the main reactor, and

[0142] ii) at least one test reactor in fluid communication with the inlet and each comprising a reaction chamber containing a catalyst.

[0143] Clause 2. The chemical reactor system according to clause 1, wherein the reaction testing module further comprises:

[0144] iii) an analyzer configured to determine a catalytic activity level of the catalyst within the at least one test reactor by analyzing gases exiting or originating from the reaction chamber of the at least one test reactor.

[0145] Clause 3. The chemical reactor system of clause 2, wherein the analyzer comprises a mass spectrometer or a gas chromatograph.

[0146] Clause 4. A chemical reactor system according to clause 2 or clause 3, wherein the analyzer is configured to generate an alarm upon detecting a decrease in the catalytic activity level of the catalyst within the at least one test reactor, the alarm indicating that the catalyst within the at least one test reactor is poisoned.

[0147] Clause 5. The chemical reactor system of Clause 4, wherein the chemical reactor system further comprises a controller configured to take corrective action when the analyzer generates the alarm.

[0148] Item 6. A chemical reactor system according to Item 5, wherein the corrective action includes changing the composition of the raw gas, reducing the flow rate of the raw gas into the reaction chamber of the main reactor, or preventing the raw gas from being fed into the reaction chamber of the main reactor.

[0149] Clause 7. A chemical reactor system according to any preceding clause, wherein the reaction testing module further comprises a separator for separating liquid and gas leaving the reaction chamber of the at least one test reactor into one or more wax and / or liquid and / or gas fractions.

[0150] Clause 8. The chemical reactor system of Clause 7, wherein the wax and liquid fraction is separated into a first product stream comprising a wax product and a second product stream comprising a light hydrocarbon product and water.

[0151] Clause 9. A chemical reactor system according to any preceding clause, 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.

[0152] Clause 10. A chemical reactor system according to any one of clauses 1 to 8, 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.

[0153] Clause 11. The chemical reactor system of any preceding clause, wherein the at least one test reactor comprises a plurality of test reactors arranged in parallel.

[0154] Clause 12. The chemical reactor system of Clause 11, wherein each of the plurality of test reactors is removable from the reaction testing module while remaining test reactors of the plurality of test reactors remain in operation.

[0155] 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.

[0156] Clause 14. A chemical reactor system according to any preceding clause, wherein each of the at least one test reactor comprises a microreactor having:

[0157] i) Less than 250cm 3 , optionally less than 200 cm 3 , optionally less than 150 cm 3 , optionally less than 100 cm 3 , optionally less than 50 cm 3 The reaction chamber volume; and / or

[0158] 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.

[0159] Clause 15. The chemical reactor system of any preceding clause, wherein the reaction testing module further comprises a heating chamber housing the at least one test reactor.

[0160] Clause 16. A chemical reactor system according to any preceding clause, wherein the reaction testing module is configured as a side stream cell arranged in parallel with a gas flow path through the main reactor.

[0161] Item 17. The chemical reactor system according to any of the preceding items further includes a diverter downstream of the raw material source and upstream of the main reactor, wherein the diverter receives the raw material gas from the raw material source; the diverter includes a first outlet for feeding the reaction chamber of the main reactor and a second outlet for feeding the at least one test reactor of the reaction test module.

[0162] Item 18. A chemical reactor system according to any of the preceding items, wherein the reaction testing module is configured to combine gas leaving the reaction testing module with gas leaving the main reactor at a point downstream of the reaction chamber of the main reactor so that the gas passing through the reaction testing module at least bypasses the reaction chamber of the main reactor.

[0163] Clause 19. A chemical reactor system according to any preceding clause, wherein the primary reactor is a Fischer-Tropsch reactor containing a Fischer-Tropsch catalyst.

[0164] Clause 20. A method for detecting catalyst poisoning in a reaction chamber, the method comprising:

[0165] a) operating a main reactor, the main reactor comprising the reaction chamber containing the catalyst, by passing a raw material gas through the reaction chamber to contact the catalyst so as to produce a reaction product by reaction of the raw material gas in the presence of the catalyst;

[0166] b) simultaneously operating a reaction test module by passing a feed gas through at least one test reactor of the reaction test module, each test reactor comprising a reaction chamber containing a catalyst; and

[0167] c) using an analyzer, determining a catalytic activity level of the catalyst within the at least one test reactor by analyzing gases exiting or originating from the reaction chamber of the at least one test reactor and / or analyzing the catalyst of the at least one test reactor.

[0168] Clause 21. The method according to Clause 20, wherein the raw material gas fed to the reaction chamber of the main reactor and the raw material gas fed to the at least one test reactor of the reaction test module are from the same raw material source.

[0169] Clause 22. The method of clause 21, wherein a gas stream from the feedstock source is separated into a first stream that feeds the reaction chamber of the main reactor and a second stream that feeds the at least one test reactor of the reaction test module.

[0170] Clause 23. The method according to any one of clauses 20 to 22, wherein during operation of the main reactor, gases leaving or originating from the reaction chamber of the at least one test reactor are analyzed in real time.

[0171] Clause 24. The method according to any one of clauses 20 to 23, wherein the gases leaving or originating from the reaction chamber of the at least one test reactor are analyzed by a mass spectrometer or a gas chromatograph.

[0172] Clause 25. The method according to any one of clauses 20 to 24, wherein the gas leaving or originating from the reaction chamber of the at least one test reactor is dried and / or cooled before being conveyed to the mass spectrometer or gas chromatograph.

[0173] Clause 26. The method of any one of Clauses 20 to 25, further comprising generating an alarm upon detecting a decrease in the catalytic activity level of the catalyst within the at least one test reactor, the alarm indicating that the catalyst within the at least one test reactor is poisoned.

[0174] Clause 27. The method of clause 26, further comprising taking corrective action when the analyzer generates the alarm.

[0175] Clause 28. A method according to Clause 27, wherein the corrective action includes changing the composition of the raw gas, reducing the flow rate of the raw gas into the reaction chamber of the main reactor, or preventing the raw gas from being fed into the reaction chamber of the main reactor.

[0176] Clause 29. The method according to any one of Clauses 20 to 28, wherein the catalyst in the reaction chamber of the at least one test reactor is the same as the catalyst present in the reaction chamber of the main reactor.

[0177] Clause 30. The method according to any one of Clauses 20 to 28, 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.

[0178] Clause 31. The method according to any one of Clauses 20 to 30, wherein the at least one test reactor comprises a plurality of test reactors arranged in parallel.

[0179] Clause 32. The method of any one of Clauses 20 to 31, wherein the analysis of the catalyst of the at least one test reactor is performed at a remote location by removing the test reactor from the reaction testing module.

[0180] Clause 33. The method of Clause 32, wherein the analysis of the catalyst comprises elemental analysis of the catalyst to identify accumulation of poisons on the catalyst.

[0181] 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 the analysis of the catalyst comprises periodically removing successive test reactors to enable identification of trends in poison accumulation on the catalyst.

[0182] Clause 35. The method of any one of Clauses 20 to 34, further comprising heating the at least one test reactor in a heating chamber.

[0183] Clause 36. The method according to any one of clauses 20 to 35, wherein the main reactor is a Fischer-Tropsch reactor containing a Fischer-Tropsch catalyst.

[0184] Clause 37. A reaction test module, the reaction test module being configured to be connected to a source of raw materials of a main reactor, the reaction test module comprising:

[0185] i) an inlet configured to receive a feedstock gas from the feedstock source; and

[0186] ii) a plurality of test reactors in fluid communication with the inlet and arranged in parallel, each test reactor comprising a reaction chamber containing a catalyst.

[0187] Clause 38. The reaction testing module of Clause 37, further comprising an analyzer configured to determine a catalytic activity level of the catalyst within the plurality of test reactors by analyzing gases exiting the reaction chambers of the plurality of test reactors.

[0188] Clause 39. The reaction testing module according to Clause 37 or Clause 38, wherein the reaction testing module further comprises a heating chamber housing the at least one test reactor.

[0189] Clause 40. A reaction test module according to any one of clauses 37 to 39, wherein the catalyst in each of the reaction chambers is a Fischer-Tropsch catalyst.

[0190] Clause 41. A microreactor configured to be removably inserted into a reaction test module, the microreactor comprising:

[0191] i) Less than 250cm 3 , optionally less than 200 cm 3 , optionally less than 150 cm 3 , optionally less than 100 cm 3 , optionally less than 50 cm 3 The reaction chamber volume; and / or

[0192] 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.

[0193] Item 42. The microreactor of Item 41, wherein the reaction chamber has a length of 30 cm to 120 cm and / or a diameter of 5 mm to 20 mm.

[0194] Clause 43. The microreactor of Clause 41 or Clause 42, wherein the catalyst in the reaction chamber is a Fischer-Tropsch catalyst.

[0195] Clause 44. The microreactor according to any one of clauses 41 to 43, wherein the reaction chamber of the microreactor is pre-loaded with the catalyst and sealed before the reaction test module is inserted.

Claims

1. A chemical reactor system, comprising: a) a main reactor, the main reactor comprising: i) a reaction chamber, said reaction chamber containing a catalyst, ii) an inlet for feeding a feed gas from a feed source into the reaction chamber to contact the catalyst, and iii) an output portion for outputting a reaction product produced by a reaction of the raw material gas in the presence of the catalyst in the reaction chamber; and b) a reaction test module, the reaction test module comprising: i) an inlet configured to receive a feed gas from the same feed source that supplies the feed gas to the main reactor, and ii) at least one test reactor in fluid communication with the inlet and each comprising a reaction chamber containing a catalyst, The main reactor is a Fischer-Tropsch reactor containing a Fischer-Tropsch catalyst.

2. The chemical reactor system according to claim 1, wherein the reaction test module further comprises: iii) an analyzer configured to determine a catalytic activity level of the catalyst within the at least one test reactor by analyzing gases exiting or originating from the reaction chamber of the at least one test reactor.

3. The chemical reactor system of claim 2, wherein the analyzer is configured to generate an alarm upon detecting a decrease in the catalytic activity level of the catalyst within the at least one test reactor, the alarm indicating that the catalyst within the at least one test reactor is poisoned.

4. The chemical reactor system of claim 3, wherein the chemical reactor system further comprises a controller configured to take corrective action when the analyzer generates the alarm; And optionally, wherein the corrective action includes changing the composition of the raw gas, reducing the flow rate of the raw gas into the reaction chamber of the main reactor, or preventing the raw gas from being fed into the reaction chamber of the main reactor.

5. A chemical reactor system according to any preceding claim, 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. The chemical reactor system of any one of claims 1 to 4, 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. A chemical reactor system according to any preceding claim, wherein the at least one test reactor comprises a plurality of test reactors arranged in parallel.

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

9. The chemical reactor system of any preceding claim, wherein each of the at least one test reactor comprises a microreactor having: i) Less than 250cm 3 , optionally less than 200 cm 3 , optionally less than 150 cm 3 , optionally less than 100 cm 3 , optionally less than 50 cm 3 The reaction chamber volume; and / or 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 cm to 120 cm and / or a reaction chamber diameter of 5 mm to 20 mm.

10. A chemical reactor system according to any preceding claim, wherein the reaction testing module further comprises a heating chamber housing the at least one test reactor.

11. A method for detecting catalyst poisoning in a reaction chamber, the method comprising: a) operating a main reactor, said main reactor comprising said reaction chamber containing said catalyst, by passing a feed gas through said reaction chamber to contact said catalyst, so as to produce a reaction product by reaction of the feed gas in the presence of the catalyst; b) simultaneously operating a reaction test module by passing a feed gas through at least one test reactor of the reaction test module, each test reactor comprising a reaction chamber containing a catalyst; as well as c) using an analyzer to determine the catalytic activity level of the catalyst within the at least one test reactor by analyzing gases leaving or originating from the reaction chamber of the at least one test reactor and / or analyzing the catalyst of the at least one test reactor, The main reactor is a Fischer-Tropsch reactor containing a Fischer-Tropsch catalyst.

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

13. A method according to claim 11 or claim 12, wherein during operation of the main reactor, gases leaving or originating from the reaction chamber of the at least one test reactor are analysed in real time.

14. The method of any one of claims 11 to 13, further comprising generating an alarm upon detecting a decrease in the catalytic activity level of the catalyst within the at least one test reactor, the alarm indicating that the catalyst within the at least one test reactor is poisoned.

15. The method of claim 14, further comprising taking corrective action when said analyzer generates said alarm; And optionally, wherein the corrective action includes changing the composition of the raw gas, reducing the flow rate of the raw gas into the reaction chamber of the main reactor, or preventing the raw gas from being fed into the reaction chamber of the main reactor.

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

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

18. The method of claim 17, wherein the analysis of the catalyst comprises elemental analysis of the catalyst to identify accumulation of poisons on the catalyst.

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 the analysis of the catalyst comprises periodically removing successive test reactors to enable identification of trends in poison accumulation on the catalyst.

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