Abstract:
The present disclosure may include a device for testing catalysts, and a method for controlling the flow rate and temperature parameters during the process. The device may separate mass flow control through heating elements from the mass flow through the sample, as well as separate banks for mixing oxidizing elements, carbon dioxide, and diluent gas as well as reducing agents, nitric oxide, and diluent gas. The device disclosed here may also use mass control units of a sufficiently high speed so as to allow the desired testing conditions.

Description:
CROSS-REFERENCE TO RELATED APPLICATIONS 
       [0001]    N/A 
       BACKGROUND 
       [0002]    1. Field of the disclosure 
         [0003]    The present disclosure relates to a laboratory test device and, more particularly, to a device for testing catalysts under dynamic conditions. 
         [0004]    2. Background Information 
         [0005]    Catalysts may need to be tested to evaluate their performance and their response to parameter changes. Devices of use in testing catalysts may include one or more combustion engines; however, the use of these engines may be expensive, require higher maintenance than desired, and be more time consuming. Additionally, the use of these engines may not allow individual parameter variations or calibrations of use when testing catalysts. Other test devices suitable for testing catalysts may include Laboratory Scale Reactors, commonly referred to as Test Benches, and may allow a greater control over the testing conditions of the catalyst. 
         [0006]    However, Laboratory-scale reactors may not capture the catalyst&#39;s response to dynamic changes in one or more of multiple variables, including temperature, space-velocity, and reactant gas concentration. This may be of great relevance to catalyst applications where the performance of the catalyst may be judged as a sum of its performance in one or more sequence of events, where the events may have varying space velocities, temperatures and gas systems. 
         [0007]    As such, there is a continuing need for test devices able to evaluate the performance of catalysts under a variety of dynamic conditions. 
       SUMMARY 
       [0008]    The present disclosure may include a device for testing catalysts, and a method for controlling the flow rate and temperature parameters during the process. 
         [0009]    The method may include isolating the load perceived by the heating elements from the loading perceived by the catalyst being tested, where excess gas may undergo any suitable venting, including venting over a catalyst holder, venting to a confined environment, venting to the general environment, or any suitable combination. This may allow the space-velocity of gas processed by the heater to vary from the space-velocity of the gas flowing through the sample. 
         [0010]    The unit that may control the flow of gas through the catalyst sample may include one or more suitable mass controllers, where the mass controllers may be heated above the dew-point that may be associated with the water vapor concentration. Where a plurality of mass controllers may be used, the mass controllers may be placed in parallel. Suitable mass controllers of use in controlling the flow through the heater and controlling the gas composition may be of a suitably high speed, including mass controllers able to change flow from about 10% flow potential to about 90% of flow potential in less than one second. Mass flow controllers of use may include mass controllers able to make the change in 0.1 seconds. 
         [0011]    The method may also include using separate banks of mass flow controllers for mixing the gas composition to the desired composition and for controlling the flow of the gas composition through the heater. A separate bank may be used for controlling any suitable mix of reducing agents, nitric oxide, and diluent gas; while another separate bank may be used for controlling any suitable mix of oxidizing gases, carbon dioxide, and diluent gas. The flow of gas through each bank may be controlled so as to result in any suitable gas composition, including embodiments where the amount of gas flowing through each bank may be controlled to be about half of the flow, where the amount of gas flowing through each bank may be regulated by regulating the amount of diluent gas flowing through each bank. Embodiments where each of the banks may contribute about half of the flow may allow the events that may be generated in each of the banks to reach the catalyst sample at about the same time. 
         [0012]    Numerous other aspects, features and advantages of the present disclosure may be made apparent from the following detailed description, taken together with the drawing figures. 
     
    
     
       BRIEF DESCRIPTION OF THE DRAWINGS 
         [0013]    These and further features, aspects and advantages of the embodiments of the present disclosure will be apparent with regard to the following description, appended claims and accompanying drawings where: 
           [0014]      FIG. 1  illustrates a flow chart for the testing process in a test bench reactor. 
           [0015]      FIG. 2  illustrates a Gas Feed System. 
           [0016]      FIG. 3  illustrates a Test Gas Generator. 
           [0017]      FIG. 4  illustrates a Sample Tester. 
           [0018]      FIG. 5  illustrates a Test Bench. 
       
    
    
       [0019]    It should be understood that these drawings are not necessarily to scale and they can illustrate a simplified representation of the features of the embodiments of the disclosure. 
       DETAILED DESCRIPTION 
     Definitions 
       [0020]    As used here, the following terms have the following definitions: 
         [0021]    Mass flow controller (MFC) refers to any computer controlled analog or digital device of use in controlling the flow rate of fluids and/or gases. 
         [0022]    Temperature controller refers to any device of use in controlling temperature in a process. 
         [0023]    Laboratory Scale Reactor/Test Bench refers to any apparatus suitable for testing a material with a test gas. 
         [0024]    Oxidizing agent refers to any substance that may take electrons from another substance in a redox chemical reaction. 
         [0025]    Reducing agents refers to any substance that may give electrons to another substance in a redox chemical reaction. 
         [0026]    Gas mixture refers to the mixture obtained from combining oxidizing agents, reducing agents, inert gases, or any other suitable gases. 
         [0027]    Water-gas mixture refers to the mixture obtained from combining water vapor with a gas mixture. 
         [0028]    Test Gas refers to any gas mixture of use in chemically testing an interaction between it and one or more materials. 
         [0029]    Catalyst refers to one or more materials that may be of use in the conversion of one or more other materials. 
       Description 
       [0030]    The description of the drawings, as follows, illustrates the general principles of the present disclosure with reference to various alternatives and embodiments. The present disclosure may, however, be embodied in different forms and should not be limited to the embodiments here referred. Suitable embodiments for other applications will be apparent to those skilled in the art. 
         [0031]      FIG. 1  is a flowchart for a method of testing a material in a Laboratory Scale Reactor. Testing Process  100  may include the preparation of Oxidizing Component Mixture  102  and may include the preparation of Reducing Component Mixture  104 . Oxidizing Component Mixture  102  and Reducing Component Mixture  104  may then be mixed and may form Full Component Mixture  106 , which may then undergo Preheating  108 . Full Component Mixture  106  may then undergo Water Vapor Addition  110 , where Full Component Mixture  106  may then undergo Heating  112 . A portion of Full Component Mixture  106  may then undergo Catalyst Sample Treatment  114 , where any portion not undergoing Catalyst Sample Treatment  114  may undergo venting in Vent  116 . A portion of Full Component Mixture  106  having undergone Catalyst Sample Treatment  114  may then be analyzed in any suitable Untreated Analysis  118 . Another portion may undergo Analysis Pretreatment  120  previous to undergoing Analysis  122 . Any portion not undergoing analysis may be vented in Vent  124 , as well as any portion having already undergone Untreated Analysis  118  or Analysis  122 . 
         [0032]      FIG. 2  shows Gas Feed System  200 . Gas Feed System  200  may include Gas Source  202 , Control Valve  204 , Pressure Regulator  206 , one or more Mass Flow Controllers  208 , and one or more Output Lines  210 . 
         [0033]    Gas Source  202  may be any source suitable for delivering any suitable gas to the system, including any tank or line able to provide N2, C3H6, C3H8, H2, CO, NO, NO2, CO2, SO2 or any suitable combination thereof at any suitable concentration. 
         [0034]    Control Valve  204  may be any valve suitable for restricting or allowing flow from Gas Source  202 , including solenoid valves, hydraulic valves, pneumatic valves, or any suitable combination. 
         [0035]    Pressure Regulator  206  may be any device suitable for regulating the pressure of gas in Gas Feed System  200 , including devices including any suitable pressure gauge or pressure transducer as well as any suitable valve, including solenoid valves, hydraulic valves, pneumatic valves, or any suitable combination. 
         [0036]    Mass Flow Controllers  208  may be any mass controller or series of mass controllers suitable for controlling the flow of gas from Gas Source  202  to one or more Output Lines  210  at a suitable frequency, including frequencies in the range of 1 to 25 Hz. Suitable Mass Flow Controllers  208  may include mass flow controllers able to provide any suitable flow rate, including flow rates between 100 cubic centimeters per minute to 60000 cubic centimeters. 
         [0037]      FIG. 3  shows Test Gas Generator  300 , having Oxidizing Components Branch  302 , Reducing Components Branch  304 , Evaporation Block  306 , Pump  308 , Water Reservoir  310 , Heater  312 , Temperature Controller  314 , and Output  316 . 
         [0038]    Oxidizing Components Branch  302  may include any number of suitable Gas Feed Systems  200 , where the included Gas Feed Systems  200  may provide any number of oxidizing gases, dilutants, and combinations thereof, including N2, O2, and CO2. 
         [0039]    Reducing Components Branch  304  may include any number of suitable Gas Feed Systems  200 , where the included Gas Feed Systems  200  may provide any number of reducing gases, dilutants, and combinations thereof, including N2, H2, CO, NO, and any suitable hydrocarbons. Suitable Hydrocarbons may include C3H8. Suitable heavy hydrocarbons may also be added using any suitable method, including liquid injection and evaporation. Suitable heavy hydrocarbons may include decane, tolune, and dodecane. 
         [0040]    The flow of the mixture of gases generated by Oxidizing Components Branch  302  and Reducing Components Branch  304  may then be preheated by any suitable means, including heated lines, where the heated lines may be heated using heat jackets. Suitable temperatures may include temperatures in the range of 130° C. to 180° C., including 150° C. 
         [0041]    Evaporation Block  306  may be any device suitable for evaporating water and adding it to the flow of gas generated by the combination of gas flows from Oxidizing Components Branch  302  and Reducing Components Branch  304  in Test Gas Generator  300 . Evaporation Block  306  may evaporate water which may be provided by Pump  308 , where Pump  308  may be any pump suitable for pumping water from Water Reservoir  310  to Evaporation Block  306 . Suitable temperatures in Evaporation Block  306  may include temperatures in the range of 110° C. to 150° C., including 130° C. 
         [0042]    The gas flowing out of Evaporation Block  306  may then be heated by Heater  312 , where Heater  312  may be any suitable heating device, including serpentine heaters. Heater  312  may be controlled by Temperature Controller  314 , which may be any suitable temperature controller, including thermocouples and thermistors. 
         [0043]    The resulting test gas exits Test Gas Generator  300  through Output  316 . 
         [0044]      FIG. 4  shows Sample Tester  400 , including Catalyst Sample  402  on Catalyst Holder  404 , Heated Block  406 , Pump  408 , Cooling Liquid Reservoir  410 , Radiator  412 , FID Unit  414 , Cooling Bath  416 , Chiller Unit  418 , Gas Analyzer  420 , Water Reservoir  422 , Vacuum  424 , Calibration Gas  426 , Filter  428 , Heated Mass Flow Controller  430 , Radiator  432 , Control Valve  434 , Water Reservoir  436 , Control Valve  438 , and Purge Valves  440 . 
         [0045]    Catalyst Sample  402  may be any material suitable for testing with test gas delivered by Output  316 , placed on any suitable Catalyst Holder  404 . Catalyst Sample  402  may interact with any suitable portion of test gas delivered by Output  316 , where any portion not of test gas delivered by Output  316  may undergo any suitable venting, including venting through Catalyst Holder  404  and venting to the environment. 
         [0046]    The temperature of test gas treated by Catalyst Sample  402  may then be controlled by Heated Block  406 , where Heated Block  406  uses cooling liquid provided by Pump  408  from Cooling Liquid Reservoir  410 . Cooling liquid in Cooling Liquid Reservoir  410  may be any suitable cooling liquid, including water, ethylene glycol, propylene glycol, or any suitable combination thereof. Cooling liquid exiting Heated Block  406  may then be cooled by Radiator  412 . 
         [0047]    A suitable portion of test gas exiting Heated Block  406  may then flow through heated lines to FID Unit  414 , where FID unit  414  may be any suitable Flame Ionization Detector device. 
         [0048]    Another suitable portion of test gas exiting Heated Block  406  may be cooled to a suitable temperate in Cooling Bath  416 . Cooling Bath  416  allows the test gas to be cooled to a temperature suitable for condensing the water vapor content in the incoming test gas, and is kept at a suitable temperature using Chiller Unit  418 , where Chiller Unit  418  may be any suitable chilling device. Dry test gas exiting Cooling Bath  416  may then be analyzed by one or more suitable Gas Analyzers  420 . Moisture condensed in Cooling Bath  416  may flow into Water Reservoir  422 , where the moisture may then exit to Vacuum  424  or be purged by Purge Valve  440 . 
         [0049]    Another suitable portion of test gas exiting Heated Block  406  may then flow through one or more suitable Filters  428 . The flow of gas may be controlled by one or more suitable Heated Mass Flow Controllers  430 , where Heated Mass Flow Controllers  430  may provide a suitable flow rate, including rates between 0 to 100 liters per minute. Test gas flowing through Heated Mass Flow Controllers  430  may then be cooled in Radiator  432 , where it may then flow through control Valve  434 . Control Valve  434  may be any valve suitable for restricting or allowing flow from Heated Mass Flow Controllers  430 , including solenoid valves, hydraulic valves, pneumatic valves, or any suitable combination. 
         [0050]    During calibration of one or more of FID Unit  414  and/or Gas Analyzers  420 , Heated Mass Flow Controllers  430  may be set to a suitably low flow value, including zero. Calibration Gas  426  may then flow to FID Unit  414  and through Cooling Bath  416  to Gas Analyzers  420 , and may also flow through Catalyst Sample  402  in a direction which may be contrary to that of flow in normal operating conditions. 
         [0051]    Test gas exiting Control Valve  434  may then flow into Water Reservoir  436 , where it may then flow through Control Valve  438  into Vacuum  424 , or may be purged intermittently along with the water when Water Reservoir  436  is emptied. 
         [0052]    Control Valve  438  may be any valve suitable for restricting or allowing flow from Water Reservoir  436 , including solenoid valves, hydraulic valves, pneumatic valves, or any suitable combination. 
         [0053]    One or more Purge Valves  440  may be used to purge Water Reservoir  422  and/or Water Reservoir  436 , where suitable valves may include solenoid valves, hydraulic valves, pneumatic valves, manually activated valves, or any suitable combination. 
         [0054]      FIG. 5  show Test Bench  500 , including Test Gas Generator  300  and Sample Tester  400 .