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CN107941986B - Device for evaluating catalytic performance of catalyst - Google Patents

Device for evaluating catalytic performance of catalyst Download PDF

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CN107941986B
CN107941986B CN201710979952.6A CN201710979952A CN107941986B CN 107941986 B CN107941986 B CN 107941986B CN 201710979952 A CN201710979952 A CN 201710979952A CN 107941986 B CN107941986 B CN 107941986B
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pipeline
gas
catalyst
hydrocarbon fuel
valve
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CN107941986A (en
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郭永胜
方文军
程欣欣
刘朝山
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Zhejiang University ZJU
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/10Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using catalysis
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/12Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using combustion
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004Gaseous mixtures, e.g. polluted air
    • G01N33/0009General constructional details of gas analysers, e.g. portable test equipment
    • G01N33/0027General constructional details of gas analysers, e.g. portable test equipment concerning the detector
    • G01N33/0036General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
    • G01N33/004CO or CO2

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Abstract

本发明涉及一种用于评价催化剂催化性能的装置,包括依次通过管路连接的配气装置、碳氢燃料鼓泡装置、放置待测催化剂的管式炉和尾气检测装置;所述碳氢燃料鼓泡装置与管式炉通过混合气管路连接,所述混合气管路上设有第一截止阀;所述管式炉进出口两端管路上并联设有辅助测试管路,所述辅助测试管路上设有第二截止阀,且所述辅助测试管路的进口端设置在第一截止阀与碳氢燃料鼓泡装置之间。该装置能够简便、高效地评价催化剂对于碳氢燃料的催化燃烧性能,从而有助于选择不同碳氢燃料的最优催化剂。

Figure 201710979952

The invention relates to a device for evaluating the catalytic performance of a catalyst, comprising a gas distribution device, a hydrocarbon fuel bubbling device, a tube furnace for placing a catalyst to be tested, and an exhaust gas detection device connected in sequence through pipelines; the hydrocarbon fuel The bubbling device and the tube furnace are connected by a mixed gas pipeline, and the mixed gas pipeline is provided with a first shut-off valve; the pipelines at both ends of the inlet and outlet of the tube furnace are provided with auxiliary test pipelines in parallel, and the auxiliary test pipelines are connected in parallel with each other. A second shut-off valve is provided, and the inlet end of the auxiliary test pipeline is arranged between the first shut-off valve and the hydrocarbon fuel bubbling device. The device can simply and efficiently evaluate the catalytic combustion performance of the catalyst for hydrocarbon fuels, thereby helping to select the optimal catalyst for different hydrocarbon fuels.

Figure 201710979952

Description

Device for evaluating catalytic performance of catalyst
Technical Field
The invention relates to the field of catalytic combustion of hydrocarbon fuels, in particular to a device for evaluating catalytic performance of a catalyst.
Background
Explosion of fuel tanks is one of the main factors threatening the safety of aerospace, so that a fuel tank inerting system for reducing the flammability of the fuel tanks is always a research hotspot for the safety of airplanes. An airborne inert gas production system (OBIGGS for short) based on an air separator becomes an inerting system which is widely applied to airplanes at home and abroad at present because the oxygen content in the space of an oil tank can be effectively reduced and the safety of the oil tank can be ensured.
However, the OBIGGS system also has certain limitations in the application process, such as certain influence on the performance of the aircraft engine, additional increase in the weight of the aircraft, high price of components, and the like. A green airborne inert gas production system (called GOBIGGS for short) developed on the basis of an OBIGGS system is an economical, efficient and environment-friendly novel fuel oil deoxygenation system in a test stage.
The main working principle of the GOBIGGS system is as follows: the fuel oil and the inert gas are fully mixed through the gas contactor, so that dissolved oxygen in the fuel oil escapes, and then the oil-water separator separates the fuel oil from the gas, so that the aim of removing oxygen is fulfilled. Introducing the separated mixed gas containing oxygen, inert gas and fuel steam into a reaction chamber containing a catalyst to enable the oxygen and the fuel steam to perform catalytic combustion reaction. The water produced by the reaction is filtered off by a condensation system, and the carbon dioxide is compressed and used as inert gas to continuously participate in the oxygen removal reaction. The system has the advantages of low power consumption, compact structure, light weight and the like on the basis of effectively ensuring the safety of the fuel tank.
The catalytic gas combustion unit is one of the core components of the GOBIGGS, and the performance of the catalyst is directly related to the inerting effect of the whole system on the oil tank. Due to the fact that the variety of catalysts capable of being used for catalytic combustion of hydrocarbon fuel is large, and the research on catalytic combustion of hydrocarbon fuel is few at present, the development of a performance evaluation device of the hydrocarbon fuel combustion catalyst is of great significance to the development of a novel oil tank inerting technology.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a device for evaluating the catalytic performance of a catalyst, which can simply, conveniently and efficiently evaluate the catalytic combustion performance of the catalyst on hydrocarbon fuel, thereby being beneficial to selecting the optimal catalyst of different hydrocarbon fuels.
The technical scheme provided by the invention is as follows:
a device for evaluating catalytic performance of a catalyst comprises a gas distribution device, a hydrocarbon fuel bubbling device, a tubular furnace for placing the catalyst to be detected and a tail gas detection device which are sequentially connected through pipelines;
the hydrocarbon fuel bubbling device is connected with the tube furnace through a mixed gas pipeline, and a first stop valve is arranged on the mixed gas pipeline; and the pipelines at the inlet and the outlet of the tubular furnace are provided with auxiliary test pipelines in parallel, the auxiliary test pipelines are provided with second stop valves, and the inlet ends of the auxiliary test pipelines are arranged between the first stop valves and the hydrocarbon fuel bubbling device.
In the above technical solution, the provided device can be used for evaluating the catalytic effect of the catalyst on various hydrocarbon fuels, and the hydrocarbon fuels can include model fuels such as n-dodecane, n-tridecane, n-tetradecane, decalin, cyclohexane, ethylcyclohexane, methylcyclohexane, and the like.
In addition, because the auxiliary test pipeline is arranged, the condition of the device passage is measured by closing the first stop valve and opening the second stop valve, and the composition of the raw material gas is measured at any time.
Preferably, the tubular furnace is an OTF-1200X-II tubular furnace, the length of the quartz reaction tube is 500-800mm, the inner diameter is 6-12mm, and the catalyst is fixed in the middle of the quartz reaction tube through quartz wool. The tubular furnace can accurately control the catalytic combustion temperature within the range of 10-800 ℃, and the detection result has guiding significance for the actual application of each catalyst.
Preferably, the gas distribution device is a gas-carrying steel cylinder and is connected with the hydrocarbon fuel bubbling device through a gas-carrying pipeline. The carrier gas cylinder may be filled with a gas such as air, and used to form a mixed gas by bubbling a liquid hydrocarbon fuel, and then the mixed gas is sent into the tube furnace to be combusted.
Preferably, a third stop valve, a flow controller and a one-way valve are sequentially arranged on the gas carrying pipeline.
Preferably, the carrier gas steel cylinder is further provided with a supplementary gas pipeline connected with the mixed gas pipeline. The make-up gas pipeline and the carrier gas pipeline are both connected to a pressure reducing valve of the carrier gas steel cylinder, so that gas in the carrier gas steel cylinder is divided into two paths, and the two paths can be used for adjusting the proportion of the hydrocarbon fuel in the mixed gas.
Preferably, a fourth stop valve, a flow controller and a one-way valve are sequentially arranged on the air supplementing pipeline.
Preferably, the tube furnace is connected with the tail gas absorber through a tail gas pipeline. The tail gas absorber is used for collecting tail gas, and the tail gas is prevented from directly entering the atmosphere to cause pollution.
Preferably, the tail gas detection device comprises a gas chromatograph, and the gas chromatograph is respectively connected with a tail gas pipeline and a tail gas absorber. Preferably, the gas chromatograph adopts a GC-2014AFsc type gas chromatograph of Shimadzu corporation, and adopts a six-way valve for automatic sample injection, so that the composition and the content of the components in the catalytic combustion tail gas can be accurately detected, and the catalytic combustion effect of the catalyst on the hydrocarbon fuel can be better evaluated.
Preferably, the tail gas detection device further comprises CO2Detector, the CO2Detector passing CO2The detection pipeline is connected with the tail gas pipeline, and the CO is2And a fifth stop valve is arranged on the detection pipeline. The flow of the measured hydrocarbon fuel can be quantitatively calibrated, the combustion condition of the hydrocarbon fuel can be detected at any time, and whether the consumed part is completely combusted or not can be judged.
Preferably, the pipeline is wound with a heating belt. The heating belt is wound on the pipeline, so that the gas state of the hydrocarbon fuel can be kept all the time, and thus, the high boiling range fuels such as aviation kerosene and rocket kerosene can be evaluated. The pipeline can be a mixed gas pipeline, an auxiliary test pipeline, a gas carrying pipeline, a supplementary gas pipeline, a tail gas pipeline and CO2And detecting the pipeline.
Preferably, a temperature sensor is arranged in a quartz tube of the tube furnace. The thermocouple is connected into the quartz tube, and the temperature sensor is externally connected, so that the temperature can be further accurately controlled, and the measurement result is more accurate and meaningful.
Compared with the prior art, the invention has the beneficial effects that:
(1) the device provided by the invention can be used for evaluating the catalytic effect of the catalyst on various high boiling range hydrocarbon fuels, such as model fuels or actual fuels including aviation kerosene, rocket kerosene and the like, because the heating belt is wound on the pipeline.
(2) The device provided by the invention is provided with CO2The detector can quantitatively calibrate the flow of the measured hydrocarbon fuel, and can detect the combustion condition of the hydrocarbon fuel at any time to judge whether the consumed part is completely combusted.
(3) The device provided by the invention is provided with the auxiliary test pipeline, and the condition of the device passage is measured by closing the first stop valve and opening the second stop valve, so that the composition of the feed gas can be measured at any time.
(4) The temperature sensor is connected in the quartz tube, so that the actual temperature in the tube can be known more accurately, and the experimental result is more accurate.
Drawings
FIG. 1 is a schematic view showing the structure of an apparatus for evaluating catalytic performance of a catalyst in the example.
Wherein, 1, a gas distribution device; 2. a carrier gas line; 3. a make-up gas line; 4. a hydrocarbon fuel bubbling device; 5. a mixed gas pipeline; 6. a tube furnace; 7. a temperature sensor; 8. auxiliary testing of the pipeline; 9. a gas chromatograph; 10. a tail gas pipeline; 11. a tail gas absorber; 12. CO22Detecting a pipeline; 13. CO22A detector; 14. a third stop valve; 15. a fourth stop valve; 16. a first shut-off valve; 17. a second stop valve; 18. and a fifth stop valve.
Detailed Description
The present invention will be described in more detail with reference to specific examples.
Examples
As shown in fig. 1, the device for evaluating the catalytic performance of the catalyst comprises a gas distribution device 1, a hydrocarbon fuel bubbling device 4, a tubular furnace 6 for placing the catalyst to be tested and an exhaust gas detection device which are sequentially connected through a pipeline.
The gas distribution device 1 is a carrier gas steel cylinder and is divided into a carrier gas pipeline 2 and a supplementary gas pipeline 3 through a pressure reducing valve of the carrier gas steel cylinder. The carrier gas steel cylinder is connected with the hydrocarbon fuel bubbling device 4 through the carrier gas pipeline 2, and the carrier gas pipeline 2 is sequentially provided with a third stop valve 14, a flow controller and a one-way valve, wherein the flow controller is used for controlling the gas flow entering the hydrocarbon fuel bubbling device 4 and the content of the hydrocarbon fuel entering a quartz reaction tube in the tube furnace 6; the stop valve is arranged before flow control and used for stopping gas flow; the check valve is arranged behind the flow controller and used for protecting the flow controller.
The carrier gas cylinder 1 is filled with air, and the hydrocarbon fuel bubbler 4 is filled with model fuels such as n-dodecane, n-tridecane, n-tetradecane, decalin, cyclohexane, ethylcyclohexane, methylcyclohexane, etc., or actual fuels such as jet fuel, rocket fuel, etc.
The hydrocarbon fuel bubbling device 4 is connected with the tube furnace 6 through a mixed gas pipeline 5, and a first stop valve 16 is arranged on the mixed gas pipeline 5. The tube furnace is an OTF-1200X-II tube furnace, the length of the quartz reaction tube is 500-800mm, the inner diameter is 6-12mm, and the catalyst is fixed in the middle of the quartz reaction tube through quartz wool. The tubular furnace can accurately control the catalytic combustion temperature within the range of 10-800 ℃, and the detection result has guiding significance for the actual application of each catalyst. In addition, a temperature sensor 7 is provided in the quartz tube of the tube furnace 6. A thermocouple is connected into the quartz tube, and the temperature sensor 7 is connected outside, so that the temperature can be further accurately controlled, and the measurement result is more accurate and meaningful.
The carrier gas steel cylinder is also provided with a supplementary gas pipeline 3 connected with the mixed gas pipeline 5, and the supplementary gas pipeline 3 is also sequentially provided with a fourth stop valve 15, a flow controller and a one-way valve. The make-up gas pipeline 3 divides the gas in the carrier gas cylinder into two paths, and can be used for adjusting the proportion of the hydrocarbon fuel in the mixed gas by adjusting the third stop valve 14 and the fourth stop valve 15.
The mixed gas pipeline 5 and the tail gas pipeline 10 are respectively connected with the inlet end and the outlet end of the tube furnace 6, the auxiliary test pipeline 8 is arranged on the pipeline at the inlet end and the outlet end of the tube furnace 6 in parallel, the second stop valve 17 is arranged on the auxiliary test pipeline 8, and the inlet end of the auxiliary test pipeline 8 is arranged between the first stop valve 5 and the hydrocarbon fuel bubbling device 4.
The tube furnace 6 is connected to a tail gas absorber 11 through a tail gas pipeline 10. The tail gas absorber is used for collecting tail gas, and the tail gas is prevented from directly entering the atmosphere to cause pollution.
The tail gas detection device comprises a gas chromatograph 9 and CO2The detector 13 and the gas chromatograph 9 are respectively connected with the tail gas pipeline 10 and the tail gas absorber 11, a GC-2014AFsc type gas chromatograph of Shimadzu company is adopted, and six-way valve automatic sampling is adopted, so that the component composition and the content in the catalytic combustion tail gas can be accurately detected, and the catalytic combustion effect of the catalyst on hydrocarbon fuel can be better evaluated.
CO2Detector 13 passing CO2 A detection pipeline 12 is connected with the tail gas pipeline 10, CO2A fifth stop valve 18, CO, is arranged on the detection pipeline 122The detector 13 can quantitatively calibrate the flow rate of the hydrocarbon fuel, and can detect the combustion condition of the hydrocarbon fuel at any time to determine whether the consumed portion is completely combusted.
In addition, the pipelines are wound with heating belts (not shown in the figure), so that the gas state of the hydrocarbon fuel can be kept all the time, and thus, the high boiling range fuels such as aviation kerosene and rocket kerosene can be evaluated.
The working process is as follows:
firstly, a certain amount of catalyst is weighed and fixed in the middle of a quartz reaction tube by quartz wool, and the quartz reaction tube is arranged in a tube furnace 6, and then a flow controller, a heating belt controller, the tube furnace 6, a gas chromatograph 9 and a computer are started.
And secondly, sequentially opening a carrier gas steel cylinder valve, a pressure reducing valve and a stop valve, adjusting a flow controller to a certain value, reducing the pressure of the gas by the pressure reducing valve, dividing the gas into two paths by a carrier gas pipeline 2 and a supplementary gas pipeline 3, and mixing the gas in the carrier gas pipeline 2 and the gas in the supplementary gas pipeline 3 after passing through a hydrocarbon fuel bubbling device 4 to form mixed gas and introducing the mixed gas into the quartz reaction tube. A certain amount of catalyst to be measured with 20 meshes to 40 meshes is placed in the quartz reaction tube, and two ends of the catalyst are fixed by quartz cotton. And the mixed gas is subjected to catalytic degradation reaction under the action of the catalyst to be detected. Finally, the degraded mixed gas is connected with a tail gas absorber 11 through a tail gas pipeline 10. The gas chromatograph 9 collects a certain amount of degraded mixed gas from the tail gas pipeline 10 through the six-way valve, and accurately analyzes the composition and concentration of the mixed gas.

Claims (5)

1.一种用于评价催化剂催化性能的装置,其特征在于,包括依次通过管路连接的配气装置、碳氢燃料鼓泡装置、放置待测催化剂的管式炉和尾气检测装置;1. a device for evaluating the catalytic performance of a catalyst, is characterized in that, comprises a gas distribution device, a hydrocarbon fuel bubbling device, a tube furnace and a tail gas detection device that are connected by pipeline successively; 所述碳氢燃料鼓泡装置与管式炉通过混合气管路连接,所述混合气管路上设有第一截止阀;所述管式炉进出口两端管路上并联设有辅助测试管路,所述辅助测试管路上设有第二截止阀,且所述辅助测试管路的进口端设置在第一截止阀与碳氢燃料鼓泡装置之间;由于设置了辅助测试管路,实现随时测定原料气的成分组成;The hydrocarbon fuel bubbling device and the tube furnace are connected through a mixed gas pipeline, and the mixed gas pipeline is provided with a first shut-off valve; the pipelines at both ends of the inlet and outlet of the tube furnace are connected in parallel with auxiliary test pipelines, so The auxiliary test pipeline is provided with a second cut-off valve, and the inlet end of the auxiliary test pipeline is set between the first cut-off valve and the hydrocarbon fuel bubbling device; due to the auxiliary test pipeline, the raw material can be measured at any time. composition of gas; 所述配气装置为载气钢瓶,通过载气管路连接碳氢燃料鼓泡装置,所述载气钢瓶还设有与混合气管路连接的补充气管路;The gas distribution device is a carrier gas cylinder, which is connected to the hydrocarbon fuel bubbling device through a carrier gas pipeline, and the carrier gas cylinder is also provided with a supplementary gas pipeline connected to the mixed gas pipeline; 所述载气管路上依次设有第三截止阀、流量控制器和单向阀;所述补充气管路上依次设有第四截止阀、流量控制器和单向阀;The carrier gas pipeline is provided with a third stop valve, a flow controller and a one-way valve in sequence; the supplementary gas pipeline is sequentially provided with a fourth stop valve, a flow controller and a one-way valve; 所述管式炉的石英管内设有温度传感器。A temperature sensor is provided in the quartz tube of the tube furnace. 2.根据权利要求1所述的用于评价催化剂催化性能的装置,其特征在于,所述管式炉通过尾气管路连接尾气吸收器。2 . The device for evaluating the catalytic performance of a catalyst according to claim 1 , wherein the tubular furnace is connected to an exhaust gas absorber through an exhaust gas pipeline. 3 . 3.根据权利要求2所述的用于评价催化剂催化性能的装置,其特征在于,所述尾气检测装置包括气相色谱仪,所述气相色谱仪分别连接尾气管路和尾气吸收器。3 . The device for evaluating the catalytic performance of a catalyst according to claim 2 , wherein the exhaust gas detection device comprises a gas chromatograph, and the gas chromatograph is respectively connected to the exhaust gas pipeline and the exhaust gas absorber. 4 . 4.根据权利要求3所述的用于评价催化剂催化性能的装置,其特征在于,所述尾气检测装置还包括CO2检测器,所述CO2检测器通过CO2检测管路与尾气管路连接,所述CO2检测管路上设有第五截止阀。4. The device for evaluating the catalytic performance of a catalyst according to claim 3, wherein the exhaust gas detection device further comprises a CO2 detector, and the CO2 detector is connected to the exhaust gas pipeline through a CO2 detection pipeline, so The CO2 detection pipeline is provided with a fifth stop valve. 5.根据权利要求1所述的用于评价催化剂催化性能的装置,其特征在于,所述管路上缠绕有加热带。5 . The device for evaluating the catalytic performance of a catalyst according to claim 1 , wherein a heating tape is wound around the pipeline. 6 .
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CN109061033A (en) * 2018-07-10 2018-12-21 华电电力科学研究院有限公司 SCR denitration demercuration integration catalyst integrated experiment device and test method
CN109406703A (en) * 2018-11-13 2019-03-01 华电电力科学研究院有限公司 A kind of catalyst performance test device and its test method removing hydro carbons organic pollutant
CN109799314A (en) * 2019-03-27 2019-05-24 盛守祥 A kind of catalyst activity evaluating apparatus and method

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