CN107478764B - Hydrocarbon steam conversion catalyst activity evaluation device and test method and application thereof - Google Patents
Hydrocarbon steam conversion catalyst activity evaluation device and test method and application thereof Download PDFInfo
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Abstract
The invention relates to an activity evaluation device of a hydrocarbon steam conversion catalyst, a test method and application thereof, belonging to the technical field of petrochemical industry. The evaluation device comprises a pressure reducing valve, a gas mass flowmeter, a metering pump, a vaporizer, a mixer, a reactor, an electric heating furnace, a condenser, a gas-liquid separator, a voltage stabilizer, a liquid level meter, a wet flowmeter, a dryer and a gas chromatograph; the test method comprises a hydrocarbon steam reforming process and a methane carbon dioxide reforming process; the invention is suitable for the product quality control of manufacturing enterprises of hydrocarbon steam conversion catalysts and the performance index test of catalyst samples in the development process of hydrocarbon steam conversion catalysts. The hydrocarbon steam conversion catalyst activity evaluation device provided by the invention is safe and stable in operation, controllable in temperature difference of the catalyst bed layer of the reactor, constant in reaction temperature, safe, environment-friendly and convenient to use.
Description
Technical Field
The invention relates to an activity evaluation device of a hydrocarbon steam conversion catalyst, a test method and application thereof, belonging to the technical field of petrochemical industry.
Background
The preparation of hydrogen and synthesis gas by hydrocarbon steam conversion is an important chemical process, and the performance requirement of hydrocarbon steam conversion reaction on a catalyst is strict. The activity evaluation of the catalyst is always a crucial link in the aspects of hydrocarbon steam reforming catalyst development, production performance index test, product quality control and the like. Reliable and accurate hydrocarbon steam reforming catalyst activity evaluation data depends on an activity evaluation device which is carefully designed and manufactured and an evaluation method which is summarized through tests accumulated in a daily period. At present, the activity evaluation device and the test method of the hydrocarbon steam reforming catalyst used at home and abroad are approximately the same.
A experiment of ' oil-to-gas ' for raw material of hydrogen production device in oil refinery ' published in 30 vol.2 of Qilu petrochemical engineering 2002 introduces a small-sized hydrogen production pressurization evaluation device and a catalyst activity evaluation method, and has certain defects, such as improper heating mode, no water vaporizer, mixing and vaporizing of water and hydrocarbon raw materials in a mixer, and because of large heat capacity of water and poor vaporization mixing effect, water vapor pulse feeding is easy to occur, so that water-carbon ratio imbalance at the inlet of a catalyst bed layer is caused, and long-term evaluation of a conversion catalyst is not facilitated. The water-gas separator has no liquid level control capability, unreacted water is stored in the separator, manual discharge is relied on, water is completely discharged, a large amount of gas escapes, the gas mainly comprises methane, carbon monoxide and carbon dioxide, and is flammable, explosive and dangerous, and the gas escapes suddenly, so that the pressure fluctuation of the whole system is inevitably caused, a large amount of materials are impacted on a catalyst bed layer, the instant feeding amount exceeds the catalyst treatment capability, and the normal operation of the catalyst activity evaluation reaction is influenced.
A pressurized micro-reverse evaluation device and a catalyst activity evaluation method are introduced in a gaseous hydrocarbon low-temperature adiabatic conversion catalyst published in Shanghai chemical industry 2006, volume 31 and 6. There are disadvantages in that: the catalyst loading is only 5mL, and the representativeness is weak; the process gas completely passes through the dryer and then enters a six-way valve of the chromatograph, and the adsorbent in the dryer is easily and quickly saturated, so that the process gas containing water vapor is introduced into the gas chromatograph to damage the chromatograph.
"research and development and performance test of a miniature hydrogen production reactor for oxidizing and reforming natural gas", published in proceedings of xu zhou institute of engineering (nature science edition) 2013, 9, 28, volume 3, introduces a design and evaluation method for an integrated hydrogen production reactor for oxidizing and reforming natural gas, and has the following disadvantages: the reforming reactor test system adopts open fire for heat supply, belongs to dangerous behaviors in a laboratory and violates safety regulations; water is vaporized in the mixer and mixed with methane, so that the vaporization mixing effect is poor; water is introduced into the system in a nitrogen pressurization mode, the water inflow is influenced by the pressure difference between the output pressure of the nitrogen cylinder and the system pressure, the water inflow cannot be kept constant, and the long-term evaluation of the catalyst is not facilitated; the reforming reaction evaluation adopts normal pressure, and industrial actual conditions cannot be simulated.
In summary, the prior art has the following disadvantages:
(1) the mixing effect of the steam and the hydrocarbon is poor, and the water-carbon ratio is easy to be disordered;
(2) the water-vapor separator has no liquid level control capability;
(3) the condition that process gas containing water vapor enters the gas chromatography exists, and the chromatograph is damaged;
(4) the heat supply mode cannot meet the safety regulation of a laboratory, and the personal safety of evaluation personnel cannot be ensured;
(5) the pulse feeding is easy to realize, and the operation life of the catalyst is influenced, so that the accuracy of output result data is influenced.
Disclosure of Invention
The invention aims to provide an activity evaluation device for a hydrocarbon steam conversion catalyst, which has the characteristics of stable operation, safety, reliability, convenient use, accurate test data and good repeatability; the invention also provides a test method and application for evaluating the hydrocarbon steam reforming catalyst by adopting the hydrocarbon steam reforming catalyst activity evaluation device.
The hydrocarbon steam conversion catalyst activity evaluation device comprises a pressure reducing valve, a gas mass flow meter, a metering pump, a vaporizer, a mixer, a reactor, an electric heating furnace, a condenser, a gas-liquid separator, a voltage stabilizer, a liquid level meter, a wet flow meter, a dryer and a gas chromatograph; the top of the reactor is connected with a mixer, and the mixer is respectively connected with a hydrogen storage tank, a carbon dioxide storage tank, a methane storage tank, a water storage tank and a naphtha storage tank; the bottom of the reactor is sequentially connected with a condenser and a gas-liquid separation tank, the top of the gas-liquid separation tank is connected with a gas chromatograph through a dryer, and the bottom of the gas-liquid separation tank is connected with a liquid level control valve; wherein the reactor is located inside an electric heating furnace; the mixer is connected with the water storage tank through a water vaporizer and is connected with the naphtha storage tank through a hydrocarbon vaporizer; the gas chromatograph is connected with a computer control system.
Wherein:
the electric heating furnace adopts a multi-section heating mode, the top of the electric heating furnace is provided with a blower, and the blower is connected with the upper part of the reactor through an air duct.
The reactor is made of high-alloy austenitic heat-resistant steel pipes, and the material of the reactor is any one of 40Cr25Ni20, 4Cr25Ni35, 4Cr25Ni35Nb, 4Cr25Ni35WNb and 5Cr25Ni35Co015W5, preferably 4Cr25Ni35 Nb; the reactor is internally provided with a thermowell which is made of 40Cr25Ni20, 4Cr25Ni35 or 4Cr25Ni35Nb, preferably 4Cr25Ni35Nb, the size of the thermowell is preferably phi 8 multiplied by 1mm, and 5 temperature measuring points are arranged.
The computer control system consists of a computer, a single-loop regulator and a programmable controller, and adopts the centralized operation management of the computer or the operation on the single-loop regulator.
The computer control system is controlled by an on-site instrument and a computer, automatically collects data, automatically stores the data, automatically prints the data, automatically controls the temperature, the pressure, the liquid flow and the gas flow, and can display a process flow chart with real-time state data, a real-time trend chart and a historical trend chart.
The test method comprises a hydrocarbon steam reforming process and a methane carbon dioxide reforming process, and comprises the following steps:
(1) hydrocarbon steam reforming process
Measuring naphtha and water, respectively entering a hydrocarbon vaporizer and a water vaporizer for heating, heating the naphtha to be vaporized, heating the water to form superheated steam, mixing the naphtha, methane and the superheated steam in a mixer, entering a reactor, performing conversion reaction with hydrocarbon steam of a catalyst to be detected filled in the reactor, separating water and process gas from the reacted gas through a condenser and a gas-liquid separation tank, and discharging the process gas to the atmosphere after the process gas is analyzed by a chromatograph;
(2) methane carbon dioxide reforming process
The methane and the carbon dioxide enter the mixer and the reactor in sequence after being measured, the methane and the carbon dioxide are subjected to reforming reaction with a catalyst to be measured filled in the reactor, water and process gas are separated from the reacted gas through the condenser and the gas-liquid separation tank, and the process gas is analyzed by the chromatograph and then discharged to the atmosphere.
Wherein, the test process conditions are as follows:
preferably, the experimental process conditions are as follows:
the test method described in the present invention is the overall reaction for steam reforming of hydrocarbons: cnHm+H2O→eCO+bCO2+cH2+dCH4+eH2O is used as an index to evaluate the conversion activity and selectivity of the hydrocarbon steam conversion catalyst; naphtha with a dry point of 200 ℃ is used as a raw material, the water-carbon ratio is 2.0, the operation is carried out for 8h under the feeding condition, a gas chromatograph is used for analyzing the composition of the emptying process gas once per hour, and the conversion rate gamma and the methane selectivity of the catalyst are calculated according to the following formula:
wherein ∑ C% is CO and CO in the emptying process gas2The sum of the volume percentages of (A); vTailThe flow rate of the process gas is in mL/min; m is the loading of the catalyst and is in g;
in the formula: the total carbon at the outlet is CH4、CO、CO2、C2H4、C2H6。
The application of the hydrocarbon steam reforming catalyst activity evaluation device is suitable for product quality control of manufacturing enterprises of hydrocarbon steam reforming catalysts, performance index test of catalyst samples in the development and development processes of the hydrocarbon steam reforming catalysts, side line analysis of development and amplification test stages of the hydrocarbon steam reforming catalysts, application tracking analysis of the hydrocarbon steam reforming catalysts in operation of production devices and monitoring and indicating of catalyst activity decline.
Compared with the prior art, the invention has the following advantages:
(1) a multi-section type electric heating furnace is adopted, and a reactor is arranged in the electric heating furnace; the top of the electric heating furnace is provided with a blower, so that air between the reactor and the heating furnace can be forced to convect, and the temperature distribution of a hearth of the industrial reforming furnace can be simulated;
(2) the water vaporizer is additionally arranged on an outlet pipeline of the water pump, the vaporizer can vaporize water into steam completely and overheat the steam to form overheated steam, so that the pulse feeding of the steam is avoided, and the stability of the water-carbon ratio of a test is facilitated;
(3) the liquid level control of the gas-liquid separator is added, the condensed material is subjected to gas-liquid separation in the enterprise separator, and the storage and discharge of the liquid are in a controllable state, so that system pressure fluctuation caused by manual liquid discharge is avoided, and the stability of test data is facilitated;
(4) a carbon dioxide gas circuit and corresponding accessories are additionally arranged and used for experimental research on hydrocarbon carbon dioxide reforming reaction;
(5) the system is provided with a computer control system which consists of a computer, a single-loop regulator and a programmable controller; the computer system is provided with a high, low and low limit alarm system, the control system adopts computer centralized operation management or operates on a single-loop regulator, and the control software adopts open-loop control. The control system is designed with three-level alarm functions of high-limit and low-limit alarm, high-limit and high-limit emergency treatment and emergency power failure, so that the safety of the system is ensured.
The invention has the following beneficial effects:
(1) the hydrocarbon steam conversion catalyst activity evaluation device is safe and stable in operation, controllable in temperature difference of a catalyst bed layer of the reactor, constant in reaction temperature, safe, environment-friendly and convenient to use;
(2) the blower arranged at the top of the electric heating furnace can lead the air between the reactor and the electric heating furnace to carry out forced convection, thereby being capable of simulating the temperature distribution of a hearth of the industrial reforming furnace;
(3) the test data is accurate and reliable, the activity deviation of the measured catalyst is below 1%, and the data repeatability is good.
Drawings
FIG. 1 is a process flow diagram of the present invention.
FIG. 2 is a schematic view of the structure of an electric heating furnace and a reactor in the present invention.
FIG. 3 is a process flow diagram of a prior art hydrocarbon steam reforming catalyst activity evaluation apparatus.
In the figure: 1. a hydrogen storage tank; 2. a carbon dioxide storage tank; 3. a methane storage tank; 4. a water storage tank; 5. a naphtha storage tank; 6. a water vaporizer; 7. a hydrocarbon vaporizer; 8. a mixer; 9. a reactor; 10. a condenser; 11. a gas-liquid separation tank; 12. a dryer; 13. a gas chromatograph; 14. a computer control system; 15. a liquid level control valve; 16. a blower; 17. an electric heating furnace; 18. a resistance wire; 19. an air duct; 20. a tray; 21. a thermowell; 22. an oil metering pump; 23. a water metering pump; 24. a vaporizer; 25. a raw material mixer; 26. a tubular reactor; 27. a cooler; 28. a separator; 29. a voltage regulator; 30. a wet flowmeter.
Detailed Description
The present invention is further described below with reference to examples.
Example 1
As shown in fig. 1-2, the hydrocarbon steam reforming catalyst activity evaluation device of the present invention comprises a reactor 9, a mixer 8 is connected to the top of the reactor 9, and the mixer 8 is connected to a hydrogen storage tank 1, a carbon dioxide storage tank 2, a methane storage tank 3, a water storage tank 4 and a naphtha storage tank 5; the bottom of the reactor 9 is connected with a condenser 10 and a gas-liquid separation tank 11 in sequence, the top of the gas-liquid separation tank 11 is connected with a gas chromatograph 13 through a dryer 12, and the bottom of the gas-liquid separation tank 11 is connected with a liquid level control valve 15.
The reactor 9 is positioned inside the electric heating furnace 17, the resistance wire 18 is wound outside the electric heating furnace 17, a multi-section heating mode is adopted, the top of the electric heating furnace 17 is provided with a blower 16, and the blower 16 is connected with the upper part of the reactor 9 through an air duct 19; the mixer 8 is connected with the water storage tank 4 through the water vaporizer 6, and the mixer 8 is connected with the naphtha storage tank 5 through the hydrocarbon vaporizer 7; the gas chromatograph 13 is connected to a computer control system 14.
The temperature of five temperature measuring points at the upper part, the middle part A, the middle part B, the middle part C and the lower part of the catalyst bed layer are measured by temperature control measurement at different temperatures on the hydrocarbon steam reforming catalyst activity evaluation device disclosed by the invention and are shown in table 1.
TABLE 1 measurement data of temperature measurement points at different temperatures
As can be seen from Table 1, the temperature difference of the catalyst bed at each measurement point was less than 1 ℃.
Example 2
When the inlet pressure of the hydrocarbon steam reforming catalyst activity evaluation device is 3.0MPa, temperature control measurement is carried out at different carbon airspeeds, and the measured temperatures of five temperature measuring points of the upper part, the middle part A, the middle part B, the middle part C and the lower part of a catalyst bed layer are shown in a table 2.
TABLE 2 measurement data of temperature measurement points at different carbon airspeeds
As can be seen from Table 2, the temperature difference of the catalyst bed at each measurement point was less than 1 ℃.
Example 3
For the hydrocarbon steam reforming catalyst of the inventionActivity evaluation device at carbon airspeed of 6000h-1During the process, temperature control measurement is carried out under different pressures, and the measured temperatures of five measurement points of the upper part, the middle part A, the middle part B, the middle part C and the lower part of a catalyst bed layer are shown in
TABLE 3 measurement data of temperature measurement points under different pressures
As can be seen from Table 3, the temperature difference of the catalyst bed at each measurement point was less than 1 ℃.
Example 4
The test method and the evaluation device of the invention are adopted to take the Z412Q/Z413Q catalyst developed by the research institute of Qilu petrochemical company as a research object, natural gas is taken as a raw material, the water-carbon ratio is 1.97, the inlet pressure of a reactor is 2.4MPa, and long-period tests are carried out on 2015 from 5 months to 7 days to 6 months to 13 days, and the results are shown in Table 4.
TABLE 4 Long-period test results
Comparative example 1
Temperature control measurement is carried out at different temperatures by using a small hydrogen production pressurization evaluation device of the institute of the middle petrochemical and Qilu division in the background art, and the measured temperatures of five temperature measurement points of the upper part, the middle part A, the middle part B, the middle part C and the lower part of a catalyst bed layer are shown in a table 5.
TABLE 5 measurement data of temperature measurement points at different temperatures
As can be seen from Table 5, the catalyst bed temperature difference was large at each measurement point.
Comparative example 2
The temperature of five temperature measuring points, namely the upper part, the middle part A, the middle part B, the middle part C and the lower part of a catalyst bed layer, are measured by using a small hydrogen production pressurization evaluation device of the research institute of the middle petrochemical Qilu division company in the background technology and performing temperature control measurement at different carbon airspeeds when the inlet pressure of a reactor is 3.0MPa, and the measured temperatures are shown in a table 6.
TABLE 6 measurement data of temperature measurement points at different carbon airspeeds
As can be seen from Table 6, the catalyst bed temperature difference at each measurement point was large.
Claims (6)
1. An apparatus for evaluating the activity of a hydrocarbon steam reforming catalyst, comprising a reactor (9), characterized in that: the top of the reactor (9) is connected with a mixer (8), and the mixer (8) is respectively connected with a hydrogen storage tank (1), a carbon dioxide storage tank (2), a methane storage tank (3), a water storage tank (4) and a naphtha storage tank (5); the bottom of the reactor (9) is sequentially connected with a condenser (10) and a gas-liquid separation tank (11), the top of the gas-liquid separation tank (11) is connected with a gas chromatograph (13) through a dryer (12), and the bottom of the gas-liquid separation tank (11) is connected with a liquid level control valve (15); wherein the reactor (9) is located inside an electrically heated furnace (17); the mixer (8) is connected with the water storage tank (4) through a water vaporizer (6), and the mixer (8) is connected with the naphtha storage tank (5) through a hydrocarbon vaporizer (7); the gas chromatograph (13) is connected with a computer control system (14);
a resistance wire (18) is wound outside the electric heating furnace (17), and a multi-section heating mode is adopted; the top of the electric heating furnace (17) is provided with a blower (16), and the blower (16) is connected with the upper part of the reactor (9) through an air duct (19);
the material of the reactor (9) is any one of 40Cr25Ni20, 4Cr25Ni35, 4Cr25Ni35Nb, 4Cr25Ni35WNb and 5Cr25Ni35Co015W 5; a thermowell (21) is arranged in the reactor (9) and is made of 40Cr25Ni20, 4Cr25Ni35 or 4Cr25Ni35 Nb; the bottom of the reactor (9) is provided with a tray (20) for supporting a catalyst bed layer;
the computer control system (14) consists of a computer, a single-loop regulator and a programmable controller, and adopts the centralized operation management of the computer or operates on the single-loop regulator;
the computer control system (14) adopts an on-site instrument and a computer for control, automatically collects, stores and prints data, automatically controls temperature, pressure, liquid flow and gas flow, and can display a process flow chart with real-time state data, a real-time trend chart and a historical trend chart.
2. A method for conducting a test using the apparatus for evaluating the activity of a hydrocarbon steam reforming catalyst according to claim 1, characterized in that: the method comprises a hydrocarbon steam conversion process and a methane carbon dioxide reforming process, and comprises the following steps:
(1) hydrocarbon steam reforming process
Naphtha and water are metered and then respectively enter a hydrocarbon vaporizer (7) and a water vaporizer (6) for heating, naphtha is heated to be vaporized, water is heated to form superheated steam, then the naphtha, methane and the superheated steam are mixed in a mixer (8) and then enter a reactor (9) to carry out hydrocarbon steam conversion reaction with a catalyst to be tested filled in the reactor (9), the reacted gas is sequentially subjected to a condenser (10) and a gas-liquid separation tank (11) to separate water and process gas, and the process gas is analyzed by a gas chromatograph (13) and then discharged to the atmosphere;
(2) methane carbon dioxide reforming process
The methane and the carbon dioxide are measured and then sequentially enter a mixer (8) and a reactor (9), the methane and the carbon dioxide are subjected to reforming reaction with a catalyst to be detected filled in the reactor (9), the reacted gas is sequentially subjected to separation of water and process gas by a condenser (10) and a gas-liquid separation tank (11), and the process gas is analyzed by a gas chromatograph (13) and then discharged to the atmosphere.
3. The method of claim 2, wherein:
the experimental process conditions were as follows:
4. the method of claim 2, wherein: the experimental process conditions were as follows:
5. the method of claim 2, wherein: overall reaction with steam reforming of hydrocarbons: CnHm + H2O→eCO+bCO2+cH2+dCH4+eH2O is used as an index to evaluate the conversion activity and selectivity of the hydrocarbon steam conversion catalyst; naphtha with a dry point of 200 ℃ is used as a raw material, the water-carbon ratio is 2.0, the operation is carried out for 8h under the feeding condition, a gas chromatograph is used for analyzing the composition of the emptying process gas once per hour, and the conversion rate gamma and the methane selectivity of the catalyst are calculated according to the following formula:
in the formula: Σ C% is the sum of the volume percentages of CO, CO2 in the vent process gas; the V tail is the flow of the process gas, and the unit is mL/min; m is the loading of the catalyst and is in g;
in the formula: the total carbon at the outlet is CH4、CO、CO2、C2H4、C2H6。
6. Use of the apparatus for evaluating the activity of a hydrocarbon steam reforming catalyst according to claim 1, wherein: the method is suitable for product quality control of hydrocarbon steam conversion catalyst manufacturing enterprises, performance index test of catalyst samples in the hydrocarbon steam conversion catalyst research and development process, side line analysis of hydrocarbon steam conversion catalyst research and development amplification test stages, application tracking analysis of hydrocarbon steam conversion catalysts in production device operation and monitoring indication of catalyst activity decline.
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| JP2008224257A (en) * | 2007-03-09 | 2008-09-25 | Tokyo Electric Power Co Inc:The | Catalytic activity evaluation device and evaluation method |
| CN202649187U (en) * | 2012-06-15 | 2013-01-02 | 北京恒德水沐土地修复环保科技有限公司 | Activity evaluation device of catalyst |
| CN103512966A (en) * | 2012-06-27 | 2014-01-15 | 中国石油化工股份有限公司 | Sulfur recovery catalyst activity evaluating device and test method |
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