CN107478732B - Volatile organic compound catalytic combustion evaluation device and test method - Google Patents
Volatile organic compound catalytic combustion evaluation device and test method Download PDFInfo
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- CN107478732B CN107478732B CN201610407526.0A CN201610407526A CN107478732B CN 107478732 B CN107478732 B CN 107478732B CN 201610407526 A CN201610407526 A CN 201610407526A CN 107478732 B CN107478732 B CN 107478732B
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- G—PHYSICS
- G01—MEASURING; TESTING
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
- F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
- F23G7/00—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals
- F23G7/06—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases
- F23G7/07—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases in which combustion takes place in the presence of catalytic material
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- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
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Abstract
The invention belongs to the technical field of catalyst evaluation, and particularly relates to a volatile organic compound catalytic combustion evaluation device and a test method. The volatile organic compound catalytic combustion evaluation device comprises a reactor, wherein the reactor is respectively connected with a gas mass flowmeter and a metering pump, the reactor, a heat exchanger, a condenser, a gas-liquid separator, a wet flowmeter, a drying pipe and a gas chromatograph are sequentially connected with a computer, the heat exchanger is connected with an air blower, the gas-liquid separator is connected with a liquid storage tank, and an exhaust head is respectively connected with the wet flowmeter and the drying pipe. The invention has large catalyst loading amount, can load a whole honeycomb monolithic catalyst, has strong authenticity of the obtained test data, and is beneficial to converting from a laboratory device to an industrial device; be provided with the heat exchanger, make full use of heat reduces the laboratory and uses electricity.
Description
Technical Field
The invention belongs to the technical field of catalyst evaluation, and particularly relates to a volatile organic compound catalytic combustion evaluation device and a test method.
Background
Along with the increasing strictness of environmental protection, chemical and petrochemical process waste gases containing Volatile Organic Compounds (VOCs), petroleum and chemical product storage tank gases, printing and paint production waste gases, extraction waste gases, wood dry distillation waste gases, pharmaceutical factory waste gases, automobile exhaust gases and the like are increasingly treated by incineration or catalytic combustion. Compared with the traditional condensation method, absorption method, adsorption method and biological method, the combustion method is used for treating VOCSThe treatment is more thorough and complete, and becomes a preferred method for treating high-concentration waste gas with complex pollutant components.
CN 01207962.6 discloses a regenerative incinerator for organic waste gas, which uses two regenerative beds to switch alternately to complete the processes of gas heating, purification and heat storage. CN 200320116750.2 discloses a three-heat-storage bed structure.
The above patent is bulky, high in manufacturing cost, complex in control, and can not be conveniently used for scientific research.
The research on the industrial organic tail gas catalytic combustion technology of the university of eastern science and technology of China, paper P21 and P25, which provides the process flow of 2 catalyst laboratory evaluation devices, can be judged from the introduction of the process flow, the test device is a fixed bed reactor, and the mode of electric heating outside the tube of the reactor is adopted. Wherein P21, catalyst loading is 50 ml, thermocouple inserted into catalyst bed layer is set before and after reaction to measure temperature, and is controlled by temperature programmed controller. The loading amount of the catalyst P21 is not disclosed, the loading length is 15-25 mm, and the catalyst is in a constant temperature area of a heating furnace. The introduction of 2 laboratory evaluation devices P21 and P25 can judge that the temperature measurement of the P21 device has defects, and VOCs can emit large amount of heat during catalytic combustion, so that when a thermocouple is positioned in a catalyst bed layer, the measured temperature is higher than the preheating temperature of materials, and test data cannot directly assist industrial design; in addition, the loading amount of the catalyst is small, so that the catalyst needs to be crushed before being loaded, and the device cannot load the honeycomb monolithic catalyst, which is not favorable for the industrial conversion of test results. The P22 device is an intrinsic dynamic device, on one hand, the catalyst is broken and is always in a constant temperature area of the reactor, on the other hand, the reaction state is too ideal, and the industrial actual situation cannot be simulated.
Disclosure of Invention
The invention aims to provide a volatile organic compound catalytic combustion evaluation device which is stable in operation, safe, reliable, convenient and fast to use, accurate in test data and good in repeatability; the invention also provides a test method of the device for evaluating the catalytic combustion of the volatile organic compound, which is scientific, reasonable, simple and feasible.
The volatile organic compound catalytic combustion evaluation device comprises a reactor, wherein the reactor is respectively connected with a gas mass flowmeter and a metering pump, the reactor, a heat exchanger, a condenser, a gas-liquid separator, a wet flowmeter, a drying pipe and a gas chromatograph are sequentially connected with a computer, the heat exchanger is connected with an air blower, the gas-liquid separator is connected with a liquid storage tank, and an exhaust head is respectively connected with the wet flowmeter and the drying pipe.
The reactor is internally provided with a sprayer, a heating plate and a steel wire mesh from left to right in sequence, and the outside of the reactor is respectively connected with a temperature measuring instrument and a pressure measuring instrument.
The number of the temperature measuring instruments is 2.
The number of the pressure measuring instruments is 2.
And a catalyst is filled in the steel wire mesh.
The catalyst to be tested is filled in a reactor, raw materials and air enter the reactor together, the materials enter a catalyst bed layer after the temperature is raised to the reaction temperature, the reacted gas is subjected to heat exchange, condensation and separation by a separator to obtain water and process gas, and the tail gas is discharged after chromatographic analysis.
The invention adopts the testing method of the volatile organic compound catalytic combustion evaluation device, and the steps are as follows:
(1) filling a catalyst to be tested in a reactor, introducing air into a system by using an air blower, exchanging heat of the air through a heat exchanger, mixing the heated air and a volatile organic compound, entering the reactor, heating to a reaction temperature, and then entering a catalyst bed layer for reaction;
(2) and (3) the reacted materials enter a heat exchanger to exchange heat, then are condensed, are subjected to water-vapor separation, are measured by a wet flowmeter to measure the tail gas amount, and are subjected to chromatographic analysis, and the tail gas is discharged.
The evaluation test of the VOCs catalytic combustion evaluation device has the specific process flow that:
the method comprises the steps of introducing air into a system by utilizing an air blower, enabling the air to fully exchange heat with reacted materials through a heat exchanger, enabling the heated air and volatile organic compounds from a gas mass flow meter and/or a metering pump to be mixed and enter a reactor, firstly heating the air at a heater, judging whether the materials reach reaction temperature through the temperature measured by a thermocouple in front of a catalyst, enabling the materials reaching the reaction temperature to pass through a catalyst bed layer, enabling the materials to be subjected to catalytic combustion on the catalyst bed layer, enabling the reacted materials to enter the heat exchanger for heat exchange, then condensing, separating water and vapor, metering tail gas amount by a wet flowmeter, and emptying purified tail gas to the atmosphere after an emptying unit absorbs alkali liquor.
The test process conditions of the test method for evaluating the catalytic combustion of the VOCs by using the VOCs catalytic combustion evaluation device are shown in table 1.
TABLE 1 test Process conditions in test methods for VOCs catalytic Combustion evaluation
The preferable test process conditions of the test method for evaluating the catalytic combustion of the VOCs by using the VOCs catalytic combustion evaluation device are shown in Table 2.
TABLE 2 optimized test Process conditions in test methods for catalytic Combustion evaluation of VOCs
Conversion rate of VOCs (VOCs content in raw material gas-VOCs content in tail gas)/VOCs content in raw material gas 100%
Air volume (m)3(h) organic Compound feed amount (g/h)/organic Compound content in gas sample (g/m)3)
The evaluation device for VOCs catalytic combustion is suitable for product quality control of enterprises manufacturing VOCs catalytic combustion catalysts, performance index test of catalyst samples in the research and development process of the VOCs catalytic combustion catalysts, side line analysis of the research and development amplification test stage of the VOCs catalytic combustion catalysts, application tracking analysis of the VOCs catalytic combustion catalysts in operation of production devices and monitoring indication of catalyst activity decline.
All be provided with the temperature measurement point around the catalyst that awaits measuring loads the position, wire net central authorities are arranged in to the temperature measurement point, and the measurement point before the catalyst can fully reflect the temperature that the material preheated, and the measurement point after the catalyst can fully reflect the material temperature after the catalytic combustion of VOCs, and the data that obtain these 2 temperatures are favorable to the industrial device design.
Pressure measuring points are arranged before and after the filling position of the catalyst to be detected, and pressure drop of materials passing through a catalyst bed layer is detected, so that on one hand, industrial design is assisted, on the other hand, the pressure drop condition caused by the honeycomb monolithic catalyst or the catalyst prepared by an irregular carrier is detected, and on the other hand, the long-period operation condition of the catalyst can be monitored, and if carbon deposition blockage occurs on the catalyst bed layer, the pressure drop change before and after the bed layer can be found.
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 computer control system in the VOCs catalytic combustion evaluation device is controlled by an on-site instrument and a computer, data are automatically acquired, automatically stored and printed, and the temperature, the pressure, the liquid flow and the gas flow are automatically controlled; the process flow chart with real-time state data, the real-time trend chart and the historical trend chart can be seen on the display.
And the process tail gas after the reaction is treated by adopting an alkali liquor absorption mode, so that no pollutants such as sulfur, NOx and the like exist, and then the process tail gas is discharged to the atmosphere.
The material composition before and after the reaction was analyzed by chromatography.
Compared with the prior art, the invention has the following beneficial effects:
(1) the heating is non-open fire electric heating, and the temperature control and the explosion-proof control are simpler and more reliable than the auxiliary fuel open fire direct combustion type preheating.
(2) The catalyst to be tested is placed between the steel wire meshes, and can be used for evaluating honeycomb monolithic catalysts and catalysts prepared from irregular carriers.
(3) The loading amount of the catalyst is large, the monolithic honeycomb monolithic catalyst can be loaded, the obtained test data has strong authenticity, and the conversion from a laboratory device to an industrial device is facilitated.
(4) Be provided with the heat exchanger, make full use of heat reduces the laboratory and uses electricity.
(5) 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 schematic view of the structure of a VOCs catalytic combustion evaluation device of the present invention;
FIG. 2 is a schematic diagram of the reactor configuration;
in the figure: 1. a gas mass flow meter; 2. a metering pump; 3. a reactor; 4. a heat exchanger; 5. a blower; 6. a condenser; 7. a gas-liquid separator; 8. a liquid storage tank; 9. a wet flow meter; 10. a drying tube; 11. a gas chromatograph; 12. a computer; 13. an exhaust head; 14. a sprayer; 15. heating plates; 16. a temperature measuring instrument; 17. a pressure gauge; 18. steel wire mesh; 19. a catalyst.
Detailed Description
The present invention is further described below with reference to examples.
Example 1
As shown in fig. 1, the volatile organic compound catalytic combustion evaluation device of the present invention includes a reactor 3, wherein the reactor 3 is connected to a gas mass flow meter 1 and a metering pump 2, respectively, the reactor 3, a heat exchanger 4, a condenser 6, a gas-liquid separator 7, a wet flow meter 9, a drying pipe 10, a gas chromatograph 11 and a computer 12 are sequentially connected, the heat exchanger 4 is connected to an air blower 5, the gas-liquid separator 7 is connected to a liquid storage tank 8, and an exhaust head 13 is connected to the wet flow meter 9 and the drying pipe 10, respectively.
As shown in fig. 2, the sprayer 14, the heating plate 15 and the steel wire mesh 18 are sequentially arranged inside the reactor 3 from left to right, and the outside of the reactor 3 is respectively connected with the temperature measuring instrument 16 and the pressure measuring instrument 17.
The number of the temperature measuring instruments 16 is 2.
The number of the pressure measuring instruments 17 is 2.
The wire mesh 18 is filled with a catalyst 19.
3kg of honeycomb monolithic catalyst is filled in the VOCs catalytic combustion evaluation device, air is introduced into the system by using an air blower, the air exchanges heat through a heat exchanger, the heated air and volatile organic compounds are mixed and enter a reactor, and after the temperature is raised to the reaction temperature, the materials enter a catalyst bed layer for reaction; and (3) the reacted materials enter a heat exchanger to exchange heat, then are condensed, are subjected to water-vapor separation, are measured by a wet flowmeter to measure the tail gas amount, and are subjected to chromatographic analysis, and the tail gas is discharged. The ethanol was subjected to an evaluation test, and the evaluation data are shown in Table 3.
TABLE 3 ethanol decontamination results
Example 2
3kg of honeycomb monolith catalyst was loaded on the apparatus for evaluating catalytic combustion of VOCs of the present invention, and toluene was subjected to an evaluation test according to the test method of example 1, and the evaluation data are shown in Table 4.
TABLE 4 toluene decontamination results
Example 3
On the apparatus for evaluating catalytic combustion of VOCs of the present invention, 3.5kg of a catalyst prepared from an irregular carrier was loaded, and evaluation tests were carried out on toluene in accordance with the test method of example 1, and the evaluation data are shown in Table 5.
TABLE 5 toluene purge results
Claims (4)
1. A volatile organic compound catalytic combustion evaluation device comprises a reactor (3), and is characterized in that the reactor (3) is respectively connected with a gas mass flow meter (1) and a metering pump (2), the reactor (3), a heat exchanger (4), a condenser (6), a gas-liquid separator (7), a wet flow meter (9), a drying pipe (10) and a gas chromatograph (11) are sequentially connected with a computer (12), the heat exchanger (4) is connected with an air blower (5), the gas-liquid separator (7) is connected with a liquid storage tank (8), and an exhaust head (13) is respectively connected with the wet flow meter (9) and the drying pipe (10);
the reactor (3) is internally provided with a sprayer (14), a heating plate (15) and a steel wire mesh (18) in sequence from left to right, and the outside of the reactor (3) is respectively connected with a temperature measuring instrument (16) and a pressure measuring instrument (17);
the number of the temperature measuring instruments (16) is 2; temperature measuring points are arranged at the front and the back of the filling position of the catalyst to be measured, and the temperature measuring points are arranged in the center of the steel wire mesh;
the number of the pressure measuring instruments (17) is 2;
the inside of the steel wire mesh (18) is filled with a catalyst (19);
the catalyst is 80X 100mm honeycomb monolithic catalyst or catalyst prepared by irregular carrier with the same volume, and the weight of the catalyst is 3.5kg at most.
2. A test method using the apparatus for evaluating catalytic combustion of volatile organic compounds according to claim 1, characterized by comprising the steps of:
(1) filling a catalyst to be tested in a reactor, introducing air into a system by using an air blower, exchanging heat of the air through a heat exchanger, mixing the heated air and a volatile organic compound, entering the reactor, heating to a reaction temperature, and then entering a catalyst bed layer for reaction;
(2) and (3) the reacted materials enter a heat exchanger to exchange heat, then are condensed, are subjected to water-vapor separation, are measured by a wet flowmeter to measure the tail gas amount, and are subjected to chromatographic analysis, and the tail gas is discharged.
3. The test method according to claim 2, characterized in that the test process conditions are as follows:
catalyst loading 3.5Kg
Catalyst size 80 x 100mm honeycomb monolithic catalyst or catalyst prepared from same volume of irregular carrier
Between 2 layers of high temperature resistant steel wire nets in the catalyst filling position reactor
Gas chromatography GC-14C; FID, double column
Gas chromatograph for on-line detection of organic matter content and CO in gas
The reaction temperature is 200 ℃ and 950 DEG C
Air volume of blower is 1-1000m3
Test gas airspeed of 5000-30 kilo L/h Kgcat
Inlet organic compound concentration of at most 10g/m3
The pressure is between the normal pressure and 0.2 MPa.
4. The test method according to claim 2, characterized in that the test process conditions are as follows:
catalyst loading 3.0Kg
Catalyst size 80 x 100mm honeycomb monolithic catalyst or catalyst prepared from same volume of irregular carrier
Between 2 layers of high temperature resistant steel wire nets in the catalyst filling position reactor
Gas chromatography GC-14C; FID, double column
Gas chromatograph for on-line detection of organic matter content and CO in gas
The reaction temperature is 200 ℃ and 700 DEG C
Blower air volume 500-3
Test gas airspeed of 5-15 kilo L/h Kgcat
Inlet organic compound concentration of at most 6g/m3
The pressure is between the normal pressure and 0.1 MPa.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004195386A (en) * | 2002-12-19 | 2004-07-15 | Mitsui Eng & Shipbuild Co Ltd | Apparatus and method for testing catalytic activity |
| CN101858901A (en) * | 2010-07-07 | 2010-10-13 | 中国汽车技术研究中心 | System and method for testing activity of vehicle exhaust purification catalytic material |
| CN201848239U (en) * | 2010-11-18 | 2011-06-01 | 天津市先权工贸发展有限公司 | Full-automatic hydrogenation reaction device |
| 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 |
| CN204214820U (en) * | 2014-08-28 | 2015-03-18 | 天津市鹏翔科技有限公司 | A kind of integrating device for hydrogenation process evaluating catalyst |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004195386A (en) * | 2002-12-19 | 2004-07-15 | Mitsui Eng & Shipbuild Co Ltd | Apparatus and method for testing catalytic activity |
| CN101858901A (en) * | 2010-07-07 | 2010-10-13 | 中国汽车技术研究中心 | System and method for testing activity of vehicle exhaust purification catalytic material |
| CN201848239U (en) * | 2010-11-18 | 2011-06-01 | 天津市先权工贸发展有限公司 | Full-automatic hydrogenation reaction device |
| 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 |
| CN204214820U (en) * | 2014-08-28 | 2015-03-18 | 天津市鹏翔科技有限公司 | A kind of integrating device for hydrogenation process evaluating catalyst |
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