CN117686643A - Gaseous pollutant adsorption-desorption and catalysis evaluation system of solid adsorbent/catalyst - Google Patents
Gaseous pollutant adsorption-desorption and catalysis evaluation system of solid adsorbent/catalyst Download PDFInfo
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- 239000003344 environmental pollutant Substances 0.000 title claims abstract description 149
- 231100000719 pollutant Toxicity 0.000 title claims abstract description 149
- 239000003463 adsorbent Substances 0.000 title claims abstract description 55
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 43
- 239000003054 catalyst Substances 0.000 title claims abstract description 41
- 238000002336 sorption--desorption measurement Methods 0.000 title claims abstract description 35
- 239000007787 solid Substances 0.000 title claims abstract description 29
- 238000011156 evaluation Methods 0.000 title claims abstract description 26
- 238000002309 gasification Methods 0.000 claims abstract description 56
- 238000001179 sorption measurement Methods 0.000 claims abstract description 39
- 238000003795 desorption Methods 0.000 claims abstract description 23
- 238000001514 detection method Methods 0.000 claims abstract description 21
- 238000012360 testing method Methods 0.000 claims abstract description 14
- 238000010521 absorption reaction Methods 0.000 claims abstract description 12
- 238000009413 insulation Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000011056 performance test Methods 0.000 claims abstract description 8
- 230000001105 regulatory effect Effects 0.000 claims abstract description 4
- 230000001276 controlling effect Effects 0.000 claims abstract description 3
- 239000007789 gas Substances 0.000 claims description 77
- 238000006243 chemical reaction Methods 0.000 claims description 64
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 25
- 238000004321 preservation Methods 0.000 claims description 22
- 230000003197 catalytic effect Effects 0.000 claims description 17
- 239000010453 quartz Substances 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 229920000742 Cotton Polymers 0.000 claims description 6
- 239000000523 sample Substances 0.000 claims description 6
- 239000000356 contaminant Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000012159 carrier gas Substances 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 238000010998 test method Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 abstract description 10
- 238000002156 mixing Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 229920006395 saturated elastomer Polymers 0.000 abstract description 2
- TXCDCPKCNAJMEE-UHFFFAOYSA-N dibenzofuran Chemical compound C1=CC=C2C3=CC=CC=C3OC2=C1 TXCDCPKCNAJMEE-UHFFFAOYSA-N 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 239000000835 fiber Substances 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 238000009835 boiling Methods 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000035515 penetration Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000012494 Quartz wool Substances 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- KVGZZAHHUNAVKZ-UHFFFAOYSA-N 1,4-Dioxin Chemical compound O1C=COC=C1 KVGZZAHHUNAVKZ-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- FFHWARDRFNJTLA-UHFFFAOYSA-N [C].C1=CC=CC=2OC3=C(C21)C=CC=C3 Chemical class [C].C1=CC=CC=2OC3=C(C21)C=CC=C3 FFHWARDRFNJTLA-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000002156 adsorbate Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
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- -1 dibenzofuran/dioxin analog compounds Chemical class 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 229920001973 fluoroelastomer Polymers 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
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- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229940008718 metallic mercury Drugs 0.000 description 1
- 125000001997 phenyl group Chemical class [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 150000003071 polychlorinated biphenyls Chemical group 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to a gaseous pollutant adsorption-desorption and catalysis evaluation system of a solid adsorbent/catalyst, which comprises a pollutant gasification unit, a fixed bed adsorption-desorption/catalysis unit and a tail gas detection unit; an insulation box I is arranged between the pollutant gasification unit and the fixed bed adsorption/desorption/catalysis unit. The beneficial effects of the invention are as follows: the pollutant gasifying unit is used for gasifying the pollutants which are liquid and solid at normal temperature, so that the pollutant gasifying unit can be used for carrying out adsorption and desorption/catalysis performance test on the gasified pollutants by the adsorbent/catalyst; by arranging three gas paths in front of the pollutant gasification unit, uniform mixing of various gaseous pollutants is realized, the gas concentration is regulated, and the high-temperature working condition in the actual application process is simulated; the high-temperature three-way valve is used for controlling the airflow to flow into the fixed bed adsorption/desorption/catalysis unit or the tail gas absorption device, so that the initial concentration of pollutants can be conveniently read and calibrated, and the adsorbent or the catalyst is filled after the inner wall of the pipeline is saturated in adsorption, so that the test error is effectively reduced.
Description
Technical Field
The invention belongs to the technical field of adsorption and desorption and catalytic performance evaluation, and particularly relates to a gaseous pollutant adsorption and desorption and catalytic evaluation system of a solid adsorbent/catalyst.
Background
Along with the rapid development of the industry in China, the adsorbent and the catalyst are widely applied in the fields of environment, chemical industry and the like, for example, a garbage incineration power plant adopts activated carbon to treat dioxin substances in high-temperature flue gas at 100-200 ℃. Aiming at the pollutants which are in a gaseous state under the actual high-temperature working condition but are in a solid state at normal temperature, the conventional gas adsorption/catalysis system is difficult to realize the gasification of the solid pollutants and perform adsorption and desorption or catalysis performance evaluation. In order to avoid resource waste and environmental risks caused by ineffective use of the adsorbent/catalyst, it is highly desirable to develop a gas-phase desorption and catalytic performance evaluation system that satisfies various contaminants, particularly high-boiling-point, difficult-to-volatilize contaminants.
CN115144296a discloses a multi-mode adsorption performance testing system, which can realize in-situ pressure swing adsorption testing of adsorbents by adopting various adsorbents under the working condition of rapid temperature rise and drop. Compared with a fixed bed reactor, the adsorption performance is evaluated by testing a dynamic penetration curve, the static adsorption technology adopted by the system has a large gap from the actual application scene, and the industrial production is difficult to predict and guide accurately.
Publication number CN104792932B discloses a catalyst/adsorbent evaluation device for multicomponent feed, which can achieve uniform mixing of a plurality of component gases of feed and perform catalytic/adsorption performance evaluation by a fixed bed reaction device. However, the device can only perform adsorption/catalysis performance test of gaseous pollutants, and cannot perform adsorption or catalysis performance evaluation of pollutants which are liquid or solid at normal temperature.
Publication number CN115452984a discloses an adsorbent adsorption performance evaluation system that can evaluate the adsorption performance of adsorbents at different temperatures and different amounts. However, the adsorbate used is still limited to substances which are gaseous at normal pressure and normal temperature.
In summary, the dynamic adsorption and desorption or catalytic performance test performed by the fixed bed reactor is limited to the liquid pollutant with gaseous state or partial low boiling point at normal temperature and normal pressure, and the adsorption and desorption or catalytic performance evaluation of the existing reactor system is difficult to complete for the pollutant with high boiling point and difficult volatilization.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a gaseous pollutant adsorption-desorption and catalysis evaluation system of a solid adsorbent/catalyst.
The gaseous pollutant adsorption-desorption and catalysis evaluation system of the solid adsorbent/catalyst comprises: the device comprises a pollutant gasification unit, a fixed bed adsorption/desorption/catalysis unit and a tail gas detection unit; an insulation box I is arranged between the pollutant gasification unit and the fixed bed adsorption/desorption/catalysis unit;
a high-temperature three-way valve is arranged in one end of the heat preservation box connected with the pollutant gasification unit, an outlet of the pollutant gasification unit is connected to an inlet of the high-temperature three-way valve, and two outlets of the high-temperature three-way valve are respectively connected with the fixed bed adsorption/desorption/catalysis unit and the tail gas absorption device;
the fixed bed adsorption/desorption/catalysis unit comprises a gaseous pollutant reaction tube, an adsorbent/catalyst is supported in the gaseous pollutant reaction tube through a quartz sand core and quartz cotton, the outlet end of the gaseous pollutant reaction tube is connected with a tail gas detection unit, and the tail gas detection unit comprises a gas chromatograph.
Preferably, the pollutant gasification unit comprises a pollutant gasification pipe and a high-temperature reaction furnace I, the middle part of the pollutant gasification pipe is arranged in the high-temperature reaction furnace I, and a quartz crucible is arranged in the pollutant gasification pipe; the fixed bed adsorption/desorption/catalysis unit comprises a gaseous pollutant reaction tube and a high-temperature reaction furnace II, and the middle part of the gaseous pollutant reaction tube is arranged in the high-temperature reaction furnace II.
Preferably, a second insulation box is further arranged between the fixed bed adsorption/desorption/catalysis unit and the tail gas detection unit, a filter is arranged in the second insulation box, and temperature sensing probes are arranged in the pollutant gasification pipe, the first insulation box, the gaseous pollutant reaction pipe and the second insulation box.
Preferably, the inlet of the pollutant gasification unit is connected with three gas paths which are respectively used for introducing nitrogen, oxygen and pollutant gas, the three gas paths are sequentially provided with a filter, a switch valve, a mass flowmeter and a one-way valve, the three gas paths are connected to the mixer and then connected to the inlet of the pollutant gasification unit, and a pressure gauge is arranged between the mixer and the pollutant gasification unit.
The method for using the solid adsorbent/catalyst gaseous pollutant adsorption-desorption and catalysis evaluation system comprises the following steps:
step one, under the condition of not filling an adsorbent/catalyst, a high-temperature three-way valve is regulated to enable a gas path to enter a tail gas detection unit;
step two, after the gaseous pollutant reaction tube and the gas chromatograph are heated to the set temperature, starting the pollutant gasification unit and carrying gas until the gas chromatograph shows that the tail gas concentration is constant;
and step three, rotating the high-temperature three-way valve to enable the pollutant air flow to be discharged outside and enter the tail gas absorption device, simultaneously filling the adsorbent/catalyst in the gaseous pollutant reaction tube, and rotating the high-temperature three-way valve to enable the air flow to flow through the fixed bed adsorption/desorption/catalysis unit and the tail gas detection unit to perform adsorption/catalysis performance test.
Preferably, the step three is repeated, and the adsorption/catalytic performance continuous test of a plurality of samples can be realized by replacing the adsorbent/catalyst samples each time.
Preferably, when the adsorbent is filled in the gaseous pollutant reaction tube, the third step further comprises a fourth step of: and after the adsorbent reaches an adsorption saturation state, the high-temperature three-way valve is rotated to control the pollutant air flow to be discharged outside and enter the tail gas absorption device, and then the gas pollutant air inlet is stopped or the heating of the pollutant gasification unit is stopped.
Preferably, the method further comprises a desorption test method, and step five is implemented after step four: and (3) enabling the temperature of the gaseous pollutant reaction tube to reach a set desorption temperature, rotating the high-temperature three-way valve, controlling carrier gas to enter the gaseous pollutant reaction tube to blow off the adsorbent, and carrying out desorption test.
The beneficial effects of the invention are as follows:
1) Besides gaseous pollutants, the invention also realizes the gasification of the pollutants which are liquid and solid at normal temperature through the pollutant gasification unit, so that the pollutants can be subjected to adsorption and desorption/catalysis performance test of the adsorbent/catalyst on the gasified pollutants.
2) According to the invention, the three gas paths are arranged in front of the pollutant gasification unit, so that uniform mixing of various gaseous pollutants is realized, the gas concentration is regulated, and the high-temperature working condition in the practical application process is simulated.
3) According to the invention, the high-temperature three-way valve can control the airflow to flow into the fixed bed adsorption/desorption/catalysis unit or the tail gas absorption device, so that the initial concentration of pollutants can be conveniently read and calibrated, and the adsorbent or the catalyst is filled after the inner wall of the pipeline is adsorbed and saturated, so that the test error can be effectively reduced.
4) According to the invention, through the slender structure of the quartz crucible in the pollutant gasification pipe, the full gasification of solid and liquid pollutants can be realized, the fluctuation of the gasified airflow concentration is within 1.0%, and the test precision is improved.
Drawings
FIG. 1 is a schematic diagram of the structure of the present invention;
FIG. 2 is a graph showing the concentration of contaminant gas stream in accordance with the third embodiment;
FIG. 3 is a graph of dynamic permeation profile of an adsorbent in a third embodiment.
Reference numerals illustrate: the device comprises a pollutant gasification pipe 1, a first high-temperature reaction furnace 2, a quartz crucible 3, a high-temperature three-way valve 4, a first heat preservation box 5, a second high-temperature reaction furnace 6, an adsorbent/catalyst 7, a quartz sand core 8, quartz wool 9, a gaseous pollutant reaction pipe 10, a second heat preservation box 11, a filter 12, a heat preservation pipe sleeve 13, a one-way valve 14, a mass flowmeter 15, a switch valve 16 and a filter 17.
Detailed Description
The invention is further described below with reference to examples. The following examples are presented only to aid in the understanding of the invention. It should be noted that it will be apparent to those skilled in the art that modifications can be made to the present invention without departing from the principles of the invention, and such modifications and adaptations are intended to be within the scope of the invention as defined in the following claims.
Example 1
As an example, as shown in fig. 1, the gaseous pollutant adsorption-desorption and catalysis evaluation system of the solid adsorbent/catalyst comprises: the device comprises a pollutant gasification unit, a fixed bed adsorption/desorption/catalysis unit and a tail gas detection unit; an insulation box I5 is arranged between the pollutant gasification unit and the fixed bed adsorption/desorption/catalysis unit;
the inlet of the pollutant gasification unit is connected with three gas paths which are respectively used for introducing nitrogen, oxygen and pollutant gases including but not limited to carbon dioxide, sulfur dioxide, ammonia, nitrogen oxides and other pollutants which are gaseous at normal temperature. The three gas paths are sequentially provided with a filter 17, a switch valve 16, a mass flowmeter 15 and a one-way valve 14, and are connected to the inlets of the pollutant gasification units after being connected to the mixer, and a pressure gauge is arranged between the mixer and the pollutant gasification units and used for judging the blocking condition of the rear-end gas path.
The pollutant gasification unit comprises a pollutant gasification pipe 1 and a high-temperature reaction furnace I2, the middle part of the pollutant gasification pipe 1 is arranged in the high-temperature reaction furnace I2, and a quartz crucible 3 is arranged in the pollutant gasification pipe 1 and is used for gasifying liquid and solid pollutants to obtain stable pollutant air flow; the first high-temperature reaction furnace 2 is an open type furnace chamber integrating furnace wires and sintered fibers.
The first heat preservation box 5 is internally provided with an M-type heater, the heat preservation temperature is RT-600 ℃, one end of the first heat preservation box 5, which is connected with the pollutant gasification unit, is internally provided with a high-temperature three-way valve 4 and is also opened, the high-temperature three-way valve 4 is convenient to adjust, the outlet of the pollutant gasification unit is connected to the inlet of the high-temperature three-way valve 4, two outlets of the high-temperature three-way valve 4 are connected with a fixed bed adsorption/desorption/catalysis unit, and the other end of the first heat preservation box 5 is externally connected with a tail gas absorption device.
The fixed bed adsorption/desorption/catalysis unit comprises a gaseous pollutant reaction tube 10 and a second high-temperature reaction furnace 6, the middle part of the gaseous pollutant reaction tube 10 is arranged in the second high-temperature reaction furnace 6, the second high-temperature reaction furnace 6 is an open type furnace, and the furnace wires are sintered into fiber integrated hearth.
The inside of the gaseous pollutant reaction tube 10 is supported with an adsorbent/catalyst 7 through a quartz sand core 8 and a quartz cotton 9, the quartz cotton 9 is internally provided with a liner tube for fixation, the outlet end of the gaseous pollutant reaction tube 10 is connected with a tail gas detection unit, and the tail gas detection unit comprises a gas chromatograph and is used for tail gas concentration measurement.
And a second insulation box 11 is arranged between the fixed bed adsorption/desorption/catalysis unit and the tail gas detection unit, and a filter 12 with a filter element with a pore diameter of 3 mu m is arranged in a pipeline in the second insulation box 11 and is used for intercepting the powder of the escaping adsorbent/catalyst 7. The second heat preservation box 11 adopts a detachable hose to heat a heat preservation sleeve, a temperature sensing probe is arranged in the heat preservation sleeve, and the heat preservation temperature is RT-600 ℃. The pollutant gasification pipe 1, the first insulation box 5, the gaseous pollutant reaction pipe 10 and the second insulation box 11 are respectively provided with a temperature sensing probe.
Example two
As another embodiment, in the second embodiment, on the basis of the first embodiment, a gaseous pollutant adsorption/desorption and catalysis evaluation system of the solid adsorbent/catalyst is provided:
the pipelines in the system are all made of 316L stainless steel pipe fittings, and the pipelines are connected with the valve parts by adopting 316L stainless steel cutting ferrule. The gaseous pollutant reaction tube 10 is made of 316L stainless steel, graphite gaskets at two ends are sealed, and threads are fastened; the built-in liner tube is placed in a quartz crucible 3 for gasifying pollutants which are liquid or solid at normal temperature, wherein the liquid pollutants comprise but are not limited to acetone, ethanol, benzene series and the like, and the solid pollutants comprise but are not limited to dibenzofuran/dioxin analog compounds, polychlorinated biphenyl, metallic mercury and the like; the quartz crucible 3 adopts an elongated cylindrical structure so as to ensure that liquid or molten pollutants have constant volatilization area in the long-time testing process, and improve the concentration stability of the pollutants.
The first high-temperature reaction furnace 2 in the pollutant gasification unit adopts a furnace wire sintering fiber integrated hearth, the heating temperature of the furnace wire is RT-1200 ℃, and the hearth adopts an open type design, so that the gasification pipe is convenient to install.
The gaseous pollutant reaction tube 10 in the fixed bed adsorption/desorption/catalysis unit can be a 316L stainless steel tube or a quartz tube according to the reaction temperature, and the quartz tube is sealed by fluororubber and fastened by threads. The adsorbent/catalyst 7, the quartz sand core 8 and the quartz cotton 9 are respectively arranged in the gaseous pollutant reaction tube 10 according to the airflow direction. The quartz wool 9 is used for fixing the quartz sand core 8 and filling gaps between the quartz sand core 8 and the inner wall of the gaseous pollutant reaction tube 10; the quartz sand core 8 can select 10-550 mu m aperture for supporting adsorbents/catalysts 7 with different particle diameters; the adsorbent/catalyst 7 can be filled with more than 300 meshes of particle size, so that the testing requirements of most adsorbents/catalysts 7 are met.
The second high-temperature reaction furnace 6 in the fixed bed adsorption/desorption/catalysis unit adopts a furnace wire sintering fiber integrated hearth, the heating temperature of the furnace wire is RT-1200 ℃, and the hearth adopts an open type design, so that the gaseous pollutant reaction tube 10 is convenient to install.
The gas chromatograph in the tail gas detection unit is provided with an automatic sample injection six-way valve, so that the concentration is automatically monitored. The gas chromatograph gas outlet is externally connected with a tail gas absorption device, so that pollutant leakage is avoided.
It should be noted that, in this embodiment, the same or similar parts as those in the first embodiment may be referred to each other, and will not be described in detail in this application.
Example III
As another embodiment, the third embodiment is provided based on the first and second embodiments, and an embodiment of the method for using the solid adsorbent/catalyst for adsorption, desorption and catalytic evaluation of gaseous pollutants, including the steps of:
step one, filling 0.8g of dibenzofuran solid in a gasification pipe, and adjusting a high-temperature three-way valve 4 to enable a gas path to enter a gas chromatograph through a gaseous pollutant reaction pipe 10 under the condition that the gaseous pollutant reaction pipe 10 is not filled with active carbon, wherein the melting point of the dibenzofuran is 86 ℃ and the boiling point of the dibenzofuran is 287 ℃;
setting a first 5 target heat preservation temperature of a heat preservation box at 150 ℃, a second 6 target adsorption temperature of a high-temperature reaction furnace at 150 ℃, a second 11 heat preservation temperature of the heat preservation box at 300 ℃, a heat preservation pipe sleeve at 13 heat preservation temperature of 300 ℃ and a gas chromatographic column at 240 ℃.
When the first heat preservation box, the second reaction furnace, the second heat preservation box, the heat preservation pipe sleeve and the gas chromatograph reach the target temperature; starting a first reaction furnace, setting a target volatilization temperature of 130 ℃, and heating at a rate of 10 ℃/min; turn on N 2 And (3) carrying out carrier gas, and setting the airflow flow to be 0.2L/min.
When the gas chromatograph shows that the concentration of the tail gas is stable within 1h, according to the concentration fluctuation rate= (real-time concentration-average concentration)/average concentration multiplied by 100%, and when the gas flow concentration fluctuation is within 1.0%, as shown in fig. 2, it is explained that the pipeline, the quartz sand core 8 and the quartz cotton 9 reach adsorption saturation, and meanwhile, the pollutant gasification unit enters a stable operation state.
And step three, rotating the high-temperature three-way valve 4 to control the air flow to enter the tail gas absorption device, wherein the pollutant gasification unit operates normally at the moment, and the pollutant concentration is not fluctuated.
Taking down the gaseous pollutant reaction tube 10, filling 0.2g of active carbon with the particle size of 100-200 meshes as an adsorbent, and after the gaseous pollutant reaction tube 10 reaches the set adsorption temperature, rotating the high-temperature three-way valve 4 to control the airflow to flow through the pollutant reaction tube 10 for adsorption performance test, wherein the test result is shown in figure 3.
And step three, the adsorption performance of a plurality of samples can be continuously tested by replacing different adsorbents each time, and the stable operation of the pollutant gasification unit is not affected during the continuous test.
From the penetration curve obtained in fig. 3, the penetration time and the adsorption amount can be calculated, and the results are shown in table 1.
TABLE 1 dynamic adsorption data for activated carbon dibenzofurans
Example IV
As another embodiment, the fourth embodiment proposes a desorption performance test embodiment based on the third embodiment, and the third step is followed by the fourth step and the fifth step:
and step four, after the tail gas detection unit shows that the adsorbent reaches an adsorption saturation state, rotating the high-temperature three-way valve 4 to control the discharge of the pollutant air flow to enter the tail gas absorption device, and then closing the gas pollutant air inlet valve or removing the quartz crucible 3 in which the liquid and solid pollutants are placed.
And fifthly, when the gas flow does not contain pollutants, the high-temperature reaction furnace II 6 reaches the set desorption temperature, the high-temperature three-way valve 4 is rotated, and carrier gas is controlled to enter the gaseous pollutant reaction tube 10 to blow off the adsorbent.
And finally, calculating desorption performance according to the concentration of the desorption tail gas measured by the tail gas detection unit.
Example five
As another embodiment, the fifth embodiment provides, based on the third embodiment, that the gaseous pollutant reaction tube 10 may be loaded with a catalyst, and the catalytic performance may be calculated according to the concentration of the catalytic product measured by the exhaust gas detection unit by using the solid adsorbent/catalyst gaseous pollutant adsorption-desorption and catalytic evaluation system.
In this specification, each embodiment is described in a progressive manner, and each embodiment is mainly described by a difference from other embodiments, and identical and similar parts between the embodiments are referred to each other.
Claims (8)
1. A solid adsorbent/catalyst gaseous contaminant adsorption and catalytic evaluation system comprising: the device comprises a pollutant gasification unit, a fixed bed adsorption/desorption/catalysis unit and a tail gas detection unit; an insulation box I is arranged between the pollutant gasification unit and the fixed bed adsorption/desorption/catalysis unit;
a high-temperature three-way valve is arranged in one end of the heat preservation box connected with the pollutant gasification unit, an outlet of the pollutant gasification unit is connected to an inlet of the high-temperature three-way valve, and two outlets of the high-temperature three-way valve are respectively connected with the fixed bed adsorption/desorption/catalysis unit and the tail gas absorption device;
the fixed bed adsorption/desorption/catalysis unit comprises a gaseous pollutant reaction tube, an adsorbent/catalyst is supported in the gaseous pollutant reaction tube through a quartz sand core and quartz cotton, the outlet end of the gaseous pollutant reaction tube is connected with a tail gas detection unit, and the tail gas detection unit comprises a gas chromatograph.
2. The system for adsorption, desorption and catalysis evaluation of gaseous pollutants of solid adsorbent/catalyst according to claim 1, wherein the pollutant gasification unit comprises a pollutant gasification pipe and a high-temperature reaction furnace I, the middle part of the pollutant gasification pipe is arranged in the high-temperature reaction furnace I, and a quartz crucible is arranged in the pollutant gasification pipe; the fixed bed adsorption/desorption/catalysis unit comprises a gaseous pollutant reaction tube and a high-temperature reaction furnace II, and the middle part of the gaseous pollutant reaction tube is arranged in the high-temperature reaction furnace II.
3. The system for adsorption, desorption and catalysis evaluation of gaseous pollutants of solid adsorbent/catalyst according to claim 2, wherein a second incubator is further arranged between the fixed bed adsorption, desorption/catalysis unit and the tail gas detection unit, a filter is arranged in the second incubator, and temperature sensing probes are arranged in the pollutant gasification pipe, the first incubator, the gaseous pollutant reaction pipe and the second incubator.
4. The system for adsorption, desorption and catalytic evaluation of gaseous pollutants of solid adsorbent/catalyst according to claim 1, wherein the inlet of the pollutant gasification unit is connected with three gas paths for introducing nitrogen, oxygen and pollutant gases, the three gas paths are sequentially provided with a filter, a switch valve, a mass flowmeter and a one-way valve, the three gas paths are connected to the mixer and then connected to the inlet of the pollutant gasification unit, and a pressure gauge is installed between the mixer and the pollutant gasification unit.
5. A method of using the solid adsorbent/catalyst gaseous contaminant adsorption and catalytic evaluation system according to any one of claims 1 to 4, comprising the steps of:
step one, under the condition of not filling an adsorbent/catalyst, a high-temperature three-way valve is regulated to enable a gas path to enter a tail gas detection unit;
step two, after the gaseous pollutant reaction tube and the gas chromatograph are heated to the set temperature, starting the pollutant gasification unit and carrying gas until the gas chromatograph shows that the tail gas concentration is constant;
and step three, rotating the high-temperature three-way valve to enable the pollutant air flow to be discharged outside and enter the tail gas absorption device, simultaneously filling the adsorbent/catalyst in the gaseous pollutant reaction tube, and rotating the high-temperature three-way valve to enable the air flow to flow through the fixed bed adsorption/desorption/catalysis unit and the tail gas detection unit to perform adsorption/catalysis performance test.
6. The method of claim 5, wherein the step three is repeated, and each time the adsorbent/catalyst sample is replaced, the continuous test of the adsorption/catalytic performance of a plurality of samples can be realized.
7. The method of using a solid adsorbent/catalyst gaseous pollutant adsorption/desorption and catalytic evaluation system according to claim 5, wherein when the gaseous pollutant reaction tube is filled with adsorbent, step three is followed by step four: and after the adsorbent reaches an adsorption saturation state, the high-temperature three-way valve is rotated to control the pollutant air flow to be discharged outside and enter the tail gas absorption device, and then the gas pollutant air inlet is stopped or the heating of the pollutant gasification unit is stopped.
8. The method of using a solid adsorbent/catalyst gaseous pollutant adsorption/desorption and catalytic evaluation system according to claim 7, further comprising a desorption test method, wherein step four is followed by step five: and (3) enabling the temperature of the gaseous pollutant reaction tube to reach a set desorption temperature, rotating the high-temperature three-way valve, controlling carrier gas to enter the gaseous pollutant reaction tube to blow off the adsorbent, and carrying out desorption test.
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