CN111773876A - Precise gas adsorption system for temperature programmed desorption - Google Patents
Precise gas adsorption system for temperature programmed desorption Download PDFInfo
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- CN111773876A CN111773876A CN202010547258.9A CN202010547258A CN111773876A CN 111773876 A CN111773876 A CN 111773876A CN 202010547258 A CN202010547258 A CN 202010547258A CN 111773876 A CN111773876 A CN 111773876A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
- B01D53/0407—Constructional details of adsorbing systems
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2259/00—Type of treatment
- B01D2259/40—Further details for adsorption processes and devices
- B01D2259/40083—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption
- B01D2259/40088—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption by heating
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Abstract
The invention discloses a precise gas adsorption system for temperature programmed desorption, which comprises a vacuum subsystem, a gas circuit subsystem and a gas sample injection head, wherein the vacuum subsystem comprises a backing pump, a vacuum cavity and a vacuum gauge; the gas path subsystem comprises a single gas path, two gas paths or a plurality of gas paths, and each gas path comprises a sample pool, a gas storage tank and a precise vacuum gauge; the gas sample injection head is an overflow molecular beam sample injection head, the outlet end of the gas sample injection head is a porous micro-channel plate, and the gas sample injection head is provided with a heating part. Compared with the traditional gas adsorption mode, the precise gas adsorption system realizes the precise adsorption of different gases in the temperature programmed desorption system, wherein the adsorption is less than 0.1 Monolayer (ML), the gas system of the device can rapidly switch different gases, and can also rapidly expand/reduce the number of parallel gas paths.
Description
Technical Field
The invention relates to the technical field of instrument equipment, in particular to a precise gas adsorption system for temperature programmed desorption.
Background
Temperature programmed desorption analysis (TPD) systems are widely used for catalytic process research. After adsorption of molecules onto the catalyst surface, the molecules adsorbed on the catalyst surface desorb from the catalyst surface when the catalyst is heated to a point where the energy barrier (commonly referred to as desorption activation energy) that the molecules need to overcome to escape is overcome. The energy required for desorption is different due to the different binding capacities between different adsorbates and the same surface, or between the same adsorbate and adsorption centres with different properties on the surface. Therefore, the thermal desorption experimental results not only reflect the binding capacity between the adsorbate and the solid surface, but also reflect the kinetic behavior at the temperature and surface coverage at which desorption occurs.
The gas adsorption is one of the steps of the TPD experiment, the main function of the gas adsorption is to enable different molecules to be adsorbed on the surface of the catalyst, the control of the adsorption quantity and the adsorption uniformity degree are the key points of the accuracy of the TPD experiment. The traditional gas adsorption mode is a background adsorption mode, which cannot accurately control gas adsorption, and the adsorption uniformity degree cannot be ensured. A precise gas adsorption system capable of precisely controlling the adsorption process is a necessary condition for realizing a high-precision temperature programmed desorption experiment. How to design a precise gas adsorption system with high applicability is one of the bottlenecks in the development of the TPD experimental device.
Disclosure of Invention
The invention aims to provide a precise gas adsorption system for temperature programmed desorption, which aims to overcome the defects of the prior art.
The invention adopts the following technical scheme:
a precise gas adsorption system for programmed temperature desorption, which comprises a vacuum subsystem, a gas circuit subsystem and a gas sample injection head,
the vacuum subsystem comprises a backing pump, a vacuum cavity and a vacuum gauge, wherein the backing pump is connected with the vacuum pump through a backing pump valve and a pipeline; the vacuum cavity is provided with a vacuum gauge;
the gas path subsystem comprises a single gas path, two gas paths or a plurality of gas paths, and each gas path comprises a sample pool, a gas storage tank and a precise vacuum gauge; the sample tank and the vacuum cavity are respectively connected to an air inlet pipeline of the air storage tank through pipelines, the sample tank is provided with a valve, the pipeline connecting the sample tank and the air inlet pipeline of the air storage tank and the pipeline connecting the vacuum cavity and the air inlet pipeline of the air storage tank are provided with valves, the air inlet pipeline of the air storage tank is provided with a valve, the air storage tank is provided with a precision vacuum gauge, and the air outlet pipeline of the air storage tank is provided with a valve; an outlet of an air outlet pipeline of the air storage tank of each air path is connected to an air inlet pipeline of the gas sample injection head in parallel, the air inlet pipeline of the gas sample injection head is connected with an air inlet end of the gas sample injection head, and an air inlet valve is arranged on the air inlet pipeline of the gas sample injection head;
the gas inlet end of the gas sampling head is connected with the vacuum cavity through a first bypass pipeline, a gas outlet valve is arranged at the position, close to the gas sampling head, of the first bypass pipeline, and a first bypass valve is arranged at the position, close to the vacuum cavity, of the first bypass pipeline; a gas inlet pipeline of a gas sample injection head between the gas inlet valve and each gas outlet pipeline of the gas circuit and gas storage tank is connected with the vacuum cavity through a second bypass pipeline, a second bypass valve is arranged at the position, close to the gas inlet valve, of the second bypass pipeline, and a valve is arranged at the position, close to the vacuum cavity, of the second bypass pipeline;
the gas sample injection head is an overflow molecular beam sample injection head, the outlet end of the gas sample injection head is a porous micro-channel plate, and the gas sample injection head is provided with a heating part.
Further, an integral toasting subsystem is also provided.
Furthermore, a heating component is arranged in the sample cell.
Furthermore, the backing pump is a dry backing pump, and the vacuum pump is a molecular pump.
Further, the air path subsystem comprises three or four air paths.
Furthermore, the opening and closing time of the air inlet valve and the air outlet valve is automatically controlled.
The invention has the beneficial effects that:
1. the invention relates to a precise gas adsorption system for programmed temperature desorption, which comprises a vacuum subsystem, a gas circuit subsystem and a gas sample injection head, wherein the amount of adsorbed gas can be precisely controlled by precisely controlling the opening and closing time of an air inlet valve and an air exhaust valve and measuring the pressure change in a gas storage tank according to a precise vacuum gauge; the gas is uniformly adsorbed through the gas sample introduction head with the porous micro-channel plate, so that the purpose of accurately controlling gas sample introduction adsorption is achieved, and the applicability of an adsorption system to different gases is improved. The invention can be used for the precise adsorption sample injection of less than 0.1 Monolayer (ML) of different gases in a vacuum system.
2. The gas circuit subsystem comprises a single gas circuit, double gas circuits or a plurality of gas circuits, wherein the plurality of gas circuits are connected in parallel, so that different gases can be rapidly switched, and the number of the parallel gas circuits (mixed sample measurement) can be rapidly expanded/reduced.
3. The outlet end of the gas sample injection head is provided with a porous micro-channel plate, so that samples are uniformly dispersed and injected. The gas sampling head is provided with a heating part, the gas sampling head can be heated after the sampling is finished, and residual gas adsorbed in the gas sampling head pipe is removed by matching with the gas outlet valve, the first bypass and the vacuum pump.
4. After the sample introduction is finished, the residual gas in the pipeline between the gas circuit subsystem and the sample introduction valve can be quickly cleaned by matching the second bypass and the vacuum pump, so that the sample in another parallel pipeline can be detected, and the parallel pipeline can be quickly switched to different gases. And gas mixing sampling of two or more pipelines can be realized simultaneously.
5. The invention is provided with an integral baking subsystem, after the integral precise gas adsorption system is vacuumized, the integral baking subsystem is utilized to bake while vacuumizing so as to remove water and other gases in the system, thus leading the vacuum degree of the whole system to be better.
6. The sample cell is internally provided with the heating part, so that the sample cell can contain gas and liquid, and the liquid can be heated and gasified to enter the gas storage tank.
Drawings
Fig. 1 is a schematic structural diagram of a precision gas adsorption system for temperature programmed desorption according to the present invention.
Fig. 2 is a schematic side view of a temperature programmed desorption precision gas adsorption system according to the present invention.
Fig. 3 is a schematic view of a gas sample injection structure.
Fig. 4 is a schematic view of the end structure of the gas injection head.
1 gas sample injection head, 2 gas outlet valves, 3 gas inlet valves, 4 second bypass valves, 5 first bypass pipelines, 6 valves, 7 valves, 8 valves, 9 precision vacuum gauges, 10 precision vacuum gauges, 11 precision vacuum gauges, 12 second bypass pipelines, 13 gas storage tanks, 14 gas storage tanks, 15 gas storage tanks, 16 valves, 17 valves, 18 valves, 19 valves, 20 valves, 21 valves, 22 first bypass valves, 23 valves, 24 valves, 25 valves, 26 valves, 27 valves, 28 valves, 29 valves, 30 blind flange, 31 sample tanks, 32 sample tanks, 33 sample tanks, 34 vacuum pumps, 35 backing pumps, 36 valves, 37 vacuum pump valves, 38 vacuum gauges, 39 flanges, 40 heating wires, 41 porous microchannel plates, 42 temperature control temperature measurement elements and 43 backing pump valves.
Detailed Description
The invention is explained in more detail below with reference to exemplary embodiments and the accompanying drawings. The following examples are provided only for illustrating the present invention and are not intended to limit the scope of the present invention.
A precise gas adsorption system for temperature programmed desorption, which is shown in figures 1-4 and comprises a vacuum subsystem, a gas circuit subsystem and a gas sample injection head,
the vacuum subsystem comprises a backing pump 35, a vacuum pump 34, a vacuum cavity and a vacuum gauge 38, wherein the backing pump 35 can be a dry backing pump, the vacuum pump 34 can be a molecular pump, the backing pump 35 and the vacuum pump 34 are connected through a backing pump valve 43 and a pipeline, the backing pump 35 is connected with the vacuum cavity through a backing pump valve 43, a pipeline and a valve 36, and the vacuum pump 34 is connected with the vacuum cavity through a vacuum pump valve 37 and a pipeline; the vacuum cavity is provided with a vacuum gauge 38 for detecting the vacuum degree in the vacuum cavity, and the vacuum gauge with an Agilent model FRG-702 can be selected;
the air path subsystem comprises a single air path, two air paths or a plurality of air paths, preferably three air paths or four air paths, and fig. 1 shows three air paths, wherein each air path comprises sample pools 31, 32 and 33, air storage tanks 13, 14 and 15, and precision vacuum gauges 9, 10 and 11; preferably, heating parts are arranged in the sample tanks 31, 32 and 33, so that the sample tanks 31, 32 and 33 can contain gas and liquid, and the liquid can be heated and gasified to enter the gas storage tanks 13, 14 and 15; the sample tanks 31, 32, 33 and the vacuum cavities are respectively connected to an air inlet pipeline of the air storage tank through pipelines, the sample tanks 31, 32 and 33 are provided with valves 27, 28 and 29, the pipelines for connecting the sample tanks 31, 32 and 33 and the air inlet pipeline of the air storage tank are provided with valves 23, 24 and 25, and the pipelines for connecting the vacuum cavities and the air inlet pipeline of the air storage tank are provided with valves 19, 20 and 21, the air inlet pipeline of the air storage tank is provided with valves 16, 17 and 18, the air storage tanks 13, 14 and 15 are provided with precision vacuum gauges 9, 10 and 11, the precision vacuum gauges 9, 10 and 11 can detect the gas pressure in the air storage tanks 13, 14 and 15, and the vacuum gauges with model number of ZKJ-210Z of Shanghai Zhe; the air outlet pipeline of the air storage tank is provided with valves 6, 7 and 8; an outlet of an air outlet pipeline of the air storage tank of each air path is connected in parallel to an air inlet pipeline of the gas sample injection head, the air inlet pipeline of the gas sample injection head is connected with an air inlet end of the gas sample injection head 1, and an air inlet valve 3 is arranged on the air inlet pipeline of the gas sample injection head;
the gas inlet end of the gas sampling head 1 is connected with the vacuum cavity through a first bypass pipeline 5, a gas outlet valve 2 is arranged at the position, close to the gas sampling head 1, of the first bypass pipeline 5, and a first bypass valve 22 is arranged at the position, close to the vacuum cavity, of the first bypass pipeline 5; a gas inlet pipeline of a gas sample injection head between the gas inlet valve 3 and each gas outlet pipeline of the gas circuit and gas storage tank is connected with the vacuum cavity through a second bypass pipeline 12, a second bypass valve 4 is arranged at the position, close to the gas inlet valve 3, of the second bypass pipeline 12, and a valve 26 is arranged at the position, close to the vacuum cavity, of the second bypass pipeline 12;
the gas sample injection head 1 is an overflow molecular beam sample injection head, the outlet end is a porous micro-channel plate 41 which is a capillary array, so that a gas sample is uniformly dispersed and injected; the gas sampling head 1 is provided with a heating part which is an independent heating part and comprises a heating wire 40 (partial heating wire is drawn in fig. 3 and fig. 4) and a temperature control and measurement element 42, after sampling is completed, the heating wire 40 is electrified to heat the gas sampling head 1, and then residual gas adsorbed in the gas sampling head 1 is removed.
Preferably, the opening and closing time of the inlet valve 3 and the outlet valve 2 is automatically controlled by an intelligent control device such as a computer, and the amount of the sample gas can be accurately controlled according to the pressure change in the gas storage tanks 13, 14 and 15.
Preferably, the whole precision gas adsorption system is further equipped with a whole baking subsystem (not shown in fig. 1), the whole baking subsystem is a heating belt, and after the whole precision gas adsorption system is vacuumized, before the whole precision gas adsorption system is used, the whole precision gas adsorption system is covered by the heating belt except for the backing pump 35 and the vacuum pump 34, and baking is carried out while vacuumizing, so as to remove water and other gases in the system, and the vacuum degree of the whole system is better.
The TPD experiments were performed in ultra-high vacuum chambers and the invention is not further described.
Before use, all valves (including the backing pump valve 43 and the valve 36, excluding the inlet valve 3, the outlet valve 2 and the vacuum pump valve 37) are opened, the backing pump 35 is started, and the vacuum chamber and the gas circuit subsystem are vacuumized to 1 × 10-2Torr～1*10-3Torr, closing valve 36, opening vacuum pump valve 37, starting vacuum pump 34, and vacuumizing the vacuum cavity and gas circuit subsystem to 1 × 10- 6Torr～1*10-8On the Torr scale. Except for the pre-pump 35, the vacuum pump 34 and the gas sampling head 1, the whole system is coated by a heating belt, and the baking is carried out while vacuumizing, optionally, the baking temperature is 100 ℃, and the baking time is 48 hours, so that water and other gases in the system are removed, and the vacuum degree of the whole system is better. After baking is finished, all valves are closed, and the whole system is cooled to room temperature.
Before the gas circuit subsystem samples, all valves are ensured to be closed. Taking an air path as an example, a sample is loaded into the sample cell 31, the valve 23 and the valve 16 are opened, the sample enters the air storage tank 13, the precision vacuum gauge 9 records the pressure change in the air storage tank 13, the valve 23 and the valve 16 are closed, the valve 6 and the air inlet valve 3 are opened, the opening and closing time of the air inlet valve 3 is accurately controlled through a computer, and the amount of sample injection gas can be accurately controlled according to the pressure change in the air storage tank 13.
The outlet end of the gas sample injection head 1 is a porous micro-channelPlate 41, sample introduction for uniform sample dispersion. After the sample introduction is finished, residual gas in the gas sample introduction head 1 needs to be removed, and the gas sample introduction head 1 is provided with an independent heating component. After the sample introduction is finished, the gas outlet valve 2, the first bypass valve 22 and the vacuum pump valve 37 are opened, the heating system of the gas sample introduction head 1 is opened, the vacuum pump 34 is started to pump away the residual sample in the gas sample introduction head 1, and the vacuum of the sample introduction head 1 is up to 1 x 10-6Torr～1*10-8After the Torr level, the gas outlet valve 2 and the first bypass valve 22 are closed.
The second bypass valve 4 and the valve 26 are opened due to the residual gas in the pipeline between the valve 6 and the air inlet valve 3, and the vacuum pump 34 is started to vacuumize the section of the air pipeline to 1 × 10-6Torr～1*10-8After the Torr magnitude, the second bypass valve 4, the valve 26 and the vacuum pump valve 37 are closed, and the gas path is cleaned quickly. After the rapid cleaning, samples in other parallel pipelines can be detected, and different gases can be rapidly switched in the parallel pipelines. The invention can also realize gas mixing sampling of two or more pipelines simultaneously.
The flow of changing the sample in a single gas path will be described below with reference to the gas paths in which the valves 6 and 19 are located. Before the sample is replaced, firstly, the normal operation of the gas circuit system is determined, before the sample is replaced, the closing of the valve 6 and the valve 27 is determined, the valve 16, the valve 23, the valve 19, the evacuation gas circuit and the existing gas in the gas storage tank 13 are opened in sequence, and the vacuum pumping is carried out until the vacuum pumping is 1 x 10-5On the Torr level, the valves 16, 23 and 19 are closed. Using a wrench to disassemble the pipeline connection head between the valve 27 and the valve 23, removing the sample cell 31 and the valve 27, replacing the sample cell 31 and the valve 27 with new samples, opening the valve 23 and the valve 19 in sequence after replacing the screwed connection head, evacuating the air entering the connection head due to replacement, and vacuumizing to 1 x 10-6Torr～1*10-8When the Torr is in a magnitude, the valve 16 is opened, the whole gas path is baked while the vacuum is maintained (if a plurality of gas paths are replaced, the plurality of gas paths can be baked at the same time), and the pipeline is thoroughly cleaned. The vacuum of the cavity is firstly worsened and then improved during baking to 1 x 10-6Torr～10-8After the Torr level, heating is stopped, the valves 16, 23 and 19 are closed, and the sample is completely replaced.
Claims (6)
1. A precise gas adsorption system for programmed temperature desorption is characterized by comprising a vacuum subsystem, a gas circuit subsystem and a gas sample injection head,
the vacuum subsystem comprises a backing pump, a vacuum cavity and a vacuum gauge, wherein the backing pump is connected with the vacuum pump through a backing pump valve and a pipeline; the vacuum cavity is provided with a vacuum gauge;
the gas path subsystem comprises a single gas path, two gas paths or a plurality of gas paths, and each gas path comprises a sample pool, a gas storage tank and a precise vacuum gauge; the sample tank and the vacuum cavity are respectively connected to an air inlet pipeline of the air storage tank through pipelines, the sample tank is provided with a valve, the pipeline connecting the sample tank and the air inlet pipeline of the air storage tank and the pipeline connecting the vacuum cavity and the air inlet pipeline of the air storage tank are provided with valves, the air inlet pipeline of the air storage tank is provided with a valve, the air storage tank is provided with a precision vacuum gauge, and the air outlet pipeline of the air storage tank is provided with a valve; an outlet of an air outlet pipeline of the air storage tank of each air path is connected to an air inlet pipeline of the gas sample injection head in parallel, the air inlet pipeline of the gas sample injection head is connected with an air inlet end of the gas sample injection head, and an air inlet valve is arranged on the air inlet pipeline of the gas sample injection head;
the gas inlet end of the gas sampling head is connected with the vacuum cavity through a first bypass pipeline, a gas outlet valve is arranged at the position, close to the gas sampling head, of the first bypass pipeline, and a first bypass valve is arranged at the position, close to the vacuum cavity, of the first bypass pipeline; a gas inlet pipeline of a gas sample injection head between the gas inlet valve and each gas outlet pipeline of the gas circuit and gas storage tank is connected with the vacuum cavity through a second bypass pipeline, a second bypass valve is arranged at the position, close to the gas inlet valve, of the second bypass pipeline, and a valve is arranged at the position, close to the vacuum cavity, of the second bypass pipeline;
the gas sample injection head is an overflow molecular beam sample injection head, the outlet end of the gas sample injection head is a porous micro-channel plate, and the gas sample injection head is provided with a heating part.
2. The precision gas adsorption system for temperature programmed desorption of claim 1 further equipped with an integral bake out subsystem.
3. The precision gas adsorption system for temperature programmed desorption of claim 1 or 2, wherein a heating element is provided within the sample cell.
4. The precision gas adsorption system for temperature programmed desorption according to claim 1 or 2, wherein the backing pump is a dry backing pump and the vacuum pump is a molecular pump.
5. The precision gas adsorption system for temperature programmed desorption of claim 1 or 2, wherein the gas circuit subsystem comprises three or four gas circuits.
6. The precision gas adsorption system for temperature programmed desorption according to claim 1 or 2, wherein the on-off time of the gas inlet valve and the gas outlet valve is automatically controlled.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113976090A (en) * | 2020-12-31 | 2022-01-28 | 苏州开洛泰克科学仪器科技有限公司 | Centralized self-diagnosis vacuum desorption device and use method thereof |
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