CN110702578A - Volumetric method isobaric adsorption tester - Google Patents
Volumetric method isobaric adsorption tester Download PDFInfo
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- CN110702578A CN110702578A CN201910986477.4A CN201910986477A CN110702578A CN 110702578 A CN110702578 A CN 110702578A CN 201910986477 A CN201910986477 A CN 201910986477A CN 110702578 A CN110702578 A CN 110702578A
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- 238000001179 sorption measurement Methods 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000012360 testing method Methods 0.000 claims abstract description 47
- 230000000087 stabilizing effect Effects 0.000 claims abstract description 25
- 230000003068 static effect Effects 0.000 abstract description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 239000007789 gas Substances 0.000 description 10
- 239000003463 adsorbent Substances 0.000 description 9
- 239000007788 liquid Substances 0.000 description 7
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 238000005086 pumping Methods 0.000 description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002156 adsorbate Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N2015/0866—Sorption
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- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Examining Or Testing Airtightness (AREA)
Abstract
The invention discloses a volumetric method isobaric adsorption tester, which structurally comprises a reference cavity, a pressure stabilizing valve, a test cavity, a stop valve, a vacuum pump, an air source, a Dewar cup, a pressure sensor, a control system and the like, wherein the reference cavity is connected with the stop valve through a pipeline, the stop valve is communicated with the air inlet end of the pressure stabilizing valve through a pipeline, the air outlet end of the pressure stabilizing valve is communicated with the test cavity through a pipeline, air can be controlled to enter the test cavity from the reference cavity, the reference cavity is simultaneously communicated with the vacuum pump and the air source tank through the pipeline and the stop valve respectively, the reference cavity can be vacuumized and aerated, the test cavity and the reference cavity are connected with a pressure gauge, the pressure in the cavity can be recorded and monitored through the control system, the control system can automatically control the testing process of the tester. The invention is different from the traditional static volumetric method test instrument in that a pressure stabilizing device is added at the air inlet end of the test cavity, so that the test cavity can be always kept constant in the sample adsorption process.
Description
Technical Field
The invention relates to the field of instruments and equipment for testing physical adsorption, in particular to a volumetric method isobaric adsorption tester.
Background
The main principle of the apparatus for testing and evaluating the adsorption performance of the adsorption materials such as porous materials, catalysts and the like is a static capacity method, and the method is that an adsorbent sample is arranged in an adsorption cavity with a certain volume, a certain amount of adsorbent gas is put into the adsorption cavity through a reference cavity with a known volume, and the adsorption quantity of the adsorbent to the adsorbent gas is obtained according to the pressure change of the reference cavity before and after adsorption, and conversely, the desorption quantity can also be obtained. The principle can obtain the adsorption capacity of the adsorbent material under different pressures at a certain temperature, namely an adsorption and desorption isotherm. However, in the test process according to this principle, the pressure of the environment (adsorption chamber) in which the sample is placed is changed, and the pressure is quantified by the pressure change before and after adsorption, so that the adsorption rate and the adsorption amount under a constant pressure condition (constant pressure or constant pressure) cannot be obtained. According to the invention, the pressure stabilizing device is arranged between the reference cavity and the adsorption cavity, so that the pressure of the reference cavity is changed before and after adsorption in the adsorption test process, and the pressure in the adsorption cavity is constant at a certain value, so that the adsorption quantity and the adsorption speed of the adsorbent under the constant pressure condition can be obtained.
Disclosure of Invention
In order to overcome the defect that the traditional static capacity method can not finish the adsorption quantity test of the adsorbent to the adsorbate gas under the constant pressure, the invention provides a capacity method isobaric adsorption tester, and the aim of realizing the constant pressure of a test cavity is fulfilled by adding a pressure stabilizing device between a reference cavity and the test cavity.
The technical scheme adopted by the invention for solving the technical problems is as follows: a volumetric method isobaric adsorption tester, comprising: the device comprises a reference cavity, a pressure stabilizing valve, a test cavity, a vacuum pump, an air source, a pressure sensor, a stop valve, a Dewar cup, a control system and the like. The reference cavity is provided with four interfaces, namely a vacuumizing pipeline interface, an air inlet pipeline interface, an air outlet pipeline interface and a pressure sensor interface. The interface of the vacuum pumping pipeline of the reference cavity is connected with a stop valve through an air path pipe, and the other end of the stop valve is connected with a vacuum pump through the air path pipe to realize the vacuum pumping of the reference cavity; the air inlet pipeline interface of the reference cavity is connected with a stop valve through an air path pipe, and the other end of the stop valve is connected with an air source through the air path pipe to realize air feeding of the reference cavity; the air outlet pipeline interface of the reference cavity is connected with one end of a stop valve through an air path pipe, the other end of the stop valve is connected with an air inlet of a pressure stabilizing valve through the air path pipe, and an air outlet of the pressure stabilizing valve is connected with the test cavity through the air path pipe; the interface of the reference cavity pressure sensor is connected with a pressure sensor. The pressure stabilizing valve is a pressure stabilizing device, the testing cavity is an adsorption cavity of the adsorbent sample, and the testing cavity is connected with a pressure sensor. Liquid nitrogen is filled in the Dewar cup, and the test cavity can be immersed in the liquid nitrogen in the test process. The control system comprises a main control board, a relay, a computer, software and the like, the control system is connected with the stop valve, the vacuum pump, the Dewar cup lifting motor and the pressure sensor through leads, the control system can control the starting and stopping of the vacuum pump, the on-off of the stop valve and the lifting of the Dewar cup through leads, meanwhile, signals of the pressure sensor are collected, a test result is obtained through the calculation and analysis of the software, and the constant-pressure tester system adopting the volumetric method is formed.
The pressure stabilizing device is additionally arranged in front of the test cavity, so that the pressure of the test cavity is ensured to be constant in the adsorption test process of the adsorbent sample, and the problem that the pressure of the test cavity cannot be ensured to be constant in the test process of the traditional static capacity method is solved.
Drawings
The invention is further illustrated with reference to the following figures and examples.
FIG. 1 is a schematic diagram of the inventive system;
in the figure, 1, a reference cavity, 2, a pressure stabilizing valve, 3, a test cavity, 4, a first pressure sensor, 5, a second pressure sensor, 6, a vacuum pump, 7, a first air source, 8, a second air source, 9, a first stop valve, 10, a second stop valve, 11, a third stop valve, 12, a fourth stop valve, 13, a fifth stop valve, 14, a Dewar cup, 15, a lifting motor and 16 are control systems.
Detailed Description
[ example 1 ]
The volumetric method isobaric adsorption tester comprises a reference cavity 1, a pressure stabilizing valve 2, a testing cavity 3, a first pressure sensor 4, a second pressure sensor 5, a vacuum pump 6, a first air source 7, a second air source 8, a first stop valve 9, a second stop valve 10, a third stop valve 11, a fourth stop valve 12, a fifth stop valve 13, a Dewar cup 14, a lifting motor 15 and a control system 16. The reference cavity 1 is connected with a first stop valve 9 through a pipeline, the other end of the first stop valve 9 is connected with the air inlet end of a pressure stabilizing valve 2 through a pipeline, and the air outlet end of the pressure stabilizing valve 2 is connected with the test cavity 3 through a pipeline; the reference cavity 1 is connected with a second stop valve 10 through a pipeline, and the other end of the second stop valve 10 is connected with a vacuum pump 6 through a pipeline; the reference cavity 1 is connected with a fourth stop valve 12 through a pipeline, and the other end of the fourth stop valve 12 is connected with a first air source 7 through a pipeline; the reference cavity 1 is connected with a fifth stop valve 13 through a pipeline, and the other end of the fifth stop valve 13 is connected with a second air source 8 through a pipeline; the reference chamber 1 is connected with a first pressure sensor 4. The test cavity 3 is connected with a third stop valve 11 through a pipeline, the other end of the third stop valve 11 is connected with a vacuum pump 6 through a pipeline, and the test cavity 3 is connected with a second pressure sensor 5 through a pipeline. The first pressure sensor 4, the second pressure sensor 5, the vacuum pump 6, the first stop valve 9, the second stop valve 10, the third stop valve 11, the fourth stop valve 12, the fifth stop valve 13 and the lifting motor 15 are connected with a control system 16 through leads.
When the device works, the control system 16 controls the dewar cup 14 to ascend through the lifting motor 15, liquid nitrogen is filled in the dewar cup 14, the dewar cup 14 ascends to enable the testing cavity 3 to be immersed in the liquid nitrogen of the dewar cup 14, and the temperature environment required by the experiment is obtained. If cooling is not required, control system 16 controls dewar 14 to be lowered by lift motor 15 and test chamber 3 is disengaged from dewar 14.
The control system 16 controls the first stop valve 9, the second stop valve 10 and the third stop valve 11 to be opened, the fourth stop valve 12 and the fifth stop valve 13 to be closed, the vacuum pump 6 is controlled to be started, and the vacuum pump 6 starts to vacuumize the reference cavity 1 and the test cavity 3. The control system 16 records the pressure of the reference cavity 1 and the pressure of the test cavity 3 through the first pressure sensor 4 and the second pressure sensor 5, and after the vacuum requirement is met, the control system 16 controls the first stop valve 9, the second stop valve 10 and the third stop valve 11 to be closed, controls the vacuum pump 6 to stop, and completes the vacuum pumping of the reference cavity 1 and the test cavity 3.
After the vacuum pumping is finished, the control system 16 controls the fourth stop valve 12 to be opened, the first stop valve 9, the second stop valve 10, the third stop valve 11 and the fifth stop valve 13 to be closed, the gas in the gas source 1 enters the reference cavity 1, and the control system 16 controls the opening time of the fourth stop valve 12 to control the air inflow amount in the reference cavity 1. If the gas of the gas source 2 needs to be filled, the control system 16 controls the following modes: the fifth cut-off valve 13 is opened, and the first cut-off valve 9, the second cut-off valve 10, the third cut-off valve 11, and the fourth cut-off valve 12 are closed. After the dosing is complete, the control system 16 records the stabilized pressure of the reference chamber 1 via the first pressure sensor 4 as P1.
After the reference cavity 1 is filled with gas, the output pressure of the pressure stabilizing valve 2 is set, the control system 16 controls the first stop valve 9 to be opened, the second stop valve 10, the third stop valve 11, the fourth stop valve 12 and the fifth stop valve 13 to be closed, the gas enters the test cavity 3 from the reference cavity 1 through the first stop valve 9 and the pressure stabilizing valve 2, and the sample starts to be adsorbed. The control system 16 records the pressure of the reference chamber 1 and the pressure of the test chamber 3 through the first pressure sensor 4 and the second pressure sensor 5, and when the pressure of the reference chamber 1 is not changed any more, the completion of the adsorption can be judged. The control system 16 records the opening time of the first stop valve 9 and the time when the pressure of the reference cavity 1 starts to stabilize, and the time difference between the opening time of the first stop valve and the time is the time when the sample finishes adsorption under constant pressure and is counted as t; the control system 16 records the pressure P2 of the reference cavity 1 and the pressure P3 of the test cavity 3 after adsorption is finished, and in combination with the pressure P1 after the reference cavity 1 is aerated, according to an ideal gas state equation, the volumes of the reference cavity 1 and the test cavity 3 are both known, so that the adsorption quantity of the sample can be calculated; the adsorption time t is measured, and the adsorption speed of the sample under the set pressure can be calculated.
The adsorption quantity and the adsorption speed of the sample under different pressure conditions can be obtained by changing the output pressure of the pressure stabilizing valve 2. The pressure fluctuation range of the test chamber 3 can be verified by the pressure data of the second pressure sensor 5 collected by the control system 16 during the sample adsorption process.
[ example 2 ]
The cooling medium in the dewar 14 may be ice water mixture, liquid carbon dioxide, liquid argon, in addition to liquid nitrogen, according to the test requirements.
[ example 3 ]
The pressure stabilizing valve 2 can be a manually controlled pressure stabilizing valve or an automatically controlled pressure stabilizing valve.
Claims (2)
1. A volumetric method isobaric adsorption tester comprises a reference cavity (1), a pressure stabilizing valve (2), a test cavity (3), a first pressure sensor (4), a second pressure sensor (5), a vacuum pump (6), a first air source (7), a second air source (8), a first stop valve (9), a second stop valve (10), a third stop valve (11), a fourth stop valve (12), a fifth stop valve (13), a Dewar cup (14), a lifting motor (15) and a control system (16), and is characterized in that the reference cavity (1) is connected with the first stop valve (9) through a pipeline, the other end of the first stop valve (9) is connected with the air inlet end of the pressure stabilizing valve (2) through a pipeline, the air outlet end of the pressure stabilizing valve (2) is connected with the test cavity (3) through a pipeline, the reference cavity (1) is connected with the second stop valve (10) through a pipeline, the other end of the second stop valve (10) is connected with the vacuum pump (6) through a pipeline, benchmark chamber (1) links to each other with fourth stop valve (12) through the pipeline, fourth stop valve (12) other end passes through pipe connection first air supply (7), benchmark chamber (1) links to each other with fifth stop valve (13) through the pipeline, fifth stop valve (13) other end passes through pipe connection second air supply (8), benchmark chamber (1) has connect first pressure sensor (4), test chamber (3) link to each other with third stop valve (11) through the pipeline, third stop valve (11) other end pipe connection vacuum pump (6), test chamber (3) are connected with second pressure sensor (5) through the pipeline, control system (16) pass through wire and first pressure sensor (4), second pressure sensor (5), vacuum pump (6), first stop valve (9), second stop valve (10), third stop valve (11), fourth stop valve (12), The fifth stop valve (13) is connected with a lifting motor (15).
2. The volumetric method isobaric adsorption tester according to claim 1, characterized in that the pressure-maintaining valve (2) can be a manually controlled pressure-maintaining valve or an automatically controlled pressure-maintaining valve.
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| CN201910986477.4A CN110702578A (en) | 2019-10-17 | 2019-10-17 | Volumetric method isobaric adsorption tester |
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| CN201910986477.4A CN110702578A (en) | 2019-10-17 | 2019-10-17 | Volumetric method isobaric adsorption tester |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111141644A (en) * | 2020-02-28 | 2020-05-12 | 贝士德仪器科技(北京)有限公司 | Filter membrane aperture analyzer with liquid sealing pressure relief protection device |
| CN114136837A (en) * | 2021-10-28 | 2022-03-04 | 贝士德仪器科技(北京)有限公司 | Volumetric method constant-voltage tester and voltage control method |
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| CN114136837A (en) * | 2021-10-28 | 2022-03-04 | 贝士德仪器科技(北京)有限公司 | Volumetric method constant-voltage tester and voltage control method |
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