CN111307653A - Gas absorption and desorption performance testing device - Google Patents
Gas absorption and desorption performance testing device Download PDFInfo
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- CN111307653A CN111307653A CN202010086866.4A CN202010086866A CN111307653A CN 111307653 A CN111307653 A CN 111307653A CN 202010086866 A CN202010086866 A CN 202010086866A CN 111307653 A CN111307653 A CN 111307653A
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Abstract
The application discloses a gas absorption and desorption performance testing device which comprises a controller, an air inlet cavity, a sample cavity and a pressure measuring component, wherein the air inlet cavity is formed in the controller; the air inlet cavity and the sample cavity are sequentially arranged along the airflow direction; the pressure measuring component is positioned in the air inlet cavity and used for measuring the pressure in the air inlet cavity; the controller is respectively electrically connected with the air inlet cavity and the sample cavity and is used for controlling the pressure in the air inlet cavity and the sample cavity according to the pressure measured by the pressure measuring component. The gas absorption and desorption performance testing device is simple in structure and capable of accurately detecting gas absorption and desorption performance under set temperature and pressure.
Description
Technical Field
The application relates to the technical field of material detection, and particularly discloses a gas adsorption and desorption performance testing device.
Background
The performance of the material is usually closely related to the composition and structure of the material, wherein the absorption and desorption performance test of the material is to test the volume and mass changes of the material during gas absorption or desorption at precisely set temperature and pressure, and the volume and mass changes of the material during absorption and desorption can be automatically and directly measured by various instruments for representing the absorption and desorption performance of the material, so that the absorption and desorption isothermicity and isobars of the material to various gases under different temperature, pressure and operation conditions are obtained, so as to evaluate the kinetic and thermodynamic parameters in the absorption and desorption process, and the method can be used as a characterization method for obtaining the performance of the material in a wider range. However, it is expected that the change of the structure of the material can be studied while the properties of the material are studied.
Ultraviolet-visible, infrared, Raman and other spectrum techniques are powerful material research techniques for characterizing the structure of compounds and understanding chemical reactions. The spectroscopic technology is a technology for obtaining information of gas components on the surface layer of a sample and adsorbed on the surface of the sample by light through the sample or a reflection signal of the light on the surface of the sample, does not need to put the sample, and cannot damage the sample in a testing process, so that the spectroscopic technology can be used as one of important means for researching the structure of a material.
In the related art, the sample chamber of the instrument for characterizing the adsorption and desorption performance of the material needs to adapt to the temperature change from the liquid nitrogen temperature to the 500 ℃ (or 1000 ℃) range and the high vacuum (10 ℃)-6mbar) or high pressure (20bar), and strict test conditions put higher demands on the test device, and the research on the material structure of the instrument while testing the adsorption and desorption performance is limited to a certain extent, so that the research on the spectral change in the process of researching the adsorption and desorption performance of the material is challenged.
Disclosure of Invention
According to an aspect of the application, a gaseous desorption performance testing arrangement that inhales is provided, the device passes through temperature, the pressure variation in air inlet chamber, the sample chamber in the controller controlling means to around putting into the sample based on the sample intracavity, the pressure variation in air inlet chamber and the sample chamber inhales the desorption performance and characterizes to the sample, can realize the gaseous desorption performance research of inhaling under the harsh condition with simple structure's testing arrangement.
A gas absorption and desorption performance testing device comprises a controller, an air inlet cavity, a sample cavity and a pressure measuring component;
the air inlet cavity and the sample cavity are sequentially arranged along the airflow direction;
the pressure measuring component is positioned in the air inlet cavity and used for measuring the pressure in the air inlet cavity;
the controller is respectively electrically connected with the air inlet cavity and the sample cavity and is used for controlling the pressure in the air inlet cavity and the sample cavity according to the pressure measured by the pressure measuring component.
Optionally, the device further comprises an air outlet channel and at least one air inlet channel, wherein each air inlet channel sequentially comprises a first mass flow meter and a first electromagnetic valve along the air flow direction;
the air outlet channel sequentially comprises a second electromagnetic valve and a second mass flow meter along the air flow direction.
Preferably, the device comprises an air outlet channel and at least two air inlet channels, wherein each air inlet channel sequentially comprises a first mass flow meter and a first electromagnetic valve along the air flow direction; the air outlet channel sequentially comprises a second electromagnetic valve and a second mass flow meter along the air flow direction.
Optionally, each intake passage further comprises:
the first filter valve is arranged at the air inlet end of the first mass flow meter;
and the first one-way valve is arranged between the first mass flow meter and the first electromagnetic valve.
Optionally, the air outlet channel further comprises:
the second filter valve is arranged between the second electromagnetic valve and the second mass flowmeter;
and the second one-way valve is arranged at the air outlet end of the second mass flow meter.
Optionally, the device further comprises a cavity valve located between the gas inlet cavity and the sample cavity and used for adjusting the communication state of the gas inlet cavity and the sample cavity;
preferably, the gas inlet chamber and the sample chamber have the same volume.
Optionally, the intake chamber further comprises:
the pressure release valve is arranged at the air inlet end of the pressure measurement component;
the first exhaust valve is arranged at the air inlet end of the pressure measurement component;
forming the volume of the air inlet cavity according to the first electromagnetic valve, the pressure release valve, the first exhaust valve, the pressure measuring part, the cavity valve and the connecting pipeline among the second electromagnetic valve, the pressure release valve, the first exhaust valve, the pressure measuring part and the cavity valve;
the first electromagnetic valve, the pressure measuring component and the cavity valve are sequentially arranged in the air inlet cavity along the air flow direction.
Optionally, the sample chamber further comprises a sample placing pool and a second exhaust valve arranged at the gas outlet end of the sample placing pool;
forming the volume of a sample cavity according to the cavity valve, the sample placing pool, the second exhaust valve and the second electromagnetic valve and the connecting pipelines among the cavity valve, the sample placing pool, the second exhaust valve and the second electromagnetic valve;
the cavity valve, the sample placing pool, the second exhaust valve and the second electromagnetic valve are sequentially arranged in the sample cavity along the airflow direction.
Optionally, the air outlet channel further comprises a metering valve disposed in a bypass connected in parallel with the second solenoid valve, the second filter valve, the second mass flow meter, and the second check valve.
Optionally, the apparatus further comprises a vacuum pump having a vacuum gauge that is displayed with the pressure at which the pressure within the apparatus is below a pressure threshold;
the device also includes a temperature controller for controlling the temperature in the gas inlet chamber and the sample chamber.
Optionally, the sample placing pool is provided with a light-transmitting window, and the sample in the sample placing pool is subjected to in-situ spectral monitoring through the light-transmitting window;
the light-transmitting window is a transmission window or a reflection window.
Preferably, the number of the light transmission windows is at least 2, and the light transmission windows are respectively used for incidence and emergence of the light source.
The beneficial effects that this application can produce include:
the temperature and pressure changes in the gas inlet cavity and the sample cavity in the device are controlled by the controller, the adsorption performance of the sample on gas is calculated by an ideal gas state equation based on the pressure changes in the gas inlet cavity and the sample cavity before and after the sample is placed in the sample cavity, so that the characterization of the adsorption and desorption performance of the sample is realized, the structure of the testing device is simple, and the gas adsorption and desorption performance under the set temperature and pressure can be accurately detected;
furthermore, in the process of absorbing and desorbing the sample, a light source of a spectrometer irradiates the sample in the sample storage tank through a light-transmitting window arranged on the sample storage tank, so that the spectral change of the gas absorbing and desorbing process of the sample in the tank is obtained according to the emergent light, the absorption and desorption performance and the spectral change of the material are tested in the same process, the advantages of two testers are integrated, the device has a simple structure, the tester for the absorption and desorption performance of the material develops towards the direction of multifunctionality, and convenience is provided for the performance and structure research of the material;
furthermore, the controller is electrically connected with the air inlet cavity and the sample cavity to control the opening and closing of each valve in the cavities, so that the pressure and the temperature in the device can be automatically controlled and stabilized at a preset value, the controllability of detection conditions is improved, and automatic control is realized;
furthermore, one gas is introduced into each gas inlet channel through a plurality of parallel gas inlet channels, so that the test and research of the adsorption and desorption performance of the material on various gases can be realized; meanwhile, the spectral change conditions of reactants, intermediates and products caused by the change of the conditions such as the proportion of reaction raw material gas, flow rate, reaction temperature, reaction pressure and the like in the catalytic reaction process can be monitored in real time through a plurality of parallel gas inlet channels, so that the optimal conditions of the catalytic reaction can be conveniently screened, and support is provided for the research of the reaction mechanism of the catalytic reaction;
furthermore, the device of the present application can be at room temperature to 450 ℃ and 10 DEG C-5Testing the isothermal adsorption and desorption curve of the sample adsorbed gas under the condition of mbar-30 bar, and realizing in-situ monitoring of the spectral change in the adsorption and desorption process;
in addition, through the arrangement of the pressure release valve, the exhaust valve and the metering valve in the device, when a fault occurs in the test process, the pressure in the system can be quickly adjusted and the air can be quickly exhausted, so that the system safety of the whole test device is further ensured.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the present application and together with the description, serve to explain the principles of the application. It is obvious that the drawings in the following description are only some embodiments of the application, and that for a person skilled in the art, other drawings can be derived from them without inventive effort.
Fig. 1 is a schematic structural diagram of a gas adsorption and desorption performance testing device according to the present application;
fig. 2 is a schematic structural diagram of an air inlet cavity and a sample cavity in a gas adsorption and desorption performance testing device according to the present application;
FIG. 3 is a schematic structural diagram of a sample well according to an embodiment of the present disclosure;
fig. 4 is a schematic structural diagram of a sample well according to an embodiment of the present application.
List of parts and reference numerals:
i an air inlet channel; II, an air inlet cavity;
III a sample chamber; IV, an air outlet channel;
1a first filter valve; 1b a first mass flow meter;
1c a first one-way valve; 1d first electromagnetic valve;
3d cavity valve; 2a second filter valve;
2b a second mass flow meter; 2c a second one-way valve;
2d second electromagnetic valve; e, releasing the valve;
1v a first exhaust valve; 2v second exhaust valve;
f a pressure sensor; j a mechanical pressure gauge;
g, metering valve; r is placed in a sample pool;
an M controller; p vacuum pump with vacuum gauge.
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples.
A gas absorption and desorption performance testing device comprises a controller, an air inlet cavity, a sample cavity and a pressure measuring component;
the air inlet cavity and the sample cavity are sequentially arranged along the airflow direction;
the pressure measuring component is positioned in the air inlet cavity and used for measuring the pressure in the air inlet cavity;
the controller is respectively electrically connected with the air inlet cavity and the sample cavity and is used for controlling the pressure in the air inlet cavity and the sample cavity according to the pressure measured by the pressure measuring component.
The gas to among the correlation technique is inhaled desorption capability test device simple structure, and because of can't inhale desorption appearance and spectrum appearance antithetical couplet usefulness with gas, has restricted and has carried out the gaseous desorption capability test in-process that inhales of material, inhales this problem of spectral change test of desorption in-process simultaneously, and this application provides a gaseous desorption capability test device that inhales. The device controls the temperature and pressure changes in the air inlet cavity and the sample cavity in the device through the controller, and represents the adsorption and desorption performance of the sample based on the pressure changes in the air inlet cavity and the sample cavity before and after the sample is placed in the sample cavity; further, in the sample adsorption and desorption process, through the light-through window arranged on the sample tank, the sample in the test bin can absorb the spectrum change in the gas adsorption and desorption process, the test of material adsorption and desorption performance and spectrum change can be realized in the same process, the advantages of two types of testers are integrated, the material adsorption and desorption performance tester can be developed towards the direction of multiple functions, and convenience is provided for the performance and structural research of the material.
Optionally, the device further comprises an air outlet channel and at least one air inlet channel, wherein each air inlet channel sequentially comprises a first mass flow meter and a first electromagnetic valve along the air flow direction; the air outlet channel sequentially comprises a second electromagnetic valve and a second mass flow meter along the air flow direction.
Optionally, each intake passage further comprises: the first filter valve is arranged at the air inlet end of the first mass flow meter; and the first one-way valve is arranged between the first mass flow meter and the first electromagnetic valve.
Alternatively, the device may comprise a plurality of parallel intake passages, and the composition of each intake passage is the same;
preferably, the device comprises at least two air inlet channels.
Specifically, a plurality of air inlet channels (namely air inlet gas channels) with the same structure and parts can be configured in the device for performing the characterization of the adsorption and desorption performance of a plurality of different gases on a sample; the number of the parallel air inlet channels can be 2, 3, 5, etc., and the number of the air inlet channels is not particularly limited in the present application.
The parallel air inlet channels sequentially comprise a first filter valve, a first mass flow meter, a first one-way valve and a first electromagnetic valve along the air flow direction, and the volume of the air inlet cavity is formed according to the first electromagnetic valve, the pressure measuring component, the cavity valve and connecting pipelines among the first electromagnetic valves, the pressure measuring component and the cavity valve in each air inlet channel.
In some possible embodiments, through a plurality of parallel gas inlet channels, one gas is introduced into each gas inlet channel, so that the test research on the adsorption and desorption performance of multiple gases of the material can be realized. For example, if the device comprises 2 parallel inlet channels, CO gas is introduced through the first inlet channel and CO is introduced through the second inlet channel2And the variation range of the amount of the introduced CO gas is 0-100 percent, and the introduced CO gas is CO2The variation range of the gas amount is 100-0 percent, so that the introduction of CO and CO with different proportions can be studied2In the case of (2), adsorption/desorption properties of the material.
Optionally, the air outlet channel further comprises: the second filter valve is arranged between the second electromagnetic valve and the second mass flowmeter; and the second one-way valve is arranged at the air outlet end of the second mass flow meter.
Optionally, the device further comprises a cavity valve located between the gas inlet cavity and the sample cavity and used for adjusting the communication state of the gas inlet cavity and the sample cavity;
preferably, the volume of the gas inlet chamber and the sample chamber is the same;
specifically, in order to avoid the error influence caused by the large difference between the volumes of the air inlet cavity and the sample cavity, the volumes of the air inlet cavity and the sample cavity are kept the same in the application. Therefore, when the gas absorption and desorption performance testing device is used, the standard values of the volumes of the gas inlet cavity and the sample cavity are firstly measured so as to know whether the volumes of the gas inlet cavity and the sample cavity of the device are the same or not or whether the volumes of the gas inlet cavity and the sample cavity are similar or not, so that the number of workers doing the test is increased.
Specifically, the method for calibrating the standard volumes of the air inlet cavity and the sample cavity comprises the following steps: firstly, vacuumizing the device, then closing a cavity valve, and introducing gas into an air inlet cavity through an air inlet channel to ensure that the air inlet cavity has first initial pressure; then, opening a cavity valve to enable the air inlet cavity and the sample cavity to have the same first test pressure; finally, based on the gas state approach (PV ═ nRT, where P is the ideal gas pressure, V is the ideal gas volume, n is the physical quantity of the ideal gas, R is the ideal gas constant, and T is the thermodynamic temperature of the ideal gas), the intake chamber standard volume and the sample chamber standard volume are calculated from the first initial pressure and the first test pressure.
Based on the obtained standard volume of the air inlet cavity and the standard volume of the sample cavity, a tester can know whether the volumes of the air inlet cavity and the sample cavity influence the test result, and the number of the air inlet cavity and the sample cavity is in the heart, and under the normal condition, the standard volumes of the air inlet cavity and the sample cavity are close to each other or even the same.
It should be noted that, under the condition that the device only includes a inlet channel, when carrying out the sample test at every turn, if used gas is different with the examination desorption gas that adsorbs of awaiting measuring when survey the standard value of inlet chamber volume, the standard value of sample chamber volume, then need switch over gas and wash the gas circuit, and under the condition that the device includes at least two inlet channels, one of them is fixed as the inlet gas circuit when surveying the standard value of inlet chamber volume, the standard value of sample chamber volume before the sample test at every turn, other inlet channels are as the inlet gas circuit of the gas that awaits measuring, based on this, demarcate the gas circuit of gas and the gas circuit of the gas that awaits measuring and distinguish, avoided the operation of switching gas and washing gas circuit, comparatively speaking, the operation is more convenient, of course, this application can be according to the actual work demand, select the quantity of inlet channel in the testing arrangement.
Optionally, the intake chamber further comprises: and the pressure relief valve is arranged at the air inlet end of the pressure measuring part and used for ensuring that the pressure in the device does not exceed the preset highest pressure value.
Specifically, if the pressure value in the device obtained by the pressure measuring part exceeds the preset highest pressure value, the air pressure in the device is rapidly reduced to the preset pressure value by the pressure relief valve.
Optionally, the air inlet chamber further comprises a first exhaust valve (i.e. a stop valve) arranged at the air inlet end of the pressure measurement component, and used for rapidly exhausting gas when the testing device fails in the testing process; in some possible embodiments, the first exhaust valve is located in the intake chamber in parallel with the pressure relief valve (as shown in fig. 1), and of course, the position of the first exhaust valve may also be selected in the intake chamber according to implementation requirements, and the application does not specifically limit the position of the exhaust valve in the intake chamber.
Forming the volume of the air inlet cavity according to the first electromagnetic valve, the pressure release valve, the first exhaust valve, the pressure measuring part, the cavity valve and the connecting pipeline among the second electromagnetic valve, the pressure release valve, the first exhaust valve, the pressure measuring part and the cavity valve;
the first electromagnetic valve, the pressure measuring component and the cavity valve are sequentially arranged in the air inlet cavity along the air flow direction.
Specifically, in the air inlet channel, a first filter valve is arranged in the air inlet direction of the first mass flow meter, a first check valve and a first electromagnetic valve are sequentially arranged in the air outlet direction of the first mass flow meter along the air flow direction, and the first electromagnetic valve, the pressure testing component, the cavity valve and a pipeline connecting the first electromagnetic valve, the pressure testing component and the cavity valve form the air inlet cavity volume of the device and are used for quantitatively introducing air into the sample cavity.
Optionally, valves such as the first filter valve, the first check valve, the first electromagnetic valve, the second filter valve, the second check valve, the pressure relief valve, the first exhaust valve, and a connection pipeline connecting the valves are all made of stainless steel, and parts of the valves are connected in a surface sealing manner, such as VCR connection (Vacuum coupling radial Seal); the cover of the sample placing pool is sealed by a perfluoroether rubber Ring O-Ring (Kalrez O-Ring).
Optionally, the sample chamber further comprises a sample placing pool and a second exhaust valve arranged at the gas outlet end of the sample placing pool;
forming the volume of a sample cavity according to the cavity valve, the sample placing pool, the second exhaust valve and the second electromagnetic valve and the connecting pipelines among the cavity valve, the sample placing pool, the second exhaust valve and the second electromagnetic valve; the cavity valve, the sample placing pool, the second exhaust valve and the second electromagnetic valve are sequentially arranged in the sample cavity along the airflow direction.
Specifically, in the air outlet channel, a second electromagnetic valve and a second filter valve are sequentially arranged in the air inlet direction of the second mass flow meter along the air flow direction, a second one-way valve is arranged in the air outlet direction of the second mass flow meter along the air flow direction, and the cavity valve, the sample placing pool inner space, the second electromagnetic valve and a pipeline connecting the cavity valve, the sample placing pool inner space and the second electromagnetic valve form the sample cavity volume of the device.
Optionally, the second exhaust valve is also made of stainless steel, and the components associated with the second exhaust valve are connected in a face-sealing manner, such as a VCR connection (Vacuum Coupling radial Seal).
Optionally, the air outlet channel further comprises a metering valve, which is disposed in a bypass connected in parallel with the second solenoid valve, the second filter valve, the second mass flow meter and the second check valve, and is used for vacuumizing the device. Specifically, a bypass including a metering valve is connected to the parallel sides of the second electromagnetic valve, the second filter valve, the second mass flow meter and the second check valve, so that the device can be quickly vacuumized, for example, during sample activation.
Optionally, the apparatus further comprises a vacuum pump having a vacuum gauge for displaying the pressure when the pressure within the apparatus is below a pressure threshold. For example, when the pressure in the device is lower than 1bar, the pressure in the device is indicated by vacuum; correspondingly, the pressure measuring part is used for displaying high pressure (namely when the pressure in the device is 1-30 bar).
Preferably, the high pressure is in the range of 1-30 bar;
the low pressures indicated a pressure range of < 1 bar.
In some possible embodiments, the pressure measurement means comprise a mechanical pressure gauge and a pressure sensor for sending the pressure values in the form of numerical signals to the controller (for example by connecting with a LabView controller using a compiled program) so that the controller automatically controls the pressure inside the device and stabilizes it at preset pressure values (for example 100mbar, 5bar, 20bar, etc.). The mechanical pressure gauge is used for feeding back pressure values to operators on site, and the accuracy of pressure in the device can be ensured in a double-pressure display mode, so that faults can be found and eliminated in time when the pressure displays differences.
In some possible embodiments, the pressure measuring component may be a sensor combining a high pressure sensor and a low pressure sensor, so that the simultaneous monitoring of high pressure and low pressure can be realized on the same pressure measuring component, thereby simplifying the device and expanding the application range of the pressure measuring component.
Optionally, a controller in the device is electrically connected with the air inlet cavity and the sample cavity and used for controlling the pressure in the air inlet cavity and the sample cavity according to the pressure measured by the pressure measuring part;
specifically, the controller is electrically connected with the first mass flow meter, the first electromagnetic valve, the pressure measurement component, the cavity valve, the second electromagnetic valve and the second mass flow meter, and automatically controls the pressure in the device through each mass flow meter and the electromagnetic valve, and enables the pressure to be stabilized at a preset pressure value.
Optionally, the apparatus further comprises a temperature controller for controlling the temperature in the gas inlet chamber and the sample chamber; in some possible embodiments, the pressure controller may be integrated with the temperature controller in the same controller, and the present application is not limited thereto.
Optionally, the sample storage pool is provided with a light-transmitting window, and the sample in the sample storage bin is subjected to in-situ spectral monitoring through the light-transmitting window.
Specifically, a light-transmitting window of the optical lens may be installed in the sample storage cell to allow a light source of the spectrometer to enter the sample storage cell to irradiate on the sample, and the emitted light returns to the spectrometer, so that in the process of detecting the gas absorption and desorption performance of the sample, the spectrum information of the sample is obtained at the same time.
Preferably, the number of the light transmission windows is at least 2, and the light transmission windows are respectively used for incidence and emergence of the light source.
In some possible embodiments, the light-transmitting window may be a transmissive window, and referring to fig. 3, a schematic view of a sample cell according to an embodiment of the present application is shown, lines with arrows are light rays, a light source of a spectrometer is incident on a sample from a first light-transmitting window, light transmitted through the sample is emitted to a detector from a second light-transmitting window corresponding to the first light-transmitting window, and a spectrum of the sample placed in the sample cell is detected in a transmissive manner.
In some possible embodiments, the light-transmitting window may be a reflective window, and referring to fig. 4, which is a schematic view of a sample well according to an embodiment of the present application, a line with an arrow is a light ray, a light source of a spectrum is incident on a sample from a first light-transmitting window, and light reflected by the sample is emitted from a second light-transmitting window to a detector, so as to perform spectrum detection on the sample in the sample well in a reflective manner. In practical application, a corresponding light-transmitting window can be selected according to the actual working environment so as to facilitate detection.
Optionally, the temperature resistance range of the sample placing pool of the device is between room temperature and 450 ℃, and the room temperature in the application is 25 ℃.
Optionally, the device has a sealed pressure-resistant range of the sample-placing tankIs 10-5mbar～30bar。
Specifically, the device of the application can activate the sample at room temperature to 450 ℃, test and characterize the absorption and desorption performance of the sample to gas, and can resist pressure of 10 times in a closed state in the reaction-5mbar～30bar；
Preferably, the device of the application can control the pressure between 10mbar and 30bar, and accurately represents the adsorption and desorption performance of the material.
The temperature and pressure changes in the air inlet cavity and the sample cavity in the device are controlled by the controller, and the absorption and desorption performances of the sample are represented based on the pressure changes in the air inlet cavity and the sample cavity before and after the sample is put into the sample cavity; in the process of absorbing and desorbing a sample, the spectral change of the sample in the test bin in the process of absorbing and desorbing gas is tested through a light-transmitting window arranged on a sample placing pool, the absorption and desorption performance and the spectral change of the material are tested in the same process, the advantages of the two testers are integrated, the absorption and desorption performance tester of the material is developed towards the direction of multiple functions, and convenience is provided for the research on the performance and the structure of the material;
furthermore, the spectral change conditions of reactants, intermediates and products caused by the change of the conditions such as the proportion of reaction raw material gas, the flow rate, the reaction temperature, the reaction pressure and the like in the catalytic reaction process can be monitored in real time through a plurality of parallel gas inlet channels, so that the optimal conditions of the catalytic reaction can be conveniently screened, and the reaction mechanism of the catalytic reaction can be conveniently researched.
Example 1
Fig. 1 is a schematic structural diagram of a gas adsorption and desorption performance testing apparatus provided in this embodiment, and the following describes this embodiment with reference to fig. 1.
As shown in fig. 1, the gas adsorption and desorption performance testing device sequentially comprises a gas inlet channel I, a gas inlet cavity II, a sample cavity III and a gas outlet channel IV along the gas flow direction. The air inlet channel I sequentially comprises a first filter valve 1a, a first mass flow meter 1b, a first one-way valve 1c and a first electromagnetic valve 1d along the air flow direction; the air inlet cavity II sequentially comprises a first electromagnetic valve 1d, a pressure release valve e (also comprising a first exhaust valve 1v in parallel), a pressure measuring component (comprising a pressure sensor f and a mechanical pressure gauge j) and a cavity valve 3d along the air flow direction; the sample cavity III sequentially comprises a cavity valve 3d, a sample placing pool R, a second exhaust valve 2v and a second electromagnetic valve 2d along the airflow direction; the air outlet channel IV sequentially comprises a second electromagnetic valve 2d, a second filter valve 2a, a second mass flow meter 2b and a second one-way valve 2c along the air flow direction; a vacuum pump P with a vacuum gauge is arranged behind the air outlet channel IV along the air flow direction; besides, a controller M is arranged outside the device, and the controller M is connected with the first mass flow meter 1b, the first electromagnetic valve 1d, the pressure sensor f, the mechanical pressure gauge j, the cavity valve 3d, the second electromagnetic valve 2d and the second mass flow meter 2 b.
It should be noted that, the sample cell R in the present application is provided with a light-transmitting window, which allows a light source of the spectrometer to shine into the sample cell R from the light-transmitting window and to strike on the sample, and the light source that is emitted is received by detecting to test the spectral change in the gas adsorption process.
The following describes a process of testing the gas adsorption and desorption performance testing device by using a spectrometer with reference to fig. 1 and 2:
firstly, confirming that a first exhaust valve 1v and a second exhaust valve 2v are in a normally closed state, and vacuumizing the device by using a vacuum pump P; subsequently, all the first electromagnetic valve 1d, the chamber valve 3d, the second electromagnetic valve 2d and the metering valve g are closed, and helium gas is used as standard gas in the embodiment;
secondly, opening the first electromagnetic valve 1d, introducing helium into the air inlet cavity II through the air inlet channel I, so that the pressure in the air inlet cavity is P0At this time, no sample is placed in the sample placing pool (the pressure in the sample cavity is 0); then, the cavity valve 3d is opened, so that the gas in the gas inlet cavity II flows into the sample cavity III, and the pressure in the gas inlet cavity II and the pressure in the sample cavity III are obtained through the pressure measuring part to be equal to P1(ii) a Further, a known volume V is placed in the sample placing poolsdAnd repeating the above steps, wherein the gas in the gas inlet cavity II flows into the sample cavity III by opening the cavity body valve 3d again, and the pressure in the gas inlet cavity II and the pressure in the sample cavity III are obtained to be the same as P through the pressure measuring part2；
Then, based on Vsd、P0、P1、P2And an ideal gas state equation, and calculating the standard volume V of the air inlet cavity IIDoseComprises the following steps:
standard volume V of sample chamber IIIsamComprises the following steps:
based on the volume, whether the volumes of the air inlet cavity II and the sample cavity III of the device are similar or even identical is determined, wherein in order to further avoid the influence caused by calculation errors, the standard volume V of the air inlet cavity II obtained for multiple times can be usedDoseAnd the standard volume V of the sample chamber IIIsamCalculating an average value;
then, the standard volume V of the air inlet cavity II is calibratedDoseAnd the standard volume V of the sample chamber IIIsamAnd then, starting to test the gas adsorption and desorption performance of the sample, and comprising the following specific processes:
opening the first electromagnetic valve 1d, introducing helium gas into the air inlet cavity II through the air inlet channel I, so that the pressure in the air inlet cavity is P3When the cavity valve 3d is closed; then, the cavity valve 3d is opened, so that the gas in the gas inlet cavity II flows into the sample cavity III, and the pressure in the gas inlet cavity II and the pressure in the sample cavity III are obtained through the pressure measuring part to be equal to P4(ii) a Further, may be according to P3、P4And the standard volume V of the air inlet cavity II obtained in the previous stepDoseCalculating the volume V of the sample chamber III after the sample has been addedb-samComprises the following steps:
finally, based on the ideal gas state mode, according to the volume V of the sample chamber IIIb-samStandard volume V of air inlet cavity IIDoseAnd P3、P4Calculating the amount of substance of the gas adsorbed by the sampleComprises the following steps:
based on this, can accurately measure the pressure change of the sample before and after the cavity valve 3d is closed and opened under constant temperature or different temperatures through the temperature and pressure of the controller control device, calculate the amount of the substance of the gas adsorbed by the sample, thereby evaluate the gas absorption and desorption performance of the material, simultaneously, in the process, the light of the spectrometer is incident to the sample through the light-transmitting window of the sample cell, and the emergent light is received through the detector, thereby realizing the spectrum change monitoring of the gas absorption and desorption process of the material.
In conclusion, the device controls the temperature and pressure changes in the air inlet cavity and the sample cavity in the device through the controller, and represents the adsorption and desorption performance of the sample based on the pressure changes in the air inlet cavity and the sample cavity before and after the sample is placed in the sample cavity, so that the device is simple in structure; in the sample adsorption and desorption process, the spectral change of the sample in the gas adsorption and desorption process is tested by the light-through window arranged on the sample placing pool, the test of the adsorption and desorption performance and the spectral change of the material is realized in the same process, the advantages of two types of testers are integrated, the material adsorption and desorption performance tester develops towards the direction of multifunctionalization, and convenience is provided for the performance and structural research of the material.
Although the present application has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application.
Claims (10)
1. The gas absorption and desorption performance testing device is characterized by comprising a controller, an air inlet cavity, a sample cavity and a pressure measuring component;
the air inlet cavity and the sample cavity are sequentially arranged along the airflow direction;
the pressure measuring component is positioned in the air inlet cavity and used for measuring the pressure in the air inlet cavity;
the controller is respectively electrically connected with the air inlet cavity and the sample cavity and is used for controlling the pressure in the air inlet cavity and the sample cavity according to the pressure measured by the pressure measuring component.
2. The device of claim 1, further comprising an outlet channel and at least one inlet channel, each inlet channel comprising in sequence, in the direction of gas flow, a first mass flow meter, a first solenoid valve;
the air outlet channel sequentially comprises a second electromagnetic valve and a second mass flow meter along the air flow direction.
3. The apparatus of claim 2, wherein each intake passage further comprises:
the first filter valve is arranged at the air inlet end of the first mass flow meter;
and the first one-way valve is arranged between the first mass flow meter and the first electromagnetic valve.
4. The apparatus of claim 2, wherein the outlet channel further comprises:
the second filter valve is arranged between the second electromagnetic valve and the second mass flowmeter;
and the second one-way valve is arranged at the air outlet end of the second mass flow meter.
5. The device of claim 2, further comprising a chamber valve located intermediate the gas inlet chamber and the sample chamber for regulating communication between the gas inlet chamber and the sample chamber;
preferably, the gas inlet chamber and the sample chamber have the same volume.
6. The apparatus of claim 5, wherein the air intake chamber further comprises:
the pressure release valve is arranged at the air inlet end of the pressure measurement component;
the first exhaust valve is arranged at the air inlet end of the pressure measurement component;
forming the volume of an air inlet cavity according to the first electromagnetic valve, the pressure release valve, the first exhaust valve, the pressure measuring part, the cavity valve and the connecting pipeline;
the first electromagnetic valve, the pressure measuring component and the cavity valve are sequentially arranged in the air inlet cavity along the air flow direction.
7. The device of claim 5, wherein the sample chamber further comprises a sample placing pool and a second exhaust valve arranged at the gas outlet end of the sample placing pool;
forming the volume of a sample cavity according to the cavity valve, the sample placing pool, the second exhaust valve, the second electromagnetic valve and the connecting pipeline;
the cavity valve, the sample placing pool, the second exhaust valve and the second electromagnetic valve are sequentially arranged in the sample cavity along the airflow direction.
8. The apparatus of claim 4, wherein the outlet passage further comprises a metering valve disposed in a bypass in parallel with the second solenoid valve, second filter valve, second mass flow meter, and second check valve.
9. The device of claim 1, further comprising a vacuum pump having a vacuum gauge that is displayed with a pressure when the pressure within the device is below a pressure threshold;
the device also includes a temperature controller for controlling the temperature in the gas inlet chamber and the sample chamber.
10. The device according to claim 7, wherein the sample placing pool is provided with a light-transmitting window through which the sample in the sample placing pool is subjected to in-situ spectral monitoring;
preferably, the number of the light transmission windows is at least 2, and the light transmission windows are respectively used for incidence and emergence of the light source.
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