CN109164002B - A gas adsorption test method - Google Patents
A gas adsorption test method Download PDFInfo
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- CN109164002B CN109164002B CN201811137836.0A CN201811137836A CN109164002B CN 109164002 B CN109164002 B CN 109164002B CN 201811137836 A CN201811137836 A CN 201811137836A CN 109164002 B CN109164002 B CN 109164002B
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- G01N5/02—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by absorbing or adsorbing components of a material and determining change of weight of the adsorbent, e.g. determining moisture content
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Abstract
The invention relates to the technical field of gas adsorption and desorption related to adsorbents, in particular to a gas adsorption test method, which comprises a test method when adsorption gas is introduced into a device from bottom to top, a test method when adsorption gas is introduced into the device from top to bottom and a gas adsorption efficiency measurement method.
Description
Technical Field
The invention relates to the technical field of gas adsorption and desorption related to adsorbents, in particular to a gas adsorption test method capable of carrying out bidirectional adsorption test on gas.
Background
Adsorption is an important chemical operation process, and is widely applied to the fields of petroleum, chemical industry, metallurgy, food, medicine and the like, and the basic principle is that flowing gas or liquid contacts with an adsorbent and interacts with the adsorbent, so that part of components in the gas or liquid to be adsorbed are adsorbed by the adsorbent, and the purpose of separating the gas or liquid to be adsorbed is achieved, wherein the adsorbent can be liquid or solid and can be stationary phase or mobile phase. The weighing method is a common method for researching the adsorption process, and the adsorption capacity, density and other characteristics of the adsorbent are researched by weighing the adsorbent with a certain mass before and after adsorption, however, in the prior art, only the condition that the gas is introduced into the device from top to bottom can be measured, the scene in industrial application cannot be simulated, and secondly, the adsorption experiment process of certain liquid adsorbents on the gas is slower due to insufficient contact of the gas and the liquid, so that the problem can be solved by the gas adsorption test method.
Disclosure of Invention
In order to solve the problems, the method adopts a double-sample-cavity structure which is arranged up and down, is suitable for two conditions that adsorption air flows pass through the device from top to bottom and from bottom to top, adopts a nested air pipe structure to ensure that the contact area between the liquid adsorbent and the air is large, accelerates the adsorption process, and has high air tightness of the sample cavity when the air adsorption efficiency measurement is carried out, thereby improving the accuracy of the measurement result.
The technical scheme adopted by the invention is as follows:
the gas adsorption testing device comprises a computer, a controller, a microbalance, a hanging rod, an electromagnet, a testing cavity, a vent I, a permanent magnet, a steel wire, a displacement sensor, an induction coil, a standard sample, a supporting position I, a tray I, a supporting position II, a bracket, a tray II, a supporting position III, a connecting pipe, a gas pipe I, a sample cavity I, a gas pipe II, a sample cavity II and a vent II, xyz is a three-dimensional space coordinate system, the standard sample is inert to the tested adsorption gas, the adsorption gas is not adsorbed by the standard sample, and the weight m of the standard sample in a vacuum environment rvac Volume V rvac The weights of the permanent magnet, the steel wire, the displacement sensor, the tray I, the bracket, the tray II, the connecting pipe, the air pipe I, the sample cavity I, the air pipe II and the sample cavity II are all known, and the buoyancy in the gas is negligible; the testing cavity comprises a cavity I and a cavity II, the position of the microbalance is fixed, the electromagnet is connected below the microbalance through a hanging rod, the hanging rod and the electromagnet are connected with a controller through cables, the length of the hanging rod can be adjusted through the controller, the electromagnet can be enabled to move in the y direction, the controller is connected with a computer through cables, the controller can adjust the current of the electromagnet so as to change the magnetic field distribution generated by the electromagnet, the testing cavity is positioned under the electromagnet, the testing cavity is sequentially provided with a cavity I and a cavity II from top to bottom, the inner wall of the cavity I is provided with a vent I, a supporting position II and a supporting position III from top to bottom, the permanent magnet, the steel wire, the displacement sensor, the induction coil, the standard sample, the tray I, the bracket and the tray II are positioned in the cavity I from top to bottom, the induction coil is positioned on two sides of the displacement sensor and used for detecting the displacement of the displacement sensor in the y direction and inputting the displacement sensor into the computer; the method comprises the steps that a preset value of the displacement of a permanent magnet in the y direction is input into a computer, the computer reads the real-time displacement of a displacement sensor measured by an induction coil in the y direction, a controller can adjust the current of an electromagnet and the length of a hanging rod according to the preset value of the displacement and the real-time displacement, the position of the permanent magnet can be adjusted, the relative positions of the permanent magnet, the displacement sensor, a tray I and a tray II are unchanged and are sequentially connected through steel wires, the permanent magnet, the displacement sensor, the tray I and the tray II can integrally move in the y direction, a standard sample is placed on a supporting position I, and the standard sample is placed on the supporting position I The permanent magnet is positioned at the initial position, the tray I is positioned at a position 3 mm below the standard sample, the standard sample can be lifted upwards by the tray I when the permanent magnet moves upwards by a distance exceeding 3 mm in the positive y direction, the standard sample is separated from the supporting position I, the tray II is limited in the bracket, the bracket is positioned between the supporting position II and the supporting position III, a flange is arranged below the side surface of the bracket, the initial position of the bracket is a position where the flange is contacted with the supporting position III, the flange and the supporting position III have air tightness when the bracket is positioned at the initial position, the bracket can be lifted upwards by the tray II when the permanent magnet moves upwards by a distance exceeding 5 mm in the positive y direction from the initial position, the bracket is separated from the supporting position III, and the flange is contacted with the supporting position II and has air tightness when the permanent magnet moves upwards by a distance exceeding 10 mm in the positive y direction from the initial position; connecting pipe, sample chamber I and sample chamber II all are located chamber II, bracket, connecting pipe, sample chamber I and sample chamber II connect gradually from the top down, connect through the trachea II along y direction between sample chamber I and the sample chamber II, trachea II's upper end and lower extreme link up, trachea II's internal diameter is 2 millimeters, the external diameter is 2.4 millimeters, trachea II's lower extreme is 3 millimeters from sample chamber II's interior lower surface, trachea I is located sample chamber I, trachea I's internal diameter is 3.2 millimeters, trachea I nests in trachea II's outside, trachea I's upper end is sealed, trachea I's interior upper end face is 2 millimeters from trachea II's upper end, trachea I's lower extreme is 3 millimeters from sample chamber I's interior lower surface, sample chamber I's higher authority has the gas pocket, sample chamber II's side has the gas pocket, there is air vent II below the chamber II.
Principle that the computer changes the position of the permanent magnet by adjusting the length of the suspension rod and the current of the electromagnet:
the method comprises the steps that a preset value of displacement of a permanent magnet in the y direction is input into a computer, the preset value is compared with displacement of a displacement sensor measured by an induction coil in the y direction, the length of a hanging rod is adjusted through a controller to initially change the position of the electromagnet, the weight connected below the hanging rod is changed due to the position change of the permanent magnet, in order to enable the permanent magnet to keep a suspension state, attractive force between the electromagnet and the permanent magnet is changed, the relative position between the electromagnet and the permanent magnet is also changed, the current of the electromagnet is required to be adjusted through the controller by the computer, for example, under the condition that the weight connected below the permanent magnet is increased, the current of the electromagnet is increased by the controller, the distribution of a magnetic field generated by the electromagnet is changed, the distance between the permanent magnet and the electromagnet is reduced, the length of the hanging rod and the current of the electromagnet are required to be alternately adjusted until the position of the permanent magnet reaches the preset value of the displacement.
Through remove along y direction the bracket, make the flange of the side lower limb of bracket can contact support position II respectively with support position III and have the gas tightness, can reduce gaseous turbulent flow in adsorbing the two kinds of circumstances that the air current from the top down and from the bottom up through the device, simulate industrial application scene more accurately.
The double-sample cavity and the inner and outer air pipe designs which are connected up and down are suitable for two conditions that adsorption air flows pass through the device from top to bottom and from bottom to top, and gas is led in from the bottom of the adsorbent sample solution, compared with a common sample cavity, the area of a contact area between liquid and gas in the double-sample cavity designs which are connected up and down is much larger, in addition, bubbles in the liquid rise to cause generation of a turbulent flow field, so that an adsorption process is not limited by a diffusion process of the gas any more, concentration gradient in fluid can be ignored, turbulent convection mass transfer is obviously increased, and adsorption experiments in the liquid can be carried out more quickly.
The gas adsorption test method adopts the gas adsorption test device and comprises a test method when adsorption gas is introduced into the device from bottom to top, a test method when adsorption gas is introduced into the device from top to bottom and a gas adsorption efficiency measurement method.
The testing method for the adsorption gas when the adsorption gas is introduced into the device from bottom to top comprises the following steps:
a known volume V 1 Weight m in vacuum 0vac Is placed in the sample chamber I;
secondly, adjusting the length of the suspension rod and the magnetic field distribution generated by the electromagnet through the controller, enabling the electromagnet to move in the y direction, enabling the permanent magnet to move, enabling the tray II to move upwards in the y positive direction, enabling the flange below the side face of the tray to be in contact with the supporting position II and enabling the tray II to be airtight;
introducing the adsorption gas into the cavity II from the air port II, wherein the gas flow rate value is 5-10 SCCM, and the duration time T is 30 minutes to 8 hours;
the adsorption gas enters the sample cavity II from the vent II and then enters the gas pipe I from the bottom to the top through the gas hole on the side surface of the sample cavity II, and enters the sample cavity I through a gap between the gas pipe I and the gas pipe II and then contacts with the adsorbent sample, and the adsorption gas which is not adsorbed by the adsorbent sample is discharged into the cavity I through the gas hole on the upper surface of the sample cavity I;
stopping introducing the adsorption gas from the air port II to the cavity II, and standing the device for five minutes;
the length of the suspension rod and the magnetic field distribution generated by the electromagnet are regulated by the controller, so that the electromagnet moves in the y direction, the permanent magnet moves, the tray II moves downwards for 3 mm along the y positive direction, and the total weight m of the adsorbent sample and the standard sample in the adsorbed gas environment is measured by the microbalance 1 +m r ；
Seventhly, adjusting the length of the suspension rod and the magnetic field distribution generated by the electromagnet through the controller, enabling the electromagnet to move in the y direction, enabling the permanent magnet to move to a position 4 mm above the initial position, and enabling the bracket to be located at the initial position again;
measuring the total weight m of the standard sample in the adsorbed gas environment by a microbalance r Calculating the weight m of the adsorbent sample in the adsorbed gas environment 1 ；
Ninth, calculate the density of the adsorbed gas
Calibration of buoyancy in weight measurement, calculation of the actual weight m of the adsorbent sample after gas adsorption 1vac ＝m 1 +V 1 ρ g ；
Eleven, comparing the weight change of the adsorbent sample before and after adsorbing the gas and the duration T of gas introduction, and researching the adsorption capacity of the adsorbent sample on different gases.
The testing method for the adsorption gas when the adsorption gas is introduced into the device from top to bottom comprises the following steps:
step 1, known volume V 1 Weight m in vacuum 0vac Is placed in the sample chamber II;
step 2, adjusting the length of the suspension rod and the magnetic field distribution generated by the electromagnet through the controller, so that the electromagnet moves in the y direction, the permanent magnet moves to a position 7 mm above the initial position, the tray II moves upwards along the y positive direction, and the bracket is separated from the supporting position III;
Step 3, introducing the adsorption gas into the sample cavity I from the vent I, wherein the gas flow rate is 5-10 SCCM, and the duration time T is 30 minutes to 8 hours;
step 4, after the adsorption gas is introduced into the cavity I from the vent I, the adsorption gas enters the sample cavity I through the connecting pipe and the air hole on the sample cavity I, and enters the air pipe II through a gap between the air pipe I and the air pipe II, then enters the sample cavity II from top to bottom through the air pipe II and contacts the adsorbent sample, and the adsorption gas which is not adsorbed by the adsorbent sample enters the cavity II through the air hole on the side surface of the sample cavity II and is finally discharged from the vent II;
step 5, stopping introducing the adsorption gas from the vent I to the cavity I, and standing the device for five minutes;
step 6, measuring the total weight m of the adsorbent sample and the standard sample in the adsorption gas environment through a microbalance 1 +m r The method comprises the steps of carrying out a first treatment on the surface of the Step 7, adjusting the length of the suspension rod and the magnetic field distribution generated by the electromagnet through the controller, so that the electromagnet moves in the y direction, and the permanent magnet moves to a position 4 mm above the initial position, so that the bracket is positioned at the initial position again;
step 8, measuring the total weight m of the standard sample in the gas adsorption environment through a microbalance r Calculating the weight m of the adsorbent sample in the adsorbed gas environment 1 ；
Step 9, calculating to obtain the density of the adsorbed gas
Step 10, calibrating the buoyancy in the weight measurement, and calculating to obtain the actual weight m of the adsorbent sample after adsorbing the gas 1vac ＝m 1 +V 1 ρ g ；
Step 11, comparing the weight change of the adsorbent sample before and after adsorbing the gas and the duration T of gas introduction, and researching the adsorption capacity of the adsorbent sample on different gases.
In the case of gas adsorption efficiency measurement, it is necessary to record the mass m of the gas introduced into the chamber II from the vent II total And measuring the mass m of the gas adsorbed by the adsorbent sample sop Calculating to obtain the gas adsorption efficiency m sop /m total In order to reduce errors, the chamber II needs to have good tightness during the gas adsorption process.
The method for measuring the gas adsorption efficiency comprises the following steps:
step one, a known volume V 1 Weight m in vacuum 0vac Placing an adsorbent sample in the sample cavity I;
step two, keeping the bracket at the initial position;
step three, the mass m total The adsorption gas is introduced into the cavity II from the air vent II, enters the sample cavity II from the air vent II through an air hole on the side surface of the sample cavity II, enters the air pipe I from the lower part to the upper part after passing through the air pipe II, enters the sample cavity I through a gap between the air pipe I and the air pipe II, contacts with an adsorbent sample, is kept for 1 hour, and the air pressure P at the air vent II is measured 2 ；
Step four, adsorbing gas is introduced into the cavity I from the air vent I, the gas flow speed value is 1SCCM, and the air pressure at the air vent I is P 2 Stopping introducing gas from the vent I;
step five, adjusting the length of the suspension rod and the magnetic field distribution generated by the electromagnet through the controller, so that the electromagnet moves in the y direction, the permanent magnet moves to a position 7 mm above the initial position, the tray II moves upwards along the y positive direction, the bracket is lifted upwards from the initial position, and the bracket is separated from the supporting position III;
step six, measuring the total weight m of the adsorbent sample and the standard sample in the adsorption gas environment through a microbalance 1 +m r ；
Step seven, adjusting the length of the suspension rod and the magnetic field distribution generated by the electromagnet through the controller, so that the electromagnet moves in the y direction, and the permanent magnet moves to a position 4 mm above the initial position, so that the bracket is positioned at the initial position again;
step eight, measuring the total weight m of the standard sample in the gas adsorption environment through a microbalance r Calculating the weight m of the adsorbent sample in the adsorbed gas environment 1 ；
Step nine, calculating to obtain the density of the adsorbed gas
Step ten, calibrating the buoyancy in the weight measurement, and calculating to obtain the actual weight m of the adsorbent sample after adsorbing the gas 1vac ＝m 1 +V 1 ρ g ；
Step eleven, calculating the weight m of the gas adsorbed by the adsorbent sample sop ＝m 1vac -m 0vac Calculating to obtain the gas adsorption efficiency m sop /m total 。
The beneficial effects of the invention are as follows:
the method can be used for researching two adsorption processes of adsorbing air flow from top to bottom and from bottom to top through the device respectively, the experimental operation flow is simple, the adsorption process time is short, and in addition, the accuracy of the measurement result of the gas adsorption efficiency is higher.
Drawings
The following is further described in connection with the figures of the present invention:
FIG. 1 is a schematic illustration of the present invention;
FIG. 2 is one of the schematic diagrams of sample chamber I and sample chamber II;
FIG. 3 is a second schematic view of sample chamber I and sample chamber II.
In the figure, 1, a computer, 2, a controller, 3, a microbalance, 4, a hanging rod, 5, an electromagnet, 6, a test cavity, 6-1, a cavity I,6-2, a cavity II,7, a vent I,8, a permanent magnet, 9, a steel wire, 10, a displacement sensor, 11, an induction coil, 12, a standard sample, 13, a support position I,14, a tray I,15, a support position II,16, a bracket, 17, a tray II,18, a support position III,19, a connecting pipe, 20, an air pipe I,21, a sample cavity I,22, an air pipe II,23, a sample cavity II,24 and a vent II.
Detailed Description
As shown in fig. 1, xyz is a three-dimensional space coordinate system and comprises a computer (1), a controller (2), a microbalance (3), a suspension rod (4), an electromagnet (5), a test cavity (6), a vent I (7), a permanent magnet (8), a steel wire (9), a displacement sensor (10), an induction coil (11), a standard sample (12), a supporting position I (13), a tray I (14), a supporting position II (15), a bracket (16), a tray II (17), a supporting position III (18), a connecting pipe (19), an air pipe I (20), a sample cavity I (21), an air pipe II (22), a sample cavity II (23) and a vent II (24), the test cavity (6) comprises a cavity I (6-1) and a cavity II (6-2), the microbalance (3) is fixed in position, the electromagnet (5) is connected below the microbalance (3) through the suspension rod (4), the suspension rod (4) and the electromagnet (5) are connected with the controller (2) through cables, the length of the suspension rod (4) can be adjusted through the controller (2) so that the electromagnet (5) can move in the y direction of the controller (2), the controller (2) can adjust the current of the electromagnet (5) so as to change the magnetic field distribution generated by the electromagnet (5), the test cavity (6) is positioned under the electromagnet (5), the test cavity (6) is sequentially provided with a cavity I (6-1) and a cavity II (6-2) from top to bottom, the inner wall of the cavity I (6-1) is provided with a vent I (7), a supporting position I (13), a supporting position II (15) and a supporting position III (18) from top to bottom, the permanent magnet (8), the steel wire (9), the displacement sensor (10), the induction coil (11), the standard sample (12), the tray I (14), the bracket (16) and the tray II (17) are positioned in the cavity I (6-1) from top to bottom, the induction coil (11) is positioned at two sides of the displacement sensor (10) and used for detecting the displacement of the displacement sensor (10) in the y direction and inputting the displacement sensor to the computer (1); the computer (1) is input with a preset value of the displacement of the permanent magnet (8) in the y direction, and the meter The computer (1) reads the real-time displacement of the displacement sensor (10) measured by the induction coil (11) in the y direction, the controller (2) can adjust the current of the electromagnet (5) and the length of the hanging rod (4) according to the preset value of the displacement and the real-time displacement, the position of the permanent magnet (8) can be adjusted, the relative positions of the permanent magnet (8), the displacement sensor (10), the tray I (14) and the tray II (17) are unchanged and are sequentially connected through the steel wire (9), the permanent magnet (8), the displacement sensor (10), the tray I (14) and the tray II (17) can integrally move in the y direction, the standard sample (12) is placed on the supporting position I (13), the standard sample (12) is provided with a through hole in the vertical y direction, the steel wire (9) passes through the through hole in a non-contact manner, when the permanent magnet (8) is positioned at the initial position, the tray I (14) is positioned at the position of 3 mm below the standard sample (12), when the permanent magnet (8) moves upwards by more than 3 mm in the y direction, the tray I (14) and the tray I (16) can be lifted up to the standard sample (16) in the position of the standard sample (16) in the vertical direction, the standard sample (16) is separated from the standard sample (16) in the supporting position II (16) in the vertical direction, the standard sample (12) is positioned between the standard sample (16) and the standard sample (16) in the standard sample (13) in the supporting position and the standard sample in the standard position of the standard position in the vertical direction. The lower side of the side face of the bracket (16) is provided with a flange, the initial position of the bracket (16) is the contact position of the flange and the supporting position III (18), when the bracket (16) is at the initial position, the flange and the supporting position III (18) are airtight, when the permanent magnet (8) moves upwards from the initial position in the positive y direction for more than 5 mm distance, the bracket (16) can be lifted upwards by the tray II (17), so that the bracket (16) is separated from the supporting position III (18), and when the permanent magnet (8) moves upwards from the initial position in the positive y direction for 10 mm distance, the flange is in contact with the supporting position II (15) and is airtight; connecting pipe (19), sample cavity I (21) and sample cavity II (23) are all located in cavity II (6-2), bracket (16), connecting pipe (19), sample cavity I (21) and sample cavity II (23) are connected in proper order from top to bottom, cavity II (6-2) is below to have air vent II (24), and standard sample (12) is inert to the adsorption gas that is tested, and adsorption gas can not be adsorbed by standard sample (12), and weight m of standard sample (12) in vacuum environment rvac Volume V rvac Is known, the weight of the permanent magnet (8), the steel wire (9), the displacement sensor (10), the tray I (14), the bracket (16), the tray II (17), the connecting pipe (19), the air pipe I (20), the sample cavity I (21), the air pipe II (22) and the sample cavity II (23)The amounts are known and the buoyancy in the gas is negligible.
Fig. 2 is one of the schematic diagrams of the sample cavity I and the sample cavity II, fig. 3 is the second schematic diagram of the sample cavity I and the sample cavity II, the sample cavity I (21) and the sample cavity II (23) are connected through an air pipe II (22) along the y direction, the upper end and the lower end of the air pipe II (22) are communicated, the inner diameter of the air pipe II (22) is 2 mm, the outer diameter of the air pipe II (22) is 2.4 mm, the lower end of the air pipe II (22) is 3 mm away from the inner bottom surface of the sample cavity II (23), the air pipe I (20) is positioned in the sample cavity I (21), the inner diameter of the air pipe I (20) is 3.2 mm, the air pipe I (20) is nested outside the air pipe II (22), the upper end of the air pipe I (20) is sealed, the inner upper end of the air pipe I (20) is 2 mm away from the inner bottom surface of the sample cavity I (21), the upper surface of the sample cavity I (21) is provided with air holes, and the side surface of the sample cavity II (23) is provided with air holes. As shown in fig. 2, corresponding to the condition that the adsorption gas is introduced into the device from bottom to top, the adsorption gas enters the cavity II (6-2) from the vent hole II (24) and then enters the sample cavity II (23) through the air holes on the side surface of the sample cavity II (23), the adsorption gas enters the air pipe I (20) from bottom to top after passing through the air pipe II (22), and enters the sample cavity I (21) through the gap between the air pipe I (20) and the air pipe II (22) and then contacts with the adsorbent sample, and the adsorption gas which is not adsorbed by the adsorbent sample is discharged through the air holes on the upper surface of the sample cavity I (21); referring to fig. 3, in response to the condition that the adsorption gas is introduced into the device from top to bottom, the adsorption gas enters the sample chamber I (21) through the air hole on the connecting pipe (19) and the sample chamber I (21) after being introduced into the chamber I (6-1) from the air port I (7), enters the air pipe II (22) through the gap between the air pipe I (20) and the air pipe II (22), then enters the sample chamber II (23) from top to bottom through the air pipe II (22) and contacts the adsorbent sample, and the adsorption gas which is not adsorbed by the adsorbent sample enters the chamber II (6-2) through the air hole on the side surface of the sample chamber II (23) and is finally discharged from the air port II (24).
The gas adsorption testing device comprises a computer (1), a controller (2), a microbalance (3), a suspension rod (4), an electromagnet (5), a testing cavity (6), a vent I (7), a permanent magnet (8), a steel wire (9), a displacement sensor (10), an induction coil (11), a standard sample (12), a supporting position I (13), a tray I (14), a supporting position II (15), a bracket (16), a tray II (17), a supporting position III (18),Connecting pipe (19), air pipe I (20), sample cavity I (21), air pipe II (22), sample cavity II (23) and air port II (24), xyz is a three-dimensional space coordinate system, standard sample (12) is inert to the tested adsorption gas, the adsorption gas is not adsorbed by standard sample (12), and the weight m of standard sample (12) in vacuum environment rvac Volume V rvac The weights of the permanent magnet (8), the steel wire (9), the displacement sensor (10), the tray I (14), the bracket (16), the tray II (17), the connecting pipe (19), the air pipe I (20), the sample cavity I (21), the air pipe II (22) and the sample cavity II (23) are known, and the buoyancy in gas is negligible; the test cavity (6) comprises a cavity I (6-1) and a cavity II (6-2), the microbalance (3) is fixed in position, the electromagnet (5) is connected to the lower part of the microbalance (3) through a hanging rod (4), the hanging rod (4) and the electromagnet (5) are connected with a controller (2) through cables, the length of the hanging rod (4) can be adjusted through the controller (2), the electromagnet (5) can move in the y direction, the controller (2) is connected with a computer (1) through cables, the controller (2) can adjust the current of the electromagnet (5) so as to change the magnetic field distribution generated by the electromagnet (5), the test cavity (6) is positioned under the electromagnet (5), the test cavity (6) is sequentially provided with a cavity I (6-1) and a cavity II (6-2) from top to bottom, the inner wall of the cavity I (6-1) is provided with a vent I (7), a supporting position I (13), a supporting position II (15) and a supporting position III (18), the permanent magnet (8), a steel wire (9), a displacement sensor (10), an induction coil (11), a supporting sample (14), a supporting sample (16) and a tray (16) are positioned in the tray (1) from top to bottom (16) and a tray (1) in the tray (17) from top to bottom, the induction coils (11) are positioned at two sides of the displacement sensor (10) and are used for detecting the displacement of the displacement sensor (10) in the y direction and inputting the displacement into the computer (1); the controller (2) can adjust the position of the permanent magnet (8) according to the preset value of the displacement of the permanent magnet (8) in the y direction input in the computer (1) and the displacement of the displacement sensor (10) in the y direction measured by the induction coil (11), the position of the permanent magnet (8) can be adjusted by adjusting the current of the electromagnet (5) and the length of the suspension rod (4), the relative positions of the permanent magnet (8), the displacement sensor (10), the tray I (14) and the tray II (17) are unchanged and are sequentially connected through the steel wire (9), the permanent magnet (8), the displacement sensor (10), the tray I (14) and the tray II (17) can integrally move in the y direction, the standard sample (12) is arranged on the supporting position I (13), and the standard sample (12) is provided with a through hole in the vertical y direction The steel wire (9) passes through the through hole in a non-contact way, when the permanent magnet (8) is positioned at the initial position, the tray I (14) is positioned at a position 3 mm below the standard sample (12), when the permanent magnet (8) moves upwards in the y positive direction by more than 3 mm distance, the tray I (14) can lift the standard sample (12) upwards, so that the standard sample (12) is separated from the supporting position I (13), the tray II (17) is limited in the tray (16), the tray (16) is positioned between the supporting position II (15) and the supporting position III (18), a flange is arranged below the side surface of the tray (16), the initial position of the bracket (16) is a position where the flange is contacted with the supporting position III (18), when the permanent magnet (8) is positioned at the initial position, the flange is airtight with the supporting position III (18), when the permanent magnet (8) moves upwards in the y positive direction by more than 5 mm distance, the tray II (17) can lift the tray (16) upwards, so that the tray (16) is separated from the supporting position III (18) and the permanent magnet (8) is separated from the supporting position II) by more than 5 mm distance in the y positive direction, and when the permanent magnet (8) moves upwards in the y positive direction, the initial position is contacted with the flange (10 mm) and has the initial position; connecting pipe (19), sample chamber I (21) and sample chamber II (23) all are located chamber II (6-2), bracket (16), connecting pipe (19), sample chamber I (21) and sample chamber II (23) connect gradually from the top down, connect through trachea II (22) along the y direction between sample chamber I (21) and sample chamber II (23), the upper end and the lower extreme of trachea II (22) link up, the internal diameter of trachea II (22) is 2 millimeters, the external diameter is 2.4 millimeters, the lower extreme of trachea II (22) is 3 millimeters from the interior lower surface of sample chamber II (23), trachea I (20) are located sample chamber I (21), the internal diameter of trachea I (20) is 3.2 millimeters, trachea I (20) nest in the outside of trachea II (22), the upper end of trachea I (20) is sealed, the interior upper end face of trachea I (20) is 2 millimeters from the upper end of trachea II (22), the lower extreme of trachea I (20) is 3 millimeters from the interior lower surface of sample chamber I (21), the mask has gas pocket II (24) on the side has gas pocket II (24) of sample chamber II.
The principle that the computer (1) changes the position of the permanent magnet (8) by adjusting the length of the hanging rod (4) and the current of the electromagnet (5):
the method comprises the steps that a preset value of displacement of a permanent magnet (8) in the y direction is input into a computer (1), the preset value is compared with the displacement of a displacement sensor (10) measured by an induction coil (11) in the y direction by the computer (1), the length of a hanging rod (4) is adjusted through a controller (2) to primarily change the position of the electromagnet (5), the distance between the permanent magnet (8) and the electromagnet (5) is reduced due to the change of the position of the permanent magnet (8), in order to enable the permanent magnet (8) to keep a suspension state, attractive force between the electromagnet (5) and the permanent magnet (8) is changed, the relative position between the electromagnet (5) and the permanent magnet (8) is also changed, the computer (1) needs to adjust the current of the electromagnet (5) through the controller (2), for example, under the condition that the weight connected below the permanent magnet (8) is increased, the current of the electromagnet (5) is increased, the magnetic field distribution generated by the electromagnet (5) is changed, the distance between the permanent magnet (8) and the electromagnet (5) is reduced, and the relative position between the preset value and the induction coil (11) is required to be compared again, the current of the electromagnet (5) is adjusted, and the displacement of the electromagnet (5) is not changed, and the displacement of the permanent magnet (10) is adjusted in the y direction.
The testing method for the adsorption gas when the adsorption gas is introduced into the device from bottom to top comprises the following steps:
a known volume V 1 Weight m in vacuum 0vac Is placed in a sample chamber I (21);
secondly, the length of the hanging rod (4) and the magnetic field distribution generated by the electromagnet (5) are regulated by the controller (2), so that the electromagnet (5) moves in the y direction, the permanent magnet (8) moves, the tray II (17) moves upwards in the y positive direction, and the flange at the lower side of the side surface of the bracket (16) is contacted with the supporting position II (15) and has air tightness;
introducing the adsorbed gas from the gas port II (24) into the cavity II (6-2), wherein the gas flow rate is 5-10 SCCM, and the duration T is 30 minutes to 8 hours;
fourth, the adsorption gas enters the cavity II (6-2) from the vent II (24), enters the sample cavity II (23) through the air holes on the side surface of the sample cavity II (23), enters the air pipe I (20) from bottom to top after passing through the air pipe II (22), enters the sample cavity I (21) through the gap between the air pipe I (20) and the air pipe II (22), contacts with the adsorbent sample, and the adsorption gas which is not adsorbed by the adsorbent sample is discharged into the cavity I (6-1) through the air holes on the upper surface of the sample cavity I (21);
stopping introducing the adsorption gas from the air port II (24) to the cavity II (6-2), and standing the device for five minutes;
Regulating the length of the hanging rod (4) and the magnetic field distribution generated by the electromagnet (5) through the controller (2), enabling the electromagnet (5) to move in the y direction and enabling the permanent magnet (8) to move, enabling the tray II (17) to move downwards for 3 mm distance along the y positive direction, and measuring the total weight m of the adsorbent sample and the standard sample (12) in the adsorbed gas environment through the microbalance (3) 1 +m r ；
Seventhly, the length of the hanging rod (4) and the magnetic field distribution generated by the electromagnet (5) are regulated by the controller (2), so that the electromagnet (5) moves in the y direction, the permanent magnet (8) moves to the position 4 mm above the initial position, the bracket (16) is positioned at the initial position again,
measuring the total weight m of the standard sample (12) in the adsorbed gas environment by means of a microbalance (3) r Calculating the weight m of the adsorbent sample in the adsorbed gas environment 1 ；
Ninth, calculate the density of the adsorbed gas
Calibration of buoyancy in weight measurement, calculation of the actual weight m of the adsorbent sample after gas adsorption 1vac ＝m 1 +V 1 ρ g ；
Eleven, comparing the weight change of the adsorbent sample before and after adsorbing the gas and the duration T of gas introduction, and researching the adsorption capacity of the adsorbent sample on different gases.
The testing method for the adsorption gas when the adsorption gas is introduced into the device from top to bottom comprises the following steps:
Step 1, known volume V 1 Weight m in vacuum 0vac Is placed in a sample chamber II (23);
step 2, adjusting the length of the hanging rod (4) and the magnetic field distribution generated by the electromagnet (5) through the controller (2), enabling the electromagnet (5) to move in the y direction, enabling the permanent magnet (8) to move to a position 7 mm above the initial position, enabling the tray II (17) to move upwards in the y positive direction, and enabling the bracket (16) to be separated from the supporting position III (18);
step 3, introducing the adsorption gas into the sample cavity I (6-1) from the vent I (7), wherein the gas flow rate value is 5-10 SCCM, and the duration time T is 30 minutes to 8 hours;
step 4, after the adsorption gas is introduced into the cavity I (6-1) from the vent I (7), the adsorption gas enters the sample cavity I (21) through the connecting pipe (19) and the air hole above the sample cavity I (21), enters the air pipe II (22) through a gap between the air pipe I (20) and the air pipe II (22), then enters the sample cavity II (23) from top to bottom through the air pipe II (22) and contacts with the adsorbent sample, and the adsorption gas which is not adsorbed by the adsorbent sample enters the cavity II (6-2) through the air hole at the side surface of the sample cavity II (23) and is finally discharged from the vent II (24);
step 5, stopping introducing the adsorption gas from the vent I (7) to the cavity I (6-1), and standing the device for five minutes;
Step 6, measuring the total weight m of the adsorbent sample and the standard sample (12) in the adsorption gas environment through a microbalance (3) 1 +m r ；
Step 7, adjusting the length of the hanging rod (4) and the magnetic field distribution generated by the electromagnet (5) through the controller (2), enabling the electromagnet (5) to move in the y direction, enabling the permanent magnet (8) to move to a position 4 mm above the initial position, and enabling the bracket (16) to be located at the initial position again;
step 8, measuring the total weight m of the standard sample (12) in the adsorption gas environment through the microbalance (3) r Calculating the weight m of the adsorbent sample in the adsorbed gas environment 1 ；
Step 9, calculating to obtain the density of the adsorbed gas
Step 10, calibrating the buoyancy in the weight measurement, and calculating to obtain the actual weight m of the adsorbent sample after adsorbing the gas 1vac ＝m 1 +V 1 ρ g ；
Step 11, comparing the weight change of the adsorbent sample before and after adsorbing the gas and the duration T of gas introduction, and researching the adsorption capacity of the adsorbent sample on different gases.
In the case of gas adsorption efficiency measurement, it is necessary to record the mass m of the gas introduced into the chamber II (6-2) from the vent II (24) total And measuring the mass m of the gas adsorbed by the adsorbent sample sop Calculating to obtain the gas adsorption efficiency m sop /m total In order to reduce errors, the chamber II (6-2) needs to have good tightness during the gas adsorption process.
The method for measuring the gas adsorption efficiency comprises the following steps:
step one, a known volume V 1 Weight m in vacuum 0vac The adsorbent sample is placed in a sample cavity I (21);
step two, keeping the bracket (16) at a starting position;
step three, the mass m total Is introduced into the cavity II (6-2) from the air vent II (24), is introduced into the cavity II (6-2) from the air vent II (24) and then enters the sample cavity II (23) through an air hole on the side surface of the sample cavity II (23), is introduced into the air pipe I (20) from bottom to top through the air pipe II (22), is introduced into the sample cavity I (21) through a gap between the air pipe I (20) and the air pipe II (22), is contacted with an adsorbent sample, and is kept for 1 hour, and the air pressure P at the air vent II (24) is measured 2 ；
Step four, adsorbing gas is introduced into the cavity I (6-1) from the air port I (7), the gas flow speed value is 1SCCM, and the air pressure at the air port I (7) is P 2 Stopping introducing gas from the air port I (7);
step five, adjusting the length of the hanging rod (4) and the magnetic field distribution generated by the electromagnet (5) through the controller (2), enabling the electromagnet (5) to move in the y direction, enabling the permanent magnet (8) to move to a position 7 mm above the initial position, enabling the tray II (17) to move upwards in the y positive direction, lifting the tray (16) upwards from the initial position, and enabling the tray (16) to be separated from the supporting position III (18);
Step six, measuring the total weight m of the adsorbent sample and the standard sample (12) in the adsorption gas environment through a microbalance (3) 1 +m r ；
Step seven, the length of the hanging rod (4) and the magnetic field distribution generated by the electromagnet (5) are adjusted through the controller (2), so that the electromagnet (5) moves in the y direction, the permanent magnet (8) moves to the position 4 mm above the initial position, and the bracket (16) is located at the initial position again;
step eight, measuring the total weight m of the standard sample (12) in the adsorption gas environment through a microbalance (3) r Calculating the weight m of the adsorbent sample in the adsorbed gas environment 1 ；
Step nine, calculating to obtain the density of the adsorbed gas
Step ten, calibrating the buoyancy in the weight measurement, and calculating to obtain the actual weight m of the adsorbent sample after adsorbing the gas 1vac ＝m 1 +V 1 ρ g ；
Step eleven, calculating the weight m of the gas adsorbed by the adsorbent sample sop ＝m 1vac -m 0vac Calculating to obtain the gas adsorption efficiency m sop /m total 。
The method adopts the design that the two sample cavities are arranged up and down, can be used for researching the adsorption process of the adsorption air flow passing through the device from top to bottom and from bottom to top respectively, adopts the inner and outer nested air pipes to enable the adsorption process to be faster, and adopts the design of the sample cavities with air tightness to enable the accuracy to be higher when the gas adsorption efficiency measurement is carried out.
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