CN107367440B - Method for acetylene adsorption measurement - Google Patents
Method for acetylene adsorption measurement Download PDFInfo
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- CN107367440B CN107367440B CN201710506863.XA CN201710506863A CN107367440B CN 107367440 B CN107367440 B CN 107367440B CN 201710506863 A CN201710506863 A CN 201710506863A CN 107367440 B CN107367440 B CN 107367440B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
- G01N7/02—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder
- G01N7/04—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder by absorption or adsorption alone
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/32—Hydrogen storage
Abstract
The invention relates to the field of performance test of adsorption materials, in particular to a method for acetylene adsorption measurement, which comprises the steps of placing a nano material sample subjected to drying and degassing treatment into a sample cavity; starting a vacuum pump and an electromagnetic valve to carry out vacuum degassing on the device; filling high-purity nitrogen into the reference cavity, the sample cavity and other areas in the vacuum system of the device, and recording related data; determining the number of moles of gas entering the vacuum system of the device from the mass flow controller data and calculating the volume of gas flowing through the mass flow controller; starting a vacuum pump and an electromagnetic valve to pump out nitrogen in the device; acetylene gas is filled into the reference cavity; expanding acetylene gas in a reference cavity into the sample cavity, and recording a barometer reading and a thermocouple reading; starting a vacuum pump and an electromagnetic valve to pump out acetylene gas in the device; recording barometer and thermocouple readings at each equilibrium state pressure; calculating the gas adsorption quantity expressed in terms of mole number; and drawing the obtained gas adsorption quantity data points under each equilibrium state of air pressure into curves to obtain adsorption isotherms.
Description
Technical Field
The invention relates to the field of performance testing of adsorption materials, in particular to a method for acetylene adsorption measurement, which can more accurately determine the vacuum system volume of a device, reduce errors in the calibration process and measure the total vacuum system volume by using a mass flow controller, thereby avoiding using a calibration sample.
Background
The basic method for measuring gas adsorption by the capacity method is that a vacuum system comprises a container I and a container II, a certain amount of adsorbent sample is placed in the container I, the container I is emptied of gas and kept at a certain temperature, then a known amount of gas is introduced into the container I through a container II with a certain volume, after the adsorbent adsorbs a certain amount of gas, the gas pressure in the container I and the container II reaches equilibrium, and the adsorption amount can be calculated according to the change of the gas pressure before and after adsorption. And gradually increasing the pressure of the gas in the container II to the vacuum system, repeating the steps to obtain the gas adsorption quantity under different equilibrium pressures, drawing data points of the gas adsorption quantity under each equilibrium state pressure on a two-dimensional graph and connecting the two-dimensional graph to form a curve, wherein the ordinate is the gas adsorption quantity, and the abscissa is the equilibrium state pressure, so that an adsorption isotherm under a certain temperature condition can be obtained.
In the prior art, the dynamic volumes of acetylene molecules are often different from the gases such as helium, nitrogen, etc. used for device volume determination, which results in inaccurate estimates of sample density for certain materials, such as materials with larger distributions of pore sizes or materials with pore sizes close to the gas molecules, and thus require more accurate testing devices, especially in terms of determination of vacuum system volumes. In addition, the valves used in the existing different types of testing devices can cause errors in volume measurement, and the method for measuring acetylene adsorption can solve the problem.
Disclosure of Invention
In order to solve the problems, the invention can reduce the systematic error in the gas adsorption measurement, and the air pressure range for testing is 10 -10 The mbar to 500bar is a capacity method adsorption measurement method with higher experimental accuracy.
The technical scheme adopted by the invention is as follows:
the method for acetylene adsorption measurement mainly comprises an air storage tank I, an air storage tank II, an electromagnetic valve I, a mass flow controller, an electromagnetic valve II, a reference cavity, an electromagnetic valve III, a barometer, a thermocouple, an electromagnetic valve IV, a vacuum pump, an electromagnetic valve V, a sample cavity and an air pipe, wherein one end of the electromagnetic valve I is connected with the air storage tank I and the air storage tank II through a valve air pipe, the other end of the electromagnetic valve I is sequentially connected with the mass flow controller, the electromagnetic valve II, the reference cavity, the electromagnetic valve IV and the vacuum pump through the electromagnetic valve III, the barometer is connected with the reference cavity through the electromagnetic valve III, the thermocouple is positioned outside the reference cavity, the sample cavity is connected with the reference cavity through the electromagnetic valve V, acetylene gas for testing is filled in the air storage tank I, the gas storage tank II is filled with high-purity nitrogen, the barometer and the thermocouple are respectively used for monitoring the pressure and the temperature of gas in the reference cavity, the vacuum pump is used for vacuumizing the device, the sample cavity is positioned in a constant temperature tank to maintain the required temperature, the mass flow controller controls the flow rate of the gas entering the reference cavity and can be adjusted between 0SLM and 30SLM, the error is +/-0.2%, the types of the electromagnetic valve I, the electromagnetic valve II, the electromagnetic valve III, the electromagnetic valve IV and the electromagnetic valve V are respectively of Burset 2400, and the internal volume of the electromagnetic valve I, the electromagnetic valve III, the electromagnetic valve IV and the electromagnetic valve V are not changed in the changing process between opening and closing, and the method for measuring the acetylene adsorption comprises the following steps:
firstly, placing a nano material sample subjected to drying and degassing treatment into the sample cavity;
secondly, starting the vacuum pump, and starting the electromagnetic valve I, the electromagnetic valve II, the electromagnetic valve III, the electromagnetic valve IV and the electromagnetic valve V to perform vacuum degassing on the device;
closing the electromagnetic valve IV and the electromagnetic valve V, and opening valves on the gas storage tank II to enable high-purity nitrogen to be filled into the reference cavity, the sample cavity and other areas in the device vacuum system, wherein in the process, the mass flow controller sets a certain parameter to control the gas flow rate and records related data;
determining the number of moles of gas entering the vacuum system of the device from the flow data of the mass flow controller and calculating the volume of gas flowing through the mass flow controllerWith air pressure P and total volume of vacuum system V tot The relation of->Wherein T is N And P N Is the temperature and air pressure under normal conditions, T is the temperature of the vacuum system volume, estimated +.>The slope of the curve enables the determination of V tot =V S +V R +V other Wherein V is S V being the volume of the sample chamber R V being the volume of the reference chamber other Is the volume of other areas within the device vacuum system;
fifthly, starting the vacuum pump, and starting the electromagnetic valve I, the electromagnetic valve II, the electromagnetic valve III, the electromagnetic valve IV and the electromagnetic valve V to pump out nitrogen in the device;
closing the electromagnetic valve IV and the electromagnetic valve V, opening a valve on the gas storage tank I, filling acetylene gas into the reference cavity, and closing the electromagnetic valve I after the acetylene gas reaches an equilibrium state;
seventhly, opening the electromagnetic valve V to enable acetylene gas in the reference cavity to expand into the sample cavity, and recording the reading of the barometer and the reading of the thermocouple after the air pressure is balanced;
opening the vacuum pump, opening the electromagnetic valve I, the electromagnetic valve II, the electromagnetic valve III, the electromagnetic valve IV and the electromagnetic valve V, and pumping out acetylene gas in the device;
ninth, repeating the steps six to eight until the air pressure reaches 500bar, repeating the steps for N times, and recording the barometer reading and thermocouple reading under each balanced state air pressure;
ten, calculating the gas adsorption quantity, wherein the gas adsorption quantity is expressed in terms of mole number, and after the gas expands from the reference cavity to enter the sample cavity, when the gas pressure reaches an equilibrium state, the mole number of the gas is reduced, namely the mole number of the gas to be absorbed; at each equilibrium state pressure, the gas adsorption quantity n is calculated through the true gas law ads =r i [V R (r 0 /r i -1)-V S ]+r i-1 V S Wherein r is i =P i /(Z(T i ,P i )RT i ) Is the molar density of the gas, i is an integer from 1 to N, Z (T i ,P i ) Is the gas at the temperature T i And air pressure P i Compression coefficient under the condition, r 0 Is the molar density in the reference chamber, r, before gas expansion i Is the molar density of the gas after expansion in the sample chamber and absorption by the sample; and drawing the data points of the gas adsorption quantity under each equilibrium state gas pressure on a two-dimensional graph and connecting the two-dimensional graph into a curve, wherein the ordinate is the adsorption mole number, and the abscissa is the equilibrium state gas pressure, so that an adsorption isotherm is obtained.
The beneficial effects of the invention are as follows:
the invention can more accurately determine the vacuum system volume of the device, reduce errors in the calibration process, use the mass flow controller to measure the total vacuum system volume, reduce the uncertainty of experimental results, avoid using calibration samples, and is a capacity method adsorption measurement method with higher experimental precision.
Drawings
The following is further described in connection with the figures of the present invention:
FIG. 1 is a schematic diagram of the present invention.
In the figure, a gas tank I, a gas tank II, a solenoid valve I, a mass flow controller 4, a solenoid valve II, a reference cavity 6, a solenoid valve III, a barometer 8, a thermocouple 9, a solenoid valve 10, a solenoid valve IV, a vacuum pump 11, a solenoid valve V, and a sample cavity 13.
Detailed Description
As shown in FIG. 1, the measuring device mainly comprises an air storage tank I1, an air storage tank II2, an electromagnetic valve I3, a mass flow controller 4, an electromagnetic valve II5, a reference cavity 6, an electromagnetic valve III7, a barometer 8, a thermocouple 9, an electromagnetic valve IV10, a vacuum pump 11, an electromagnetic valve V12, a sample cavity 13 and an air pipe, wherein one end of the electromagnetic valve I3 is connected with the air storage tank I1 and the air storage tank II2 through valve air pipes, the other end of the electromagnetic valve I3 is connected with the mass flow controller 4, the electromagnetic valve II5, the reference cavity 6, the electromagnetic valve IV10 and the vacuum pump 11 through air pipes in sequence, the barometer 8 is connected with the reference cavity 6 through the electromagnetic valve III7, the thermocouple 9 is positioned outside the reference cavity 6, the sample cavity 13 is connected with the reference cavity 6 through the electromagnetic valve V12, the gas tank I1 is filled with acetylene gas for test, the gas tank II2 is filled with high-purity nitrogen, the barometer 8 and the thermocouple 9 are respectively used for monitoring the pressure and the temperature of the gas in the reference cavity 6, the vacuum pump 11 is used for vacuumizing the device, the sample cavity 13 is positioned in a constant temperature tank to maintain the required temperature, the mass flow controller 4 controls the flow rate of the gas entering the reference cavity 6 and can be adjusted between 0 and 30SLM, the error is +/-0.2%, the types of the electromagnetic valve I3, the electromagnetic valve II5, the electromagnetic valve III7, the electromagnetic valve IV10 and the electromagnetic valve V12 are of the type Burnet 2400, and are specially designed so that the internal volume of the electromagnetic valve is not changed in the changing process between opening and closing, and the method for measuring the acetylene adsorption comprises the following steps:
firstly, placing a nano material sample subjected to drying and degassing treatment into the sample cavity 13;
secondly, starting the vacuum pump 11, and starting the electromagnetic valves I3, II5, III7, IV10 and V12 to perform vacuum degassing on the device;
closing the electromagnetic valve IV10 and the electromagnetic valve V12, and opening valves on the gas storage tank II2 to enable high-purity nitrogen to be filled into the reference cavity 6, the sample cavity 13 and other areas in a device vacuum system, wherein in the process, the mass flow controller 4 sets a certain parameter to control the gas flow rate and records related data;
determining the number of moles of gas entering the vacuum system of the device from the flow data of the mass flow controller 4 and calculating the volume of gas flowing through the mass flow controller (4)With air pressure P and total volume of vacuum system V tot The relation of->Wherein T is N And P N Is the temperature and air pressure under normal conditions, T is the temperature of the vacuum system volume, estimated +.>The slope of the curve enables the determination of V tot =V S +V R +V other Wherein V is S V being the volume of the sample chamber 13 R V being the volume of the reference chamber 6 other Is the volume of other areas within the device vacuum system;
fifthly, starting the vacuum pump 11, and starting the electromagnetic valves I3, II5, III7, IV10 and V12 to pump out nitrogen in the device;
closing the electromagnetic valve IV10 and the electromagnetic valve V12, opening a valve on the air storage tank I1, filling acetylene gas into the reference cavity 6, and closing the electromagnetic valve I3 after the equilibrium state is reached;
seventhly, opening the electromagnetic valve V12 to enable acetylene gas in the reference cavity 6 to expand into the sample cavity 13, and recording the reading of the barometer 8 and the reading of the thermocouple 9 after the air pressure is balanced;
starting the vacuum pump 11, and starting the electromagnetic valves I3, II5, III7, IV10 and V12 to pump out acetylene gas in the device;
ninth, repeating the steps six to eight until the air pressure reaches 500bar, repeating the steps for N times, and recording the reading of the barometer 8 and the thermocouple 9 under each balanced state air pressure;
ten, calculating the gas adsorption quantity, wherein the gas adsorption quantity is expressed in terms of mole number, and after the gas is expanded from the reference cavity 6 into the sample cavity 13, when the gas pressure reaches an equilibrium state, the mole number of the gas is reduced, namely the mole number of the gas absorbed; at each equilibrium state pressure, the gas adsorption quantity n is calculated through the true gas law ads =r i [V R (r 0 /r i -1)-V S ]+r i-1 V S Wherein r is i =P i /(Z(T i ,P i )RT i ) Is the molar density of the gas, i is an integer from 1 to N, Z (T i ,P i ) Is the gas at the temperature T i And air pressure P i Compression coefficient under the condition, r 0 Is the molar density in the reference chamber, r, before gas expansion i Is the molar density of the gas after expansion in the sample chamber 13 and absorption by the sample; and drawing the data points of the gas adsorption quantity under each equilibrium state gas pressure on a two-dimensional graph and connecting the two-dimensional graph into a curve, wherein the ordinate is the adsorption mole number, and the abscissa is the equilibrium state gas pressure, so that an adsorption isotherm is obtained.
In summary, the invention can more accurately measure the total vacuum system volume and reduce the uncertainty of the adsorption experimental result by using the mass flow controller and the specially designed solenoid valve.
Claims (1)
1. The measuring device mainly comprises an air storage tank I (1), an air storage tank II (2), an electromagnetic valve I (3), a mass flow controller (4), an electromagnetic valve II (5), a reference cavity (6), an electromagnetic valve III (7), a barometer (8), a thermocouple (9), an electromagnetic valve IV (10), a vacuum pump (11), an electromagnetic valve V (12), a sample cavity (13) and an air pipe, wherein one end of the electromagnetic valve I (3) is connected with the air storage tank I (1) and the air storage tank II (2) through a valve air pipe, the other end of the electromagnetic valve I (3) is connected with the mass flow controller (4), the electromagnetic valve II (5), the reference cavity (6), the electromagnetic valve IV (10) and the vacuum pump (11) through the electromagnetic valve III (7), the thermocouple (9) is positioned outside the reference cavity (6), the sample cavity (13) is connected with the reference cavity (6) through the electromagnetic valve V (12), the air storage tank I (1) is filled with tested gas, the air storage tank II (2) is filled with high-purity acetylene gas and the thermocouple (8) is used for monitoring the pressure of the acetylene gas and the temperature in the reference cavity (6), the vacuum pump (11) is used for vacuumizing the device, the sample cavity (13) is positioned in a constant temperature tank to maintain the required temperature, the mass flow controller (4) controls the gas flow rate entering the reference cavity (6) and can be adjusted between 0 and 30SLM, the error is +/-0.2%, the types of the electromagnetic valve I (3), the electromagnetic valve II (5), the electromagnetic valve III (7), the electromagnetic valve IV (10) and the electromagnetic valve V (12) are of the Burnet 2400 type, and are specially designed so that the internal volume of the electromagnetic valve I (3), the electromagnetic valve II (5) and the electromagnetic valve IV (10) cannot change in the process of changing between opening and closing,
the method is characterized in that: the method for acetylene adsorption measurement comprises the following steps:
firstly, placing a nano material sample subjected to drying and degassing treatment into the sample cavity (13);
secondly, starting the vacuum pump (11), and starting the electromagnetic valve I (3), the electromagnetic valve II (5), the electromagnetic valve III (7), the electromagnetic valve IV (10) and the electromagnetic valve V (12), so as to carry out vacuum degassing on the device;
closing the electromagnetic valve IV (10) and the electromagnetic valve V (12), and opening valves on the gas storage tank II (2) to enable high-purity nitrogen to be filled into the reference cavity (6), the sample cavity (13) and other areas in the device vacuum system, wherein in the process, the mass flow controller (4) sets certain parameters to control the gas flow rate and records related data;
fourth, the number of flows through the mass flow controller (4)Determining the number of moles of gas entering the vacuum system of the device and calculating the volume of gas flowing through the mass flow controller (4)With air pressure P and total volume of vacuum system V tot The relation of->Wherein T is N And P N Is the temperature and air pressure under normal conditions, T is the temperature of the vacuum system volume, estimated +.>The slope of the curve enables the determination of V tot =V S +V R +V other Wherein V is S V being the volume of the sample chamber (13) R For the volume of the reference chamber (6), V other Is the volume of other areas within the device vacuum system;
fifthly, starting the vacuum pump (11), and starting the electromagnetic valve I (3), the electromagnetic valve II (5), the electromagnetic valve III (7), the electromagnetic valve IV (10) and the electromagnetic valve V (12), and pumping out nitrogen in the device;
closing the electromagnetic valve IV (10) and the electromagnetic valve V (12), opening a valve on the gas storage tank I (1) to enable acetylene gas to be filled into the reference cavity (6), and closing the electromagnetic valve I (3) after the equilibrium state is reached;
seventhly, opening the electromagnetic valve V (12) to enable acetylene gas in the reference cavity (6) to expand into the sample cavity (13), and recording the reading of the barometer (8) and the reading of the thermocouple (9) after the air pressure is balanced;
starting the vacuum pump (11), and starting the electromagnetic valve I (3), the electromagnetic valve II (5), the electromagnetic valve III (7), the electromagnetic valve IV (10) and the electromagnetic valve V (12), and pumping out acetylene gas in the device;
ninth, repeating the steps six to eight until the air pressure reaches 500bar, repeating the steps N times, and recording the readings of the barometer (8) and the thermocouple (9) under each balanced state air pressure;
ten, calculating the gas adsorption quantity, wherein the gas adsorption quantity is expressed in terms of mole number, and after the gas is expanded into the sample cavity (13) from the reference cavity (6), when the gas pressure reaches an equilibrium state, the mole number of the gas is reduced, namely the mole number of the gas absorbed; at each equilibrium state pressure, the gas adsorption quantity n is calculated through the true gas law ads =r i [V R (r 0 /r i -1)-V S ]+r i-1 V S Wherein r is i =P i /(Z(T i ,P i )RT i ) Is the molar density of the gas, i is an integer from 1 to N, Z (T i ,P i ) Is the gas at the temperature T i And air pressure P i Compression coefficient under the condition, r 0 Is the molar density in the reference chamber, r, before gas expansion i Is the molar density of the gas after expansion in the sample chamber (13) and absorption by the sample; and drawing the data points of the gas adsorption quantity under each equilibrium state gas pressure on a two-dimensional graph and connecting the two-dimensional graph into a curve, wherein the ordinate is the adsorption mole number, and the abscissa is the equilibrium state gas pressure, so that an adsorption isotherm is obtained.
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CN109142130B (en) * | 2018-09-16 | 2024-02-13 | 金华职业技术学院 | Adsorbent testing method |
CN109238905B (en) * | 2018-09-16 | 2024-02-09 | 金华职业技术学院 | Gas adsorption testing device |
CN112945794B (en) * | 2021-02-02 | 2023-02-07 | 南昌师范学院 | Used for detecting SO of activated carbon fiber pair 2 Method for measuring adsorption amount |
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