CN114646573A - Device for measuring adsorption quantity of material mixed gas and transfer weighing method - Google Patents
Device for measuring adsorption quantity of material mixed gas and transfer weighing method Download PDFInfo
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- 238000005259 measurement Methods 0.000 claims abstract description 25
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- 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
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- 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
- G01N7/14—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference
- G01N7/16—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference by heating the material
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Abstract
The invention discloses a device for measuring the adsorption capacity of a material mixed gas and a transfer weighing method, wherein the device comprises a gas supply unit and an adsorption unit which are sequentially connected through a pipeline, and further comprises a pure gas unit, a desorption unit and a detection unit which are respectively connected with the adsorption unit through pipelines, the gas supply unit comprises a raw material gas cylinder, a valve assembly I, a valve assembly II and a valve assembly III, the adsorption unit comprises an adsorbent column tube and a valve assembly IV, the pure gas unit comprises a valve assembly V and a high-purity gas cylinder, the desorption unit comprises a valve assembly VI and a plurality of buffer gas cylinders, and the detection unit comprises a valve assembly VII and a chromatograph. The transfer weighing method utilizes the device to provide mixed gas through the gas supply unit, completely desorbs adsorbed gas after dynamic adsorption balance, transfers the adsorbed gas into a buffer gas cylinder, and then carries out weighing measurement. The measuring device and the measuring method effectively avoid the influence of factors such as gas buoyancy and the like in the existing gravimetric method, and effectively improve the measuring accuracy of the adsorption quantity.
Description
Technical Field
The invention belongs to the technical field of measurement, relates to measurement of gas adsorption capacity, and particularly relates to a device for measuring adsorption capacity of material mixed gas and a transfer weighing method.
Background
In recent years, along with the large application of adsorbing materials such as adsorbents, catalysts, battery materials, composite materials, powder metals and the like in various industries, tests on the surface and interface physical properties of materials are increasingly common, wherein the adsorption quantity is an important parameter reflecting the characteristics of the materials, such as the adsorption rate, the pore diffusion coefficient and the mass transfer coefficient of the materials can be obtained by measuring the adsorption quantity; by measuring the adsorption capacity of nitrogen under different pressures at the liquid nitrogen temperature, parameters such as specific surface area, pore volume, pore size distribution and the like of the adsorption material can be obtained; the method is combined with gas chromatography to measure the adsorption amount of the multicomponent components, so that the separation coefficients of the adsorption material to different gases can be calculated. The adsorption amount refers to the mass (or amount of substance) of the adsorbent per unit mass or unit surface area of the adsorbent, and is a main parameter of the adsorption performance of the reaction material.
The conventional methods for measuring the gas adsorption amount include a volumetric method and a gravimetric method. The volumetric method is a method of calculating the amount of gas adsorbed by measuring the pressure P and the volume V of the gas before and after a certain mass of adsorbent is contacted at a certain temperature. The capacitance method needs to accurately measure parameters such as PVTZ, and the measurement precision is influenced by the precision, the installation precision and the like of the PVT sensor; the V value is calculated based on the fact that helium is not adsorbed, accuracy is not high, and the difference from the actual value is large, and the difference of measurement results in different laboratories is also large. The weight rule is to calculate the amount of adsorbed gas by directly measuring the change in weight of the adsorbent during the adsorption process. The gravimetric method measurement is influenced by the spring balance precision, the buoyancy of gas and the temperature difference, the accuracy is not high, and the error is possibly larger than that of the volumetric method.
In the existing inspection of the adsorption performance of the material, the measurement equipment of the adsorption amount of the material gas can only measure the adsorption amount of the material to a single pure gas generally, but cannot meet the measurement of the measured material to the adsorption amount of the mixed gas. In practical production, it is usually necessary to adsorb the multi-component mixed gas by using an adsorbent to obtain a high-purity gas, for example, in helium purification, it is necessary to purify crude helium by using multiple impurity gases (Ne/H)2/O2/N2Etc.) to obtain high purity helium gas. Different components in the mixed gas have competitive adsorption, so that the requirement of actual production on the judgment of the adsorption performance of the material cannot be met only by measuring the pure gas adsorption quantity of the material.
Disclosure of Invention
The invention aims to solve the problems that the conventional volumetric method and gravimetric method for measuring the gas adsorption capacity in the prior art have low accuracy and large error, and the conventional test device can only measure single gas adsorption capacity.
In order to achieve the above purpose, the device for measuring the adsorption quantity of the material mixed gas provided by the invention comprises a gas supply unit, an adsorption unit, a pure gas unit, a desorption gas buffer unit and a detection unit, wherein the gas supply unit and the adsorption unit are sequentially connected through a pipeline;
the gas supply unit comprises a raw material gas cylinder for providing mixed gas, and a valve component I, a valve component II and a valve component III which are sequentially connected with the raw material gas cylinder through pipelines, and the mixed gas sequentially passes through the valve component I, the valve component II and the valve component III and regulates the flow and the pressure;
the adsorption unit comprises an adsorbent column tube and a valve assembly IV, wherein two ends of the adsorbent column tube are respectively connected with the air outlet end of the valve assembly I and the air outlet end of the valve assembly II through pipelines, and the valve assembly IV is arranged on the pipelines at the air inlet end and the air outlet end of the adsorbent column tube and used for sealing the adsorbent column tube when adsorption is saturated; the mixed gas can enter the adsorption unit through the valve component I and then is discharged through the valve component III;
the pure gas unit comprises a valve component V and a high-purity gas cylinder which are sequentially connected with the gas inlet end of the adsorbent column tube through a pipeline, the high-purity gas cylinder is used for providing high-purity gas, and the high-purity gas enters the adsorption unit through the valve component V;
the desorption gas buffer unit comprises a valve assembly VI and a plurality of buffer gas cylinders which are sequentially connected with the gas outlet end of the adsorbent column tube through a pipeline, the adsorbent column tube carries out gas desorption at the gas desorption temperature, and desorption gas is transferred through the valve assembly VI and stored into the buffer gas cylinders under the action of decompression or negative pressure suction of the buffer gas cylinders;
the detection unit comprises a valve assembly VII and a chromatograph, the valve assembly VII and the chromatograph are sequentially connected with a valve assembly VI through pipelines, gas at an outlet of the adsorbent column tube enters the buffer gas cylinder or the detection unit through the valve assembly VI, and the chromatograph is used for detecting whether adsorption of the adsorbent column tube is saturated or not and measuring the component content of mixed gas in the buffer gas cylinder.
Above-mentioned a device for measuring material mixed gas adsorption capacity, the pipeline bore that uses in process of production can design according to actual demand, and when the pipeline bore that uses was great, in order to make to wait that the adsorbed gas can cool off to corresponding adsorption temperature fast when reaching the adsorbent column pipe, this measuring device still preferred includes the precooling pipe, and the precooling pipe is around establishing on the connecting tube between valve component I and adsorption unit. The precooling pipe can cool the gas to be adsorbed in advance, so that the effect of rapid cooling is achieved when the gas reaches the adsorbent column pipe.
The main factors influencing the adsorption capacity of the device for measuring the adsorption capacity of the material mixed gas are gas pressure, gas flow and adsorption temperature. The adsorption temperature is mainly determined by controlling the temperature of the adsorbent column, and the gas pressure and the gas flow are mainly controlled by the valve component. Therefore, each valve assembly is mainly used to control the flow of the gas, the gas pressure and the flow rate. In the present invention, the valve assembly i preferably includes a pressure reducing valve i, a needle valve i and a pneumatic valve i which are sequentially installed on a connection pipe between the raw material gas cylinder and the adsorbent column tube. The main function of the valve assembly II is to allow the mixed gas to directly flow from the raw gas cylinder through the valve assembly II to the valve assembly III before adsorption is started so as to adjust the gas flow and adsorption pressure, and the valve assembly II preferably comprises a pneumatic valve II. The valve component III is mainly used for controlling the flow and the on-off of mixed gas in initial state setting and a dynamic adsorption process to safely discharge the gas, and preferably comprises a pneumatic valve III, a needle valve II, a stop valve I, a stop valve II, a flow meter and a stop valve III which are sequentially connected through pipelines. The pressure reducing valve I is used for adjusting gas pressure and keeping the gas pressure stable; the needle valve has the function of cutting off fluid, but the more important function is to accurately adjust the fluid flow, and the needle valve I and the needle valve II are mainly used for adjusting the gas flow; pneumatic valves (I/II/III) are used to control the flow of gas. Each stop valve (I/II/III) controls the on-off of gas by opening and closing.
In the device for measuring the adsorption capacity of the material mixed gas, in the dynamic gas adsorption, the temperature of the gas coming out of the adsorbent column tube is low, and in order to reduce the requirement on the cold resistance of the valve and further reduce the cost, the device also preferably comprises a heat recovery tube which is wound on a pipeline between the pneumatic valve III and the needle valve II. The heat recovery pipe can heat the adsorbed gas to restore the gas to normal temperature or other set temperature, so that the performance requirements of the valves are reduced, and each valve can be realized by using a conventional valve.
According to the device for measuring the adsorption quantity of the material mixed gas, the valve assembly IV is mainly used for controlling the on-off of the gas, the adsorbent column tube can be closed when the valve assembly IV is closed, and the valve assembly IV preferably comprises a pneumatic valve IV arranged on a pipeline at the gas inlet end of the adsorbent column tube and a pneumatic valve V arranged on a pipeline at the gas outlet end of the adsorbent column tube. Further, the valve assembly IV further comprises a pneumatic valve VI, and the pneumatic valve VI is arranged on a pipeline between the pneumatic valve V and the adsorbent column tube.
Above-mentioned a device for measuring material gas mixture adsorption capacity, in actual production process, it is unchangeable usually to wait that adsorbed gas, but for further reinforcing the device application scope, guarantees the accuracy of adsorption capacity test, and this measuring device still preferredly includes the vacuum unit, the vacuum unit includes valve member VIII and the vacuum pump that connects gradually through pipeline and I exit end of stop valve, valve member VIII includes pneumatic valve VII, and thereby the vacuum pump can be used to get rid of impurity gas to whole device pipeline evacuation processing, further improves measuring accuracy.
Above-mentioned a device for measuring material gas mixture adsorption capacity, for the holistic security of further reinforcing device, improve the reliability of device, gas supply unit still preferably includes valve assembly IX, and valve assembly IX includes relief pressure valve II, stop valve IV and stop valve V, pressure reducing valve II passes through the pipe connection between needle valve II and flowmeter, stop valve IV and stop valve V insert the pipeline between needle valve II and stop valve I through the pipeline parallel connection respectively. The valve component IX is designed as a safety redundancy, and when the air pressure of the pipeline breaks through the set safety air pressure, the pressure reducing valve II can be opened for reducing the pressure, and/or the stop valve IV and the stop valve V are opened for discharging the gas.
In the device for measuring the adsorption capacity of the material mixed gas, the valve assembly V is mainly used for controlling the on-off of the high-purity gas, and preferably comprises a stop valve VI arranged on a connecting pipeline between a high-purity gas cylinder and the gas inlet end of the adsorbent column tube. Further, the high purity gas should generally be the main component gas of the mixed gas to be tested, such as neon, hydrogen, oxygen, nitrogen, etc. in helium, and the high purity gas should be high purity helium.
The valve assembly VI is mainly used for controlling the on-off of the gas at the outlet of the adsorbent column tube so that the gas at the outlet of the adsorbent column tube enters the buffer gas cylinder or the detection unit through the valve assembly VI, and preferably comprises a stop valve VII and a stop valve VIII which are arranged on a connecting pipeline between the adsorbent column tube and the buffer gas cylinder.
Above-mentioned a device for measuring material mist adsorption capacity, buffer gas cylinder are the cylinder of taking out air, for making desorption gas get into to buffer gas cylinder smoothly, and buffer gas cylinder's volume size design principle is littleer for making the atmospheric pressure of the atmospheric pressure in the buffer gas cylinder than the atmospheric pressure of left side pipe, and on this basis, buffer gas's volume size can be set for according to actual production demand. In general, the volume of the buffer cylinder is larger than the volume of the adsorbent column tube, so that the above requirements can be met. The pressure reduction is realized by utilizing the larger difference of the volumes of the buffer gas cylinder and the adsorbent column tube, thereby being beneficial to desorption and transfer of adsorbed gas. The number of buffer cylinders is not particularly limited, and in the present invention, the number of buffer cylinders is preferably two, including a buffer cylinder i and a buffer cylinder ii. Wherein, the buffer gas cylinder I is a main storage gas cylinder, can reduce pressure and continue pumping in the subsequent process after the first adsorption, and then balance the residual pressure by using the buffer gas cylinder II after reaching the pressure balance, thereby realizing negative pressure pumping and promoting the rapid desorption and transfer of the adsorbed gas. The high-purity gas is repeatedly filled for dilution, and then the pressure is reduced and the negative pressure suction is carried out, so that the adsorbed gas can be completely desorbed and completely transferred.
The device for measuring the adsorption capacity of the material mixed gas has the main function that the chromatograph detects the concentration change of impurity gas in the dynamic adsorption process so as to determine adsorption saturation, so the chromatograph can be directly connected with the gas outlet end of the adsorbent column tube through a pipeline, and the valve assembly VII is arranged on a connecting pipeline between the chromatograph and the gas outlet end of the adsorbent column tube. The valve assembly vii preferably comprises a needle valve iii. In order to further improve the detection efficiency of the device, in the invention, the chromatograph is preferably connected with a connecting pipeline between the stop valve VII and the stop valve VIII through a pipeline, and the valve assembly VII is arranged on a pipeline at the gas inlet end of the chromatograph. In this preferred embodiment, the chromatograph is connected not only to the adsorbent column but also to a buffer gas cylinder. When the adsorption saturation state needs to be judged, the mixed gas can enter a chromatograph by opening the stop valve VII and the needle valve III. When the content of impurity gas components in the buffer gas cylinder needs to be detected, the stop valve VIII and the needle valve III are opened to detect, so that the buffer gas cylinder is not required to be externally connected with a chromatograph independently, the manual operation cost is reduced, and the detection efficiency is effectively improved.
Above-mentioned a device for measuring material gas mixture adsorption capacity, for better detection pipeline internal pressure and temperature, the device still preferably includes pressure measurement subassembly and temperature measurement subassembly. The pressure measuring assembly comprises a plurality of pressure test meters, and the temperature measuring assembly comprises a plurality of temperature test meters. The specific installation positions of the pressure test meter and the temperature test meter can be installed according to actual monitoring requirements. Generally, at least one pressure test meter can be arranged at the joint of each unit, and the pressure test meter can be installed in each unit as occasion demands. The temperature test meter can be installed in front of and behind the pre-cooling pipe, the rewarming pipe and the adsorbent column pipe.
The invention also provides a transfer weighing method for measuring the adsorption quantity of the material mixed gas, which is used for measurement by using the device for measuring the adsorption quantity of the material mixed gas and comprises the following steps:
s11, initial state adjustment: in the initial state, the flow and the pressure of the mixed gas discharged by the raw material gas bottle are regulated through each valve component until the flow and the pressure are stable and reach the initial set pressure and the initial set flow; the specific implementation mode is as follows: at the beginning, all valve components are in a closed state, the valve component I, the valve component II and the valve component III are opened in sequence, mixed gas provided by the raw material gas bottle is discharged through the valve component I, the valve component II and the valve component III in sequence, and the gas flow and pressure are regulated through the valve components until the flow and pressure are stable and reach the initial set pressure and the initial set flow;
s12, impurity purging: carrying out impurity residual gas purging on the adsorbent column pipe and the first detection unit by using high-purity gas provided by a high-purity gas bottle, and regulating the pressure of the high-purity gas in the pipeline to an initial set pressure through each valve assembly; the specific implementation mode is as follows: opening the valve assembly V, the valve assembly VI and the valve assembly VII, discharging high-purity gas provided by the high-purity gas bottle through the valve assembly V, the adsorbent column tube, the valve assembly VI and the detection unit so as to purge the impurity gas, closing the valve assembly VI and the valve assembly VII after purging is finished, and regulating the gas pressure in the pipeline to an initial set pressure through each valve assembly;
s13, low-temperature adsorption: cooling the adsorbent column pipe filled with the adsorption material to the gas adsorption temperature, continuously supplementing high-purity gas until the pressure is greater than the initial set pressure in the step S11 and is stable, and then closing the valve assembly V; closing the valve component II and opening the valve component IV, adsorbing the mixed gas at low temperature by the adsorbent column tube at the gas adsorption temperature, opening the valve component VI and the valve component VII to enable the gas at the outlet of the adsorbent column tube to enter a chromatograph, detecting the concentration change of the mixed gas component by using the chromatograph, judging that the mixed gas component reaches adsorption saturation when the chromatograph detects the mixed gas component with a set quantitative value, closing the valve component IV to seal the adsorbent column tube, opening the valve component II, and closing the valve component VI and the valve component VII at the same time;
s14, negative pressure desorption: reheating the adsorbent column tube to a gas desorption temperature, opening the valve assembly VI to enable gas at the outlet of the adsorbent column tube to enter the buffer gas cylinder, carrying out gas desorption at the gas desorption temperature, transferring desorbed gas by using the negative pressure of the buffer gas cylinder and storing the desorbed gas in the buffer gas cylinder, wherein a plurality of buffer gas cylinders (401) can be alternately used until the pressure of the finally used buffer gas cylinder is balanced;
s15, dilution and transfer: closing the valve component VI, simultaneously opening the valve component V, and providing high-purity gas by using a high-purity gas bottle to dilute the residual desorption gas until the pressure of the adsorbent column tube is set pressure; closing the valve component V, simultaneously opening the valve component VI, transferring the desorption gas and storing the desorption gas in the buffer gas cylinder by utilizing the decompression or negative pressure suction of the buffer gas cylinder again to achieve the pressure balance (when more than two first buffer gas cylinders are arranged, all the gas cylinders can be alternately used until the pressure of the first buffer gas cylinder used finally is balanced); then closing the valve assembly VI, simultaneously opening the valve assembly V, repeating the step for a plurality of times until the gas in the adsorbent column tube is consistent with the high-purity gas (indicating that the mixed gas in the adsorbent column tube is completely desorbed at the moment), and closing the valve assembly VI;
s16, component measurement: the amount of increase of the buffer gas cylinder is weighed to obtain the mass of the gas stored in the buffer gas cylinder, and the buffer gas cylinder is connected to a chromatograph in the device or an external chromatograph to measure the content of each component of the mixed gas, so that the adsorption amount and the volume of each component of the mixed gas in a standard state are calculated.
The weighing transfer method for measuring the adsorption quantity of the mixed gas has the following principle: when the temperature of the adsorbent column tube and a cooling device (usually a liquid nitrogen cylinder) reaches a balance, mixed gas with a certain flow is introduced under a certain pressure, the concentration change of impurities in high-purity gas is detected at the outlet of the adsorbent column tube, when a certain impurity component with a certain quantitative value is detected at the outlet, the adsorption is considered to be saturated, then the adsorbed impurity gas is completely desorbed and is completely transferred into a buffer gas cylinder by the high-purity gas, and the mass of the impurity component and the volume under a standard state are calculated by weighing the mass of the mixed gas and measuring the content of the impurity component in the gas. Obviously, the volume of the mixed gas discharged from the buffer gas bottle may be measured and the mass thereof may be weighed, thereby calculating the volume of the impurity component.
The initial set pressure and the initial set flow rate in steps S11-S16 of the method for measuring the transfer volume for measuring the pure gas adsorption amount may be set by referring to the flow rate and the pressure value used in the conventional gas adsorption operation in the art, and the present invention is not limited thereto.
In the above transfer volume measurement method for measuring the adsorption amount of the mixed gas, in step S12, the temperature reduction treatment method for reducing the temperature of the adsorbent column tube to the gas adsorption temperature may adopt a conventional temperature reduction method in the art, and generally, the low temperature of the gas adsorption temperature refers to the liquid nitrogen temperature, and the liquid nitrogen barrel sleeve is adopted to carry out liquid nitrogen bath temperature reduction on the adsorbent column tube until the temperature is balanced.
In the transfer volume measuring method for measuring the adsorption amount of the mixed gas, in step S13, the high-purity gas is continuously supplied until the gas pressure in the adsorbent column tube is higher than the initial set pressure in step S11, so as to prevent the mixed gas outside the adsorbent column tube from instantaneously penetrating through the adsorbent layer when entering the adsorbent column tube when the pneumatic valves iv and the gas valve v are opened, and thus, the chromatographic detection cannot obtain accurate adsorption saturation time, and thus, the false judgment is generated. In order to achieve the above object, the specific value of the gas pressure in the adsorbent column is not particularly limited, and is usually slightly larger than the initial set pressure in step S11. Further, the mixed gas usually has a main gas component and an impurity gas component, and here, mainly, a change in concentration of the impurity gas component is detected. When the chromatograph detects a predetermined amount of the mixed gas component, the adsorption saturation is considered to be reached, and the predetermined amount is not particularly limited, and those skilled in the art can make corresponding determinations according to the specific impurity gas.
In the above-described transfer volume measurement method for measuring the amount of adsorbed mixed gas, in step S14, the heating method for rewarming the adsorbent column to the gas desorption temperature may be a heating method that is conventional in the art, and there is no particular requirement. In the invention, after the liquid nitrogen barrel is removed, the adsorbent column tube is heated by adopting a water bath and heating furnace until the gas desorption temperature is reached. The gas desorption temperature is usually set by heating the adsorbent column to 100 ℃ and the adsorbent filled in the adsorbent column to a temperature of at least 80 ℃.
The above-mentioned transfer volume measuring method for measuring the amount of adsorbed mixed gas, step S15, is proved by the test of the inventor: and repeatedly using the high-purity gas cylinder to provide the high-purity gas to dilute and desorb the residual desorbed gas for 10 times or more, wherein the gas in the adsorbent column tube has the same composition with the high-purity gas. Therefore, the dilution transfer operation of step S15 is preferably repeated 10 times or more to achieve complete transfer of the desorption gas.
The above-described transfer volume measurement method for measuring the amount of adsorbed mixed gas, in step S16, the manner of calculating the amount of adsorbed mixed gas components and the volume in the standard state is well known to those skilled in the art. The specific calculation method is as follows:
the mass of each component in the mixed gas is calculated by adopting the formula (1):
mi＝mmixed gas (es)×yi (1)
In the formula, miIs the mass (g), m of component iMixed gas (es)Is the total mass (g), y of the gas mixtureiIs the concentration of component i in the gas mixture (g/g).
The volume of gas at standard conditions is calculated using equation (2):
Vi＝Vi label×mi/Mi……(2)
In the formula miIs the mass (g), M of component iiIs the molar mass (g), V, of component iiVolume of component i gas in standard conditions (ml), VI labelIs the molar volume of the i component gas in the standard state (ml/mol).
The volume of part of the mixed gas can be measured by adopting a volume measurement method at normal temperature and normal pressure, the volume of each component gas in the mixed gas is calculated according to the formula (3), and then the volume is converted into the volume under a standard state.
In the formula ViVolume (ml) of impurity component i, VDischarge of mixed gasFor introducing volume measuring devices from gas cylindersVolume (ml) of gas mixture (m) of (1)Gas mixture assemblyIs the total mass (g), m, of the gas mixture in the gas cylinderDischarge of mixed gasThe mass (g), X, of the gas mixture being introduced from the gas cylinder into the volume measuring deviceiIs the concentration (V/V) of component i in the gas mixture.
Compared with the prior art, the technical scheme provided by the invention has the following beneficial effects:
(1) the device for measuring the adsorption quantity of the material mixed gas provided by the invention has the advantages that the gas supply unit is used for supplying the mixed gas, the adsorbent column tube is closed after the adsorption balance of the adsorbent column tube is realized, the gas adsorbed on the adsorbent is desorbed, the adsorbed gas is sucked and transferred into the buffer gas cylinder by utilizing decompression or negative pressure, and the weighing and chromatographic analysis quantification are used, so that the errors caused by the factors such as the sensor precision, the installation precision, the spring balance precision, the buoyancy of the gas, the temperature difference influence and the like in the in-situ measurement in the prior art are avoided, the precision requirement on a metering device is greatly reduced, the complete transfer and accurate measurement of the adsorbed gas are realized, and the problem of accurate measurement of the adsorption quantity of the multi-element mixed gas is solved. The weighing method is an internationally recognized method, the weighing is carried out after the transfer, the influence of gas buoyancy and temperature difference on the weighing is effectively avoided, and meanwhile, the weighing after the gas amount is increased greatly reduces the requirement on the precision of the balance.
(2) The device for measuring the adsorption quantity of the material mixed gas provided by the invention has the advantages that the factors influencing the adsorption quantity of the gas generally comprise pressure, temperature and flow, and the device can adjust the initial gas pressure and the initial gas flow through the valve assembly I, the valve assembly II and the valve assembly III, so that the dynamic adsorption test requirements of the gas at low temperature (generally liquid nitrogen temperature) and different pressures (0.03-16MPa) can be met.
(3) The transfer weighing method for measuring the adsorption quantity of the material mixed gas, provided by the invention, is based on the measuring device, realizes low-temperature high-pressure steady-flow adsorption, heating and depressurization desorption, transfer measurement, quick switching and purging replacement, avoids errors caused by factors such as sensor precision, installation precision, spring balance precision, gas buoyancy and temperature difference influence in situ measurement in the prior art, greatly reduces the requirement on the precision of a measuring instrument, realizes complete transfer and accurate measurement of adsorbed gas, is simple in experimental steps, easy to operate, has strong practicability and good application prospect, and is worthy of popularization and application.
Drawings
FIG. 1 is a schematic view of the gas path flow of the device for measuring the adsorption quantity of the material mixed gas according to the present invention.
Description of reference numerals: 1. an air supply unit; 101. a raw material gas cylinder; 102. a pressure reducing valve I; 103. a needle valve I; 104. a pneumatic valve I; 105. a pneumatic valve II; 106. a pneumatic valve III; 107. a needle valve II; 108. a stop valve I; 109. a stop valve II; 110. a flow meter; 111. a stop valve III; 112. a pressure reducing valve II; 113. a stop valve IV; 114. a stop valve V; 115. a pre-cooling tube; 116. a heat recovery pipe; 2. an adsorption unit; 201. an adsorbent column tube; 202. a pneumatic valve IV; 203. a pneumatic valve V; 204. a pneumatic valve VI; 3. a pure gas unit; 301. a high-purity gas cylinder; 302. a stop valve VI; 4. a desorption gas buffer unit; 401. a buffer gas cylinder; 402. the stop valve VII; 403; a stop valve VIII; 5. a detection unit; 501. a chromatograph; 502. a needle valve III; 6. a vacuum unit; 601. a vacuum pump; 602. and the pneumatic valve VII.
Detailed Description
So that the technical solutions of the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings, it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, belong to the present invention.
Example 1
The device for measuring the adsorption capacity of the mixed gas of the material provided by the embodiment comprises a gas supply unit 1, an adsorption unit 2, a pure gas unit 3, a desorption gas buffer unit 4, a detection unit 5, a pressure measurement component and a temperature measurement component, wherein the gas supply unit 1 and the adsorption unit 2 are sequentially connected through pipelines, and the pure gas unit 3, the desorption gas buffer unit 4 and the detection unit 5 are respectively connected with the adsorption unit 2 through pipelines, as shown in fig. 1.
The gas supply unit 1 comprises a raw material gas bottle 101 and a valve assembly I, a valve assembly II and a valve assembly III which are sequentially connected with the raw material gas bottle 101 through pipelines. The raw material gas bottle 101 is used for providing mixed gas to sequentially pass through the valve assembly I, the valve assembly II and the valve assembly III to regulate the flow and the pressure and then discharge the mixed gas. The valve assembly I comprises a pressure reducing valve I102, a needle valve I103 and a pneumatic valve I104 which are sequentially arranged on a connecting pipeline between the raw material gas bottle 101 and the adsorption unit 2. The valve assembly II comprises a pneumatic valve II 105. The valve assembly III comprises an air-operated valve III 106, a needle valve II 107, a stop valve I108, a stop valve II 109, a flow meter 110 and a stop valve III 111 which are sequentially connected through pipelines. The mixed gas flows through the pressure reducing valve I102, the needle valve I103, the air-operated valve I104 and the adsorption unit 2 in sequence or directly flows through the air-operated valve II 105, then flows through the air-operated valve III 106, the needle valve II 107, the stop valve I108, the stop valve II 109, the flow meter 110 and the stop valve III 111 in sequence and is discharged. The pressure reducing valve i 102 adjusts the pressure of the mixed gas to reach a set adsorption pressure. The needle valve I103 and the needle valve II 107 regulate the flow rate of the raw material gas.
In order to further enhance the safety and reliability of the device for measuring the adsorption quantity of the material mixed gas provided by the embodiment, a safety redundant component is further added in the measuring device. Specifically, the gas supply unit 1 further comprises a valve assembly IX, the valve assembly IX comprises a pressure reducing valve II 112, a stop valve IV 113 and a stop valve V114, the pressure reducing valve II 112 is connected between the needle valve II 107 and the flow meter 110 through a pipeline, and the stop valve IV 113 and the stop valve V114 are respectively connected in parallel to the pipeline between the needle valve II 107 and the stop valve I108 through pipelines.
In order to pre-cool the raw gas before entering the adsorption unit 2 when required by production, a pre-cooling pipe 115 is wound on a connecting pipeline between the pneumatic valve I104 and the air inlet end of the adsorption unit 2. In order to reduce the requirements on the valve performance, in the present embodiment, a reheat pipe 116 is further wound on the pipeline between the air-operated valve iii 106 and the needle valve ii 107.
The adsorption unit 2 comprises an adsorbent column 201 and a valve assembly iv. The two ends of the adsorbent column tube 201 are respectively connected with the air outlet end of the valve component I and the air outlet end of the valve component II through pipelines. The adsorbent column 201 is filled with an adsorbent for adsorbing gas, such as activated carbon, molecular sieve, silica gel, activated aluminum, and other common adsorbents in the art. In this embodiment, a pipeline of DN15 Φ 21 × 3 and 400mm in length is used as the adsorbent column 201, and activated carbon is filled inside as the adsorbent. The valve assembly iv includes an air-operated valve iv 202, an air-operated valve v 203, and an air-operated valve vi 204. The air-operated valve IV 202 is arranged on a connecting pipeline between the air inlet end of the adsorbent column pipe 201 and the air-operated valve I104, the air-operated valve V203 is arranged on a connecting pipeline between the air outlet end of the adsorbent column pipe 201 and the air-operated valve III 106, and the air-operated valve VI 204 is arranged between the air-operated valve V203 and the adsorbent column pipe 201. Upon saturation of adsorption, simultaneous closing of pneumatic valve iv 202 and pneumatic valve v 203 closes adsorbent column 201.
The pure gas unit 3 comprises a valve assembly V and a pure gas bottle 301 which are sequentially connected with the gas inlet end of the adsorbent column pipe 201 through a pipeline. The valve assembly v includes a shut-off valve vi 302 mounted on the connecting conduit between the high purity gas cylinder 301 and the gas inlet end of the adsorbent column 201. The high purity gas cylinder 301 is used to supply high purity gas. High purity gas enters the adsorbent column 201 through a shut-off valve vi 302. The high-purity gas is a main component gas of the mixed gas to be tested, such as neon, hydrogen, oxygen, nitrogen and other mixed gases in helium, and the high-purity gas is high-purity helium.
The desorption gas buffer unit 4 comprises a valve component VI and a buffer gas bottle 401 which are sequentially connected with the gas outlet end of the adsorbent column pipe 201 through a pipeline. The gas at the outlet of the adsorbent column pipe 201 enters the buffer gas cylinder 401 or the detection unit 5 through the valve assembly VI. The number of the buffer gas cylinders 401 is two, and the two buffer gas cylinders are a buffer gas cylinder I and a buffer gas cylinder II respectively. The valve assembly vi comprises a shut-off valve vii 402 and a shut-off valve viii 403 mounted on the connecting line between the adsorbent column 201 and the buffer gas cylinder 401. The adsorbent column 201 performs gas desorption at the gas desorption temperature, and desorbed gas is transferred and stored into the buffer gas cylinder 401 through the stop valve VII 402 and the stop valve VIII 403 under the action of pressure reduction or negative pressure of the buffer gas cylinder 401.
The detection unit 5 comprises a chromatograph 501 and a valve assembly VII. Chromatograph 501 is connected with a connecting pipeline between stop valve VII 402 and stop valve VIII 403 through a pipeline, and the valve assembly VII comprises a needle valve III 502 arranged on a pipeline at the air inlet end of chromatograph 501. The chromatograph 501 is used for detecting whether the adsorption of the adsorbent column 201 is saturated or not and measuring the content of the mixed gas component in the buffer gas cylinder 401.
The pressure measuring assembly comprises four pressure test meters, namely a pressure test meter P1, a pressure test meter P2, a pressure test meter P3 and a pressure test meter P4. A pressure gauge P1 was installed on the conduit between shut-off valve vi 302 and sorbent cartridge 201. And the pressure test meter P2 is installed on the pipeline at the air outlet end of the pneumatic valve VI 204. A pressure test meter P3 is installed on the pipeline at the air outlet end of the stop valve V114. The pressure test meter P4 is installed on the pipeline at the air outlet end of the air-operated valve V203. In the embodiment, the pressure precision of the pressure test meter P2 is high, the measurement range (0-4MPa) is small, and the pneumatic valve VI 204 is mainly used for connecting or disconnecting the pressure test meter P2 and preventing the overpressure of the pressure test meter P2 from being damaged. A pressure test meter P1 (pressure measurement range (0-20 MPa)) is arranged between the adsorbent column tube and the pneumatic valve II, and when the pressure is higher than 4MPa, the gas pressure can be measured by the pressure test meter P1.
The temperature measuring component comprises two temperature test meters, namely a temperature test meter T1 and a temperature test meter T2. And a temperature test meter T1 is arranged on a pipeline at the air inlet end of the stop valve VII 402. And the temperature test meter T2 is installed on the pipeline at the air outlet ends of the pressure reducing valve II 112 and the stop valve II 109.
In this embodiment, for further reinforcing device test accuracy, this measuring device still includes the vacuum unit 6 of being connected with air feed unit 1, and vacuum unit 6 includes valve member VIII and the vacuum pump 601 that connects gradually through pipeline and I108 exit ends of stop valve, and valve member VIII includes pneumatic valve VII 602, and vacuum pump 601 is used for carrying out evacuation processing to the pipeline.
Example 2
The transfer weighing method for measuring the adsorption amount of the material mixed gas provided by the embodiment performs the measurement of the adsorption amount of the mixed gas by using the adsorption measuring device provided by the embodiment 1, and specifically comprises the following steps:
s11, initial state adjustment: in an initial state, all valve components are in a closed state, a pressure reducing valve I102, a needle valve I103, a pneumatic valve I104, a pneumatic valve II 105, a pneumatic valve III 106, a needle valve II 107, a stop valve I108, a stop valve II 109 and a stop valve III 111 are sequentially opened, mixed gas provided by a raw material gas bottle 101 is sequentially discharged through the pressure reducing valve I102, the needle valve I103, the pneumatic valve I104, the pneumatic valve II 105, the pneumatic valve III 106, the needle valve II 107, the stop valve I108, the stop valve II 109, a flow meter 110 and the stop valve III 111, the gas flow and pressure are regulated through the valves until the initial set flow reaches and stabilizes at 10l/min, and the initial set pressure stabilizes at 15 MPa;
s12, impurity purging: opening a stop valve VI 302, a stop valve VII 402 and a needle valve III 502, discharging high-purity gas provided by a high-purity gas bottle 301 through the stop valve VI 302, an adsorbent column tube 201, the stop valve VII 402, the needle valve III 502 and a chromatograph 501 to purge impurity residual gas, closing the stop valve VII 402 and the needle valve III 502 after purging is completed, and adjusting the pressure of the high-purity gas in the pipeline to 15 MPa;
s13, low-temperature adsorption: sleeving a liquid nitrogen barrel on the adsorbent column tube 201 to enable the adsorbent column tube 201 to be placed in a liquid nitrogen bath, achieving temperature balance, continuously supplementing high-purity gas until the pressure is 15.2MPa, namely slightly higher than the pressure outside the adsorbent column tube, preventing mixed gas outside the adsorbent column tube from returning to an outlet end, stabilizing the pressure for 1-2 min, and closing a stop valve VI 302; closing the pneumatic valve II 105, opening the pneumatic valves IV 202 and V203, carrying out low-temperature adsorption on the mixed gas by the adsorbent column tube 201 at the gas adsorption temperature, opening the stop valve VII 402 and the needle valve III 502, detecting the concentration change of the mixed gas component by using the chromatograph 501, and when the chromatograph 501 detects the mixed gas component with a set quantitative value, determining that the mixed gas component reaches adsorption saturation (if helium is used as high-purity gas and hydrogen in helium is used as mixed gas, the hydrogen reaches 3 x 10-6V/V can be regarded as saturation), the pneumatic valve IV 202 and the pneumatic valve V203 are closed to seal the adsorbent column tube 201, the stop valve VII 402 and the needle valve III 502 are closed, the pneumatic valve II 105 is opened, and the raw material gas bottle 101 is closed;
s14, negative pressure desorption: placing an adsorbent column tube 201 in a hot water bath, continuously heating by using a heating furnace, heating to 100 ℃, enabling the temperature of activated carbon in the adsorber to reach at least 80 ℃, opening a stop valve VII 402 and a stop valve VIII 403, carrying out gas desorption at a gas desorption temperature, transferring and storing part of desorbed gas in a buffer gas cylinder I by using the negative pressure of the buffer gas cylinder I, opening a buffer gas cylinder II when the pressure of the buffer gas cylinder I is balanced, balancing the residual pressure by using the buffer gas cylinder II to realize negative pressure suction, transferring and storing part of desorbed gas in the buffer gas cylinder II again until the pressure of the buffer gas cylinder II is balanced;
s15: dilution and transfer: closing the stop valve VII 402, simultaneously opening the stop valve VI 302, providing high-purity gas by using a high-purity gas bottle 301 to dilute residual impurity gas in the pipeline, and filling the high-purity gas until the pressure of the adsorbent column pipe 201 is 0.5 MPa; closing a stop valve VI 302, simultaneously opening a stop valve VII 402, opening a buffer gas I, decompressing and pumping the gas and storing the gas in the buffer gas cylinder I until the pressure of the buffer gas cylinder I is balanced, closing a cylinder valve of the buffer gas cylinder I, opening the buffer gas cylinder I, balancing the residual pressure by using a buffer gas cylinder II, realizing negative pressure pumping, transferring part of desorbed gas again and storing the desorbed gas in the buffer gas cylinder II until the pressure of the buffer gas cylinder II is balanced, and closing a cylinder valve of the buffer gas cylinder II; then closing the valve assembly VI, simultaneously opening the valve assembly V, repeating the step for 10 times (proved by the test that after repeating for 10 times, the gas in the adsorbent column tube 201 is tested to have the same composition with the raw material high-purity gas); filling high-purity gas for dilution and transferring the desorbed gas until the pressure of the final buffer gas cylinder II is 0.4MPa, and closing the cylinder valve;
s16, component measurement: the increase amounts of the buffer gas cylinder I and the buffer gas cylinder II are weighed to obtain the mass of the desorbed gas stored in the buffer gas cylinder I/II, the stop valve VIII 403 and the needle valve III 502 are opened to enable the gas in the buffer gas cylinder I/II to enter a chromatograph 501, and the chromatograph 501 is used for measuring the content of impurity components in the gas, so that the mass of the impurity gas and the volume of the impurity gas in a standard state are calculated.
In step S16, the specific calculation method of the adsorption amount and the volume in the standard state of each component of the mixed gas is as follows:
the mass of each component in the mixed gas is calculated by adopting the formula (1):
mi＝mmixed gas (es)×yi (1)
In the formula, miIs the mass (g), m of component iMixed gas (es)Is the total mass (g), y of the gas mixtureiIs the concentration of component i in the gas mixture (g/g).
The volume of gas at standard conditions is calculated using equation (2):
Vi＝Vi label×mi/Mi……(2)
In the formula miIs the mass (g), M of component iiIs the molar mass (g), V, of component iiVolume of component i gas in standard conditions (ml), VI labelIs the molar volume of the i component gas in the standard state (ml/mol).
The volume of part of the mixed gas can be measured by adopting a volume measurement method at normal temperature and normal pressure, the volume of each component gas in the mixed gas is calculated according to the formula (3), and then the volume is converted into the volume under a standard state.
In the formula ViVolume (ml) of impurity component i, VDischarge of mixed gasVolume (ml) of gas mixture put into volume measurer from gas cylinder, mGas mixture assemblyIs the total mass (g), m of the gas mixture in the gas cylinderDischarge of mixed gasThe mass (g), X, of the gas mixture being introduced from the gas cylinder into the volume measuring deviceiIs the concentration (V/V) of component i in the gas mixture.
Example 3
In this example, the apparatus for measuring the amount of adsorbed material mixed gas provided in example 1 and the transfer weighing method provided in example 2 were used to conduct a repetitive experiment in which a mixed gas of argon in helium, nitrogen in helium, and oxygen in helium was used as a test gas, and the results of the repetitive experiment are shown in table 1.
TABLE 1 transfer weighing method repeatability test results
Total relative uncertainty of transfer-weighing measurements:
uncertainty of gas mass weighing: the minimum weighed mass is 5.300g, the uncertainty is 0.0104g, the relative standard uncertainty is 0.196%, and the relative uncertainty of the two mass weighings is 0.392%.
Uncertainty of component content measurement: the relative uncertainty of the standard gas is 1%, the relative standard deviation of the reproducibility of the chromatographic analysis is 1%, and the uncertainty of the component content measurement is 1.74%.
The relative standard uncertainty determined by transfer-weighing was 1.78% and the total relative uncertainty was 3.6%.
As can be seen from Table 1, the relative standard deviation of the results of 6 repeated measurements by the transfer weighing method is maximally 1.26, and the total relative uncertainty is 3.6%, which indicates that the results of the transfer weighing method are accurate and reliable.
Example 4
In this example, the apparatus for measuring the amount of adsorbed material mixed gas provided in example 1 and the transfer weighing method provided in example 2 were used, and the accuracy of the transfer weighing method was verified by performing a test to obtain the amount of adsorbed material mixed gas and the volume in the standard state using a mixed gas of carbon monoxide in helium, a mixed gas of neon, hydrogen, oxygen, and methane in helium, as raw material gases, and helium as a high purity gas, and measuring the volume of the discharged portion of the mixed gas with a volume measuring instrument and converting the volume into the volume in the standard state, respectively, and the test results are shown in table 2.
TABLE 2 comparison of gas measurement volume and weighing calculation volume
As can be seen from table 2, for the transfer weighing method, the relative deviation between the calculated result and the actual measurement result is at most 3.0%, and less than 5%, which proves that the transfer weighing method measurement result is accurate.
It will be appreciated by those of ordinary skill in the art that the examples provided herein are intended to assist the reader in understanding the principles of the invention and are to be construed as being without limitation to such specifically recited examples and embodiments. Those skilled in the art can make various other specific changes and combinations based on the teachings of the present invention without departing from the spirit of the invention, and these changes and combinations are within the scope of the invention.
Claims (10)
1. An apparatus for measuring the adsorption amount of a material mixture gas, characterized in that: the device comprises a gas supply unit (1) and an adsorption unit (2) which are sequentially connected through a pipeline, and further comprises a pure gas unit (3), a desorption gas buffer unit (4) and a detection unit (5) which are respectively connected with the adsorption unit (2) through pipelines;
the gas supply unit (1) comprises a raw material gas cylinder (101) for providing mixed gas and a valve component I, a valve component II and a valve component III which are sequentially connected with the raw material gas cylinder (101) through pipelines;
the adsorption unit (2) comprises an adsorbent column tube (201) and a valve assembly IV, wherein two ends of the adsorbent column tube (201) are respectively connected with the air outlet end of the valve assembly I and the air outlet end of the valve assembly II through pipelines, and the valve assembly IV comprises pipelines which are arranged at the air inlet end and the air outlet end of the adsorbent column tube (201) and used for sealing the adsorbent column tube (201) when adsorption is saturated; the mixed gas can enter the adsorption unit (2) through the valve component I and then is discharged through the valve component III;
the pure gas unit (3) comprises a valve assembly V and a high-purity gas cylinder (301) which are sequentially connected with the gas inlet end of the adsorbent column tube (201) through a pipeline, the high-purity gas cylinder (301) is used for providing high-purity gas, and the high-purity gas enters the adsorption unit (2) through the valve assembly V;
the desorption gas buffer unit (4) comprises a valve assembly VI and more than one first buffer gas cylinder (401), wherein the valve assembly VI is sequentially connected with the gas outlet end of the adsorbent column tube (201) through a pipeline, the adsorbent column tube (201) is subjected to gas desorption at the gas desorption temperature, and desorption gas is transferred through the valve assembly VI and stored in the buffer gas cylinder (401) under the suction action of decompression or negative pressure of the buffer gas cylinder (401);
the detection unit (5) comprises a valve assembly VII and a chromatograph (501) which are sequentially connected with a valve assembly VI through a pipeline, gas at an outlet of the adsorbent column tube (201) enters the buffer gas cylinder (401) or the detection unit (5) through the valve assembly VI, and the chromatograph (501) is used for detecting whether the adsorption of the adsorbent column tube (201) is saturated or not and measuring the content of mixed gas components in the buffer gas cylinder (401).
2. The apparatus for measuring the amount of adsorption of a material mixture gas according to claim 1, wherein: the measuring device also comprises a pre-cooling pipe (115), wherein the pre-cooling pipe (115) is wound on a connecting pipeline between the valve component I and the adsorption unit (2).
3. The apparatus for measuring the amount of adsorption of a material mixture gas according to claim 1, wherein: the valve component I comprises a pressure reducing valve I (102), a needle valve I (103) and a pneumatic valve I (104) which are sequentially arranged on a connecting pipeline between the raw material gas bottle (101) and the adsorbent column tube (201); the valve assembly II comprises a pneumatic valve II (105).
4. The apparatus for measuring the amount of adsorption of a material mixture gas according to claim 1, wherein: the valve assembly III comprises a pneumatic valve III (106), a needle valve II (107), a stop valve I (108), a stop valve II (109), a flow meter (110) and a stop valve III (111) which are sequentially connected through pipelines; the measuring device also comprises a heat recovery pipe (116), and the heat recovery pipe (116) is wound on a pipeline between the pneumatic valve III (106) and the needle valve II (107).
5. The apparatus for measuring the amount of adsorption of a material mixture gas according to claim 1, wherein: and the valve assembly IV comprises a pneumatic valve IV (202) arranged on a pipeline at the air inlet end of the adsorbent column pipe (201) and a pneumatic valve V (203) arranged on a pipeline at the air outlet end of the adsorbent column pipe (201).
6. The apparatus for measuring an adsorption amount of a material mixture gas according to claim 1, wherein: the measuring device further comprises a vacuum unit (6), wherein the vacuum unit (6) comprises a valve assembly VIII and a vacuum pump (601), the valve assembly VIII and the vacuum pump (601) are sequentially connected with the air outlet end of the stop valve I (108) through a pipeline, the valve assembly VIII comprises a pneumatic valve VII (602), and the vacuum pump (601) is used for vacuumizing the pipeline.
7. The apparatus for measuring the amount of adsorption of a material mixture gas according to claim 1, wherein: the gas supply unit (1) further comprises a valve assembly IX, the valve assembly IX comprises a pressure reducing valve II (112), a stop valve IV (113) and a stop valve V (114), the pressure reducing valve II (112) is connected between the needle valve II (107) and the flow meter (110) through a pipeline, and the stop valve IV (113) and the stop valve V (114) are respectively connected into a pipeline between the needle valve II (107) and the stop valve I (108) through pipelines in parallel.
8. The apparatus for measuring the amount of adsorption of a material mixture gas according to claim 1, wherein: the valve assembly V comprises a stop valve VI (302) arranged on a connecting pipeline between the high-purity gas cylinder (301) and the gas inlet end of the adsorbent column tube (201); the valve assembly VI comprises a stop valve VII (402) and a stop valve VIII (403) which are arranged on a connecting pipeline between the adsorbent column tube (201) and the buffer gas cylinder (401).
9. The apparatus for measuring a material mixed gas adsorption amount according to claim 8, characterized in that: the chromatograph (501) is connected with a connecting pipeline between the stop valve VII (402) and the stop valve VIII (403) through a pipeline, and the valve assembly VII comprises a needle valve III (502) arranged on a pipeline at the air inlet end of the chromatograph (501).
10. A transfer weighing method for measuring the adsorption quantity of a material mixed gas is characterized in that: the measuring method is used for measuring the adsorption quantity of the material mixed gas by using the device for measuring the adsorption quantity of any one of claims 1 to 9, and comprises the following steps:
s11, initial state adjustment: in the initial state, the flow and the pressure of the mixed gas discharged by the raw material gas bottle are regulated through each valve component until the flow and the pressure are stable and reach the initial set pressure and the initial set flow;
s12, impurity purging: the method comprises the following steps of (1) carrying out impurity residual gas purging on an adsorbent column pipe (201) and a first detection unit (5) by using high-purity gas provided by a high-purity gas bottle (301), and regulating the pressure of the high-purity gas in a pipeline to an initial set pressure through valve components;
s13, low-temperature adsorption: cooling the adsorbent column tube (201) weighed with the adsorption material to the gas adsorption temperature, continuously supplementing high-purity gas until the pressure is greater than the initial set pressure in the step S11 and is stable, and then closing the valve assembly V; closing the valve component II and opening the valve component IV, adsorbing the mixed gas at low temperature by the adsorbent column tube (201) at the gas adsorption temperature, opening the valve component VI and the valve component VII to enable the gas at the outlet of the adsorbent column tube (201) to enter a chromatograph (501), detecting the concentration change of the mixed gas component by using the chromatograph (501), closing the valve component IV to seal the adsorbent column tube (201) when the chromatograph (501) detects the mixed gas component with a set quantitative value, opening the valve component II, closing the valve component VI and the valve component VII, closing the valve component I and the raw material gas cylinder;
s14, negative pressure desorption: reheating the adsorbent column tube (201) to a gas desorption temperature, opening the valve assembly VI to enable gas at the outlet of the adsorbent column tube (201) to enter the buffer gas cylinder (401), desorbing the gas at the gas desorption temperature, transferring the desorbed gas by using the negative pressure of the buffer gas cylinder (401) and storing the desorbed gas in the buffer gas cylinder (401), wherein a plurality of buffer gas cylinders (401) can be alternately used until the pressure of the finally used buffer gas cylinder (401) is balanced;
s15: dilution and transfer: closing the valve component VI, simultaneously opening the valve component V, and providing high-purity gas by using a high-purity gas bottle (301) to dilute the residual desorption gas until the pressure of the adsorbent column tube (201) is set pressure; closing the valve component V, simultaneously opening the valve component VI, reducing pressure or sucking negative pressure by using the buffer gas bottle (401) again, transferring desorption gas and storing the desorption gas in the buffer gas bottle (401) to achieve pressure balance; then closing the valve component VI, simultaneously opening the valve component V, repeating the step for a plurality of times until the composition of the gas in the adsorbent column tube (201) is consistent with that of the high-purity gas, and closing the valve component VI;
s16, component measurement: the amount of increase of the buffer gas cylinder (401) is weighed to obtain the mass of the gas stored in the buffer gas cylinder (401), and the buffer gas cylinder (401) is connected to a chromatograph (501) to measure the content of each component of the mixed gas, so that the adsorption amount and the volume of each component of the mixed gas in a standard state are calculated.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110775841.XA CN114646573A (en) | 2021-07-09 | 2021-07-09 | Device for measuring adsorption quantity of material mixed gas and transfer weighing method |
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| CN115683923A (en) * | 2023-01-04 | 2023-02-03 | 杭州嘉隆气体设备有限公司 | Device and method for measuring residual water content in adsorbent regeneration |
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