CN211603064U - Gas chromatography hydrogen permeation testing device - Google Patents
Gas chromatography hydrogen permeation testing device Download PDFInfo
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- CN211603064U CN211603064U CN201922380337.0U CN201922380337U CN211603064U CN 211603064 U CN211603064 U CN 211603064U CN 201922380337 U CN201922380337 U CN 201922380337U CN 211603064 U CN211603064 U CN 211603064U
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Abstract
The utility model relates to a gas chromatography hydrogen permeation testing arrangement belongs to energy technical field. The device comprises electrolyte ceramics, a purified gas outlet pipe, a quartz tube, a graphite seal, a raw gas inlet pipe, a flange, a cathode, a platinum wire, an alumina tube, a carrier gas inlet pipe, a tail gas outlet pipe, a vacuum-pumping system and an anode; the alumina tube is fixed in the quartz tube through a flange; the quartz tube is sealed by a flange and is provided with a feed gas inlet tube and a tail gas outlet tube; the electrolyte ceramic is respectively connected with the cathode and the anode through platinum wires, and the cathode and the anode are connected with a direct current power supply; the raw material gas inlet pipe and the carrier gas inlet pipe are respectively connected with the mass flow controller through a ball valve and a molecular pump; the purified gas delivery pipe and the tail gas delivery pipe are respectively connected with a back pressure valve and are simultaneously connected to a gas chromatograph. The utility model discloses equipment is comparatively simple, adopts proton conductive ceramics as the electrolyte, the hydrogen separation purification device of preparation, the rate of recovery of hydrogen is high, reduce the cost.
Description
Technical Field
The utility model relates to a hydrogen separation and purification device, in particular to a gas chromatography hydrogen permeation testing device; the device can be applied to the aspects of separation and purification of hydrogen, detection of separation and purification efficiency of hydrogen and the like; belongs to the technical field of energy.
Background
As a clean energy source, hydrogen is widely concerned by researchers in storage, utilization and recovery. From the current preparation approach of hydrogen, the method has important industrial significance and social significance for separating and purifying hydrogen in mixed gas. The most important thing in the hydrogen separation and purification device is the choice of the separation membrane material. The ceramic separation membrane has the characteristics of high selectivity, low cost, good mechanical strength and simple preparation process, and becomes a very promising membrane separation material.
At present, the problems of complex equipment, low hydrogen extraction efficiency and the like mainly exist for the recovery of hydrogen in mixed gas or hydrogen-containing gas.
Therefore, it is an urgent technical problem to provide a hydrogen separation and purification device that can improve the recovery rate of hydrogen and reduce the cost.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a comparatively simple hydrogen separation purification device of equipment improves hydrogen separation purification efficiency.
The above object of the utility model is achieved through the following technical scheme:
a gas chromatography hydrogen permeation testing device comprises an electrolyte ceramic wafer, a purified gas outlet pipe, a quartz pipe, a graphite seal, a raw material gas inlet pipe, a flange, a cathode, a platinum wire, an alumina pipe, a carrier gas inlet pipe, a tail gas outlet pipe, a vacuum pumping system and an anode; the electrolyte ceramic plate is positioned at the upper end of the alumina tube, the lower end of the alumina tube is provided with a graphite seal and is fixed in the quartz tube through the graphite seal and a flange, and the alumina tube is provided with a purified gas outlet tube and a carrier gas inlet tube; the quartz tube is sealed by a flange and is provided with a feed gas inlet tube and a tail gas outlet tube; the electrolyte ceramic chip is respectively connected with a cathode insulated electrode joint and an anode insulated electrode joint through platinum wires, and the cathode insulated electrode joint and the anode insulated electrode joint are connected with a direct current power supply; the raw material gas inlet pipe and the carrier gas inlet pipe are respectively connected with the mass flow controller; the purified gas delivery pipe and the tail gas delivery pipe are respectively connected with a back pressure valve and are simultaneously connected to a gas chromatograph; the purified gas outlet pipe, the raw gas inlet pipe, the carrier gas inlet pipe and the tail gas outlet pipe are all connected with a vacuum pumping system.
Preferably, the raw material gas inlet pipe and the carrier gas inlet pipe are respectively connected with the mass flow controller through a ball valve and a molecular pump.
Preferably, the electrolyte ceramic sheet is a wafer.
Preferably, the diameter of the electrolyte ceramic wafer is 5-20 mm.
Preferably, the diameter of the electrolyte ceramic wafer is 12 mm.
Preferably, the electrolyte ceramic is SrCe1-xYxO3-αX is more than 0 and less than 1, and the electrolyte ceramic is SrCe0.95Y0.05O3-α。
Preferably, the mass flow controllers are mass flow controller-1 (MFC-1) and mass flow controller-2 (MFC-2).
Preferably, a high-temperature furnace is arranged outside the alumina tube.
Has the advantages that:
the utility model discloses a gas chromatography hydrogen permeation testing arrangement, equipment are comparatively simple, adopt this equipment can also the measurement and analysis hydrogen separation to carryPure efficiency; using SrCe0.95Y0.05O3-αThe ceramic chip is used as electrolyte, and the prepared hydrogen separation and purification device can improve the recovery rate of hydrogen and reduce the cost.
The invention is further described with reference to the drawings and the detailed description, which are not meant to limit the scope of the invention.
Drawings
Fig. 1 is a schematic diagram of the gas chromatography hydrogen permeation testing device of the present invention.
Description of the main reference numerals:
1 electrolyte ceramic chip 2 purified gas outlet pipe
3 quartz tube 4 graphite seal
5 raw material gas inlet pipe 6 flange
7 cathode insulated electrode joint 8 platinum wire
9 alumina tube 10 carrier gas inlet tube
11 tail gas eduction tube 12 anode insulation electrode connects
Detailed Description
As shown in fig. 1, it is a schematic diagram of the gas chromatography hydrogen permeation testing apparatus of the present invention; wherein, 1 is an electrolyte ceramic chip, 2 is a purified gas outlet pipe, 3 is a quartz tube, 4 graphite seals, 5 is a raw material gas inlet pipe, 6 is a flange, 7 is a cathode insulated electrode joint, 8 is a platinum wire, 9 is an alumina tube, 10 is a carrier gas inlet pipe, 11 is a tail gas outlet pipe, and 12 is an anode insulated electrode joint; the utility model discloses a gas chromatography hydrogen permeation testing device, which comprises an electrolyte ceramic wafer 1, a purified gas outlet pipe 2, a quartz tube 3, a graphite seal 4, a raw gas inlet pipe 5, a flange 6, a cathode insulation electrode joint 7, a platinum wire 8, an alumina pipe 9, a carrier gas inlet pipe 10, a tail gas outlet pipe 11 and an anode insulation electrode joint 12; the upper end of an alumina tube 9 is provided with an electrolyte ceramic sheet 1, the lower end of the alumina tube 9 is sealed by a graphite seal 4, the alumina tube 9 is provided with a purified gas outlet tube 2 and a carrier gas inlet tube 10, and the electrolyte ceramic sheet 1 is SrCe with the diameter of 12mm0.95Y0.05O3-αA wafer, wherein two sides of the wafer are coated with platinum wires 8, an alumina tube 9 is fixed inside a quartz tube 3 (a sample chamber) through a flange 6, one end of the alumina tube 9 is sealed, the other end of the alumina tube 9 is fixed on the flange 6 through a graphite seal 4, the platinum wires 8 in the alumina tube 9 are connected with a direct current power supply through a cathode insulation joint electrode 7 and an anode insulation joint electrode 12 which are arranged on the flange 6, and a high-temperature furnace (a conventional high-temperature furnace is only required) is arranged outside the wafer; the quartz tube 3 is sealed by a flange 6, and the quartz tube 3 is provided with a raw material gas inlet tube 5 and a tail gas outlet tube 11; the platinum wire 8 is respectively connected with the cathode insulated electrode joint 7 and the anode insulated electrode joint 12, and the cathode insulated electrode joint 7 and the anode insulated electrode joint 12 are connected with a direct current power supply; the raw material gas inlet pipe 5 and the carrier gas inlet pipe 10 are respectively connected with mass flow controllers (MFC-1 and MFC-2) through a ball valve and a molecular pump; the purified gas delivery pipe 2 and the tail gas delivery pipe 11 are respectively connected with a Back Pressure Valve (BPV) and are simultaneously connected to a gas chromatograph; the purified gas outlet pipe 2, the raw gas inlet pipe 5, the carrier gas inlet pipe 10 and the tail gas outlet pipe 11 are all connected with a vacuum pumping system.
The principle of the gas chromatography hydrogen permeation testing device of the utility model is that the H-containing gas is introduced into the upper reaches of the electrolyte2CO of2+N2Mixing standard gas, introducing circulating or gas-flowing CO with set flow rate at downstream2Gas sampling downstream outlet of the sample chamber, analyzing CO in the sampled gas by gas chromatography2And (4) concentration.
Example 1:
(1) respectively connecting the mass flow controllers with feed gas, then connecting the feed gas into a sample chamber (a quartz tube 3, the same below), connecting platinum wires 8 to two surfaces of an electrolyte ceramic wafer 1 in the sample chamber, connecting a purified gas outlet pipe 2 and a tail gas outlet pipe 11 of the sample chamber with a back pressure valve respectively, and simultaneously connecting the back pressure valve with a gas chromatograph to complete the construction of a gas chromatography hydrogen separation testing device;
(2) the electrolyte ceramic sheet 1 is SrCe with the diameter of 12mm0.95Y0.05O3-αA round piece, two sides of which are coated with platinum electrodes, and a tube sample (one section is closed, and two sides of which are coated with platinum electrodes);
(3) the hydrogen separation test device is subjected to tightness check, and the helium detection leakage rate is not more than 4 × 10-9Pa.m3/s；
(4) Loading a sample into a sample chamber, heating the sample chamber to a test temperature, preserving heat for 60min, simultaneously vacuumizing and exhausting an upstream (raw material gas) pipeline and a downstream (carrier gas) pipeline, closing a vacuum system and a pipeline valve after exhausting is finished, and setting the temperature to an experimental temperature;
(5) the upstream (raw gas) is vacuumized and filled with H2CO of2+N2Mixed gas purge, followed by setting back pressure valve to 105Pa, setting the flow value of the mass flow controller MFC-1, and continuously introducing H into an upstream (raw gas) gas path2CO of2+N2Mixing the gas;
(6) vacuumizing the downstream (carrier gas) circulating gas path and filling high-purity CO2Cleaning gas, setting back pressure valve as selected working pressure, setting mass flow controller MFC-2 flow value, and continuously introducing high-purity CO into downstream (carrier gas) gas path2A gas;
(7) at the experimental temperature, H is chromatographed by sampling at points A and B2The hydrogen separation characteristic is calculated and analyzed to reach 100 percent.
Example 2:
(1) respectively connecting the mass flow controllers with feed gas, then connecting the feed gas into a sample chamber (a quartz tube 3, the lower part is the same), connecting platinum wires 8 to two surfaces of an electrolyte ceramic wafer 1 in the sample chamber, connecting a purified gas outlet pipe 2 and a tail gas outlet pipe 11 of the sample chamber with a back pressure valve respectively, and simultaneously connecting a gas chromatograph to complete the construction of a gas chromatography hydrogen separation test system;
(2) the electrolyte ceramic sheet 1 is SrCe with the diameter of 12mm0.9Y0.1O3-αA round piece, two sides of which are coated with platinum electrodes, and a tube sample (one section is closed, and two sides of which are coated with platinum electrodes);
(3) the leak rate of helium detection is not more than 4 × 10 when the hydrogen separation test system is subjected to a closure check-9Pa.m3/s；
(4) Loading a sample into a sample chamber, heating the sample chamber to a test temperature, keeping the temperature for 60min, simultaneously vacuumizing an upstream pipeline and a downstream pipeline, exhausting, closing a vacuum system and a pipeline valve after exhausting is finished, and setting the temperature to an experimental temperature;
(5) the upstream is evacuated and charged with H2CO of2+N2Mixed gas purge, followed by setting back pressure valve to 105Pa, setting the flow value of the mass flow controller MFC-1, and continuously introducing H into an upstream gas path2CO of2+N2Mixing the gas;
(6) vacuumizing a downstream circulating gas path and filling high-purity CO2Cleaning gas, setting back pressure valve to selected working pressure, setting mass flow controller MFC-2 flow value, and continuously introducing high-purity CO into downstream gas path2A gas;
(7) at the experimental temperature, H is chromatographed by sampling at points A and B2The hydrogen separation characteristic was calculated and analyzed, 70%.
Example 3:
(1) respectively connecting the mass flow controllers with feed gas, then connecting the feed gas into a sample chamber (a quartz tube 3), connecting platinum wires 8 to two sides of an electrolyte ceramic wafer 1 in the sample chamber, connecting a purified gas outlet pipe 2 and a tail gas outlet pipe 11 of the sample chamber with a back pressure valve respectively, and simultaneously connecting the back pressure valve with a gas chromatograph to complete the construction of a gas chromatography hydrogen separation test system;
(2) the electrolyte ceramic sheet 1 is SrCe with the diameter of 12mm0.85Y0.15O3-αA round piece, two sides of which are coated with platinum electrodes, and a tube sample (one section is closed, and two sides of which are coated with platinum electrodes);
(3) the leak rate of helium detection is not more than 4 × 10 when the hydrogen separation test system is subjected to a closure check-9Pa.m3/s；
(4) Loading the sample into a sample chamber, heating the sample chamber to a test temperature, keeping the temperature for 20-400min (60min), simultaneously vacuumizing the upstream pipeline and the downstream pipeline, exhausting, closing a vacuum system and a pipeline valve after exhausting is finished, and setting the temperature to an experimental temperature;
(5) the upstream is evacuated and charged with H2CO of2+N2Cleaning with the mixed gasBack pressure valve is set to 104-106Pa(105Pa), setting the flow value of the mass flow controller MFC-1, and continuously introducing H into an upstream gas path2CO of2+N2Mixing the gas;
(6) vacuumizing a downstream circulating gas path and filling high-purity CO2Cleaning gas, setting back pressure valve to selected working pressure, setting mass flow controller MFC-2 flow value, and continuously introducing high-purity CO into downstream gas path2A gas;
(7) at the experimental temperature, H is chromatographed by sampling at points A and B2The hydrogen separation characteristic was calculated and analyzed, 90%.
The utility model discloses a gas chromatography hydrogen permeation testing arrangement with SrCe1-xYxO3-αThe electrolyte ceramic chip is a hydrogen pump of electrolyte, and at the working temperature, after raw material gas containing hydrogen enters an electrolyte anode end of the electrolyte ceramic chip, the hydrogen is oxidized to generate protons, and under the action of direct current voltage, the protons migrate to a cathode through the electrolyte and are reduced to generate the hydrogen, so that the separation of the hydrogen from the raw material gas is realized.
In order to improve the rate of recovery of hydrogen, reduce the cost, the utility model discloses a gas chromatography hydrogen permeation testing arrangement not only can draw the mist that contains hydrogen, can also reach the purpose that the hydrogen-containing gas of separation and purification was contained through the electrolyte potsherd, theoretically speaking, the utility model discloses a gas chromatography hydrogen permeation testing arrangement's hydrogen separation purification efficiency can reach 100% the highest.
The utility model discloses a gas chromatography hydrogen permeation testing arrangement, through with SrCe1-xYxO3-αThe electrolyte ceramic chip is a hydrogen pump of electrolyte, and at the working temperature, after raw material gas containing hydrogen enters an electrolyte anode end of the electrolyte ceramic chip, the hydrogen is oxidized to generate protons, and under the action of direct current voltage, the protons migrate to a cathode through the electrolyte and are reduced to generate the hydrogen, so that the separation of the hydrogen from the raw material gas is realized. Because the electrolyte of the electrolyte ceramic plate only selectively permeates the proton, the product gas at the cathode end is pure hydrogen.
The above embodiments are only used for illustrating the present invention, and are not intended to limit the present invention, and those skilled in the relevant art can make various structural adjustments and device changes without departing from the spirit and scope of the present invention, and all equivalent technical solutions also belong to the scope and protection scope of the present invention.
Claims (7)
1. A gas chromatography hydrogen permeation testing device is characterized in that: the device comprises an electrolyte ceramic chip, a purified gas outlet pipe, a quartz pipe, a graphite seal, a raw material gas inlet pipe, a flange, a cathode, a platinum wire, an alumina pipe, a carrier gas inlet pipe, a tail gas outlet pipe, a vacuum-pumping system and an anode; the electrolyte ceramic plate is positioned at the upper end of the alumina tube, the lower end of the alumina tube is provided with a graphite seal and is fixed in the quartz tube through the graphite seal and a flange, and the alumina tube is provided with a purified gas outlet tube and a carrier gas inlet tube; the quartz tube is sealed by a flange and is provided with a feed gas inlet tube and a tail gas outlet tube; the electrolyte ceramic chip is respectively connected with a cathode insulated electrode joint and an anode insulated electrode joint through platinum wires, and the cathode insulated electrode joint and the anode insulated electrode joint are connected with a direct current power supply; the raw material gas inlet pipe and the carrier gas inlet pipe are respectively connected with the mass flow controller; the purified gas delivery pipe and the tail gas delivery pipe are respectively connected with a back pressure valve and are simultaneously connected to a gas chromatograph; the purified gas outlet pipe, the raw gas inlet pipe, the carrier gas inlet pipe and the tail gas outlet pipe are all connected with a vacuum pumping system.
2. The gas chromatography hydrogen permeation test apparatus according to claim 1, characterized in that: the feed gas inlet pipe and the carrier gas inlet pipe are respectively connected with the mass flow controller through a ball valve and a molecular pump.
3. The gas chromatography hydrogen permeation test apparatus according to claim 2, characterized in that: the electrolyte ceramic wafer is a wafer.
4. The gas chromatography hydrogen permeation test apparatus according to claim 3, characterized in that: the diameter of the electrolyte ceramic wafer is 5-20 mm.
5. The gas chromatography hydrogen permeation test apparatus according to claim 4, characterized in that: the diameter of the electrolyte ceramic wafer is 12 mm.
6. The gas chromatography hydrogen permeation test apparatus according to claim 5, characterized in that: the mass flow controllers are MFC-1 and MFC-2.
7. The gas chromatography hydrogen permeation test apparatus according to claim 6, characterized in that: a high-temperature furnace is arranged outside the alumina tube.
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| CN201922380337.0U CN211603064U (en) | 2019-12-26 | 2019-12-26 | Gas chromatography hydrogen permeation testing device |
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| CN201922380337.0U CN211603064U (en) | 2019-12-26 | 2019-12-26 | Gas chromatography hydrogen permeation testing device |
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| CN211603064U true CN211603064U (en) | 2020-09-29 |
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