CN201110673Y - Low temperature voltage transformation adsorption apparatus - Google Patents
Low temperature voltage transformation adsorption apparatus Download PDFInfo
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- CN201110673Y CN201110673Y CNU2007200145896U CN200720014589U CN201110673Y CN 201110673 Y CN201110673 Y CN 201110673Y CN U2007200145896 U CNU2007200145896 U CN U2007200145896U CN 200720014589 U CN200720014589 U CN 200720014589U CN 201110673 Y CN201110673 Y CN 201110673Y
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- 238000001179 sorption measurement Methods 0.000 title claims abstract description 87
- 230000009466 transformation Effects 0.000 title 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000007789 gas Substances 0.000 claims abstract description 24
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052802 copper Inorganic materials 0.000 claims abstract description 23
- 239000010949 copper Substances 0.000 claims abstract description 23
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 239000000919 ceramic Substances 0.000 claims abstract description 5
- OMEXLMPRODBZCG-UHFFFAOYSA-N iron rhodium Chemical compound [Fe].[Rh] OMEXLMPRODBZCG-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 41
- 239000010935 stainless steel Substances 0.000 claims description 41
- 230000001276 controlling effect Effects 0.000 claims description 11
- 238000007789 sealing Methods 0.000 claims description 11
- 238000005057 refrigeration Methods 0.000 claims description 8
- 229920001342 Bakelite® Polymers 0.000 claims description 4
- 239000004637 bakelite Substances 0.000 claims description 4
- 229920001971 elastomer Polymers 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 238000003466 welding Methods 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 20
- 239000000463 material Substances 0.000 abstract description 11
- 238000005259 measurement Methods 0.000 abstract description 9
- 239000000843 powder Substances 0.000 abstract description 9
- 238000003795 desorption Methods 0.000 abstract description 8
- 230000008859 change Effects 0.000 abstract description 5
- 239000011148 porous material Substances 0.000 abstract description 5
- 238000009826 distribution Methods 0.000 abstract description 3
- 230000008901 benefit Effects 0.000 abstract description 2
- 239000012159 carrier gas Substances 0.000 abstract 4
- 238000010521 absorption reaction Methods 0.000 description 27
- 239000001257 hydrogen Substances 0.000 description 21
- 229910052739 hydrogen Inorganic materials 0.000 description 21
- 238000000034 method Methods 0.000 description 10
- 239000003463 adsorbent Substances 0.000 description 9
- 230000008569 process Effects 0.000 description 6
- 238000011160 research Methods 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 230000007246 mechanism Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000002156 adsorbate Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 230000002631 hypothermal effect Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 240000005373 Panax quinquefolius Species 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
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- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
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- 238000012827 research and development Methods 0.000 description 1
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- 108700002783 roundabout Proteins 0.000 description 1
- 239000011555 saturated liquid Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
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- 239000011232 storage material Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
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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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A30/00—Adapting or protecting infrastructure or their operation
- Y02A30/27—Relating to heating, ventilation or air conditioning [HVAC] technologies
-
- 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
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B30/00—Energy efficient heating, ventilation or air conditioning [HVAC]
- Y02B30/62—Absorption based systems
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- Separation Of Gases By Adsorption (AREA)
Abstract
Disclosed is a low-temperature pressure swing adsorption device, which comprises a low-temperature refrigerator, a stainless multi-layer chamber body, a vacuum pump system, a carrier gas pipeline and a measurement and control element which is matched with the carrier gas pipeline, wherein a primary cold head and a secondary cold head of the low-temperature refrigerator are sealed in the stainless chamber body, the vacuum pump system vacuumizes the chamber body and the carrier gas pipeline, an adsorption chamber in the carrier gas pipeline is connected with the secondary cold head of the refrigerator, a temperature controller clings to the adsorption chamber, and a small-size rhodium iron resistance thermometer and a ceramic heating sheet are installed on a copper base. The low-temperature pressure swing adsorption device has the advantages that the low-temperature pressure swing adsorption device can guarantee the adsorption chamber to constantly and reversibly change between 4K and the room temperature, can measure surface parameters such as specific surface, micro-pore volume, pore diameter distribution and the like of ultra-micro-pore powder material which can not measured by nitrogen adsorption, the temperature change between 4K and the room temperature in the adsorption chamber crosses critical temperature points of a plurality of gases, and particularly adsorption action and desorption action of hydrogen gas which can not be researched nowadays under liquid nitrogen temperature can be obtained.
Description
Technical field
The utility model relates to subcritical and overcritical adsorbing domain, providing a sleeving temperature and pressure to distinguish especially can be in 4K～room temperature, 0～30MPa scope under the continuous change condition, the device of measurement gas absorption on adsorbent, desorption kinetic and thermodynamic parameter.
Background technology
Gas is referred to as overcritical absorption in its absorption more than critical-temperature.In recent years, to natural gas, the demand of clean fuels such as hydrogen has promoted the development of this art theory, but compare with the industrial technology of develop rapidly, research on the overcritical adsorption theory lags far behind the needs on the engineering, this mainly is because cross over before and after the critical-temperature, the type of gas absorption changes, be applicable to that the following basic model of critical-temperature can't be applicable to more than the critical-temperature again, meanwhile, lack a large amount of experiment basis data in the temperature range of gas before and after its critical point again, these all are the principal elements of the overcritical adsorption theory research and development of restriction.
Under the low pressure condition, the adsorbance of overcritical absorption is very little, only just can observe tangible absorption under higher pressure, and therefore studying overcritical absorption need adopt elevated pressures, so experimental facilities is had relatively high expectations, this has limited the research scale of overcritical absorption to a certain extent.In all gas clean energy resourcies, (Tc=33.2K) is minimum in the critical-temperature of hydrogen, thereby also the highest to the absorption environment requirement.Up to now, be based on measurement in indivedual temperature spots or the little temperature range mostly about the research of hydrogen adsorption, its reason be lack can be in wide temperature range the cryogenic thermostat device that changes of regulating and controlling temperature and pressure, people such as Jagiello had once made a high pressure Dewar bottle, by the equalizing pressure that changes the liquid nitrogen top unit temp is controlled in 77～91K scope, they have measured 78K respectively with this device, 84K, the adsorption equilibrium data of three temperature spot hydrogen of 91K on active carbon, and predicted adsorption isotherm in the wide temperature range more according to experimental result.People such as Floess utilize the organic liquid of different freezing points to bathe, and having made a cover can be in 112～184K temperature range, change in 0～500Torr pressure limit, be used to measure the device of nitrogen absorption, but this alternating temperature method are both dangerous also discontinuous.People such as Zhou Li utilize the liquid nitrogen level control develop can be in 77K～221K scope continually varying hydrogen adsorption measurement mechanism, carried out research to various energy resources gas.But up to this point, still nobody finishes temperature and is lower than 77K, near the absorption the critical-temperature of hydrogen research, illustrates that then the overcritical absorption to hydrogen is imperfect thorough.In order more comprehensively to grasp hydrogen under low temperature more, at the absorption behavior of various hydrogen storage materials, be necessary to develop can low temperature more with more carry out the device that Chu Qing measures under the high pressure.
No matter be overcritical absorption or subcritical absorption, adopt the adsorbent of powder body material more as gas.Specific area, micropore volume, pore-size distribution etc. are the important indicators of powder body material performance, because the particle of powder body material is very thin, grain shape and surface topography are intricate, and parameters such as therefore direct its surface area of measurement are impossible, have only the employing round-about way.The nitrogen physisorphtion is acknowledged as the most ripe method, and experimental temperature is liquid nitrogen boiling point 77K.But also have certain limitation: the molecular kinetic energy of nitrogen when 77K is very low, being equivalent to molecular scale or very big less than the micropore inside diffusional resistance of nitrogen molecular size, is difficult to record, for example the absorption on NaA, KA molecular sieve; The rate of adsorption of nitrogen is very low in addition, and to reach time for adsorption balance very long for every bit on the thermoisopleth.Therefore adopt the hydrogen physisorphtion can measure the powder body material performance indications of micro-porous adsorption agent effectively, the absorption measurement mechanism that this just needs development to move below 33.2K.
The utility model content
The purpose of this utility model is at the problems referred to above of present hydrogen adsorption storage and micro-porous adsorption agent performance indications mensuration, to the invention provides quick, the reliable profound hypothermia absorption of cover measurement mechanism.
A kind of low-temperature swing adsorption device is characterized in that: described low-temperature swing adsorption device comprises Cryo Refrigerator (21), stainless steel multilayer cavity (22), vavuum pump unit (25), gas-carrier pipeline (23) and supporting observing and controlling element (24) thereof; Wherein the one-level cold head (18) of Cryo Refrigerator (21) is contained in the stainless steel cavity (22) with secondary cold head (14) sealing, vavuum pump unit (25) vacuumizes cavity and gas-carrier pipeline (23), and the adsorption chamber (12) in the gas-carrier pipeline (23) links to each other with the secondary cold head (14) of refrigeration machine (21).
Described stainless steel multilayer cavity (22) is divided into inside and outside two-layer, and exocoel is a magnetism-free stainless steel; Inner chamber is divided into two sections, and epimere is a stainless steel annular sealed cavity, and hypomere is the cold screen of purple ellipse made of copper, and the contact-making surface of two sections is smooth through extruding, fits tightly.Inner chamber can provide the internal layer that is stabilized in 77K shielding by the liquid nitrogen auxiliary cooling.
The I and II cold head output cold of described refrigeration machine (21), cold head is contained in the stainless steel cavity (22) by upper cover plate (20) sealing, and upper cover plate (20) adopts rubber sealing with the stainless steel exocoel.
Described upper cover plate (20) is left four different-diameters, is run through the duct of internal layer cavity, be respectively sample column pilot hole, temperature control circuit fairlead, vacuumize hole and liquid nitrogen hand-hole, the outside connection adopts KF to connect the bite type sealing soon.The inner chamber two sections are lifted on the upper cover plate by the CF ultrahigh vacuum seal.Being flexible coupling of place, the outer aperture of sample column welding bellows formula, not only compensate for displacement but also reduce stress,
The sample column and the adsorption chamber that are in the described gas-carrier pipeline (23) in the stainless steel cavity (22) are connected with pipeline in the room temperature by control valve (7), respectively adopts pressure sensor and temp-controlling element (24) measure and the control gas-carrier pipeline in the pressure and temperature of gas.
Parallel form is adopted in being connected of high and low pressure sensor in the described gas-carrier pipeline (23) and adsorption chamber, the high and low pressure sensor can be distinguished the pressure of use test system alone, and can make the system pressure test cross over the precision index that reaches respective sensor in the pressure limit of two sensors when common the use.Pipeline one end that connects vacuum at gas observing and controlling pipeline is installed atmospheric valve (15).
Described sample column (13) is made by Φ 3 * 0.75mm high pressure stainless steel tube, and the multilayer bakelite of round is close to its outside, and sample column (13) adds filter with the joining place of adsorption chamber (12).
Described adsorption chamber (12) is made by stainless steel, pin thread is made in the outside, the red copper seat upper end with negative thread is inserted in pilot hole rotation from upper cover plate, red copper seat lower end becomes pin thread, connect again from secondary cold head red copper that extend out, that negative thread is arranged, thereby make the cold of secondary cold head output be transmitted to adsorption chamber inside completely.Ceramic heating flake passes through the screw fastener of Φ 2 in red copper seat inside, guarantees just in time to be close to the adsorption chamber bottom after adsorption chamber inserts.Bore the aperture that a diameter is 3.5mm from red copper seat side, inner placement diameter is the metal-back rhodium iron resistance thermometer of 3mm, long 10mm, is affixed on the adsorption chamber outside, regulates and control adsorption chamber inside and near temperature by temperature controller.
Generally speaking, this testing arrangement mainly is made up of Cryo Refrigerator, temperature controller, gas-carrier pipeline, stainless steel cavity, vavuum pump unit, control valve, sensor, Φ 3 capillaries etc.Cryo Refrigerator uses helium as working media, is connected flexible pipe by compressor, cold head and metal and forms, and can provide from 5K to room temperature continually varying temperature environment.Gas-carrier pipeline mainly by
The gas control element of company and Φ 3 stainless steel tubes constitute, and the pressure that can bear 0～30MPa changes.Temperature controller is measured temperature, and carries out temperature control by means of near the resistor disc that is installed in the adsorption chamber.Cold head and adsorption chamber sealing are contained in the stainless steel cavity, and the vacuum cavity under the high vacuum state guarantees that adsorption chamber obtains profound hypothermia.The vavuum pump unit vacuumizes gas observing and controlling pipeline and stainless steel cavity respectively, but vacuum reaches 10
-4Pa.
Advantage of the present utility model:
The utility model combines Cryo Refrigerator first with adsorbent equipment, provide a cover convenient and practical low temperature pressure swing adsorption system: adsorption chamber can change by continuous reversible in 4K～room temperature; Supporting stainless steel multilayer cavity can guarantee to adsorb the constant of indoor temperature; The gas piping of system can bear 0～30MPa pressure to be changed, and installation and removal are easy; The particular design of many places details make whole system scientific and reasonable, use conveniently, measuring process is easy and simple to handle, automatic safe.Compare with other adsorbent equipments, the critical-temperature point of this device adsorption chamber temperatures span multiple gases, the thermodynamics and dynamics parameter of gas with various absorption, desorption process in subcritical and supercritical temperature zone be can more comprehensively obtain, absorption and desorption behavior that hydrogen can't be studied below liquid nitrogen temperature, so far particularly can be obtained.And under the condition of liquid hydrogen temperature, can utilize hydrogen to replace nitrogen again, finish the mensuration of a series of surface parameter of ultramicropore powder body material that nitrogen adsorption can't record.The Static Volumetric Method of this device employing standard, the random error of introducing is little, the data degree of accuracy height of surveying, be applicable to dissimilar adsorbent (as active carbon, aluminium oxide, silica gel etc.) to gas with various as (CH
4, Ar, CO etc.) absorption research.
Description of drawings
Fig. 1 is the principle schematic of this device;
Fig. 2 is the structural perspective of stainless steel cavity in this device;
Fig. 3 be under the condition of different temperatures a kind of commercially available active carbon at absorbing and storing performance chart to hydrogen.
The specific embodiment
For further understanding technology contents of the present invention, characteristics and effect, conjunction with figs. is described in detail as follows now:
Fig. 1 is the structural representation of present embodiment absorption measurement mechanism.4.2KG-M Cryo Refrigerator is done low-temperature receiver, the one-level cold head 18 of output cold is contained in the stainless steel cavity with secondary cold head 14 sealing shrouds, and guaranteeing provides enough low temperature for gas observing and controlling pipeline.Fig. 2 is the structural perspective of vacuum cavity, and cavity is divided into inside and outside two-layer, and outer cavity is made by magnetism-free stainless steel, inner polishing; The internal layer cavity is divided into two sections, and epimere is made toroidal cavity 17 by stainless steel, can load liquid nitrogen with auxiliary cooling; Hypomere is made by red copper, becomes cold screen, conducts the cold of liquid nitrogen downwards.The two contact-making surface fits tightly by bolt and screw, and integral hoisting is on the upper cover plate of stainless steel cavity.Upper cover plate 20 adopts rubber sealing with the stainless steel outer cavity, does not have oil, and is pollution-free, guarantees to produce in the stainless steel cavity high vacuum, high clean environment.The internal layer cavity is run through in the duct that upper cover plate 20 is left four different-diameters, respectively as the fairlead of sample column pilot hole, temperature control circuit, vacuumize hole and liquid nitrogen hand-hole, the sealing of itself and external environment adopts KF to connect the cutting ferrule form soon, and is simple and convenient, is easy to dismounting.In the experimental implementation process, the vacuum unit vacuumizes the stainless steel cavity, makes the multilayer cavity be vacuum state, can effectively completely cut off the heat affecting of ambient temperature to cold head and adsorption chamber.
Gas-carrier pipeline is included in the high-pressure air source 10, control valve 1,2,3,4,5,6,7, volumetric flask 11, pressure sensor 8,9 and the sample column in the stainless steel cavity 13 that (impale with chain-dotted line) in the normal temperature environment, adsorption chamber 12, resistor disc, filter etc.Gas-carrier pipeline mesohigh sensor 8, low pressure sensor 9 and adsorption chamber 12 adopt parallel way to be connected.For the pipeline dilatation that reduces to cause by the variation of various states such as vacuum and high pressure, add bellows in the pipeline many places, bellows also plays the effect of compensate for displacement simultaneously.In the practical operation, the maximum pressure of gas is determined by the upper limit of the pressure sensor on the pipeline in the gas-carrier pipeline, selects for use the high and low pressure sensor of different accuracy can satisfy dynamics and the thermodynamics needs that different absorption are measured.Adsorption chamber in the cavity is connected with pipeline 23 in the normal temperature environment by sample column 13 and valve 7, sample column 13 as a gas-carrier pipeline part is to be made by Φ 3 * 0.75mm high pressure stainless steel tube, the multilayer bakelite of round is close to its outside, also play guide effect in the reinforcing while capillaceous, can closely fasten with the red copper seat that extends out from cold head with the assurance adsorption chamber, and the bakelite of multilayer can also shield the upper cover plate bottom to the heat radiation in the cavity.Pin thread is made in the adsorption chamber outside, superior with heat conductivility, as to have negative thread red copper seat well is connected, the lower end of red copper is connected with the red copper that extends out from secondary cold head 14 by pin thread again, guarantees that the cold that comes out from the secondary cold head fully is transmitted to adsorption chamber inside.
Metal shell-type rhodium-iron resistance thermometer, and ceramic heating flake are close to adsorption chamber and are placed on red copper seat inside portion respectively, control and measure variations in temperature in the adsorption chamber by temperature controller 24, and temperature error is at ± 0.1K.
The vacuum unit is made up of mechanical pump and diffusion pump, and stainless steel cavity and gas-carrier pipeline are vacuumized, and utilizes resistance to regulate vacuum with the ionization gauge display unit, and under the state of cryogenic refrigeration, vacuum can reach 10
-5The order of magnitude.
Adsorption chamber in the present embodiment is equipped with the active carbon of 0.55g, and high-pressure air source is H
2(adsorbate) steel cylinder, H
2Purity is 99.999%, in the experimentation, measure the real time temperature of gas observing and controlling pipeline in the normal temperature environment, low, the high pressure sensor of 0～1MPa and 0～10MPa adopted in pressure measxurement respectively, precision is respectively 0.2% and 0.1%, and temperature controller 24 controls are also gathered the adsorption chamber temperature.Concrete operations are as follows:
(1) adsorption chamber of earlier the sample active carbon being packed into, link to each other with sample column, the then red copper seat close-coupled of stretching out of pilot hole and the secondary cold head 14 by stainless steel cavity upper cover plate 20, again sample column top is joined by valve 7 and the gas observing and controlling pipeline that is in the normal temperature, thereby a whole set of gas-carrier pipeline assembling is finished.
(2) start vavuum pump unit 25 the stainless steel cavity is vacuumized, start refrigeration machine 21 then, by temperature controller 24 controls and show the variations in temperature of adsorption chamber.
(3) adsorption process: reach the temperature of setting, under the state of constant temperature, shut off valve 1, after open valve 2,3,4,5,6,7, vacuum unit vacuumize gas-carrier pipeline, shut off valve 4,5,7, open valve 1 charges into a certain amount of H
2, open valve 7, hydrogen is adsorbed on adsorbent, leaves standstill after absorption reaches balance after a period of time record pressure. Open valve 4,5 then, and whole observing and controlling pipeline is vacuumized.Charge into H again
2, repeat aforesaid operations, finish the absorption of another pressure spot and measure.
Repeat aforesaid operations, carry out the experiment of next temperature spot.
(4) desorption process: reach the temperature of control, shut off valve 1, open valve 2,3,4,5,6,7, after startup vacuum unit vacuumized gas-carrier pipeline, shut off valve 4,5,7 then, and open valve 1 charges into a certain amount of H
2After, open valve 7, hydrogen is adsorbed on adsorbent, leaves standstill adsorption equilibrium after a period of time, record pressure.Shut off valve 7 then, and this moment, adsorption chamber pressure remained unchanged, open valve 4,5, and after the pipeline before the valve 7 vacuumized, open valve 7, the record hydrogen later pressure of desorption from the adsorbent.At last, 4,5 pairs of whole pipelines of open valve vacuumize, and charge into H
2, repeat aforesaid operations, finish the desorption of another pressure spot and measure.
Repeat aforesaid operations, carry out the experiment of next temperature spot, thereby obtain a series of suction, desorption isotherm.Test result as shown in Figure 3.
The volumetric method of employing standard is measured the surface parameter of porous material, installs as shown in Figure 1, and the volume of reference cell (gas-carrier pipeline of valve more than 7) is 21.63ml, places room temperature environment, and keeps room temperature constant as far as possible; Adsorption chamber 12 volumes are 5.34ml, the adsorbent that interior Sheng need detect.In order to overcome in the room temperature environment variations in temperature to the influence of pressure sensor, thereby influence whole experimental data, the variation of real time record room temperature is by the influence of equation of state of real gas correction temperature to pressure.21 pairs of adsorption chambers 12 of refrigeration machine provide cold, and the temperature fluctuation amplitude is less than 0.1K under the stable state.
Adsorption chamber 12 in the present embodiment is equipped with an amount of ultramicropore powder body material, adopts H
2(adsorbate) characterizes ultramicropore powder body material, H
2Purity is 99.999%.In the experimentation, utilize the real time temperature of gas-carrier pipeline in the thermometer measure normal temperature environment.Because the critical-temperature of hydrogen is 33.2K, critical pressure is 1.315MPa, so pressure measxurement adopts 10 respectively
-3Low, the high pressure sensor of～10Torr and 0～4MPa, certainty of measurement be for being respectively 0.2% and 0.1%, the requirement when satisfying the gas pressure transition, and adsorption chamber 12 temperature are also gathered in temperature controller 24 controls.Concrete operations are as follows:
(1) with the adsorption chamber 12 of packing into after the micropore powder body material drying, links to each other with sample column, add filter between the two,, pollute pipeline and cause data error to prevent that gas-carrier pipeline from vacuumizing the moment suck-back and going into pipeline by VCR connected mode adsorption chamber.By the pilot hole of upper cover plate 20, the red copper seat that adsorption chamber and sample column and secondary cold head 14 stretch out closely fastens, and the sample column upper end joins by valve 7 and the gas-carrier pipeline (being reference cell) that is in the normal temperature, and the gas-carrier pipeline assembling finishes.
(2) startup vavuum pump unit vacuumizes the stainless steel cavity and is lower than 10
-3Behind the Pa, start refrigeration machine, temperature descends, by the variations in temperature in temperature controller 24 controls and the demonstration adsorption chamber.
(3) adsorption process: when the adsorption chamber temperature reaches 33.2K, keep constant temperature, open valve 2,3,4,5,6,7, after 25 pairs of whole gas observing and controlling pipelines of vacuum unit vacuumize, shut off valve 4,5,7, open valve 1 charges into a certain amount of H
2, steady back open valve 7, hydrogen is adsorbed in the micro-porous adsorption agent, leaves standstill after absorption reaches balance after a period of time record pressure. Open valve 4,5 then, and whole observing and controlling pipeline is vacuumized.Charge into H again
2, repeat aforesaid operations, finish the absorption measurement of another pressure spot, thereby obtain the adsorpting data of the saturated liquid hydrogen of 33.2K.
(4) try to achieve the surface area of ultramicropore material by the BET equation, obtain the specific pore volume and the pore-size distribution of material by the DA equation.
Claims (9)
1, a kind of low-temperature swing adsorption device is characterized in that: described low-temperature swing adsorption device comprises Cryo Refrigerator (21), stainless steel multilayer cavity (22), vavuum pump unit (25), gas-carrier pipeline (23) and supporting observing and controlling element (24) thereof; Wherein the one-level cold head (18) of Cryo Refrigerator (21) is contained in the stainless steel cavity (22) with secondary cold head (14) sealing, vavuum pump unit (25) vacuumizes cavity and gas-carrier pipeline (23), adsorption chamber (12) in the gas-carrier pipeline (23) links to each other with the secondary cold head (14) of refrigeration machine (21), temperature controller (24) is by being close to adsorption chamber, and small-sized rhodium iron resistance thermometer and ceramic heating flake are installed on the red copper seat.
2, according to the described low-temperature swing adsorption device of claim 1, it is characterized in that: described stainless steel cavity (22) is divided into inside and outside two-layer, and exocoel is made by magnetism-free stainless steel, inner polishing; Inner chamber is divided into two sections, and epimere is the stainless steel annular cavity (17) with red copper substrate, is used to load liquid nitrogen, and hypomere is the cold screen of red copper ellipse, and the extruding of two sections contact-making surface is smooth, fits tightly by screw.
3, according to the described low-temperature swing adsorption device of claim 1, it is characterized in that: the I and II cold head of described refrigeration machine (21) is sealed in stainless steel cavity (22) lining through stainless steel upper cover plate (20), adopts rubber sealing between upper cover plate (20) and stainless steel exocoel.
4, according to the described low-temperature swing adsorption device of claim 3, it is characterized in that: there are four different-diameters in described upper cover plate (20), run through inner chamber pipeline up and down, respectively as the fairlead of sample column pilot hole, temperature control circuit, vacuumize hole and liquid nitrogen hand-hole, the inner chamber two sections are lifted on the upper cover plate with bolt by four ducted two stainless steel heavy wall extra heavy pipe roads.
5, according to the described low-temperature swing adsorption device of claim 4, it is characterized in that: the sealing means of described four pipe holes is: the aperture seals with the extraneous KF of employing snap joint bite type; Duct and internal layer cavity adopt the CF ultrahigh vacuum seal, and wherein, the welding of sample column guide apertures place can retractile bellows.
6. low-temperature swing adsorption device according to claim 4 is characterized in that: described sample column (13) is close to Φ 3 * 0.75mm high pressure stainless steel tube by the bakelite inside of round, multilayer and is made, as the part of gas-carrier pipeline.
7. low-temperature swing adsorption device according to claim 1, it is characterized in that: the sample column and the adsorption chamber that are in the described gas-carrier pipeline (23) in the stainless steel cavity (22) are connected with pipeline in the room temperature by control valve (7), the pressure and temperature of gas in the gas-carrier pipeline is measured and controlled to adopts pressure sensor and temp-controlling element (24) respectively, parallel form is adopted in being connected of high and low pressure sensor and adsorption chamber three, and vacuum line one end that is attached thereto loads atmospheric valve (15).
8. low-temperature swing adsorption device according to claim 1, it is characterized in that: described adsorption chamber (12) is made by stainless steel, pin thread is made in the outside, insert red copper seat upper end with negative thread by the pilot hole on the upper cover plate, pin thread is made in red copper seat lower end, with red copper that extend out, that negative thread is arranged is connected again from the secondary cold head.
9. low-temperature swing adsorption device according to claim 8, it is characterized in that: near the heat form the adsorption chamber is: resistance is that the screw of ceramic heating flake by Φ 2 of 150 Ω is fixed on red copper seat inside, guarantee that adsorption chamber inserts rear lower and just in time is close to heating plate, bore the aperture that diameter is 3.5mm from red copper seat side, inner placement diameter is the metal-back rhodium iron resistance thermometer of 3mm, long 10mm, be close to the adsorption chamber outside, temperature controller is regulated by the circuit that runs through inner chamber and near the inner and temperature of control adsorption chamber.
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| CNU2007200145896U CN201110673Y (en) | 2007-09-19 | 2007-09-19 | Low temperature voltage transformation adsorption apparatus |
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| CNU2007200145896U CN201110673Y (en) | 2007-09-19 | 2007-09-19 | Low temperature voltage transformation adsorption apparatus |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102662419A (en) * | 2012-04-25 | 2012-09-12 | 常熟市虞华真空设备科技有限公司 | Temperature control device of liquid nitrogen cold head |
| CN104596879A (en) * | 2015-01-18 | 2015-05-06 | 北京工业大学 | Temperature-controllable vacuum desorption performance testing system |
| CN109661545A (en) * | 2016-08-25 | 2019-04-19 | 莱宝有限公司 | Refrigeration machine |
| CN110118451A (en) * | 2019-04-09 | 2019-08-13 | 上海交通大学 | The profound hypothermia high accuracy temperature control device of thermal capacitance thermal resistance economic benefits and social benefits coupling |
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| CN111939732A (en) * | 2020-08-10 | 2020-11-17 | 浙江勤策空分设备有限公司 | Operation method of waste heat regeneration compressed air dryer |
| CN112880231A (en) * | 2021-02-04 | 2021-06-01 | 中国科学院理化技术研究所 | Adsorption refrigeration system |
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- 2007-09-19 CN CNU2007200145896U patent/CN201110673Y/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102662419A (en) * | 2012-04-25 | 2012-09-12 | 常熟市虞华真空设备科技有限公司 | Temperature control device of liquid nitrogen cold head |
| CN104596879A (en) * | 2015-01-18 | 2015-05-06 | 北京工业大学 | Temperature-controllable vacuum desorption performance testing system |
| CN109661545A (en) * | 2016-08-25 | 2019-04-19 | 莱宝有限公司 | Refrigeration machine |
| CN110118451A (en) * | 2019-04-09 | 2019-08-13 | 上海交通大学 | The profound hypothermia high accuracy temperature control device of thermal capacitance thermal resistance economic benefits and social benefits coupling |
| CN110354636A (en) * | 2019-07-05 | 2019-10-22 | 四川远方高新装备零部件股份有限公司 | A kind of pressure-variable adsorption splitter and its electric-control system |
| CN111939732A (en) * | 2020-08-10 | 2020-11-17 | 浙江勤策空分设备有限公司 | Operation method of waste heat regeneration compressed air dryer |
| CN112880231A (en) * | 2021-02-04 | 2021-06-01 | 中国科学院理化技术研究所 | Adsorption refrigeration system |
| CN113109454A (en) * | 2021-03-29 | 2021-07-13 | 北京科技大学 | Pore integrated module for measuring specific surface area based on flow method and test method |
| CN113109454B (en) * | 2021-03-29 | 2022-03-11 | 北京科技大学 | Pore integrated module for measuring specific surface area based on flow method and test method |
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