CN112067370B - Adsorption tube aging instrument and method - Google Patents
Adsorption tube aging instrument and method Download PDFInfo
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- CN112067370B CN112067370B CN202010953433.4A CN202010953433A CN112067370B CN 112067370 B CN112067370 B CN 112067370B CN 202010953433 A CN202010953433 A CN 202010953433A CN 112067370 B CN112067370 B CN 112067370B
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- 230000032683 aging Effects 0.000 title claims abstract description 148
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 104
- 238000000034 method Methods 0.000 title claims abstract description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 78
- 238000010438 heat treatment Methods 0.000 claims abstract description 49
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 39
- 238000009833 condensation Methods 0.000 claims abstract description 21
- 230000005494 condensation Effects 0.000 claims abstract description 21
- 239000000126 substance Substances 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 7
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 3
- 230000001737 promoting effect Effects 0.000 claims abstract description 3
- 238000010926 purge Methods 0.000 claims description 37
- 230000002431 foraging effect Effects 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 6
- 239000004065 semiconductor Substances 0.000 claims description 6
- 239000002594 sorbent Substances 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims 1
- 230000003679 aging effect Effects 0.000 abstract description 5
- 239000007789 gas Substances 0.000 description 11
- 239000010935 stainless steel Substances 0.000 description 10
- 229910001220 stainless steel Inorganic materials 0.000 description 10
- 239000003570 air Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 6
- 238000003795 desorption Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 239000012855 volatile organic compound Substances 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
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- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
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- 239000003365 glass fiber Substances 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 238000009423 ventilation Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
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- 230000008878 coupling Effects 0.000 description 2
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- 230000005484 gravity Effects 0.000 description 2
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- 238000002955 isolation Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000012080 ambient air Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
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- 238000001514 detection method Methods 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2202—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
- G01N1/2214—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling by sorption
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/708—Volatile organic compounds V.O.C.'s
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2259/00—Type of treatment
- B01D2259/40—Further details for adsorption processes and devices
- B01D2259/40083—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption
- B01D2259/40088—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption by heating
- B01D2259/4009—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption by heating using hot gas
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- Compressors, Vaccum Pumps And Other Relevant Systems (AREA)
Abstract
The invention discloses an adsorption tube aging instrument and a method, wherein the adsorption tube aging instrument comprises: the aging cabin is used for placing the adsorption tube to be aged; the vacuum pump is communicated with the aging cabin and is used for promoting the formation of a vacuum environment in the aging cabin and continuously vacuumizing the aging cabin during heating and aging so as to collect the gaseous substances desorbed from the adsorption pipe; the heater is arranged in the aging cabin and is used for heating and aging the adsorption tube; and the condensation trap is provided with a condensation trapping part positioned in the aging cabin and used for condensing part of gaseous substances desorbed from the adsorption pipe into solid or liquid state for adsorption trapping. The invention has the advantages of no need of nitrogen in the aging process, no secondary pollution to the laboratory environment, high aging efficiency, strong aging effect consistency and the like.
Description
Technical Field
The invention relates to aging regeneration of a volatile organic compounds VOCs collection adsorption tube, which eliminates adsorbed organic matters through thermal desorption and recycles the adsorption tube for sampling analysis.
Background
The sampling of the adsorption tube is an important means for analyzing constant volatile organic compounds, the sample gas is quantitatively absorbed by the constant-flow sampler at a constant flow rate and flows through the adsorption tube, and the adsorption material in the tube adsorbs and enriches the volatile organic compounds in the sample gas to complete sample collection. The laboratory desorbs the sample enriched in the tube through the thermal desorption equipment, and inputs the sample into a gas chromatography system for analysis. The adsorption tube for completing thermal desorption sample injection needs to be aged and regenerated, so that the last sampling residue is eliminated, the adsorption tube is recycled, and the adsorption tube is sampled again.
The existing technology for aging the adsorption tube basically adopts a method of high-temperature heating and continuous high-purity nitrogen purging, and volatile organic compounds trapped by the adsorption tube are brought out of the adsorption tube through high-temperature air flow, so that the purpose of aging and regeneration is achieved. Such aging methods have the following disadvantages:
1. Each adsorption tube needs to maintain high-purity nitrogen flow of 50 ml/min during high-temperature purging, and the whole aging process can take several hours to more than ten hours, so that the consumption of the high-purity nitrogen is extremely high.
2. The purity of the high-purity nitrogen directly influences the final aging effect, and the aging effect often cannot meet the detection requirement due to the quality problem of the air source.
3. Many kinds of adsorption materials are easily oxidized at high temperature, the adsorption effect is lost, oxygen impurities in the nitrogen purging can accelerate oxidation failure of the adsorption materials at high temperature, and the service life is shortened.
4. Organic impurities in the adsorption tube can cause secondary pollution to laboratory ambient air after being purged out of the adsorption tube.
5. Because the purge air flow needs to be evenly distributed, the traditional ageing instrument generally enables at most 20 adsorption tubes to be aged simultaneously, a large number of adsorption tubes need to be aged in batches, and the time and labor consumption are low.
6. The aging degree is different between different aged batches and even between the same batch of pipes due to the difference of temperature and purge flow, and the defect of poor repeatability is often expressed in the test.
Disclosure of Invention
The invention aims to solve the technical problem of providing an adsorption tube aging instrument which does not need to use nitrogen and does not cause secondary pollution to laboratory environment in the aging process so as to overcome the defects existing in the prior art.
In order to solve the technical problems, the invention adopts the following technical scheme:
An adsorption tube aging apparatus, comprising:
The aging cabin is used for placing the adsorption tube to be aged;
The vacuum pump is communicated with the aging cabin and is used for promoting the formation of a vacuum environment in the aging cabin and continuously vacuumizing the aging cabin during heating and aging so as to collect the gaseous substances desorbed from the adsorption pipe;
the heater is arranged in the aging cabin and is used for heating and aging the adsorption tube;
And the condensation trap is provided with a condensation trapping part positioned in the aging cabin and used for condensing part of gaseous substances desorbed from the adsorption pipe into solid or liquid state for adsorption trapping.
According to the invention, the adsorption tube to be aged is heated under the vacuum environment to replace nitrogen purging in the prior art, the physical characteristic that the saturated vapor pressure of volatile organic matters is far greater than the vacuum atmosphere pressure is utilized as source power for desorption of the organic matters, so that the volatile organic matters in the adsorption tube are continuously desorbed and desorbed, namely, the temperature and the saturated vapor pressure of the adsorbed matters in the adsorption tube are heated and improved under the vacuum environment, a low-pressure vacuum atmosphere is created by using a vacuum pump, limited gas and low-boiling-point gaseous matters in the aging cabin are discharged, when the saturated vapor pressure of the adsorbed matters is greater than the atmosphere pressure, the adsorbed matters are gasified into high-temperature gas and flow to the low-pressure part of the cavity, namely flow to the condensation trapping part and flow to the vacuum pump, once the adsorbed matters of the high-temperature gas flow, a part of the high-boiling-point adsorbed matters are contacted with the condensation trapping part at low temperature, cooled and condensed into liquid or solid state again, and the power is lost, so that the adsorbed matters are prevented from being condensed to other low-temperature parts to pollute pipelines, cavities or vacuum pumps, and the polluted laboratory environment is avoided, and the non-condensed and mainly contained vapor is sucked to other low-boiling-point gaseous matters in the vacuum pump.
In a further development of the invention, a nitrogen purging device is also included, which is connected to the aging chamber. The nitrogen purging device can be matched with a vacuum pump to alternately purge nitrogen and vacuumize before heating and ageing so as to promote the ageing cabin to form a vacuum environment, and can also purge and cool the adsorption tube after heating and ageing.
In a specific embodiment of the invention, the aging chamber is provided with a rear door plate, and ventilation holes for supporting the adsorption tubes are distributed on the rear door plate.
In a specific embodiment of the invention, the aging chamber is provided with a front door plate, a refrigerating semiconductor is arranged on the outer surface of the front door plate to form the condensation trap, and the inner surface of the front door plate positioned in the aging chamber forms the condensation trap part. Through such structure, can make the solid and/or liquid material that desorb from the adsorption tube concentrate and be caught on the front door plant internal surface, convenient concentrated cleaning.
In a specific embodiment of the invention, the heater is of a honeycomb structure, heating carrying holes are densely distributed, and each heating carrying hole is internally provided with one adsorption tube. The structure can realize synchronous ageing of hundreds of adsorption tubes, greatly improves the ageing efficiency and ageing uniformity of the adsorption tubes and improves analysis repeatability indexes.
In addition, the invention also provides an aging method of the adsorption tube, which is characterized by comprising the following steps:
placing an adsorption tube to be aged in a closed aging cabin;
Utilizing a vacuum pump to promote the aging cabin to form a vacuum environment;
And in the ageing cabin in the vacuum environment, heating and ageing the adsorption tube by using a heater in the vacuum environment, continuously vacuumizing the ageing cabin by using a vacuum pump to collect the gaseous substances desorbed from the adsorption tube in the heating and ageing process, and condensing part of the gaseous substances desorbed from the adsorption tube into solid or liquid state by using a condensation catcher to absorb and capture the gaseous substances.
In a specific embodiment of the invention, before heating and ageing, the ageing cabin is alternately vacuumized and flushed with nitrogen by using a vacuum pump and a nitrogen purging device to form the vacuum environment. The measures can fully replace and discharge the residual oxygen and water vapor in the aging cabin, and avoid adverse effects on the adsorption tube in the heating process (adverse effects are that oxygen accelerates oxidation loss of the adsorption filling at high temperature, and water vapor can affect the ultimate vacuum degree and the pump working efficiency if condensed in a vacuum pump).
In a specific embodiment of the invention, the nitrogen purge device is turned off during the heat aging process. In the heating aging process, the nitrogen purging device is closed, and the continuous purging with high-purity nitrogen is stopped, so that the gas consumption of a laboratory can be greatly reduced.
In the specific embodiment of the invention, after heating and ageing are completed, the vacuum pump is turned off, the nitrogen purging device is utilized to charge nitrogen into the ageing cabin, so that the pressure in the ageing cabin is raised to the atmospheric pressure, the nitrogen purging device is kept in a purging state, and the door plate of the ageing cabin is opened, so that the adsorption tube is rapidly cooled in the nitrogen purging state.
In a specific embodiment of the invention, whether the ageing process is finished is judged by measuring the limiting vacuum degree in the ageing cabin.
By adopting the technical scheme, the invention has the following advantages:
1. The invention does not need to use high-purity nitrogen to continuously purge in the heating aging process, thereby greatly saving the gas consumption of a laboratory.
2. The vacuum atmosphere avoids the problem of incomplete aging caused by the purity of the purge gas, and ensures the consistency of the aging effect.
3. The desorption efficiency of vacuum aging is 3 times of that of the traditional purging aging, and the aging efficiency can be greatly improved.
4. The vacuum aging also avoids high-temperature oxidation of the adsorption material, and can effectively prolong the cycle service life of the adsorption tube.
5. Impurities desorbed by the adsorption tube are effectively recovered and intensively discharged, so that pollution to laboratory environment is avoided.
6. The adsorption tubes with the number of being more than 100 can be aged at one time, and compared with the traditional method for aging 10 adsorption tubes, the single-batch flux of an aging instrument is greatly improved.
7. The aging process is controlled by temperature, vacuum degree and time, and the final aging degree can be judged by extreme vacuum, so that the problem that the traditional aging is empirically controlled without feedback and closed loop control is solved, and the consistency among aging batches is reliably improved.
8. The heating and heat preservation effect under the vacuum atmosphere is good, the energy loss is less, and the energy is saved and the efficiency is high.
Drawings
FIG. 1 is a schematic view of an aging apparatus of the present invention;
FIG. 2 is a schematic view of an embodiment of an aging apparatus according to the present invention;
FIG. 3 is a schematic view of the structure of the aging chamber of the present invention;
FIG. 4 is a schematic view of a heater according to the present invention;
FIG. 5 is an exploded view of the structure of the heater of the present invention;
FIG. 6 is a schematic structural view of the adsorption tube carrier of the present invention.
Detailed Description
As shown in fig. 1 and 2, the adsorption tube aging apparatus of the present invention includes a base 600, an aging chamber 100, a heater 200, a vacuum pump 300, a nitrogen purging device 400, and a condensation trap 500.
Wherein, the heater 200 is fixed in the aging chamber 100, the vacuum pump 300 is positioned outside the aging chamber 200 and is communicated with the aging chamber 100 through an air pipe, and an isolation valve 310 is arranged between the vacuum pump 300 and the aging chamber 200. The nitrogen purge device 400 is also located outside the aging chamber 100 and is in communication with the aging chamber 100 through a gas pipe.
The aging chamber 100 is composed of a chamber body 110 having a through structure, a front door panel 120 provided at a front end of the chamber body 110, and a rear door panel 130 provided at a rear end of the chamber body 110. The cabin 110 is made of aluminum alloy, and both the front end and the rear end of the cabin are provided with silica gel sealing rings, so that the cabin 110 is ensured to be airtight when the front door plate 120 and the rear door plate 130 are closed.
As shown in fig. 2 in combination with fig. 3, the base 600 has a 45 ° inclined mounting surface 610, and the cabin 110 is obliquely fixed to the mounting surface 610 by a profile bracket 611 such that the front end of the cabin 110 is located above and the rear end is located below. A slide rail 620 is also fixed to the mounting surface 100 at the rear of the cabin 100. The rear door panel 130 is made of stainless steel, and the rear door panel 130 is slidably mounted on the slide rail 620. After the aging is completed, the rear door panel may slide down the sliding rail 620 under the force of gravity.
The outer surface of the front door plate 120 is fixedly provided with the refrigerating semiconductor 510, the front door plate 120 is made of an aluminum plate with good heat conduction performance, and a refrigerating area with the wall thickness of only 1.5mm is arranged in the middle, so that the loss in the temperature conduction process can be reduced, the refrigerating effect is accelerated, and the refrigerating temperature can reach minus 10 degrees. The front door 120 and the refrigerating semiconductor 510 constitute the condensation trap 500 of the present invention, and the inner surface of the refrigerating area is located in the aging chamber 100 after the front door 120 is closed, thereby forming the condensation trap portion 520 of the condensation trap 500. In addition, the front door panel 120 is further provided with a door panel housing 121 for covering the refrigerating semiconductor 510, and the door panel housing 121 is made of aluminum sheet metal and is provided with heat dissipation holes for rapid heat dissipation.
The outside of the cabin 110 has a cabin outer shell 111, and the top of the cabin outer shell 111 has a heat radiation hole. A cooling fan is arranged below the cabin 110 in the base 600, and is started when the temperature of the cabin 110 is too high, and air flow takes away heat from bottom to top along the clearance between the cabin 110 and the periphery of the cabin shell 111, so that the cooling effect is achieved.
The heater 200 has a honeycomb structure, and 106 heating carrying holes 201 penetrating from the front end face to the rear end face and parallel to the mounting face 610 are densely arranged to receive the adsorption tube 10. A tube bracket 131 is also fixed on the inner surface of the rear door plate 130 by screws, and ventilation holes 132 corresponding to the positions of the heating carrying holes 201 are distributed on the tube bracket 131. As further shown in fig. 1, the rear door panel 130 also has an air passage 133 therein which communicates with all of the ventilation holes 132.
Since the installation surface 610 of the base 600 is inclined, the adsorption tube 10 inserted in the heating load hole 201 is also inclined, and when the rear door panel 130 is opened and slides down along the slide rail 620, the adsorption tube 10 falls freely into the vent hole 132 of the tube holder 131 by gravity.
As shown in fig. 3, the front door panel 120 is connected to the edge of the cabin 100 by a swivel hinge 140 to achieve the opening and closing. The gap position inside the swivel hinge 140 passes through the power line extended from the refrigerating semiconductor 510 to function as a hiding function. A snap door lock 150 is provided at a coupling position of the front door panel 120 and the cabin 110 and at a coupling position of the rear door panel 130 and the cabin 110, and after the front door panel 120 and the door panel 130 are closed, the front door panel 120 and the rear door panel 130 can be respectively locked with the cabin 110.
At the bottom of the chamber 110 there are electrodes 112, vacuum line connections 113, pressure and temperature sensors 114. The pressure and temperature sensor 114 is capable of detecting the pressure and temperature within the burn-in chamber 100.
As further shown in fig. 1 and 2, the vacuum pump 300 is installed in the base 600, and is connected to the vacuum pipe joint 113 through the isolation solenoid valve 310 by an air pipe, and is communicated and isolated from the vacuum pump 300 and the burn-in chamber 100 by controlling the opening and closing of the solenoid valve 310. The nitrogen purge device 400 includes a charging solenoid valve 410 in communication with a nitrogen source. The inflation solenoid valve 410 is disposed within the base 600 and communicates with the air passage 133 in the rear door panel 131. Opening the inflation solenoid valve 410 may either inflate nitrogen or purge the adsorbent tube through the rear door 130 into the aging chamber 100. The front surface of the base 600 is also embedded with a display screen 630, which can display the data such as the pressure and the temperature in the aging chamber 100.
As shown in fig. 3, bosses are machined in the aging chamber 100, and lugs 202 are formed on two sides of the heater 200, and the lugs 202 are fixed on the bosses by using screws to fix the heater in the aging chamber 100, so that threaded holes in the aging chamber are not required to be drilled, and the strength of the aging chamber 100 is ensured.
As shown in fig. 4 and 5, the heater 200 is composed of a heating housing, a heating body, and a pressing insulating layer.
The heating body is composed of 106 regular adsorption tube carriers 220 and stainless steel heating belts 230 wound around adjacent rows of adsorption tube carriers 220.
The insulating layer is located around the outside of the heating body, and compresses and insulates the adsorption tube carrier 220 and the stainless steel heating belt 230 using the zirconia ceramic plate 231, specifically, four zirconia ceramic plates 231 are respectively located at the upper, lower, left and right sides of the heating body, wherein the zirconia ceramic plate 231 located at the lower side has openings to expose two electrodes 232 of the stainless steel heating belt 230. The insulating layer may use other insulating materials such as mica in addition to ceramic plates as insulating materials.
As shown in fig. 6, the adsorption tube carrier 220 is composed of a stainless steel tube 221 and at least one layer of glass fiber sleeve 222 sleeved outside the stainless steel tube 221. In this embodiment, the sorbent tube carriers 220 are fabricated in different locations by adding a layer of glass fiber sleeves 222 per 15℃ temperature differential. Because stainless steel has low thermal conductivity, the central temperature of the heater 200 is higher than that of the peripheral edges, and thus the glass fiber bushings of the middle three rows are arranged into three layers, which can effectively control the temperature conduction uniformity. The fiberglass sleeve 222 provides both insulation and uniform heat transfer to the interior of the adsorbent tube.
As shown in fig. 4 and 5, the heating housing is composed of groove panels 211 positioned at the front and rear end surfaces of the heating body 201, front panels 212 positioned at the upper and lower end surfaces of the heating body 201, and side panels 213 positioned at both sides of the heating body 201. The two front plates 212 of the upper and lower end surfaces and the two side plates 213 of the left and right side surfaces are locked and fixed by the fixing screws 214 to compress the insulating layer 230 and the heating body therein. The two groove panels 211 on the front and rear end surfaces have waist grooves 215 which are exposed from the openings on both ends of the stainless steel pipe 221. The hole of the stainless steel pipe 221 forms a heating load hole of the heater 200. The waist-shaped groove 215 is a stepped groove, and plays a role in preventing the stainless steel tube 221 from falling out and overcoming hole site deviation.
The adsorption tube aging instrument provided by the invention is used for performing the following operation of aging the adsorption tube:
1. The rear door 130 of the burn-in chamber 100 is closed and the adsorption tube to be burned-in is loaded on the heater 200 of the honeycomb structure.
2. The front door 120 of the burn-in chamber 100 is closed, the vacuum pump 300 is started to reduce the pressure of the burn-in chamber 100 to below 90% of atmospheric pressure, and the air tightness of the system is tested.
3. Continuing to use the vacuum pump 300, the pressure in the aging chamber 100 is reduced to below 5000 Pa.
4. The vacuum pump 300 was suspended, and the nitrogen inflation solenoid valve was opened to recharge the aging chamber 100 to 90% of atmospheric pressure.
5. And repeating the steps S202, S203 for three and four times, and fully replacing and discharging residual oxygen and water vapor in the cabin, so as to avoid influencing the adsorption tube in the heating process.
6. The vacuum pump 300 is activated while the condensation trap 500 is activated, reducing the pressure of the burn-in chamber 100 to the lowest pressure that the vacuum pump 300 can maintain.
7. According to the types of different adsorption pipes, a temperature rise curve control program matched with the corresponding adsorption pipe is adopted, and the heater 200 is used for heating the adsorption pipe, so that the adsorption pipe reaches the optimized aging temperature step by step, and the adsorption pipe is fully decomposed and adsorbed for a certain time. The degree of aging can be determined based on the change in the degree of the extreme vacuum, thereby determining whether the heating aging is completed. The gaseous substances desorbed from the adsorption tube are collected by a vacuum pump and discharged into a special exhaust pipeline, and part of the gaseous substances easily condensed in the gaseous substances desorbed from the adsorption tube are condensed into solid or liquid by a condensation catcher in the process of flowing to a low-pressure part and adsorbed on the condensation catching part (namely a front door plate).
8. After the heating and ageing are completed, the heater is closed, the heating is stopped, the vacuum pump is closed, the inflation electromagnetic valve of nitrogen is opened, and the pressure of the ageing cabin 100 is raised to the atmospheric pressure.
9. The nitrogen purge is maintained, the rear door 130 of the rear aging chamber 100 is opened, the adsorption tube slides out of the chamber body 110 along with the rear door, and the adsorption tube is quickly suspended and cooled under the condition of maintaining the nitrogen purge.
10. And (5) taking down the cooled adsorption tube, and installing the sealing caps at the two ends to finish the ageing operation.
As can be seen from the above detailed description, the present invention has the following advantages:
1. The invention does not need to use high-purity nitrogen to continuously purge in the heating aging process, thereby greatly saving the gas consumption of a laboratory.
2. The vacuum atmosphere avoids the problem of incomplete aging caused by the purity of the purge gas, and ensures the consistency of the aging effect.
3. The desorption efficiency of vacuum aging is more than 3 times of that of traditional purging aging, and the aging efficiency can be greatly improved.
4. The vacuum aging also avoids high-temperature oxidation of the adsorption material, and can effectively prolong the cycle service life of the adsorption tube.
5. Impurities desorbed by the adsorption tube are effectively recovered and intensively discharged, so that pollution to laboratory environment is avoided.
6. The adsorption tubes with the number of being more than 100 can be aged at one time, and compared with the traditional method for aging 10 adsorption tubes, the single-batch flux of an aging instrument is greatly improved.
7. The aging process is controlled by temperature, vacuum degree and time, the final aging degree can be judged by limiting vacuum, entrust the traditional aging is empirically, the feedback-free and non-closed-loop control problem is avoided, and the consistency among aging batches is reliably improved.
8. The heating and heat preservation effect under the vacuum atmosphere is good, the energy loss is less, and the energy is saved and the efficiency is high.
Claims (7)
1. An adsorption tube aging apparatus comprising:
The aging cabin is used for placing the adsorption tube to be aged;
the heater is arranged in the aging cabin and is used for heating and aging the adsorption tube;
Characterized by further comprising:
The vacuum pump is communicated with the aging cabin and is used for promoting the formation of a vacuum environment in the aging cabin and continuously vacuumizing the aging cabin during heating and aging so as to collect the gaseous substances desorbed from the adsorption pipe;
The nitrogen purging device is communicated to the aging cabin;
the condensation trap is provided with a condensation trapping part positioned in the aging cabin and used for condensing part of gaseous substances desorbed from the adsorption pipe into solid or liquid state for adsorption trapping;
The heater is of a honeycomb structure, heating carrying holes are densely distributed, and each heating carrying hole is internally provided with one adsorption tube;
the aging cabin is provided with a rear door plate, vent holes for supporting the adsorption tubes are distributed on the rear door plate, and the nitrogen purging device is communicated with the vent holes;
the aging cabin is obliquely arranged on the base in a posture that the front end of the aging cabin is located above and the rear end of the aging cabin is located below, a sliding rail is arranged on the base, and the rear door plate is slidably located on the sliding rail.
2. The sorbent tube aging apparatus of claim 1, wherein: the aging cabin is provided with a front door plate, a refrigerating semiconductor is arranged on the outer surface of the front door plate to form the condensation trap, and the front door plate is positioned on the inner surface of the aging cabin to form the condensation trap part.
3. The sorbent tube aging apparatus of claim 2, wherein: the aging chamber is obliquely arranged on the base in a posture that the front door plate is high and the rear door plate is low.
4. A method for aging an adsorption tube, characterized in that the aging of an adsorption tube is performed by using the adsorption tube aging apparatus according to any one of claims 1 to 3, comprising the steps of:
placing an adsorption tube to be aged in a closed aging cabin;
Utilizing a vacuum pump to promote the aging cabin to form a vacuum environment;
And in the ageing cabin in the vacuum environment, heating and ageing the adsorption tube by using a heater in the vacuum environment, continuously vacuumizing the ageing cabin by using a vacuum pump to collect the gaseous substances desorbed from the adsorption tube in the heating and ageing process, and condensing part of the gaseous substances desorbed from the adsorption tube into solid or liquid state by using a condensation catcher to absorb and capture the gaseous substances.
5. The method for aging an adsorption tube according to claim 4, wherein: and before heating and ageing, alternately vacuumizing and flushing nitrogen into the ageing cabin by using a vacuum pump and a nitrogen purging device to form the vacuum environment.
6. The method for aging an adsorption tube according to claim 4, wherein: after the heating and ageing are finished, the vacuum pump is closed, nitrogen is filled into the ageing cabin by the nitrogen purging device, so that the pressure in the ageing cabin is increased back to the atmospheric pressure, the nitrogen purging device is kept in a purging state, and a rear door plate of the ageing cabin is opened, so that the adsorption tube is rapidly cooled in the nitrogen purging state.
7. The method for aging an adsorption tube according to claim 4, wherein: and judging whether the ageing process is finished or not through measuring the limiting vacuum degree in the ageing cabin.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB910059A (en) * | 1959-12-09 | 1962-11-07 | Balzers Patent Beteilig Ag | Improvements in and relating to the pumping-off of gases and vapours by sorption |
| CN104958995A (en) * | 2015-06-23 | 2015-10-07 | 江苏中远环保科技有限公司 | Technology and device for treating organic waste gas with activated carbon by means of nitrogen heating and vacuum desorption |
| CN205826483U (en) * | 2016-04-25 | 2016-12-21 | 广州市艾谱诺仪器设备有限公司 | A kind of intelligent used in aging of adsorption tubes instrument |
| CN109060645A (en) * | 2018-10-29 | 2018-12-21 | 国网湖南省电力有限公司 | A kind of paper oil insulation material electric-thermal joint burn-in test test method and device |
| CN109696394A (en) * | 2019-01-11 | 2019-04-30 | 北京博赛德科技有限公司 | A kind of used in aging of adsorption tubes instrument |
| CN111430157A (en) * | 2020-03-24 | 2020-07-17 | 中山市昦瑞真空科技有限公司 | Novel vacuum aging equipment for film capacitor and production process thereof |
| CN213481819U (en) * | 2020-09-11 | 2021-06-18 | 上海朋环测控技术股份有限公司 | Vacuum adsorption tube aging instrument |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4628807B2 (en) * | 2005-01-28 | 2011-02-09 | 株式会社日立ハイテクノロジーズ | Vacuum processing apparatus and vacuum processing method |
-
2020
- 2020-09-11 CN CN202010953433.4A patent/CN112067370B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB910059A (en) * | 1959-12-09 | 1962-11-07 | Balzers Patent Beteilig Ag | Improvements in and relating to the pumping-off of gases and vapours by sorption |
| CN104958995A (en) * | 2015-06-23 | 2015-10-07 | 江苏中远环保科技有限公司 | Technology and device for treating organic waste gas with activated carbon by means of nitrogen heating and vacuum desorption |
| CN205826483U (en) * | 2016-04-25 | 2016-12-21 | 广州市艾谱诺仪器设备有限公司 | A kind of intelligent used in aging of adsorption tubes instrument |
| CN109060645A (en) * | 2018-10-29 | 2018-12-21 | 国网湖南省电力有限公司 | A kind of paper oil insulation material electric-thermal joint burn-in test test method and device |
| CN109696394A (en) * | 2019-01-11 | 2019-04-30 | 北京博赛德科技有限公司 | A kind of used in aging of adsorption tubes instrument |
| CN111430157A (en) * | 2020-03-24 | 2020-07-17 | 中山市昦瑞真空科技有限公司 | Novel vacuum aging equipment for film capacitor and production process thereof |
| CN213481819U (en) * | 2020-09-11 | 2021-06-18 | 上海朋环测控技术股份有限公司 | Vacuum adsorption tube aging instrument |
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