CN102389683B - Method and device for separating krypton from xenon by using active carbon - Google Patents
Method and device for separating krypton from xenon by using active carbon Download PDFInfo
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- CN102389683B CN102389683B CN201110231863.6A CN201110231863A CN102389683B CN 102389683 B CN102389683 B CN 102389683B CN 201110231863 A CN201110231863 A CN 201110231863A CN 102389683 B CN102389683 B CN 102389683B
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Abstract
The invention relates to a method and device for separating krypton from xenon by using active carbon. In the method and device, an active carbon absorption column is cooled to reach -80DEG C, a krypton and xenon mixture gas is started to be introduced after the temperature of -80 DEG C is stabilized for 5min for absorbing; and the krypton and xenon mixture gas is separated by using different desorption temperatures of a krypton gas and an xenon gas on the active carbon, thus the enrichment and the separation of the krypton gas and the xenon gas are realized. A separation device based on the method has a reasonable design, and is simple and easy to operate. In addition, the active carbon is used as an absorbing agent, and the regeneration temperature to the active carbon is 200 DEG C, and overhigh regeneration temperature is not used, thus the complexity and the realizing difficulty of the method are reduced.
Description
Technical field
The invention belongs to the method and apparatus of adsorbing separation krypton and xenon, be specifically related to the method and apparatus of Activated Carbon Adsorption Separation krypton and xenon.Utilize krypton, the xenon difference of Dynamic Adsorption coefficient and the difference of adsorption conditions on active carbon to adsorb, utilize krypton, the xenon desorption temperature difference on active carbon to separate; The enrichment that realizes krypton, xenon with separate, for environmental monitoring provides technical support.
Background technology
Krypton in air, xenon concentration are lower, directly from air, isolate krypton and xenon is more difficult, prior art be air sample through molecular sieve except anhydrate and carbon dioxide after, cryogenic rectification is separated other main components in krypton/xenon and air, realizes concentrating of krypton/xenon.People's inventions number such as the Germany Alfred Wan Na of Linde AG are the patent of CN1929455 " obtaining the method for krypton and/or xenon by the cryogenic separation of air ", by the air that compresses and be cleaned, import in separable distillation system, extract the concentrate of krypton-xenon-133 gas through devices such as high-pressure tower, lower pressure column, evaporimeters.This method adopts low temperature distillation system to obtain the concentrate of krypton-xenon, utilizes the difference of krypton, xenon boiling point to realize the separation of krypton-xenon.The method energy consumption is large, cost is high, system complex, is only suitable for the production of integrated mill.
The patent that the Chinese People's Liberation Army's refined beautiful invention number such as the people of grade of 63653 Feng of army is 201010196384.0 " a kind of carbon molecular sieve is used for the separation methods of radon and xenon ", utilizing xenon calibrating gas and the activity that carbon molecular sieve enrichment concentration is 20-200ppm is 40 × 10
4-80 × 10
4bq/m
3radon gas body, remove after moisture content and enter the absorption of carbon molecular sieve adsorbent bed through 13X molecular sieve, the 13X sieve adsorpting bed of again flowing through after heating desorption, is adsorbed on xenon, radon respectively on the carbon molecular sieve adsorbent bed of series connection, realizes the separation of xenon, radon.The method only can separate the calibrating gas of xenon and radon; Separator has used Pyatyi adsorbent bed, two kinds of sorbing materials, has increased complexity and the operation easier of device; Carbon molecular sieve activation processing before use needs that the time is long, operating condition is complicated; The sorbing material that the method is used is carbon molecular sieve, the absorption that can not realize krypton and xenon with separate.
The present invention utilizes active carbon that krypton, xenon-133 gas are adsorbed, separated, adopt a kind of sorbing material of active carbon, utilize krypton, the xenon desorption temperature difference on active carbon to separate, by controlling that the temperature of active carbon adsorption column allows krypton desorption and xenon is retained in adsorption column, the enrichment that realizes krypton, xenon with separate.The method and device both can be used for the place such as nuclear reactor, nuclear power station krypton, xenon absorption with separate, also can be environmental monitoring, Chemical Manufacture and ecological protection new technological means and measure be provided.
Summary of the invention
The present invention proposes the method and apparatus of a kind of Activated Carbon Adsorption Separation krypton, xenon-133 gas, and the method utilizes krypton, the xenon-133 gas desorption temperature difference on active carbon to separate with device, thus the enrichment that realizes krypton, xenon-133 gas with separate.Based on the separator of the method, reasonable in design, simple to operation.
Solution of the present invention:
By a method for Activated carbon separation krypton and xenon, comprise the following steps
1] active carbon adsorption column is cooled to-80 ℃, the time stablizes after 5min and starts to pass into krypton, xenon gaseous mixture adsorbs;
2] absorption finishes afterwards to adsorption column heating, purges residual gas with carrier gas, and column temperature is risen to 30 ℃, stablizes after 5min and with membrane pump, krypton is collected in steel cylinder;
3] after krypton is collected and finished, adsorption column is continued to heat up, and purge with carrier gas, stop after being raised to 50 ℃ purging, be elevated to 200 ℃ of stable 5min, xenon is collected in steel cylinder with membrane pump.
Above-mentioned steps is also included in the step before absorption, the active carbon loading in adsorption column being activated, and wherein activation temperature is 200 ℃, and pressure is less than 1kPa.
A kind of device with Activated carbon separation krypton and xenon, comprise unstrpped gas bottle, carrier gas bottle, active carbon adsorption column, vavuum pump, diaphragm booster pump, sample collection bottle, gas concentration detector, connecting pipe and valve, its special character is: described unstrpped gas bottle is connected with the inlet end of described active carbon adsorption column by valve with carrier gas bottle, the outlet side of described active carbon adsorption column is connected with sample collection bottle by diaphragm booster pump, described vavuum pump is connected to inlet end and the outlet side of active carbon adsorption column by valve, the outlet side of described active carbon adsorption column is connected with gas concentration detector, described active carbon adsorption column is provided with adsorption column heater around, cooling device and temperature controller.
Above-mentioned active carbon is 14～25 order cocoanut active charcoals.
The carrier gas of above-mentioned carrier gas bottle is nitrogen or helium.
Technical characterstic of the present invention:
1, the present invention utilizes the difference of krypton, the xenon desorption temperature on active carbon, utilizes water bath with thermostatic control control heating-up temperature, accurately controls the desorption temperature of active carbon, realizes the separation of krypton, xenon.
2, the present invention utilizes the difference of desorption temperature to separate, and has reduced other knot screen, has reduced the complexity of device.
3, the present invention only uses a kind of adsorbent of active carbon, and is 200 ℃ to the regeneration temperature of active carbon, does not use too high regeneration temperature, has reduced the complexity of method and has realized difficulty.
Accompanying drawing explanation
Fig. 1 is the structural representation of the Dynamic adsorption device of krypton, xenon;
Fig. 2 is krypton desorption curve map;
Fig. 3 is xenon desorption curve map;
Fig. 4 purges krypton in tail gas, xenon changes of contents figure while being 50 ℃;
Wherein: 1-helium steel cylinder, 2-unstripped gas steel cylinder, 3-pressure-reducing valve, 4-mass flow controller, 5-active carbon adsorption column, 6-diaphragm booster pump, 7-TCD detector, 8-vavuum pump, 9,10-pressure sensor, 11～18-valve.
The specific embodiment
The present invention includes unstrpped gas bottle, carrier gas bottle, active carbon adsorption column, vavuum pump, diaphragm booster pump, sample collection bottle, gas concentration detector, connecting pipe and valve, unstrpped gas bottle is connected with the inlet end of described active carbon adsorption column by valve with carrier gas bottle, the outlet side of active carbon adsorption column is connected with sample collection bottle by diaphragm booster pump, vavuum pump is connected to inlet end and the outlet side of active carbon adsorption column by valve, the outlet side of active carbon adsorption column is connected with gas concentration detector, active carbon adsorption column is provided with adsorption column heater around, cooling device and temperature controller.To adsorb the adsorption column of krypton, xenon-133 gas, purge residual gas with carrier gas, adsorption column is warming up to 30 ℃, post front end purges with carrier gas, and desorption gas is collected in steel cylinder, measures the concentration of krypton, xenon in steel cylinder.Adsorption column is warmed up to 200 ℃, and post front end purges with carrier gas, and desorption gas is collected in steel cylinder, measures the concentration of krypton, xenon in steel cylinder, calculates the elution volume of krypton and xenon.Select 14～25 object cocoanut active charcoals as adsorbent, the Balance Air of carrier gas and preparation gas is helium or nitrogen, and adsorption column is the flanged (FLGD) steel pipe in two ends of filling active carbon, and material is stainless steel.With krypton, xenon concentration in gas-chromatography interval 4～5min detection adsorption column eluting gas.Active carbon needs that before use active carbon adsorption column is heated to 200 ℃ and keeps 30min, is evacuated down to < 1kPa, to its removal of impurities, recover its activity with vavuum pump simultaneously.
Below in conjunction with embodiment, the invention will be further described:
Experiment condition: active carbon needs to be seated in adsorption column before use activates at 200 ℃ of temperature under pressure < 1kPa condition.
Operating procedure:
One, krypton and xenon desorption manipulation step
Press shown in Fig. 1, unstripped gas steel cylinder 2 is krypton (or xenon) calibrating gas, after adsorbing on the active carbon adsorption column of-80 ℃, and rising column temperature, purge adsorption column with certain flow rate with helium, the concentration of krypton (xenon) in gas chromatograph gas-monitoring for rear end.Take the time as abscissa, temperature and krypton (xenon) concentration is ordinate, draws the desorption curve of krypton (xenon), as shown in Figures 2 and 3.Column temperature rose to before-42 ℃, krypton do not detected in eluting gas, showed also desorption not of krypton; Rise to after-42 ℃, start to detect krypton in eluting gas, krypton starts desorption; While rising to 0 ℃, in eluting gas, fail to detect krypton, almost desorption completely of krypton.As shown in Figure 2: after a certain amount of krypton is adsorbed on active carbon, rising charcoal absorption column temperature, by helium purge, obtains krypton desorption curve map.As shown in Figure 3: xenon is adsorbed on active carbon adsorption column, adsorption column temperature was rising to before 70 ℃, and xenon desorption is little, and adsorption column temperature rises to after 80 ℃, and xenon desorption is very fast.As shown in Figure 4: the gas steel cylinder by helium purge during by 50 ℃ of column temperatures is collected, measure the wherein content of krypton, xenon with Agilent6890 gas chromatograph, 50 ℃ time along with the increase of helium purge time, in air-flow, the concentration of krypton is reducing, and the concentration of xenon is increasing, this explanation xenon is at 50 ℃ of desorptions on a small quantity.Utilize the difference of krypton, xenon desorption temperature on active carbon adsorption column, the method that separates krypton and xenon by controlling desorption temperature is feasible.
Two, separate the operating procedure of krypton and xenon in conjunction with said method
(1) connect gas circuit by shown in Fig. 1, check the sealing of gas circuit.
(2) adsorption column 5 is cooled to-80 ℃, the time stablizes after 5min and starts to pass into krypton, xenon gaseous mixture adsorbs.
(3) unstripped gas steel cylinder 2 is krypton, xenon standard mixture, opens pressure-reducing valve 3, gas mass flow controller 4, valve 14, valve 15, valve 17, allows krypton, xenon be adsorbed on active carbon adsorption column.
(4) absorption finishes afterwards to adsorption column heating, with the residual gas of helium purge, column temperature is risen to 30 ℃ with water bath with thermostatic control, stablizes after 5min and with membrane pump, desorption gas (krypton) is collected in steel cylinder.After krypton is collected and finished, adsorption column is continued to heat up, and by helium purge, stop purging after being raised to 50 ℃, be elevated to 200 ℃ of stable 5min, desorption gas (xenon) is collected in steel cylinder with membrane pump.
(5) with gas chromatograph, the krypton in sample steel cylinder, xenon concentration are measured calculate recovery rate and decontamination factor.The rate of recovery > 90% of krypton in krypton sample, to the decontamination factor > 10 of xenon
4.The rate of recovery > 90% of xenon in xenon sample, to the decontamination factor > 10 of krypton
3.
Claims (2)
1. the method with Activated carbon separation krypton and xenon, the device adopting comprises unstrpped gas bottle, carrier gas bottle, active carbon adsorption column, vavuum pump, diaphragm booster pump, steel cylinder, gas concentration detector, connecting pipe and valve, described unstrpped gas bottle is connected with the inlet end of described active carbon adsorption column by valve with carrier gas bottle, the outlet side of described active carbon adsorption column is connected with steel cylinder by diaphragm booster pump, described vavuum pump is connected to inlet end and the outlet side of active carbon adsorption column by valve, the outlet side of described active carbon adsorption column is connected with gas concentration detector, described active carbon adsorption column is provided with adsorption column heater around, cooling device and temperature controller, it is characterized in that: comprise the following steps:
1] active carbon adsorption column is cooled to-80 ℃, the time stablizes after 5min and starts to pass into krypton, xenon gaseous mixture adsorbs;
2] absorption finishes afterwards to adsorption column heating, purges residual gas with carrier gas, and column temperature is risen to 30 ℃, krypton is collected in the steel cylinder of collection krypton after stablize 5min with diaphragm booster pump;
3] after krypton is collected and finished, adsorption column is continued to heat up, and purge with carrier gas, stop after being raised to 50 ℃ purging, be elevated to 200 ℃ of stable 5min, xenon is collected in the steel cylinder of collecting xenon with diaphragm booster pump.
2. the method with Activated carbon separation krypton and xenon according to claim 1, is characterized in that: be also included in the step before absorption, the active carbon loading in adsorption column being activated, wherein activation temperature is 200 ℃, and pressure is less than 1kPa.
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| CN102389683B true CN102389683B (en) | 2014-05-28 |
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| CN103308374A (en) * | 2013-06-21 | 2013-09-18 | 中国原子能科学研究院 | Separation device and preparation method of radiochemical pure Kr-88 |
| CN107045001A (en) * | 2017-01-09 | 2017-08-15 | 天津大学 | A kind of device for measuring carbon dioxide adsorption heat |
| CN108993417B (en) * | 2018-08-17 | 2020-10-02 | 浙江大学 | Metal organic framework material for adsorption separation of xenon and krypton and preparation and application thereof |
| CN109939538B (en) * | 2019-04-12 | 2020-07-28 | 中国原子能科学研究院 | System and method for rapidly separating Kr and Xe in complex fission product |
| CN110161139A (en) * | 2019-05-23 | 2019-08-23 | 中国辐射防护研究院 | A kind of large volume non-quantitative sample injection method using gas chromatograph separation Kr-85 |
| CN112705005B (en) * | 2019-10-25 | 2023-03-10 | 中冶长天国际工程有限责任公司 | Method and device for obtaining pollution adsorption coefficient of activated carbon |
| CN111830149B (en) * | 2020-06-23 | 2022-05-20 | 中国辐射防护研究院 | TCD gas chromatography multi-stage circulating Kr separation system and method |
| CN115862916B (en) * | 2022-12-07 | 2023-10-24 | 中国原子能科学研究院 | Method for extracting krypton-85 from fast reactor spent fuel rod |
| CN117531333B (en) * | 2024-01-08 | 2024-04-02 | 西安瑞恒测控设备有限公司 | Filtering system of gas chromatograph in krypton-xenon detection |
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