CN103759501A - Low-temperature rectification device for production of ultra-pure xenon - Google Patents
Low-temperature rectification device for production of ultra-pure xenon Download PDFInfo
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- CN103759501A CN103759501A CN201410020577.9A CN201410020577A CN103759501A CN 103759501 A CN103759501 A CN 103759501A CN 201410020577 A CN201410020577 A CN 201410020577A CN 103759501 A CN103759501 A CN 103759501A
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Abstract
The invention discloses a low-temperature rectification device for production of ultra-pure xenon. The low-temperature rectification device mainly comprises a condenser, a condensation low-temperature refrigerator, a low-temperature rectifying column, a reboiler and a heater. The condenser is connected to the top end of the low-temperature rectifying column. The reboiler is connected to the bottom end of the low-temperature rectifying column. The low-temperature rectifying column is filled with rectifying filler. A raw xenon inlet is arranged in the middle of the low-temperature rectifying column. The condensation low-temperature refrigerator is connected to the upper portion of the condenser. A waste xenon outlet is arranged on the side of the condenser. The heater is connected to the bottom of the reboiler. A finished xenon outlet is arranged on the side of the reboiler. The low-temperature rectification device has the advantages that krypton concentration of the xenon can be decreased from 10-9 to 10-12, purification rate is 5kg of xenon per hour, and the requirements of large dark matter detectors for purity of detection media and certain special requirements are met.
Description
Technical field
The invention belongs to refrigeration and cryogenic engineering field, in particular, relate to a kind of for obtaining the cryogenic rectification purifying plant of ultra-pure xenon.
Background technology
Xenon has the feature of high luminous intensity, low-yield threshold and high energy resolution ratio.Therefore liquid xenon is often used as the dielectric material in Aero-Space and particle physics detector.The atomic number higher (Z=54) of xenon and the higher (～3g/cm of density of liquid xenon
3), there is no long-standing radio isotope, this contributes to reduce environmental pollution (as gamma-rays and β ray in uranium and thorium pollution), therefore be that dark matter is surveyed the high-quality probing medium in experiment.
Xenon extracts acquisition by air.In air, the concentration of xenon is～10
-7mol/mol, the concentration of krypton is～10
-6mol/mol.The xenon of producing with distillation or adsorption method, can meet general application requirements, and in its xenon, the content of krypton is 10
-9～10
-6mol/mol.
85kr is a kind of radionuclide, and the half-life is 10.76, becomes rubidium-85 after decay, can radiate β ray, and its radiant maximum can reach 687keV, and its emission ratio is 99.57%.
85the aerial concentration measurement of Kr is approximately 1Bq/m
3, be equivalent to
85kr/Kr=10
-11left and right.And in dark matter detector, at the content of 85Kr lower than～10
-23in the situation of mol/mol, just can find out dark matter signal.This illustrates that wherein the ratio of Kr/Xe should not exceed～10
-12mol/mol.
Distillation and absorption are the common methods of removing krypton in xenon.These class methods are usually used in industrial processes, but it can not remove abundant krypton to meet the requirements for high precision of dark matter detector.The utilization such as the A.I.Bolozdynya of the U.S. now can continue the concentration of krypton in xenon to reduce to be adsorbed as basic red, orange, green, blue, yellow (ROGBY), but cannot be reduced to 10
-12mol/mol.And the low-temperature fractionating tower that First obtains ultra-pure xenon is in the world developed by Japanese K.Abe etc.But the purification rate of this tower is that 0.6kg is per hour, although meet concentration demand, because purification rate is lower, be not suitable for use of large-scale production.
Summary of the invention
For the technical problem existing in above-mentioned prior art, the invention provides a kind of low temperature distillation system that obtains ultra-pure xenon, can be by the krypton concentration in xenon from 10
-9be reduced to 10
-12, and purification rate is 5kg xenon per hour, to meet purity requirement and some particular demands of large-scale dark matter detector to probing medium.
For achieving the above object, the technical solution adopted in the present invention is as follows:
A kind of hypothermia distillation device that obtains ultra-pure xenon, mainly by condenser, condensation Cryo Refrigerator, cryogenic rectification post, reboiler and heater composition, described condenser is connected to the top of cryogenic rectification post, described reboiler is connected to the bottom of cryogenic rectification post, in described cryogenic rectification post, be filled with fractional distillation filling-material, the import of raw material xenon is positioned at described cryogenic rectification post middle part, described condensation is connected to described condenser top with Cryo Refrigerator, the outlet of waste product xenon is positioned at described condenser side, described heater is connected to described reboiler bottom, the outlet of product xenon is positioned at described reboiler side.
Described cryogenic rectification post outside is enclosed with aluminium foil heat insulation layer, prevents radiant heat transfer.
Described condenser is funneling stainless steel cone.
Described condensation is with welding a red copper expansion fin on Cryo Refrigerator cold head to increase heat exchange area.
Described raw material xenon-133 gas enters described heat exchanger heat exchange after by a gas purifier.
The liquid xenon extracting in described raw material xenon-133 gas and described reboiler passes through a heat exchanger heat exchange, then by after a pre-colod-application Cryo Refrigerator, enters described cryogenic rectification post.
Described rectifier unit is arranged in a vacuum casting, by vacuum unit, maintains vacuum.
Described fractional distillation filling-material is corrugated wire gauze packing, enlightening gram DNA releaxed circular DNA, triangle or the rectangular loop granular filler of filling silk.
The import of described raw material xenon, the outlet of waste product xenon and product xenon exit are provided with valve.
The aluminium foil of described aluminium foil heat insulation layer is 20-40 layer.
Compared with prior art, the present invention has following beneficial effect:
1, in the product xenon that hypothermia distillation device of the present invention is produced, the concentration of krypton can be less than 3 orders of magnitude of concentration of krypton in raw material xenon, and in its Raw xenon, the mol ratio of krypton and xenon is generally 3X10
-9mol/mol, therefore the mol ratio of krypton and xenon can reach 3X10 in product xenon
-12mol/mol;
2, in hypothermia distillation device of the present invention, the rate of recovery of xenon can reach 99%, and product xenon and raw material xenon ratio can reach 99%;
3, the reflux ratio of hypothermia distillation device of the present invention can reach R=191;
4, the purification rate of hypothermia distillation device of the present invention is 5kg xenon per hour, the 840kg xenon of can purifying in a week.
Accompanying drawing explanation
Fig. 1 is the structural representation of hypothermia distillation device provided by the present invention;
In figure: the outlet of 1-waste product xenon, 2-fractional distillation filling-material, 3-reboiler, the outlet of 4-product xenon, 5-heater, the import of 6-raw material xenon, 7-cryogenic rectification post, 8-condenser, 9-condensation Cryo Refrigerator;
Fig. 2 is the structural representation of one embodiment of the invention;
In figure: 10-gas purifier, 11-heat exchanger, the pre-colod-application Cryo Refrigerator of 12-, 9-condensation Cryo Refrigerator, 8-condenser, 7-cryogenic rectification post, 13-liquid level gauge, 3-reboiler, 14-vacuum casting, the outlet of 1-waste product xenon, the import of 6-raw material xenon, the outlet of 4-product xenon, 18-needle-valve, 19-stop valve, 20-vacuum pumping port.
The specific embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.Following examples will contribute to those skilled in the art further to understand the present invention, but not limit in any form the present invention.It should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, can also make some distortion and improvement.These all belong to protection scope of the present invention.
Shown in Fig. 1, hypothermia distillation device provided by the present invention, separates for the cryogenic rectification of xenon.Mainly by condenser 8, for condensation, Cryo Refrigerator 9, cryogenic rectification post 7, reboiler 3 and heater 5 form.Condenser 8 is connected to the top of cryogenic rectification post 7, and reboiler 3 is connected to the bottom of cryogenic rectification post 7, is filled with fractional distillation filling-material 2 in cryogenic rectification post 7.Raw material xenon import 6 is positioned at cryogenic rectification post 7 middle parts, and condensation is connected to condenser 8 tops with Cryo Refrigerator 9, and waste product xenon outlet 1 is positioned at condenser 8 sides, and heater 5 is connected to reboiler 3 bottoms, and product xenon outlet 4 is positioned at reboiler 3 sides.
In cryogenic rectification post 7, the gas-liquid two-phase that contains the xenon of krypton carries out mass transfer exchange on fractional distillation filling-material 2 surfaces, containing the less xenon component of krypton amount, is enriched in liquid phase, moving to post underflow; Containing the more xenon component of krypton amount, be enriched in gas phase, to capital, rise.So, through the exchange of gas-liquid repeatedly, in the interior xenon component of reboiler 3, obtain enrichment, and krypton component in capital condenser 8 obtains enrichment.Liquid xenon, at the interior heated carburation by evaporation of reboiler 3, returns to post top, is condensed device 8 condensations and is back to post bottom equally at the gas xenon of capital.Containing krypton amount, be 10
-12product xenon from taking out at the bottom of post, and be 10 containing krypton amount
-7waste product xenon from capital, take out, so realize cryogenic rectification and extract the object of high-purity xenon.
Shown in Fig. 2, in one embodiment of the invention, raw material xenon-133 gas 6 first, after gas purifier 10, passes through heat exchanger 11 heat exchange with the liquid xenon extracting in reboiler 3, then by after pre-colod-application Cryo Refrigerator 12 precoolings, enters in cryogenic rectification post 7.
In the embodiment of the present invention, waste product xenon outlet 1 for external diameter be 1/4 " stainless steel tube, for by the saturated gas of condenser---waste product xenon is exported.Product xenon outlet 4 for external diameter be 1/2 " stainless steel tube, for by the liquid xenon of reboiler---product xenon is exported.The import 6 of raw material xenon for external diameter be 1/2 " stainless steel tube, for inputting raw material xenon.
In the embodiment of the present invention, condenser 8 is the funneling vertebral body structure of stainless steel, the xenon rising is so far cooled to after liquid xenon with Cryo Refrigerator 9 by condensation, in condenser 8, be separated into after liquid xenon/saturated xenon steam, liquid xenon flows into cryogenic rectification post 7, and saturated xenon steam is derived by waste product xenon outlet 1 with 1% ratio.Condensation is with welding a red copper expansion fin on Cryo Refrigerator 9 cold heads to increase heat exchange area.
In the invention process, cryogenic rectification post 7 is the high 4m of being, diameter is the stainless steel column of Φ 80mm × 4mm.Cryogenic rectification post 7 outer walls are wrapped in the aluminium foil of 20 layers, and midfeather fibrous material, after so processing, has reduced radiant heat transfer effectively.Fractional distillation filling-material 2, for corrugated wire gauze packing, enlightening gram DNA releaxed circular DNA, triangle and the rectangular loop granular filler of filling silk, completely fills among cryogenic rectification post 7.
In the embodiment of the present invention, reboiler 3 is that a diameter is 273mm, and height is the stainless steel cylindrical chamber processed of 318mm, the liquid xenon being flowed down by cryogenic rectification post 7 for splendid attire.Heater 5 is wherein heated to be saturated vapor by part liquid xenon and turns back to the interior continuation caloic exchange of cryogenic rectification post 7 and balance.Remaining liquid xenon is exported by product xenon outlet 4 as product xenon using 99% ratio.
In the embodiment of the present invention, whole rectifier unit is positioned at vacuum casting 14.Vacuum casting 14 is maintained by vacuum pumping port 20 by vacuum unit, makes vacuum keep 10
-2pa～10
-3pa, can leak heat drop by radiation and be low to moderate 6W.Unstrpped gas enters from raw material xenon import 6, by the liquid xenon heat exchange precooling extracting in heat exchanger 11 and reboiler 3, then by pre-colod-application Cryo Refrigerator 12, continued after cooling to send into cryogenic rectification post 7, xenon is cooled to liquid xenon by condensation with Cryo Refrigerator 9 in condenser 8, by filler layer by layer, flow in reboiler 3, by electric heater 5, be heated to be xenon and return to cryogenic rectification post 7 and continue caloic and exchange until reach dynamic equilibrium.
In the embodiment of the present invention, waste product xenon outlet 1, raw material xenon import 6 and product xenon export 4 places and are provided with needle-valve 18 and stop valve 19, for controlling the turnover of gas.Reboiler 3 connects a liquid level gauge 13, for measuring the number of liquid xenon.
Rectifier unit of the present invention, for how reducing radiokrypton-85 content in the probing medium liquid xenon of dark matter detector, thereby obtains the problem of high-purity xenon.This rectifier unit can be in the situation that the rate of recovery be 99%, with 5kg/h(15SLPM) speed by the content of krypton in xenon from 10
-9be reduced to 10
-12, this is to requiring the development of large-scale dark matter detector of high accuracy, high sensitivity, low background most important.
Above specific embodiments of the invention are described.It will be appreciated that, the present invention is not limited to above-mentioned specific implementations, and those skilled in the art can make various distortion or modification within the scope of the claims, and this does not affect flesh and blood of the present invention.
Claims (10)
1. one kind obtains the hypothermia distillation device of ultra-pure xenon, it is characterized in that, mainly by condenser, condensation Cryo Refrigerator, cryogenic rectification post, reboiler and heater composition, described condenser is connected to the top of cryogenic rectification post, described reboiler is connected to the bottom of cryogenic rectification post, in described cryogenic rectification post, be filled with fractional distillation filling-material, the import of raw material xenon is positioned at described cryogenic rectification post middle part, described condensation is connected to described condenser top with Cryo Refrigerator, the outlet of waste product xenon is positioned at described condenser side, described heater is connected to described reboiler bottom, the outlet of product xenon is positioned at described reboiler side.
2. the hypothermia distillation device of the ultra-pure xenon of acquisition according to claim 1, is characterized in that, described cryogenic rectification post outside is enclosed with aluminium foil heat insulation layer, prevents radiant heat transfer.
3. the hypothermia distillation device of the ultra-pure xenon of acquisition according to claim 1, is characterized in that, described condenser is funneling stainless steel cone.
4. the hypothermia distillation device of the ultra-pure xenon of acquisition according to claim 1, is characterized in that, described condensation is with welding a red copper expansion fin on Cryo Refrigerator cold head to increase heat exchange area.
5. the hypothermia distillation device of the ultra-pure xenon of acquisition according to claim 1, it is characterized in that, the liquid xenon extracting in raw material xenon-133 gas and described reboiler passes through a heat exchanger heat exchange, then by after a pre-colod-application Cryo Refrigerator, enters described cryogenic rectification post.
6. the hypothermia distillation device of the ultra-pure xenon of acquisition according to claim 5, is characterized in that, described rectifier unit is arranged in a vacuum casting, by vacuum unit, maintains vacuum.
7. the hypothermia distillation device of the ultra-pure xenon of acquisition according to claim 5, is characterized in that, described raw material xenon-133 gas enters described heat exchanger heat exchange after by a gas purifier.
8. the hypothermia distillation device of the ultra-pure xenon of acquisition according to claim 1, is characterized in that, described fractional distillation filling-material is corrugated wire gauze packing, enlightening gram DNA releaxed circular DNA, triangle or the rectangular loop granular filler of filling silk.
9. the hypothermia distillation device of the ultra-pure xenon of acquisition according to claim 1, is characterized in that, the import of described raw material xenon, the outlet of waste product xenon and product xenon exit are provided with valve.
10. the hypothermia distillation device of the ultra-pure xenon of acquisition according to claim 2, is characterized in that, the aluminium foil of described aluminium foil heat insulation layer is 20-40 layer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410020577.9A CN103759501A (en) | 2014-01-16 | 2014-01-16 | Low-temperature rectification device for production of ultra-pure xenon |
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|---|---|---|---|
| CN201410020577.9A CN103759501A (en) | 2014-01-16 | 2014-01-16 | Low-temperature rectification device for production of ultra-pure xenon |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103983085A (en) * | 2014-06-03 | 2014-08-13 | 上海启元空分技术发展股份有限公司 | Method for controlling temperature of krypton and xenon separation tower |
| CN104538114A (en) * | 2014-12-12 | 2015-04-22 | 王凡业 | Overcooling box of superconducting cable cooling system |
| CN106642996A (en) * | 2016-12-20 | 2017-05-10 | 杭州杭氧股份有限公司 | Cryogenic rectification device and method in process argon recovery system |
| CN114508899A (en) * | 2022-02-09 | 2022-05-17 | 上海交通大学四川研究院 | Cryogenic rectification system and process capable of operating in forward and reverse directions to obtain ultra-pure xenon |
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| DE19526226A1 (en) * | 1995-07-18 | 1997-01-23 | Linde Ag | Ultra-pure xenon prodn. |
| US5832746A (en) * | 1996-05-14 | 1998-11-10 | Teisan Kabushiki Kaisha | Ultra-high purity nitrogen trifluoride production method, and unit therefor |
| US6314757B1 (en) * | 2000-08-25 | 2001-11-13 | Prakair Technology, Inc. | Cryogenic rectification system for processing atmospheric fluids |
| CN201438067U (en) * | 2009-08-13 | 2010-04-14 | 上海启元科技发展有限公司 | Device for separating depleted krypton-xenon concentrate |
| JP2010126394A (en) * | 2008-11-27 | 2010-06-10 | Taiyo Nippon Sanso Corp | Xenon rectification apparatus |
-
2014
- 2014-01-16 CN CN201410020577.9A patent/CN103759501A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19526226A1 (en) * | 1995-07-18 | 1997-01-23 | Linde Ag | Ultra-pure xenon prodn. |
| US5832746A (en) * | 1996-05-14 | 1998-11-10 | Teisan Kabushiki Kaisha | Ultra-high purity nitrogen trifluoride production method, and unit therefor |
| US6314757B1 (en) * | 2000-08-25 | 2001-11-13 | Prakair Technology, Inc. | Cryogenic rectification system for processing atmospheric fluids |
| JP2010126394A (en) * | 2008-11-27 | 2010-06-10 | Taiyo Nippon Sanso Corp | Xenon rectification apparatus |
| CN201438067U (en) * | 2009-08-13 | 2010-04-14 | 上海启元科技发展有限公司 | Device for separating depleted krypton-xenon concentrate |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103983085A (en) * | 2014-06-03 | 2014-08-13 | 上海启元空分技术发展股份有限公司 | Method for controlling temperature of krypton and xenon separation tower |
| CN103983085B (en) * | 2014-06-03 | 2019-06-04 | 上海启元空分技术发展股份有限公司 | A kind of temprature control method of krypton xenon knockout tower |
| CN104538114A (en) * | 2014-12-12 | 2015-04-22 | 王凡业 | Overcooling box of superconducting cable cooling system |
| CN106642996A (en) * | 2016-12-20 | 2017-05-10 | 杭州杭氧股份有限公司 | Cryogenic rectification device and method in process argon recovery system |
| CN114508899A (en) * | 2022-02-09 | 2022-05-17 | 上海交通大学四川研究院 | Cryogenic rectification system and process capable of operating in forward and reverse directions to obtain ultra-pure xenon |
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