CN102583280A - Device and method for purifying high-purity xenon and krypton - Google Patents
Device and method for purifying high-purity xenon and krypton Download PDFInfo
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- CN102583280A CN102583280A CN2012100204300A CN201210020430A CN102583280A CN 102583280 A CN102583280 A CN 102583280A CN 2012100204300 A CN2012100204300 A CN 2012100204300A CN 201210020430 A CN201210020430 A CN 201210020430A CN 102583280 A CN102583280 A CN 102583280A
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Abstract
The invention relates to a device and method for purifying high-purity xenon and krypton. An ammonia adsorber is arranged between a crude xenon-krypton hydrocarbon compound removing system and an xenon-krypton condensing system; a second hydrocarbon compound removing system is arranged between the xenon-krypton condensing system and an xenon-krypton rectifying system; a krypton gas outlet pipe of the xenon-krypton rectifying system is connected with a vaporizer; and an xenon gas outlet pipe of the xenon-krypton rectifying system is connected with the vaporizer and an xenon gas purifier. The device and the method disclosed by the invention can be used for respectively and effectively removing ammonia in the krypton and the xenon as well as fluoride and solving the overproof problem of the condensed hydrocarbon compound, so that the purities of krypton and xenon products meet or exceed the internal technical index requirement.
Description
Technical field
The present invention relates to the purifying plant and the method for a kind of krypton, xenon.
Background technology
At present; The method of high-purity krypton, xenon of purifying generally adopts the method for bakes to burn the article and repeatedly rectifying purify krypton, xenon-133 gas; On method, do not consider the removal of radon; And fluorochemical only relies on the discharging of portioned product to remove, and makes the finished product be difficult to reach the GB requirement because of radon content, content of fluoride exceed standard, and is difficult to use in high-end fields such as electric light sources.
Existing purifying plant is seen accompanying drawing 1; Crude krypton xenon cryogenic liquid is sent into vaporizer 3 vaporizations after cryogenic liquid pump 2 pressurizations; The crude krypton xenon is warming up to 470 ℃ in interchanger I 4 and electric heater 1; Get in the stoving oven 33 catalyzed reaction at high temperature, remove hydrocarbon polymer, in molecular sieve adsorber 5, remove the carbonic acid gas and the water of roasting reaction generation through interchanger I 4 cooling backs; Get into krypton xenon purification ice chest 26 then; Be cooled to through interchanger II 30 that liquid back entering krypton xenon upgrading tower 10 concentrates, rectifying; Krypton xenon upgrading tower low-temperature receiver is to regulate supply by equipment such as liquid nitrogen transfer valve 7, gas-liquid separator 6, nitrogen discharge valve 8 and liquid nitrogen variable valve 9; Isolated oxygen and nitrogen go out krypton xenon purification ice chest 26 through interchanger II 30, obtain 99.5% crude krypton xenon mixture at tower bottom; Then, crude krypton xenon mixture is sent into krypton xenon rectifying tower 16 and is separated, and crude krypton gas gets into pure krypton column 18 rectifying and obtains pure krypton, and thick xenon gets into pure xenon column 20 rectifying and obtains pure xenon, and krypton, xenon liquid go out krypton xenon purification ice chest 26.Each rectifying tower residual air is by bleed valve II 17, bleed valve III 19, and bleed valve IV 21 is disposed to atmosphere.
Can find out from above, radon not adsorbed removal in the existing method, not consider that the krypton xenon concentrates the removal of back fluorochemical, hydrocarbon polymer, be difficult to make the product final quality to meet relevant GB technical requirements.
Summary of the invention
In order to overcome technical barriers such as extraction yield is low in purify high-purity krypton, the xenon process, product purity is not up to standard, the purpose of this invention is to provide a kind of purifying plant and method of high-purity krypton xenon.This method makes product purity meet or exceed the GB technical requirement when improving whole process extraction yield, reaches the purpose that precious resources rationally utilizes.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of purifying plant of high-purity krypton xenon; Comprise that the crude krypton xenon removes hydrocarbon polymer system, krypton xenon concentration systems, krypton xenon distillation system; Between the crude krypton xenon is except that hydrocarbon polymer system and krypton xenon concentration systems, be provided with the radon adsorber; Between krypton xenon concentration systems and krypton xenon distillation system, be provided with secondary and remove the hydrocarbon polymer system, the krypton escape pipe of krypton xenon distillation system connects vaporizer, and the xenon escape pipe of krypton xenon distillation system connects vaporizer, xenon cleaner.
Described crude krypton xenon removes the hydrocarbon polymer system and comprises liquor pump, and liquor pump connects vaporizer through electric heater, and vaporizer is through interchanger, stoving oven link molecule formula adsorber.
Described krypton xenon concentration systems comprises the krypton xenon upgrading tower that the middle part links to each other with the radon adsorber, and krypton xenon upgrading tower top is connected with gas-liquid separator, and gas-liquid separator is provided with liquid nitrogen transfer valve, nitrogen discharge valve and liquid nitrogen variable valve.
Described krypton xenon concentration systems is in the krypton xenon concentrates ice chest.
Described secondary removes the hydrocarbon polymer system and comprises the vaporizer that links to each other with krypton xenon upgrading tower bottom, and vaporizer is connected with krypton xenon distillation system through stoving oven, molecular formula adsorber.
Described krypton xenon distillation system comprises krypton xenon rectifying tower, pure krypton column, the pure xenon column that connects successively, and krypton xenon rectifying tower, pure krypton column, pure xenon column are in krypton xenon purification ice chest.
A kind of method of purification of high-purity krypton xenon; Crude krypton xenon raw material liq through the pressurization vaporization, is removed hydrocarbon polymer and moisture through bakes to burn the article, absorption, and absorption concentrates after removing radon; Carry out re-baking, absorption removal hydrocarbon polymer and moisture after concentrating; Carry out rectifying then, vaporization gets krypton, xenon respectively after the rectifying separation, and xenon obtains high-purity xenon through purifying the removal fluorochemical.
The pressure of pressurization vaporization is at 0.6MPa.
The high temperature that described bakes to burn the article TR is 460～490 ℃, pressure 0.6MPa, roasting in continuous 24 hours; 350～380 ℃ of re-baking TRs, pressure 1.0MPa, roasting in continuous 24 hours.
Obtain krypton xenon ratio after the described rectifying and be 10: 1 crude krypton xenon mixture.
The present invention purifies in high-purity krypton, the xenon process, the radon element refining plant be the radon adsorber, avoided that the concentration of radon improves in the product, radiation strengthens and threatened the harm of personnel safety.
The present invention purifies in high-purity krypton, the xenon process; The removal of hydrocarbon polymers such as methane is to be accomplished successively before and after concentrating by two stoving ovens; Solve before concentrating only bakes to burn the article effectively, concentrated hydrocarbons content such as back methane and improve again, do not reached the problem that GB requires.
The present invention purifies in high-purity krypton, the xenon process, and the refining plant of fluorochemical is the xenon cleaner in the xenon, has avoided can't removing fluorochemical fully through rectifying merely, and has removed the problem that extraction yield is difficult to improve through partial discharge.
Description of drawings
Fig. 1 is existing purifying plant structural representation;
Fig. 2 is a purifying plant structural representation of the present invention.
Wherein, 1. electric heater, 2. liquor pump, 3. vaporizer I, 4. interchanger I, 5. molecular formula adsorber I; 6. gas-liquid separator I, 7. liquid nitrogen transfer valve I, 8. nitrogen discharge valve I, 9. liquid nitrogen variable valve I, 10. krypton xenon upgrading tower, 11. bleed valve I; 12. liquid nitrogen transfer valve II, 13. nitrogen discharge valve II, 14. gas-liquid separator II, 15. liquid nitrogen variable valve II, 16. krypton xenon rectifying tower, 17. bleed valve II; 18. pure krypton column, 19. bleed valve III, 20. pure xenon columns, 21. bleed valve IV, 22. xenon transfer valves, 23. krypton gas transfer valves; 24. the xenon cleaner, 25. vaporizer III, 26. krypton xenon purification ice chests, 27. vaporizer II, 28. stoving oven II; 29. molecular formula adsorber II, 30. interchanger II, 31. krypton xenons concentrate ice chest, 32. radon adsorbers, 33. stoving oven I.
Embodiment
Below in conjunction with accompanying drawing the present invention is further specified.
Among Fig. 2; A kind of purifying plant of high-purity krypton xenon; Comprise that the crude krypton xenon removes hydrocarbon polymer system, krypton xenon concentration systems, krypton xenon distillation system, remove between hydrocarbon polymer system and krypton xenon concentration systems at the crude krypton xenon and be provided with radon adsorber 32, between krypton xenon concentration systems and krypton xenon distillation system, be provided with secondary and remove the hydrocarbon polymer system; The krypton escape pipe of krypton xenon distillation system connects vaporizer 25, and the xenon escape pipe of krypton xenon distillation system connects vaporizer 25, xenon cleaner 24.The crude krypton xenon removes the hydrocarbon polymer system and comprises liquor pump 2, and liquor pump 2 connects vaporizer I 3 through electric heater 1, and vaporizer is through interchanger I 4, stoving oven I 33 link molecule formula adsorber I 5.Krypton xenon concentration systems comprises the krypton xenon upgrading tower 10 that the middle part links to each other with radon adsorber 32, and krypton xenon upgrading tower 10 tops are connected with gas-liquid separator I 6, and gas-liquid separator I 6 is provided with liquid nitrogen transfer valve I 7, nitrogen discharge valve I 8 and liquid nitrogen variable valve I 9.
Krypton xenon concentration systems is in the krypton xenon concentrates ice chest 31.Secondary removes the hydrocarbon polymer system and comprises the vaporizer II 27 that links to each other with krypton xenon upgrading tower 10 bottoms, and vaporizer II 27 is connected with krypton xenon distillation system through stoving oven II 28, molecular formula adsorber II 29.Krypton xenon distillation system comprises krypton xenon rectifying tower 16, pure krypton column 18, the pure xenon column 20 that connects successively, and krypton xenon rectifying tower 16, pure krypton column 18, pure xenon column 20 are in krypton xenon purification ice chest 26.
Comprise among the present invention on the basis of all devices among Fig. 1, increased radon adsorber 32, vaporizer II 27, stoving oven II28, molecular sieve adsorber II 29, vaporizer III 25 and xenon cleaner 24.Crude krypton xenon cryogenic liquid is sent into vaporizer I 3 vaporizations after cryogenic liquid pump 2 pressurizations; The crude krypton xenon is warming up to 470 ℃ in interchanger I 4 and electric heater 1; Get among the stoving oven I33 catalyzed reaction at high temperature; Remove hydrocarbon polymer, after interchanger I 4 coolings, in molecular sieve adsorber I 5, remove carbonic acid gas and the water that the roasting reaction generates; Get into the krypton xenon then and concentrate ice chest 31; Remove radon through radon adsorber 32 earlier; Be cooled to through interchanger II 30 again that liquid back entering krypton xenon upgrading tower 10 concentrates, rectifying; Krypton xenon upgrading tower low-temperature receiver is to regulate supply by equipment such as liquid nitrogen transfer valve 7, gas-liquid separator 6, nitrogen discharge valve 8 and liquid nitrogen variable valve 9, and isolated oxygen and nitrogen go out the krypton xenon through interchanger II 30 and concentrates ice chest 31, obtain 99.5% crude krypton xenon mixture in krypton xenon upgrading tower 10 bottoms; Then, crude krypton xenon mixture rises to normal temperature through vaporizer II 27, continues to heat up through stoving oven II 28 catalyzed reaction takes place, and removes hydrocarbon polymer, in molecular sieve adsorber II 29, removes carbonic acid gas and the water that reaction generates; Sending into krypton xenon rectifying tower 16 then separates; Crude krypton gets into pure krypton column 18 rectifying and obtains high-purity krypton; Thick xenon gets into pure xenon column 20 rectifying and obtains pure xenon; Krypton, xenon liquid go out krypton xenon purification ice chest 26 after vaporizer III25 returns to normal temperature, and xenon gets into xenon cleaner 24 removal fluorochemicals and obtains high-purity xenon.Each rectifying tower residual air is by bleed valve II 17, bleed valve III 19, and bleed valve IV 21 is disposed to atmosphere.
A kind of method of purification of high-purity krypton xenon; Crude krypton xenon raw material liq through the pressurization vaporization, is removed hydrocarbon polymer and moisture through bakes to burn the article, absorption, and absorption concentrates after removing radon; Carry out re-baking, absorption removal hydrocarbon polymer and moisture after concentrating; Carry out rectifying then, after the rectifying separation vaporization respectively high-purity krypton, xenon, xenon obtains high-purity xenon through purifying the removal fluorochemical.Liquid thick krypton-xenon liquid is vaporizated into 0.6MPa gas through the liquor pump pressurization, delivers to bakes to burn the article in the stoving oven, is used to remove hydrocarbon polymer, and reaction generates carbonic acid gas and water vapour, and cooling is after molecular sieve adsorber is removed carbonic acid gas and water; Get into then concentrate after rectifying tower is cooled to liquid state, rectifying, separate to remove oxygen and nitrogen, obtain 99.5% crude krypton xenon mixture; Then; Crude krypton xenon mixture is delivered to the re-baking stove and is carried out catalyzed reaction after the vaporization pressurization; Remove impurity such as hydrocarbon polymer once more; Get into adsorber and adsorb to fall moisture and the carbonic acid gas that roasting produces, get into the separation of rectifying tower low temperature fractionation again and obtain high-purity krypton gas and xenon, xenon obtains high-purity xenon after removing fluorochemical through the rear end cleaner.The high temperature that the bakes to burn the article TR is 460～490 ℃, pressure 0.6MPa, roasting in continuous 24 hours; 350～380 ℃ of re-baking TRs, pressure 1.0MPa, roasting in continuous 24 hours.
Can find out by Fig. 2; In this new method of purification to the removal of radon in krypton, the xenon, to the removal of fluorochemical; And concentrate the problem that the back hydrocarbon polymer exceeds standard effective solution is all arranged, make final krypton, xenon product purity meet or exceed the GB technical requirement.
As stated, the present invention has been gone at length explanation, but as long as not breaking away from inventive point of the present invention and effect in fact can have a lot of distortion, this will be readily apparent to persons skilled in the art.Therefore, such variation also all is included within protection scope of the present invention.
Claims (9)
1. the purifying plant of a high-purity krypton xenon; Comprise that the crude krypton xenon removes hydrocarbon polymer system, krypton xenon concentration systems, krypton xenon distillation system; It is characterized in that, remove between hydrocarbon polymer system and krypton xenon concentration systems at the crude krypton xenon and be provided with the radon adsorber, between krypton xenon concentration systems and krypton xenon distillation system, be provided with secondary and remove the hydrocarbon polymer system; The krypton escape pipe of krypton xenon distillation system connects vaporizer, and the xenon escape pipe of krypton xenon distillation system connects vaporizer, xenon cleaner.
2. the purifying plant of high-purity krypton xenon according to claim 1 is characterized in that, described crude krypton xenon removes the hydrocarbon polymer system and comprises liquor pump, and liquor pump connects vaporizer through electric heater, and vaporizer is through interchanger, stoving oven link molecule formula adsorber.
3. the purifying plant of high-purity krypton xenon according to claim 1; It is characterized in that; Described krypton xenon concentration systems comprises the krypton xenon upgrading tower that the middle part links to each other with the radon adsorber; Krypton xenon upgrading tower top is connected with gas-liquid separator, and gas-liquid separator is provided with liquid nitrogen transfer valve, nitrogen discharge valve and liquid nitrogen variable valve.
4. the purifying plant of high-purity krypton xenon according to claim 1 is characterized in that, described krypton xenon concentration systems is in the krypton xenon concentrates ice chest.
5. the purifying plant of high-purity krypton xenon according to claim 1 is characterized in that, described secondary removes the hydrocarbon polymer system and comprises the vaporizer that links to each other with krypton xenon upgrading tower bottom, and vaporizer is connected with krypton xenon distillation system through stoving oven, molecular formula adsorber.
6. the purifying plant of high-purity krypton xenon according to claim 1 is characterized in that, described krypton xenon distillation system comprises krypton xenon rectifying tower, pure krypton column, the pure xenon column that connects successively, and krypton xenon rectifying tower, pure krypton column, pure xenon column are in krypton xenon purification ice chest.
7. the method for purification of a high-purity krypton xenon is characterized in that, crude krypton xenon raw material liq is vaporized through pressurization; Remove hydrocarbon polymer and moisture through bakes to burn the article, absorption; Absorption concentrates after removing radon, carries out re-baking, absorption removal hydrocarbon polymer and moisture after concentrating, and carries out rectifying then; Vaporization gets krypton, xenon respectively after the rectifying separation, and xenon obtains high-purity xenon through purifying the removal fluorochemical.
8. the method for purification of high-purity krypton xenon according to claim 7 is characterized in that, the pressure of pressurization vaporization is at 0.6MPa.
9. the method for purification of high-purity krypton xenon according to claim 7 is characterized in that, the high temperature that described bakes to burn the article TR is 460～490 ℃, pressure 0.6MPa; 350～380 ℃ of re-baking TRs, pressure 1.0MPa.
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| CN2012100204300A CN102583280A (en) | 2012-01-29 | 2012-01-29 | Device and method for purifying high-purity xenon and krypton |
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| CN2012100204300A CN102583280A (en) | 2012-01-29 | 2012-01-29 | Device and method for purifying high-purity xenon and krypton |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109879259A (en) * | 2019-04-12 | 2019-06-14 | 山东非金属材料研究所 | A kind of ultra-pure xenon, krypton purification system and purification process |
| 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 |
| CN115364659A (en) * | 2022-07-05 | 2022-11-22 | 首钢京唐钢铁联合有限责任公司 | Krypton xenon gas purification system, method and device and electronic equipment |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1729038A (en) * | 2002-11-15 | 2006-02-01 | 米哈伊尔·尤林维奇·萨维诺夫 | Method for separating a krypton-xenon concentrate and a device for carrying out said method |
| CN101723338A (en) * | 2009-11-12 | 2010-06-09 | 上海启元科技发展有限公司 | Method for extracting krypton-xenon from liquid oxygen |
| CN202080891U (en) * | 2011-05-25 | 2011-12-21 | 俄罗斯深冷机械制造股份公司 | Krypton and xenon mixture extraction equipment |
| CN202465277U (en) * | 2012-01-29 | 2012-10-03 | 济南鲍德气体有限公司 | Device for purifying high-purity xenon-krypton |
-
2012
- 2012-01-29 CN CN2012100204300A patent/CN102583280A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1729038A (en) * | 2002-11-15 | 2006-02-01 | 米哈伊尔·尤林维奇·萨维诺夫 | Method for separating a krypton-xenon concentrate and a device for carrying out said method |
| CN101723338A (en) * | 2009-11-12 | 2010-06-09 | 上海启元科技发展有限公司 | Method for extracting krypton-xenon from liquid oxygen |
| CN202080891U (en) * | 2011-05-25 | 2011-12-21 | 俄罗斯深冷机械制造股份公司 | Krypton and xenon mixture extraction equipment |
| CN202465277U (en) * | 2012-01-29 | 2012-10-03 | 济南鲍德气体有限公司 | Device for purifying high-purity xenon-krypton |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109879259A (en) * | 2019-04-12 | 2019-06-14 | 山东非金属材料研究所 | A kind of ultra-pure xenon, krypton purification system and purification process |
| 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 |
| CN115364659A (en) * | 2022-07-05 | 2022-11-22 | 首钢京唐钢铁联合有限责任公司 | Krypton xenon gas purification system, method and device and electronic equipment |
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