CN1196331A - Method for extracting high-purity krypton, xenon from mixed gas containing oxygen, krypton, xenon. - Google Patents
Method for extracting high-purity krypton, xenon from mixed gas containing oxygen, krypton, xenon. Download PDFInfo
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- CN1196331A CN1196331A CN97103252.1A CN97103252A CN1196331A CN 1196331 A CN1196331 A CN 1196331A CN 97103252 A CN97103252 A CN 97103252A CN 1196331 A CN1196331 A CN 1196331A
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F25J3/04642—Recovering noble gases from air
- F25J3/04745—Krypton and/or Xenon
- F25J3/04751—Producing pure krypton and/or xenon recovered from a crude krypton/xenon mixture
- F25J3/04757—Producing pure krypton and/or xenon recovered from a crude krypton/xenon mixture using a hybrid system, e.g. using adsorption, permeation or catalytic reaction
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2205/00—Processes or apparatus using other separation and/or other processing means
- F25J2205/60—Processes or apparatus using other separation and/or other processing means using adsorption on solid adsorbents, e.g. by temperature-swing adsorption [TSA] at the hot or cold end
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2205/00—Processes or apparatus using other separation and/or other processing means
- F25J2205/82—Processes or apparatus using other separation and/or other processing means using a reactor with combustion or catalytic reaction
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2215/00—Processes characterised by the type or other details of the product stream
- F25J2215/34—Krypton
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2215/00—Processes characterised by the type or other details of the product stream
- F25J2215/36—Xenon
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Mechanical Engineering (AREA)
- Thermal Sciences (AREA)
- General Engineering & Computer Science (AREA)
- Separation By Low-Temperature Treatments (AREA)
Abstract
A process for extracting high-purity krypton gas or xenon gas from the mixture of oxygen, krypton and xenon includes such technological steps as passing the mixture gas into methane-removing furnace to generate CO2 and H2O, adsorbing CO2 and H2O by molecular sieve, low-temp rectification for separating O2, Kr and Xe gas to obtain high-purity Xe. Its advantages are simple process, and high quality and output rate of products.
Description
The invention relates to a method for low-temperature separation and catalytic purification of a double rectifying tower, in particular to a method for extracting krypton gas products and xenon gas products from mixed gas of oxygen, krypton and xenon.
For extractingkrypton and xenon from oxygen, krypton and xenon mixed gas, a sieve tray type tower or a rotary-vane membrane type tower and a general Raschig ring packed tower are usually adopted in a low-temperature rectifying tower part; the oxygen removing part of the krypton fraction adopts active copper and a common oxygen removing catalyst; purification of the xenon fraction by Adsorption to remove CO2And H2O, then removing H by rectification2，N2Kr or removal of Kr, H by adsorption2，N2And xenon purifiers and adsorption processes; the temperature of the condenser at the top of the second rectifying tower is controlled by adopting ethanol and dry ice or liquid nitrogen as cooling media, and the ethanol and the dry ice or the liquid nitrogen are added manually. The disadvantages of the above-mentioned parts are respectively the low separation efficiency and the large increase in the viscous flowThe balance time, the allowable upper and lower limit amplitude of the ascending air flow are small, and the operation is troublesome; the oxygen removal capacity of the oxygen removal furnace is small, and each time of treatment is 15m3After oxygen in the krypton fraction is subjected to hydrogenation reduction activation, a large amount of high-purity nitrogen is required to replace the surface hydrogen, hydrogen pollution still occurs, and the hydrogen content in the krypton product reaches 2-3 ppm; the adsorption method has low treatment capacity, complicated flow, inconvenient operation and low xenon extraction rate; the manual cooling mode is achieved, the intensity of an operator is high, and the temperature is not easy to control.
The invention aims to provide a method which has high extraction rate of krypton and xenon and is easy to operate in view of the defects.
The technical points of the invention are as follows: the mixed gas containing Kr-Xe components with the concentration of more than 18 percent is used as the raw material of the invention to extract krypton products and xenon products with the purity of 99.995 percent or higher. The mixed gas of krypton-xenon with oxygen concentration of above 18% also contains CH4，N2，CO，CO2And N2Impurities such as O and the like form the whole production process flow according to different properties of the components of the impurities, and are shown in figure 1. The feed gas is 10-15 m3The flow rate of the material is charged to 50m3The production is carried out intermittently, firstly CH in the raw material gas is added4Removing CH by methane removal furnace (1)4Adding O2Generation of CO by separation2And H2O, to CH4Down to less than 1ppm and CO2And H2O is adsorbed and removed by a molecular sieve adsorber (2) to 1ppm or less. Feeding the mixed gas into a first low-temperature rectifying tower (3), operating under the pressure of 0.3-0.5 MPa, condensing the fed mixed gas by using liquid oxygen as a cooling medium by using a tower top condenser, discharging an oxygen fraction from the tower top until the feeding is finished, then performing total reflux operation, using an electric heater or heated nitrogen as a heat source at a tower bottom to ensure that the ascending steam flow of the material reaches a stable operation state, and then continuously discharging the oxygen fraction, wherein the oxygen fraction is used as O when the content of krypton components is increased to more than 0.1% to 99.9%2-the Kr fraction is sent to a storage tank (4). More than 99.9 percent of krypton is krypton fraction, oxygen-removing impurities in the oxygen-removing furnace (5) reach less than 1ppm, and the krypton product gas is used as krypton product gas to be filled in a product bottle, so that the production of krypton products is finished. When in useWhen the concentration of xenon contained in the krypton fraction discharged from the tower top is more than 20ppm and 97%, the xenon-xenon fraction is used as Kr-Xe fraction and sent to a storage tank (6) to be used as the raw material for the next operation, and the discharge is stopped to finish the operation of the first rectifying tower, namely the material stored in the towerThe xenon fraction containing impurities of about Kr, O is fed to a storage tank (12) for storage and metering2，N2，CH4，CO2And N2O, etc. are introduced into a front-end xenon purifier (7) to lead the O to2，N2，CH4，CO2And N2Removing O to reach the specified content of the product, feeding the product into a pre-cooled second low-temperature rectifying tower (8), performing total reflux operation and keeping the tower pressure at 0.2-0.3 MPa, using ethanol and liquid nitrogen as a cooling medium to form an automatic temperature control system (10) by a tower top condenser, heating a tower bottom by nitrogen to reach a stable operation state, intermittently discharging impurities such as krypton at the tower top, and feeding the discharged impurities into a storage tank (9) for storage, stopping discharging and operating when the content of krypton in the discharged materials at the tower top is below 100ppm or lower according to requirements, wherein the materials in the tower are xenon products, and feeding the xenon products into a storage tank (11) and then respectively filling into product bottles to complete the production of xenon products. E.g. N in xenon fractions2When the impurities such as O are very little, a terminal xenon purifier can be used for the treatment as shown in the flow chart (2). It uses mixed gas containing Kr-Xe component whose concentration is above 18% as raw material, and is characterized by that the raw material gas can be passedthrough methane-removing furnace (1) to produce CO2And H2O, removal of CH4Less than 1ppm, adsorbing CO by molecular sieve adsorber (2)2And H2O, each in an amount of 1ppm or less, O2The mixed gas of-Kr-Xr enters a low-temperature rectifying tower (3) to convert O2The Kr and Xe are separated respectively, when the Kr contains O2When the concentration is below 1000ppm, the oxygen removal protector (5) is used to reduce the concentration to below 1ppm, the obtained high-purity krypton product is filled into a product bottle, and when Xe contains less than 3 percent of krypton and other impurities, Kr, O are treated by a xenon purifier (7), a low-temperature rectifying tower (8) and an automatic tower top temperature control system (10)2，N2，CH4And N2Removing O and the like to obtain a high-purity xenon product, and filling the high-purity xenon product into a product bottle.
Compared with the prior art, the stainless steel wire mesh for efficient separation is corrugated and regularCompared with the Dixon ring packing, the packing and the Dixon ring packing have the advantages that under the same tower height condition, the separation efficiency is obviously high, the oxygen content in krypton fractions can reach 10-20 ppm, meanwhile, the stagnation quantity is small, the balance time can be shortened, the allowable upper and lower limit amplitude of ascending steam flow is large, the operation is easy, and therefore the extraction rate of products is improved. Adopts a high-efficiency large-capacity deoxidization furnace and can treat 300m3The krypton fraction gas is subjected to hydrogen reduction activation, so that the operation is simplified, a large amount of high-purity nitrogen is saved, the hydrogen pollution to krypton products is avoided more importantly, and the quality of the krypton products is ensured. The xenon purifier and the low-temperature rectification method solve the defects in the prior art, can treat a large amount of xenon distillate, and have wider permission on the content of krypton components to achieve higher extraction rate. Ethanol and liquid nitrogen are taken as cooling media, a set of constant-temperature automatic control system is adopted, a temperature sensor at the top of the tower is used, so that the operation requirement is set to be-76 to-82 ℃ to give a specified temperature signal, the signal is sent to an automatic liquid nitrogen discharge valve, the opening and closing degree of the valve is controlled to give different liquid nitrogen amounts, and the specified constant-temperature condition is achieved, so that the automation is realized, the operation is improved, the freezing tower accident (the difference between the boiling point and the freezing point of xenon is 3 ℃) is reduced or avoided, and the extraction rate is improved.
The invention simplifies the production process flow, facilitates the operation, and improves the reliability of the product quality and the extraction rate of the product. The attached drawing is a process flow chart of the invention.
The double rectifying towers adopt packed towers for high-efficiency separation; the oxygen impurity in the krypton fraction is removed by adopting a large-capacity oxygen removal furnace of a high-efficiency oxygen removal catalyst, and the oxygen removal is less than 1 ppm; the purification of the impurities in the xenon fraction adopts a xenon purifier and a rectifying tower, and the impurities are completely removed to meet the specified requirements; the constant temperature of the second low-temperature rectifying tower top condenser adopts ethanol and liquid nitrogen as cooling media, and a condenser temperature sensor liquid nitrogen tank and a liquid nitrogen automatic regulating valve form an automatic temperature control system.
Example 1
The raw material gas composition is as follows: o is264.6 percent of the total weight of the raw materials, and 34 percent of the total weight of the raw materials Kr; xe 1.38%, impurity content: CH (CH)4＜100ppm；N2～50ppm；CO2～5ppm；N2O～10ppm；
The feed rate was 25M3Passing through a methane removal furnace rear CH4Less than 1ppm, CO after passage through the adsorber2＜1ppm，H2O is less than 1ppm, and the krypton fraction discharged from the top of the first rectifying tower contains O210000ppm starting until the Xe content increases to 20ppm, O after passing through an oxygen removal furnace2Less than 1ppm, the composition of the krypton product is as follows:
kr is more than or equal to 99.995 percent and the impurity content is ppm
| Xe | O2 | N2 | CH4 | CO2 | H2 | H2O |
| 17 | 3 | 5 | 1 | 1 | 1 | 3 |
The krypton product amount is 7.148m3
Composition of xenon fractions: k1～2％，N2O～100ppm，O2～3ppm，
N2～5ppm，CH4～1ppm，CO2～1ppm
The feed amount is 346L, the feed enters a second rectifying tower after passing through a front-end xenon purifier, discontinuous discharge is carried out on the tower top until the content of krypton components is 60ppm, and the composition of xenon products is as follows:
xe is more than or equal to 99.995 percent and has impurity content ppm
| Kr | O2 | N2 | CH4 | CO2 | N2O | H2 | H2O |
| 17 | 3 | 5 | 1 | 1 | 0.2 | 1 | 3 |
The xenon yield was 300.2L
The extraction rate of krypton products is about 87.27%; the xenon product extraction was about 86.76%.
Example 2
The raw material gas composition is as follows: o is2～71.45％，Kr～26.8％，Xe～1.75％；
Impurity content: CH (CH)4＜100ppm；N2～30ppm；CO2～4ppm；N2O～6ppm；
The feed rate was 47.5M3Passing through a methane removal furnace rear CH43ppm, CO after passage through the adsorber2＜1ppm，H2O is less than 1ppm, and the krypton fraction discharged from the top of the first rectifying tower contains O21000ppm starting until the Xe content increases to 5ppm, where CH4Less than 1ppm, O after passing through an oxygen removal furnace2Less than 1ppm, the composition of the krypton product is as follows:
kr is more than or equal to 99.998 percent and the content of impurities is ppm
| Xe | O2 | N2 | CH4 | CO2 | H2 | H2O |
| 5 | 1 | 5 | 1 | 1 | 1 | 3 |
Krypton product amount of 11.46m3
Composition of xenon fractions: kr-1%, N2O～40ppm，O2～3ppm，
N2～7ppm，CH4～1ppm，CO2～1ppm
The feed amount is 829.3L, the feed enters a second rectifying tower after passing through a front-end xenon purifier, the discharge is interrupted at the tower top until the content of krypton components is 20ppm, and the composition of xenon products is as follows:
xe is more than or equal to 99.998 percent and the content of impurities is ppm
The extraction rate of the krypton product is about 90 percent when the xenon product amount is 746.3L; the xenon product extraction rate is about 90%.
| Kr | O2 | N2 | CH4 | CO2 | N2O | H2 | H2O |
| 5 | 1 | 3 | 1 | 1 | 0.2 | 1 | 3 |
Claims (5)
1. A method for extracting high-purity krypton and xenon from mixed gas of oxygen, krypton and xenon is characterized in that the mixed gas containing Kr-Xe components with the concentration of more than 18 percent is used as a raw material, and the raw material gas is passed through a methane removing furnace (1) to generate CO2And H2O, except CH4Less than 1ppm, adsorbing CO by molecular sieve adsorber (2)2And H2O, eachin an amount of 1ppm or less, O2The mixed gas of-Kr-Xr enters a low-temperature rectifying tower (3) to convert O2The Kr and Xe are separated respectively, when the Kr contains O2When the concentration is below 1000ppm, the oxygen removing furnace (5) is used for removing 1ppm or less to obtain high-purity krypton products, the high-purity krypton products are filled into a product bottle, and when Xe contains less than 3 percent of krypton and other impurities, Kr and O are removed through a xenon purifier (7), a low-temperature rectifying tower (8) and an automatic tower top temperature control system (10)2，N2，CH4And N2Removing O and the like to obtain a high-purity xenon product, and filling the high-purity xenon product into a product bottle.
2. The method of claim 1, wherein the double rectification columns each employ a packed column for high efficiency separation.
3. The process of claim 1 wherein the oxygen impurities in the krypton fraction are removed in a large capacity oxygen removal furnace using a high efficiency oxygen removal catalyst to remove oxygen to less than 1 ppm.
4. The method of claim 1, wherein the impurities in the xenon fraction are purified using a xenon purifier and a rectification column, and the total removal of the impurities is carried out to a specified level.
5. The method according to claim 1, wherein the constant temperature of the top condenser of the second cryogenic rectification tower is controlled by using ethanol and liquid nitrogen as cooling media, and an automatic temperature control system is formed by a condenser temperature sensor, a liquid nitrogen tank and an automatic liquid nitrogen regulating valve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97103252A CN1085188C (en) | 1997-04-17 | 1997-04-17 | Method for extracting high-purity krypton, xenon from mixed gas containing oxygen, krypton, xenon. |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97103252A CN1085188C (en) | 1997-04-17 | 1997-04-17 | Method for extracting high-purity krypton, xenon from mixed gas containing oxygen, krypton, xenon. |
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| Publication Number | Publication Date |
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| CN1196331A true CN1196331A (en) | 1998-10-21 |
| CN1085188C CN1085188C (en) | 2002-05-22 |
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| CN97103252A Expired - Fee Related CN1085188C (en) | 1997-04-17 | 1997-04-17 | Method for extracting high-purity krypton, xenon from mixed gas containing oxygen, krypton, xenon. |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1329101C (en) * | 2001-11-19 | 2007-08-01 | 气体产品与化学公司 | Method and adsorbent for recovering kryptsn and xenon from gas stream or liquid stream |
| CN101636627B (en) * | 2007-01-16 | 2011-09-07 | 乔治洛德方法研究和开发液化空气有限公司 | Separation method using a column with a corrugated cross structure packing for separating a gaseous mixture |
| CN102389683A (en) * | 2011-08-15 | 2012-03-28 | 西北核技术研究所 | Method and device for separating krypton from xenon by using active carbon |
| CN101905884B (en) * | 2006-04-03 | 2013-06-12 | 乔治洛德方法研究和开发液化空气有限公司 | Device and method for packaging dry ice in a plastic film |
| CN104310325A (en) * | 2014-10-24 | 2015-01-28 | 武汉钢铁(集团)公司 | Krypton-xenon gas purification method and device |
| CN108609591A (en) * | 2018-04-27 | 2018-10-02 | 南京特种气体厂股份有限公司 | The removing means and removal methods of trace methane in a kind of krypton xenon gaseous mixture |
| CN111874881A (en) * | 2019-06-27 | 2020-11-03 | 南京工业大学 | Method for purifying xenon by using DD3R molecular sieve membrane |
| CN112557157A (en) * | 2021-02-28 | 2021-03-26 | 中国工程物理研究院核物理与化学研究所 | Method for separating, purifying and collecting xenon in air sample based on specific device |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1011200B (en) * | 1987-04-13 | 1991-01-16 | 中国科学院大连化学物理研究所 | Technological process equipment for purifying xenon |
| JP3256811B2 (en) * | 1992-04-15 | 2002-02-18 | 日本酸素株式会社 | Method for purifying krypton and xenon |
| JP3245788B2 (en) * | 1995-08-31 | 2002-01-15 | 日本電信電話株式会社 | Mobile terminal contract information caching method |
-
1997
- 1997-04-17 CN CN97103252A patent/CN1085188C/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1329101C (en) * | 2001-11-19 | 2007-08-01 | 气体产品与化学公司 | Method and adsorbent for recovering kryptsn and xenon from gas stream or liquid stream |
| CN101905884B (en) * | 2006-04-03 | 2013-06-12 | 乔治洛德方法研究和开发液化空气有限公司 | Device and method for packaging dry ice in a plastic film |
| CN101636627B (en) * | 2007-01-16 | 2011-09-07 | 乔治洛德方法研究和开发液化空气有限公司 | Separation method using a column with a corrugated cross structure packing for separating a gaseous mixture |
| CN102389683A (en) * | 2011-08-15 | 2012-03-28 | 西北核技术研究所 | Method and device for separating krypton from xenon by using active carbon |
| CN102389683B (en) * | 2011-08-15 | 2014-05-28 | 西北核技术研究所 | Method and device for separating krypton from xenon by using active carbon |
| CN104310325A (en) * | 2014-10-24 | 2015-01-28 | 武汉钢铁(集团)公司 | Krypton-xenon gas purification method and device |
| CN104310325B (en) * | 2014-10-24 | 2016-06-29 | 武汉钢铁(集团)公司 | Krypton, xenon-133 gas purification method and device |
| CN108609591A (en) * | 2018-04-27 | 2018-10-02 | 南京特种气体厂股份有限公司 | The removing means and removal methods of trace methane in a kind of krypton xenon gaseous mixture |
| CN111874881A (en) * | 2019-06-27 | 2020-11-03 | 南京工业大学 | Method for purifying xenon by using DD3R molecular sieve membrane |
| CN112557157A (en) * | 2021-02-28 | 2021-03-26 | 中国工程物理研究院核物理与化学研究所 | Method for separating, purifying and collecting xenon in air sample based on specific device |
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| Publication number | Publication date |
|---|---|
| CN1085188C (en) | 2002-05-22 |
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