CN101726158A - Method for removing oxygen and methane from concentrated krypton-xenon liquid - Google Patents
Method for removing oxygen and methane from concentrated krypton-xenon liquid Download PDFInfo
- Publication number
- CN101726158A CN101726158A CN200910198685A CN200910198685A CN101726158A CN 101726158 A CN101726158 A CN 101726158A CN 200910198685 A CN200910198685 A CN 200910198685A CN 200910198685 A CN200910198685 A CN 200910198685A CN 101726158 A CN101726158 A CN 101726158A
- Authority
- CN
- China
- Prior art keywords
- methane
- krypton
- xenon
- tower
- liquid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Mechanical Engineering (AREA)
- Thermal Sciences (AREA)
- General Engineering & Computer Science (AREA)
- Separation By Low-Temperature Treatments (AREA)
Abstract
The invention relates to a method for removing oxygen and methane from concentrated krypton-xenon liquid. The method comprises the following steps of: introducing materials and inert gases into a rectifying tower, wherein the tower top of the rectifying tower is provided with a condensation evaporator, and the tower bottom is heated by electric heating elements or gas; and controlling the amount of ascending gas in the tower, rectifying the raw materials by the rectifying tower, leading concentration solution of krypton-xenon out of the tower bottom, and leading nitrogen gas, oxygen gas and a mixture of methane out of the tower top. Compared with the prior art, the method has the advantages that: low-boiling point inert gases are filled to dilute the oxygen gas on the tower top; the concentration of methane is ensured for safe operation of the device; the recovery rate of krypton-xenon is improved; the nitrogen content in the gas emitted from the tower top is not more than 30ppm; the process flow is simple; the economic benefits are great, the operating safety of the device is improved; the operation is easy; equipment investment cost and energy are saved; and the removal of the methane by adopting the high-temperature chemical catalytic method is avoided.
Description
Technical field
The present invention relates to rare gas purification, purification field, especially relate to a kind of method of from concentrated krypton-xenon liquid, removing oxygen and methane.
Background technology
From the common liquid oxygen of last tower, extract krypton xenon technology, at first liquid oxygen being sent into a krypton tower carries out first time krypton xenon and concentrates, obtain poor krypton-xenon liquid, because methane, krypton, xenon all belong to high boiling material, be difficult to separate, poor krypton-xenon liquid is through the high-temperature catalytic reaction, and methane and oxygen combustion react, enter sieve purification system and remove carbon dioxide and the water that reaction generates, send into low temperature distillation system.Oxygen separation in oxygen-removing tower (two krypton towers) if rectifying is not thorough, or fills in the transportation contaminated, contain 0.2%～1% the oxygen of having an appointment in about 99.5% the krypton-xenon liquid, about 0.1% methane is directly sent into except that the methane system, because the absorption loss, the recovery rate of krypton xenon will be very low.Concentrated krypton-xenon is sent into distillation system, utilize the boiling point difference of krypton, xenon, oxygen, methane, methane and oxygen are from tower top discharge, methane and oxygen proportion are 1: 4 in the concentrated krypton-xenon liquid, methane concentration will reach 20% in the cat head oxygen, surpass 0.5% the highest permission content, directly threaten the safety of krypton xenon separation equipment operation, may cause blast, this is very dangerous.
Summary of the invention
Purpose of the present invention is exactly to provide a kind of krypton xenon rate of recovery, simple, good in economic efficiency method of removing oxygen and methane from concentrated krypton-xenon liquid of technological process of improving for the defective that overcomes above-mentioned prior art existence.
Purpose of the present invention can be achieved through the following technical solutions:
A kind of method of from concentrated krypton-xenon liquid, removing oxygen and methane, it is characterized in that, this method may further comprise the steps: raw material and inert gas are introduced rectifying column, the rectifying column cat head is provided with condenser/evaporator, the tower still adopts electrical heating elements or gas heating, the rising tolerance in the control tower, and raw material is after rectifying column rectifying, krypton xenon concentrate is drawn from the tower still, and nitrogen, oxygen and methane mixture are drawn from cat head.
Described raw material is the poor krypton xenon mixture that contains oxygen and methane, enters rectifying column middle part with liquid or gas form by supercharging of liquid pump or vaporization after supercharging.
Described inert gas comprises nitrogen or nitrogen argon mixture gas, from the rectifying column middle and upper part or the above position of material inlet or introduce rectifying column with the contour position of material inlet.
Described condenser/evaporator adopts liquid nitrogen as low-temperature receiver, makes the interior rising steam of tower be condensed into phegma, and the interior temperature of control tower is-190～-110 ℃ and carries out rectifying.
The molar concentration of krypton xenon is not less than 99.9% in the described krypton xenon concentrate.
Described rectifying column and be connected that cryogenic pipelines and valve wrap in the ice chest that is filled with heat-insulating material super glass wool or expansion pearlite thermal insulation material on the tower.
Compared with prior art, the present invention has the following advantages:
(1) adopt to fill the method dilution cat head oxygen of low boiling inert gas (for example nitrogen, argon gas or its gaseous mixture), the concentration of methane, the control methane concentration is lower than 0.5%, the assurance device safe operation in containing oxygen krypton xenon mixture;
(2) improved the rate of recovery of krypton xenon, krypton content is no more than 30ppm in the gas of top of tower discharging;
(3) make methane thoroughly remove from top of tower, methane content is no more than 0.3ppm in the tower stilling fluid;
(4) technological process simple, good in economic efficiency, improved the device operational safety performance, simple to operate, saved equipment investment expense and energy resource consumption, avoid utilizing once more the high temeperature chemistry catalysis method to remove methane.
Description of drawings
Fig. 1 is the process chart among the embodiment 1;
Fig. 2 is the process chart among the embodiment 2.
1 is that rectifying column, 2 is that inert gas, 3 is that raw material, 4 is that inert gas, 5 is that liquid nitrogen, 6 is that condenser/evaporator, 7 is that nitrogen, oxygen and methane mixture, 8 are that krypton xenon concentrate, 9 is an electrical heating elements among the figure.
The specific embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.
A kind of method of from concentrated krypton-xenon liquid, removing oxygen and methane, its technological process as shown in Figure 1, this method may further comprise the steps: the raw material 3 of the poor krypton xenon mixture of oxygen and methane is entered the middle part of rectifying column 1 with liquid form after by the supercharging of liquid pump, and the flow of raw material 3 is 0.1m
3/ h, the molar content of krypton is 78%, the molar content of xenon is 21.5%, the molar content of oxygen is 0.3%, methane with the fluoride total content be 1150ppm, inert gas 2 is a nitrogen, flow is 0.3m
3/ h introduces in the tower from the middle and upper part of rectifying column 1.The cat head of rectifying column 1 is provided with condenser/evaporator 6, adopts liquid nitrogen 5 as low-temperature receiver, makes the interior rising steam of tower be condensed into phegma, and temperature is carried out rectifying for-190 ℃ in the control tower.Inert gas 4 is a nitrogen, and flow is 0.5m
3/ h introduces in the tower from the tower still of rectifying column 1, and the tower still is provided with electrical heating elements 9, the rising tolerance in the control tower.Raw material 3 is after rectifying column 1 rectifying, and krypton xenon concentrate 8 is drawn from the tower still, and the molar concentration of krypton xenon is 99.9%, and the molar concentration of methane is 0.2 * 10
-6, nitrogen, oxygen and methane mixture 7 are drawn from cat head, and mixture consists of 99% nitrogen, 0.1% oxygen, 0.03% methane.Rectifying column 1 and be connected that cryogenic pipelines and valve wrap in the ice chest that is filled with the super glass wool heat-insulating material on the tower.
A kind of method of from concentrated krypton-xenon liquid, removing oxygen and methane, its technological process as shown in Figure 2, this method may further comprise the steps: the raw material 3 of the poor krypton xenon mixture of oxygen and methane is entered the middle part of rectifying column 1 by vaporization with gas form after supercharging, the flow of raw material 3 is 0.2m
3/ h, the molar content of krypton is 75%, the molar content of xenon is 20%, the molar content of oxygen is 0.3%, methane with the fluoride total content be 1500ppm.The cat head of rectifying column 1 is provided with condenser/evaporator 6, adopts liquid nitrogen 5 as low-temperature receiver, makes the interior rising steam of tower be condensed into phegma, and temperature is carried out rectifying for-110 ℃ in the control tower.Inert gas 4 is the nitrogen argon mixture gas, and flow is 0.4m
3/ h introduces in the tower from the tower still of rectifying column 1, and the tower still adopts gas heating, the rising tolerance in the control tower.Raw material 3 is after rectifying column 1 rectifying, and krypton xenon concentrate 8 is drawn from the tower still, and the molar concentration of krypton xenon is 99.95%, and the molar concentration of methane is 0.1 * 10
-6, nitrogen, oxygen and methane mixture 7 are drawn from cat head, and mixture consists of 99% nitrogen, 0.2% oxygen, 0.1% methane.Rectifying column 1 and be connected that cryogenic pipelines and valve wrap in the ice chest that is filled with the expansion pearlite thermal insulation material on the tower.
Claims (6)
1. method of from concentrated krypton-xenon liquid, removing oxygen and methane, it is characterized in that, this method may further comprise the steps: raw material and inert gas are introduced rectifying column, the rectifying column cat head is provided with condenser/evaporator, the tower still adopts electrical heating elements or gas heating, the rising tolerance in the control tower, and raw material is after rectifying column rectifying, krypton xenon concentrate is drawn from the tower still, and nitrogen, oxygen and methane mixture are drawn from cat head.
2. a kind of method of from concentrated krypton-xenon liquid, removing oxygen and methane according to claim 1, it is characterized in that, described raw material is the poor krypton xenon mixture that contains oxygen and methane, enters rectifying column middle part with liquid or gas form by supercharging of liquid pump or vaporization after supercharging.
3. a kind of method of from concentrated krypton-xenon liquid, removing oxygen and methane according to claim 1, it is characterized in that, described inert gas comprises nitrogen or nitrogen argon mixture gas, from the rectifying column middle and upper part or the above position of material inlet or introduce rectifying column with the contour position of material inlet.
4. a kind of method of from concentrated krypton-xenon liquid, removing oxygen and methane according to claim 1, it is characterized in that, described condenser/evaporator adopts liquid nitrogen as low-temperature receiver, makes the interior rising steam of tower be condensed into phegma, and the interior temperature of control tower is-190～-110 ℃ and carries out rectifying.
5. a kind of method of removing oxygen and methane from concentrated krypton-xenon liquid according to claim 1 is characterized in that the molar concentration of krypton xenon is not less than 99.9% in the described krypton xenon concentrate.
6. a kind of method of from concentrated krypton-xenon liquid, removing oxygen and methane according to claim 1, it is characterized in that described rectifying column and be connected that cryogenic pipelines and valve wrap in the ice chest that is filled with heat-insulating material super glass wool or expansion pearlite thermal insulation material on the tower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101986854A CN101726158B (en) | 2009-11-12 | 2009-11-12 | Method for removing oxygen and methane from concentrated krypton-xenon liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101986854A CN101726158B (en) | 2009-11-12 | 2009-11-12 | Method for removing oxygen and methane from concentrated krypton-xenon liquid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101726158A true CN101726158A (en) | 2010-06-09 |
| CN101726158B CN101726158B (en) | 2011-11-30 |
Family
ID=42447410
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009101986854A Active CN101726158B (en) | 2009-11-12 | 2009-11-12 | Method for removing oxygen and methane from concentrated krypton-xenon liquid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101726158B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103706139A (en) * | 2013-12-29 | 2014-04-09 | 康乃尔化学工业股份有限公司 | Nitrobenzene vaporization distillation mixer |
| CN103712416A (en) * | 2013-12-27 | 2014-04-09 | 上海启元空分技术发展股份有限公司 | Method for controlling power of reboiler of crude krypton and xenon evaporating tower |
| CN108031138A (en) * | 2017-12-14 | 2018-05-15 | 浙江新锐空分设备有限公司 | A kind of krypton xenon concentration tower bottom heat of evaporation source system |
| CN109224491A (en) * | 2018-10-31 | 2019-01-18 | 浙江新锐空分设备有限公司 | Pure krypton xenon tower bottom evaporates heating system in a kind of krypton xenon refining plant |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| LU81226A1 (en) * | 1979-05-04 | 1980-12-16 | Centre Etd Energie Nucleaire | PROCESS FOR EXTRACTING XENON AND / OR KRYPTON FROM A CARRIER GAS |
| DE4332870C2 (en) * | 1993-09-27 | 2003-02-20 | Linde Ag | Method and device for obtaining a krypton / xenon concentrate by low-temperature separation of air |
| DE19855486A1 (en) * | 1998-12-01 | 1999-06-10 | Linde Ag | Extraction of krypton or xenon-rich mixture |
| DE19855485A1 (en) * | 1998-12-01 | 1999-06-10 | Linde Ag | Extraction of krypton or xenon-enriched mixture |
| DE10015605A1 (en) * | 2000-03-29 | 2000-12-07 | Linde Ag | Process and assembly for the production of xenon by cryogenic fractionated distillation of oxygen and xenon |
-
2009
- 2009-11-12 CN CN2009101986854A patent/CN101726158B/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103712416A (en) * | 2013-12-27 | 2014-04-09 | 上海启元空分技术发展股份有限公司 | Method for controlling power of reboiler of crude krypton and xenon evaporating tower |
| CN103712416B (en) * | 2013-12-27 | 2016-06-22 | 上海启元空分技术发展股份有限公司 | The method controlling crude krypton xenon concentration tower reboiler power |
| CN103706139A (en) * | 2013-12-29 | 2014-04-09 | 康乃尔化学工业股份有限公司 | Nitrobenzene vaporization distillation mixer |
| CN108031138A (en) * | 2017-12-14 | 2018-05-15 | 浙江新锐空分设备有限公司 | A kind of krypton xenon concentration tower bottom heat of evaporation source system |
| CN109224491A (en) * | 2018-10-31 | 2019-01-18 | 浙江新锐空分设备有限公司 | Pure krypton xenon tower bottom evaporates heating system in a kind of krypton xenon refining plant |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101726158B (en) | 2011-11-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101407920B (en) | Technique for continuously producing high purity hydrogen by water electrolysis | |
| CN101723338B (en) | Method for extracting krypton-xenon from liquid oxygen | |
| CN101726158B (en) | Method for removing oxygen and methane from concentrated krypton-xenon liquid | |
| CN104654739A (en) | Device and method for preparing food-grade liquid carbon dioxide by rectification and purification with double towers | |
| CN109264674B (en) | Process and system for preparing sulfuric acid by using smelting flue gas | |
| CN103391802A (en) | Compression of a carbon dioxide containing fluid | |
| CN106139890A (en) | Cold-rolled steel sheet heat treatment nitrogen hydrogen mixed tail gas reclaims the apparatus and method purifying | |
| CN105233689B (en) | Organic amine wet flue gas desulphurization and desorption system with high-efficiency and low-energy consumption | |
| CN110171804B (en) | Hydrogen production and purification integrated device and use method | |
| US9206795B2 (en) | Process and apparatus for drying and compressing a CO2-rich stream | |
| CN211716983U (en) | Device for separating and purifying krypton and xenon | |
| CN101634515A (en) | Method for extracting high-yield pure krypton and pure xenon by full distillation | |
| CN101634514B (en) | Method for preparing pure krypton and pure xenon by full distillation | |
| CN201855641U (en) | Device for treating tail gas containing hydrogen chloride | |
| CN101672566B (en) | Method for removing methane in poor krypton-xenon liquid by adopting rectification method | |
| CN111174530A (en) | Method and device for separating and purifying krypton and xenon | |
| CN102952589A (en) | Method for removing acid gas out of raw gas or shifted gas of raw gas | |
| CN215138328U (en) | Tail gas recovery device of methyl ethyl ketone rectifying device | |
| CN201438067U (en) | Device for separating depleted krypton-xenon concentrate | |
| CN104555922A (en) | New technology for producing hydrogen by conversion of methyl alcohol and water vapor | |
| CN101672565A (en) | Method for preparing pure krypton and pure xenon by adopting full rectification | |
| CN213942632U (en) | Tail gas solvent absorbs recovery system | |
| CN101898752B (en) | Method for refining pure krypton and pure xenon from concentrated xenon-krypton liquid | |
| CN201488467U (en) | Full rectification pure krypton and pure xenon extracting device with high yield | |
| CN105776136A (en) | Device and method used for recycling hydrogen from chlor-alkali industry vented tail gas and preparing high purity hydrogen |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20230510 Address after: 201800 rooms 202 and 204, building 3, 150 Heyu Road, Jiading District, Shanghai Patentee after: SHANGHAI QIYUAN GAS DEVELOPMENT Co.,Ltd. Address before: 201203, room 1, building 88, 402 Darwin Road, Zhangjiang hi tech park, Shanghai Patentee before: Shanghai Qiyuan Technology Development Co.,Ltd. Patentee before: SHANGHAI QIYUAN AIR SEPARATE TECHNOLOGY DEVELOPMENT Co.,Ltd. |