CN201438068U - Device for preparing pure krypton and pure xenon through full rectification - Google Patents
Device for preparing pure krypton and pure xenon through full rectification Download PDFInfo
- Publication number
- CN201438068U CN201438068U CN 200920207828 CN200920207828U CN201438068U CN 201438068 U CN201438068 U CN 201438068U CN 200920207828 CN200920207828 CN 200920207828 CN 200920207828 U CN200920207828 U CN 200920207828U CN 201438068 U CN201438068 U CN 201438068U
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- CN
- China
- Prior art keywords
- rectifying column
- level
- rectifying
- krypton
- pure
- 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.)
- Expired - Fee Related
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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
- F25J3/04751—Producing pure krypton and/or xenon recovered from a crude krypton/xenon mixture
-
- 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
- F25J2220/00—Processes or apparatus involving steps for the removal of impurities
- F25J2220/02—Separating impurities in general from the feed stream
-
- 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
- F25J2245/00—Processes or apparatus involving steps for recycling of process streams
- F25J2245/42—Processes or apparatus involving steps for recycling of process streams the recycled stream being nitrogen
Abstract
The utility model relates to a device for preparing pure krypton and pure xenon through full rectification. The device comprises a liquid pump and seven levels of rectifying towers, wherein the bottom of a first level rectifying tower is connected with the interior of a second level rectifying tower; the bottom of the second level rectifying tower is connected with the interior of a third level rectifying tower; the bottom of the third level rectifying tower is connected with the interior of a fourth level rectifying tower; the top of the fourth level rectifying tower is connected with a fifth level rectifying tower, and the bottom thereof is connected with a sixth level rectifying tower; the top of the sixth level rectifying tower is connected with a seventh level rectifying tower; and a condensing evaporator and an electric heater are arranged at the top and the bottom of each level of rectifying tower respectively. Compared with the prior art, the utility model has the advantages of high yield, simple installation, wide application range, etc.
Description
Technical field
The utility model relates to the preparation method of a kind of high purity krypton and xenon, especially relates to the device that a kind of full rectifying prepares pure krypton and pure xenon.
Background technology
Krypton in the atmosphere and xenon content are about 1.138 * 10 respectively
-6With 0.0857 * 10
-6After trace krypton and xenon enter the low-temperature fractionating tower of air-separating plant with air, high boiling component krypton, xenon, hydrocarbon (mainly being methane) and fluoride all accumulate in the liquid oxygen of lower pressure column, and the liquid oxygen of lower pressure column is sent into a krypton additional rectification column (being commonly called as a krypton tower).Can obtain the poor krypton-xenon concentrate that krypton xenon content is 0.2～0.3%Kr+Xe, wherein methane content is about 0.3～0.4%.Methane content is too high in the oxygen (generally is no more than 0.5%CH
4) be extremely dangerous, after having only the methane that removes in advance in the poor krypton-xenon concentrate, just might continue to improve the krypton xenon concentration in the liquid oxygen, in known method, at first poor krypton-xenon concentrate is pressurized to 5.5MPa and makes its vaporization, enter the methane purification devices behind the 1.0MPa that reduces pressure again.The methane purification devices is by palladium catalyst, and under 480～500 ℃ temperature, oxygen and methane carry out behind the chemical reaction methane and is removed that (remaining methane content can be lower than 1 * 10
-6), remove chemical reaction product-carbon dioxide and water with molecular sieve adsorption then.Along with the krypton xenon concentrates step by step, methane content improves again thereupon, and therefore this chemical reaction removes methane and also will repeatedly carry out.
Remove methane in the poor krypton-xenon liquid in the prior art, by heat exchange, be heated to high temperature (500 ℃) under the effect of palladium catalyst, the catalytic methane burning generates carbon dioxide and water, molecular sieve purifier is set then adsorbs these product, this technology energy consumption is big, and (low temperature-170 ℃ is heated to 500 ℃, heat exchange lower the temperature again to-160 ℃), gas loss reaches 2% during through molecular sieve purifier, will directly have influence on the recovery rate of pure krypton and/or pure xenon.
Micro-fluoride in the poor krypton-xenon concentrate belongs to high boiling component.In the separation process of krypton xenon, will accumulate in pure krypton and the pure xenon.In known method, be to pass through activated zr aluminium getter respectively, under 700 ℃ of temperature, remove the foreign gas fluoride.
The known technology of producing pure krypton and pure xenon has following shortcoming:
(1) will consume a large amount of electric energy and precious metal (palldium alloy) and make catalyst, activated zr aluminium getter is to belong to consuming goods and materials, needs periodic replacement.
(2) device that adopts chemical reaction method to remove methane moves dangerous and will lose a part of krypton and xenon, simultaneously because process route is long, and equipment is many, reveals also increase thereupon of loss.Therefore the rate of recovery of krypton and xenon is lower, generally is no more than 60～63%.
(3) equipment and valve are many, inconvenient operation, and can not move continuously.
Summary of the invention
The purpose of this utility model is exactly to provide a kind of yield height, device full rectifying simple, applied range to prepare the device of pure krypton and pure xenon for the defective that overcomes above-mentioned prior art existence.
The purpose of this utility model can be achieved through the following technical solutions: a kind of full rectifying prepares the device of pure krypton and pure xenon, it is characterized in that, this device comprises liquid pump and seven grades of rectifying columns, wherein first order rectifier bottoms connects second level rectifying column, second level rectifier bottoms connects third level rectifying column, third level rectifier bottoms connects fourth stage rectifying column, fourth stage rectifying column top connects the level V rectifying column, the bottom connects the 6th grade of rectifying column, the 6th grade of rectifying column top connects the 7th grade of rectifying column, rectifying columns at different levels top is equipped with a condenser/evaporator, and the bottom is equipped with an electric heater.
The condenser/evaporator inlet at described first order rectifying column and rectifying column top, the second level is connected the liquid nitrogen cryogenics storage tank.
The condenser/evaporator inlet of described third level rectifying column connects rectifying column top, the second level.
The inlet of described fourth stage rectifying column, level V rectifying column, the 6th grade of rectifying column and the condenser/evaporator of the 7th grade of rectifying column is connected the condenser/evaporator outlet at first order rectifying column and rectifying column top, the second level respectively.
The condenser/evaporator outlet of described seven grades of rectifying column cats head all connects air-separating plant.
Described seven grades of rectifying columns, the cryogenic pipelines and the valve that connect between each rectifying column all wrap in the ice chest that is filled with heat-insulating material.
Described heat-insulating material comprises super glass wool or expanded perlite etc.
Compared with prior art, the utlity model has following advantage:
(1) rate of recovery height of krypton and xenon can reach more than 95%.
(2) the utility model adopts and fills inert gas such as N
2, Ar etc. goes out tower with replacement of oxygen, avoided methane aggregate concentration in liquid oxygen too high (surpassing 0.5%) in the actual production process and set off an explosion may, can thoroughly remove methane in the krypton xenon pre-concentration stage simultaneously.By rectifying step by step, remove all the low boiling component (O in the poor krypton xenon unstripped gas again
2, N
2, Ar) and high boiling component hydrocarbon (CH
4, C
2H
4, C
2H
6, C
3H
8) and fluoride (CF
4, C
2F
6, SF
6) finally obtain purity and be higher than 99.999% pure krypton and pure xenon product, wherein various impurity contents all are lower than high-purity krypton technical indicator of GB/T5829-2006 and the high-purity xenon technical indicator of GB/T5828-2006.
(3) this technological process simple, good in economic efficiency, improved the device operational safety performance, simple to operate, saved equipment investment expense and energy resource consumption.
(4) applied range, after the user was provided with poor krypton-xenon liquid oxygen and liquid nitrogen cryogenics storage tank, the utility model device can break away from air-separating plant, independent operating.Also can use by supporting existing air separation plant, realize the continuous and stable production operation.
Description of drawings
Fig. 1 is a flow chart of the present utility model.
The specific embodiment
Below in conjunction with the drawings and specific embodiments the utility model is elaborated.
Embodiment
Be a device flow chart that is used for separating poor krypton-xenon concentrate as shown in Figure 1.
Device comprises liquid pump 16, seven grades of rectifying columns, first order rectifying column 1 bottom is connected in the second level rectifying column 2, rectifying column 2 bottoms in the second level are connected in the third level rectifying column 3, third level rectifying column 3 bottoms are connected in the fourth stage rectifying column 4, fourth stage rectifying column 4 tops are connected in the level V rectifying column 5, and the bottom is connected in the 6th grade of rectifying column 6, and the 6th grade of rectifying column 6 tops connect the 7th grade of rectifying column 7.Rectifying columns at different levels top is equipped with a condenser/evaporator, the bottom is equipped with an electric heater, electric heater 8 is used in first order rectifying column 1 bottom, electric heater 9 is used in rectifying column 2 bottoms in the second level, electric heater 10 is used in third level rectifying column 3 bottoms, and electric heater 11 is used in fourth stage rectifying column 4 bottoms, and electric heater 12 is used in level V rectifying column 5 bottoms, the 6th grade of rectifying column 6 bottoms use 13, the seven grades of rectifying column 7 bottoms of electric heater to use electric heater 14.The condenser/evaporator inlet at first order rectifying column 1 and second level rectifying column 2 tops is connected the liquid nitrogen cryogenics storage tank, and the condenser/evaporator outlet connects the condenser/evaporator of other rectifying columns respectively.
First order rectifying column 1 and second level rectifying column 2 top condenser/evaporators all adopt liquid-nitrogen boiling, and the interior temperature of control tower is-190 ℃～-130 ℃ and carries out rectifying, makes the interior rising steam of tower be condensed into phegma, thereby sets up the rectifying operating mode.The nitrogen that the condenser/evaporator of other rectifying column adopts first order rectifying column 1 and second level rectifying column 2 tops to discharge, temperature is-180 ℃, make low-temperature receiver with the band normal pressure and temperature nitrogen mixture gas that closes on air-separating plant and provide, temperature is controlled at-130～-70 ℃, under this temperature, can avoid the krypton xenon crystallization in the steam in the tower, can form the phegma of the needs of rectifying operating mode in the tower simultaneously again.
The utility model is filled inert gas combustion-supporting gas oxygen is diluted separation under cryogenic conditions, avoid the too high possibility that sets off an explosion of methane concentration, by rectifying step by step, utilizes hydrocarbon (CnHm), fluoride (CF
4, C
2F
6, SF
6), krypton, xenon boiling point difference separately, separate impurities successively, under the prerequisite that keeps high extraction (being not less than 90%), production purity is higher than 99.999% pure krypton and pure xenon product.Extract from liquid oxygen that poor krypton xenon, methane are removed, the krypton xenon concentrates, high-purity krypton and or high-purity xenon realized full rectifying operating mode, reduced energy consumption and product loss.
With 200Nm
3The molar content of krypton is 0.1429% in the poor krypton-xenon concentrate 15 of/h, and the molar content of xenon is 0.012%, and hydrocarbon and fluoride total content are 0.5098% poor krypton-xenon concentrate 15, after nitrogen, methane separation tower, obtains methane content 0.2 * 10
-6, the krypton-xenon liquid of krypton content 92%, the krypton xenon is purified high-boiling-point impurity (C step by step through separating
2F
6, C
2H
4, C
2H
6, C
3H
8, N
2O, SF
6) the tower still removes in the 6th grade of rectifying column 6.Low boiling impurity SF
4In level V rectifying column 5, remove CF in level V rectifying column 5 tower base streams 43
4Molar content is 0.3%.Obtaining the pure krypton flow of product is 0.28Nm
3The molar content of/h krypton is 0.9999998, CH
4Molar content is 0.2 * 10
-6The 7th grade of pure xenon flow in rectifying column 7 bottoms is about 0.024Nm
3/ h, the molar content of xenon is 0.9999996.
Separating the concrete grammar of poor krypton-xenon concentrate implements as follows.
The poor krypton-xenon concentrate 15 that the additional tower of air separation unit krypton is produced through entering first order rectifying column 1 with liquid form 17 after 16 superchargings of liquid pump, is filled about 1000Nm in first order rectifying column 1
3/ h low temperature inert nitrogen gas 18 replace oxygen utilize them to have different relative volatilities, and oxygen separation, high boiling krypton xenon, all the other impurity are all drawn from the tower still of first order rectifying column 1 with liquid form 38 and entered next rectification cell second level rectifying column 2.The krypton xenon is all drawn from the tower still in the first order rectifying column 1, owing to the too high problem that has potential safety hazard of methane concentration has been avoided in the existence of inert gas.
Lower boiling nitrogen, oxygen and a spot of methane are discharged through cryogenic pipelines 21 from cat head in the second level rectifying column 2, it is 10～30% krypton xenon concentrate 39 that the tower still obtains molar concentration, and this krypton xenon concentrate 39 is drawn from the tower still with the form of liquid and entered next rectification cell third level rectifying column 3.Rectifying column 2 bottom krypton xenons in the second level are further purified, and nitrogen oxygen is separated.
Krypton xenon concentrate 39 is sent in the third level rectifying column 3, volatile components methane is removed, the tower still obtains molar concentration and is not less than 90% krypton xenon concentrate 40, and overhead stream 22 is a methane.
Krypton xenon concentrate 40 is sent in the fourth stage rectifying column 4, and the tower still obtains containing xenon concentrate 41, and cat head obtains containing krypton concentrate 23; Contain that key component is Xe in the xenon concentrate 41, molar content is not less than 99%, and major impurity has C
2H
4, CF
4, C
2F
6, SF
6Impurity Deng higher boiling; Contain that key component is Kr in the krypton concentrate 23, molar content is not less than 99.99%.Major impurity is CH
4, CF
4
To contain krypton concentrate 23 and send in the level V rectifying column 5, and obtain the pure krypton 24 of product fluid at cat head, wherein the molar content of Kr is not less than 99.999%, CH
4Molar content be no more than 0.3 * 10
-6, CF
4At the bottom of tower, discharge collection.
To contain xenon concentrate 41 and send in the 6th grade of rectifying column 6, and obtain containing xenon fluid 26 at cat head, wherein the molar content of Xe is not less than 99.5%, CF
4Molar content be not higher than 170 * 10
-6, impurity C
2H
4Molar content be no more than 1 * 10
-6, C
2F
6, SF
6, CH
4, C
3H
8, N
2O, C
2H
6Cryogenic pipelines 42 is discharged and is collected at the bottom of the tower.
To contain xenon fluid 26 and send in the 7th grade of rectifying column 7, and obtain liquid pure xenon 44 at the bottom of tower, wherein the molar content of Xe is not less than 99.999%, impurity C
2H
4Molar content be no more than 1 * 10
-6, and contain CF in the xenon fluid 26
4Will be at cat head along with fluid is discharged from collection along cryogenic pipelines 25.
First order rectifying column 1 and second level rectifying column 2 low-temperature receivers are selected liquid nitrogen 19 for use, liquid nitrogen 28, emit the cryogenic nitrogen 27 of latent heat, cryogenic nitrogen 29 and first order rectifying column 1 and second level rectifying column 2 separated nitrogen and nitrogen oxygen atmosphere compile by cryogenic pipelines 20 and cryogenic pipelines 21 respectively, form gaseous mixture by adding normal temperature nitrogen, respectively by cryogenic pipelines 33, cryogenic pipelines 37, cryogenic pipelines 34 is as fourth stage rectifying column 4, level V rectifying column 5, low-temperature receiver with the 6th grade of rectifying column 6, third level rectifying column 3 low-temperature receivers use second level rectifying column 2 overhead stream portion gas along cryogenic pipelines 30 inputs, discharge from cryogenic pipelines 31.
After converging, the nitrogen that all condenser/evaporators are discharged or oxygen-nitrogen mixed gas all return air-separating plant, the nitrogen or the oxygen-nitrogen mixed gas of discharging as the condenser/evaporator at fourth stage rectifying column 4 tops drain into air-separating plant by cryogenic pipelines 32, nitrogen or oxygen-nitrogen mixed gas that the condenser/evaporator at level V rectifying column 5 tops is discharged drain into air-separating plant by cryogenic pipelines 36, and nitrogen or oxygen-nitrogen mixed gas that the condenser/evaporator at the 7th grade of rectifying column 7 tops is discharged drain into air-separating plant by cryogenic pipelines 35.
All rectifying columns, cryogenic pipelines and valve all wrap in the ice chest that is filled with heat-insulating material such as super glass wool, expanded perlite etc.
Claims (6)
1. a full rectifying prepares the device of pure krypton and pure xenon, it is characterized in that, this device comprises liquid pump and seven grades of rectifying columns, wherein first order rectifier bottoms connects second level rectifying column, second level rectifier bottoms connects third level rectifying column, third level rectifier bottoms connects fourth stage rectifying column, fourth stage rectifying column top connects the level V rectifying column, the bottom connects the 6th grade of rectifying column, the 6th grade of rectifying column top connects the 7th grade of rectifying column, rectifying columns at different levels top is equipped with a condenser/evaporator, and the bottom is equipped with an electric heater.
2. a kind of full rectifying according to claim 1 prepares the device of pure krypton and pure xenon, it is characterized in that, the condenser/evaporator inlet at described first order rectifying column and rectifying column top, the second level is connected the liquid nitrogen cryogenics storage tank.
3. a kind of full rectifying according to claim 1 prepares the device of pure krypton and pure xenon, it is characterized in that, the condenser/evaporator inlet of described preceding third level rectifying column connects rectifying column top, the second level.
4. a kind of full rectifying according to claim 1 prepares the device of pure krypton and pure xenon, it is characterized in that the inlet of described fourth stage rectifying column, level V rectifying column, the 6th grade of rectifying column and the condenser/evaporator of the 7th grade of rectifying column is connected the condenser/evaporator outlet at first order rectifying column and rectifying column top, the second level respectively.
5. a kind of full rectifying according to claim 1 prepares the device of pure krypton and pure xenon, it is characterized in that, the condenser/evaporator outlet of described seven grades of rectifying column cats head all connects air-separating plant.
6. a kind of full rectifying according to claim 1 prepares the device of pure krypton and pure xenon, it is characterized in that, described seven grades of rectifying columns, the cryogenic pipelines and the valve that connect between each rectifying column all wrap in the ice chest that is filled with heat-insulating material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200920207828 CN201438068U (en) | 2009-08-13 | 2009-08-13 | Device for preparing pure krypton and pure xenon through full rectification |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200920207828 CN201438068U (en) | 2009-08-13 | 2009-08-13 | Device for preparing pure krypton and pure xenon through full rectification |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN201438068U true CN201438068U (en) | 2010-04-14 |
Family
ID=42400042
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200920207828 Expired - Fee Related CN201438068U (en) | 2009-08-13 | 2009-08-13 | Device for preparing pure krypton and pure xenon through full rectification |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN201438068U (en) |
-
2009
- 2009-08-13 CN CN 200920207828 patent/CN201438068U/en not_active Expired - Fee Related
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 201203, room 1, building 88, 402 Darwin Road, Zhangjiang hi tech park, Shanghai Co-patentee after: Shanghai Qiyuan Air Separation Technology Development Co., Ltd. Patentee after: Shanghai Qiyuan Science & Technology Development Co., Ltd. Address before: 201203, room 1, building 88, 402 Darwin Road, Zhangjiang hi tech park, Shanghai Co-patentee before: Shanghai Qiyuan Air Separation Technology Development Co., Ltd. Patentee before: Shanghai Qiyuan Science & Technology Development Co., Ltd. |
|
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20100414 Termination date: 20170813 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |