CN101857201A - A device for producing high-purity oxygen and krypton-xenon concentrate and its application method - Google Patents
A device for producing high-purity oxygen and krypton-xenon concentrate and its application method Download PDFInfo
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- CN101857201A CN101857201A CN201010190808.2A CN201010190808A CN101857201A CN 101857201 A CN101857201 A CN 101857201A CN 201010190808 A CN201010190808 A CN 201010190808A CN 101857201 A CN101857201 A CN 101857201A
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- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 80
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 239000001301 oxygen Substances 0.000 title claims abstract description 79
- PDEXVOWZLSWEJB-UHFFFAOYSA-N krypton xenon Chemical compound [Kr].[Xe] PDEXVOWZLSWEJB-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 239000012141 concentrate Substances 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims description 18
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims abstract description 55
- 239000007789 gas Substances 0.000 claims abstract description 33
- 239000002994 raw material Substances 0.000 claims abstract description 28
- 239000000203 mixture Substances 0.000 claims abstract description 16
- 229910052743 krypton Inorganic materials 0.000 claims abstract description 13
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052724 xenon Inorganic materials 0.000 claims abstract description 12
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000926 separation method Methods 0.000 claims abstract description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 78
- 239000007788 liquid Substances 0.000 claims description 46
- 229910052757 nitrogen Inorganic materials 0.000 claims description 41
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 238000009835 boiling Methods 0.000 claims description 8
- 229930195733 hydrocarbon Natural products 0.000 claims description 6
- 150000002430 hydrocarbons Chemical class 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 5
- 230000008020 evaporation Effects 0.000 claims description 4
- VVTSZOCINPYFDP-UHFFFAOYSA-N [O].[Ar] Chemical compound [O].[Ar] VVTSZOCINPYFDP-UHFFFAOYSA-N 0.000 claims description 3
- 239000004215 Carbon black (E152) Substances 0.000 claims description 2
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 241000282326 Felis catus Species 0.000 claims 6
- 239000000463 material Substances 0.000 claims 3
- 229920000642 polymer Polymers 0.000 claims 1
- 239000006200 vaporizer Substances 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 16
- 229910052786 argon Inorganic materials 0.000 description 10
- 239000000047 product Substances 0.000 description 9
- 238000010992 reflux Methods 0.000 description 5
- 238000004821 distillation Methods 0.000 description 4
- QJGQUHMNIGDVPM-BJUDXGSMSA-N Nitrogen-13 Chemical compound [13N] QJGQUHMNIGDVPM-BJUDXGSMSA-N 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000012530 fluid Substances 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012263 liquid product Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
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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
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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
- F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
- F25J3/04254—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using the cold stored in external cryogenic fluids
- F25J3/0426—The cryogenic component does not participate in the fractionation
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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
- F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
- F25J3/04333—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams
- F25J3/04351—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams of nitrogen
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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
- F25J3/08—Separating gaseous impurities from gases or gaseous mixtures or from liquefied gases or liquefied gaseous mixtures
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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
- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/04—Processes or apparatus using separation by rectification in a dual pressure main column system
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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
- F25J2210/00—Processes characterised by the type or other details of the feed stream
- F25J2210/42—Nitrogen
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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
- F25J2215/50—Oxygen or special cases, e.g. isotope-mixtures or low purity O2
- F25J2215/56—Ultra high purity oxygen, i.e. generally more than 99,9% O2
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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
- F25J2270/00—Refrigeration techniques used
- F25J2270/42—Quasi-closed internal or closed external nitrogen refrigeration cycle
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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
- F25J2270/00—Refrigeration techniques used
- F25J2270/90—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration
- F25J2270/904—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration by liquid or gaseous cryogen in an open loop
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- Separation By Low-Temperature Treatments (AREA)
Abstract
本发明涉及一种用于从含氪氙混合物的液氧中生产高纯氧及氪氙浓缩物的装置及其应用，该装置包括第一级精馏塔及第二级精馏塔，第一级精馏塔内设置数块塔板，该第一级精馏塔的塔侧设置原料液氧进料口，顶部设置冷凝蒸发器及底部设置再沸器，第二级精馏塔中部与第一级精馏塔的上部经管道连接，该第二级精馏塔内设置数块塔板，顶部设置冷凝蒸发器，底部设置再沸器，高纯气氧(或液氧)从第二级精馏塔内进料口下部数块塔板或塔釜中抽出，从第一级精馏塔釜得到含氪氙的浓缩物。与现有技术相比，本发明可实现氪氙混合物和高纯氧的同时回收，高纯氧的回收率高，且应用范围广，可脱离空气分离装置，独立运行。
The invention relates to a device for producing high-purity oxygen and a krypton-xenon concentrate from liquid oxygen containing a mixture of krypton and xenon and its application. The device includes a first-stage rectification tower and a second-stage rectification tower. A number of trays are arranged in the first-stage rectification tower. The side of the first-stage rectification tower is provided with a raw material liquid oxygen inlet, the top is provided with a condensing evaporator and the bottom is provided with a reboiler, and the middle part of the second-stage rectification tower is connected to the second stage. The upper part of the first-stage rectification tower is connected by pipelines, and several trays are arranged in the second-stage rectification tower, with a condensing evaporator on the top and a reboiler on the bottom, and high-purity gas oxygen (or liquid oxygen) from the second stage Extract from several trays or tower bottoms at the lower part of the feed inlet in the rectification tower, and obtain the concentrate containing krypton and xenon from the first stage rectification tower bottom. Compared with the prior art, the invention can realize simultaneous recovery of krypton-xenon mixture and high-purity oxygen, high recovery rate of high-purity oxygen, wide application range, independent operation without air separation device.
Description
技术领域technical field
本发明涉及一种生产高纯氧及氪氙浓缩物的方法和装置，尤其是涉及一种从液氧产品中同时提取氪氙浓缩物和高纯氧的装置及其使用方法。The invention relates to a method and device for producing high-purity oxygen and krypton-xenon concentrate, in particular to a device for simultaneously extracting krypton-xenon concentrate and high-purity oxygen from liquid oxygen products and its application method.
背景技术Background technique
工艺流程以低温精馏法制取高纯氧为普遍，原料液主要为液氧和气氧两种，根据原料液的不同，液氧中提取高纯氧工艺，主要是从主冷中抽取液氧(99.5～99.7％)，其余为氮、氩、氪、氙及碳氢化合物等进入一只高纯氧塔中，以回流的方式进行精馏，制取的高纯氧纯度为99.995％，此方法高纯氧的制取量较小。The technical process is to produce high-purity oxygen by low-temperature rectification. The raw material liquid is mainly liquid oxygen and gas oxygen. According to the difference of raw material liquid, the process of extracting high-purity oxygen from liquid oxygen is mainly to extract liquid oxygen from the main cooler ( 99.5～99.7%), the rest is nitrogen, argon, krypton, xenon and hydrocarbons, etc. enter a high-purity oxygen tower, rectify in a reflux manner, and the purity of the high-purity oxygen produced is 99.995%. This method The amount of production of high-purity oxygen is small.
另一种方式为选取粗氩塔回流液作高纯液氧的原料，从氩塔下部约5块塔板处抽取含量93.17％O2，6.8％Ar，0.013％N2的原料气，送入纯氧塔进行精馏，经过约50块塔板，塔釜产出约20Nm3/h的纯度为99.9995％的高纯氧。该方法原料液氧不是从主冷抽取，而是选取粗氩塔回流液作为原料，其提取率只有约1.43％。Another way is to select the crude argon tower reflux liquid as the raw material of high-purity liquid oxygen, extract the raw material gas with content of 93.17% O 2 , 6.8% Ar, 0.013% N 2 from about 5 trays in the lower part of the argon tower, and feed it into The pure oxygen tower performs rectification, and after about 50 trays, the tower bottom produces about 20Nm 3 /h of high-purity oxygen with a purity of 99.9995%. In this method, the raw liquid oxygen is not extracted from the main cooling, but the reflux liquid of the crude argon tower is selected as the raw material, and the extraction rate is only about 1.43%.
随着电子工业技术的不断发展，对高纯氧的需求日益增大。目前普遍采用液氧为原料进行高纯氧的制取，提取率较低。而在氪氙粗制工艺流程中，经过一次、二次纯化后的氧气，纯度达到99.5％～99.99％是制取高纯氧的极佳原料，其特点是产量大、纯度高。而这样的原料气普遍采取放空或者与其他气体混合的方式，调节冷凝蒸发器温度，未能充分利用现有资源，实现循环经济。With the continuous development of electronic industry technology, the demand for high-purity oxygen is increasing. At present, liquid oxygen is generally used as raw material for the production of high-purity oxygen, and the extraction rate is low. In the krypton-xenon crude process, the oxygen after primary and secondary purification has a purity of 99.5% to 99.99%, which is an excellent raw material for producing high-purity oxygen, which is characterized by large output and high purity. However, such raw material gas is generally vented or mixed with other gases to adjust the temperature of the condensing evaporator, which fails to make full use of existing resources and realize circular economy.
发明内容Contents of the invention
本发明的目的就是为了克服上述现有技术存在的缺陷而提供一种高纯氧的回收率高、同时生产氪氙混合物以及高纯氧、应用广泛的生产高纯氧及氪氙浓缩物的装置及其使用方法。The purpose of the present invention is to provide a device for producing high-purity oxygen and krypton-xenon concentrate with high recovery rate of high-purity oxygen, simultaneous production of krypton-xenon mixture and high-purity oxygen, and wide application in order to overcome the defects in the prior art. and how to use it.
本发明的目的可以通过以下技术方案来实现：The purpose of the present invention can be achieved through the following technical solutions:
一种生产高纯氧及氪氙浓缩物的装置，其特征在于，该装置包括第一级精馏塔及第二级精馏塔，所述的第一级精馏塔内设置数块塔板，该第一级精馏塔塔侧的管道上设置原料进料口，塔顶设置冷凝蒸发器，塔釜设置再沸器，所述的第二级精馏塔中部与第一级精馏塔的上部经管道连接，该第二级精馏塔内设置数块塔板，塔顶设置冷凝蒸发器，塔釜设置再沸器，塔侧设置高纯气/液氧抽口，所述的第一级精馏塔塔釜的再沸器经节流阀与管道与第一级精馏塔及第二级精馏塔塔顶的冷凝蒸发器连接。A device for producing high-purity oxygen and krypton-xenon concentrate, characterized in that the device includes a first-stage rectification tower and a second-stage rectification tower, and several trays are arranged in the first-stage rectification tower , the pipeline on the side of the first-stage rectification tower is provided with a raw material feed port, the top of the tower is provided with a condensing evaporator, and the bottom of the tower is provided with a reboiler, the middle part of the second-stage rectification tower and the first-stage rectification tower The upper part of the rectification tower is connected by pipelines, several trays are arranged in the second-stage rectification tower, a condensing evaporator is arranged on the top of the tower, a reboiler is arranged in the bottom of the tower, and a high-purity gas/liquid oxygen suction port is arranged on the side of the tower. The reboiler in the bottom of the first-stage rectification tower is connected with the condensing evaporator at the top of the first-stage rectification tower and the second-stage rectification tower through a throttling valve and a pipeline.
所述的原料进料口设在距第一级精馏塔塔釜的至少一块塔板的高度。The raw material inlet is set at the height of at least one tray from the bottom of the first-stage rectification column.
所述的第一级精馏塔内的塔板数为8～20块，第二级精馏塔内的塔板数为40～100块，优选68块。The number of trays in the first-stage rectification tower is 8-20, and the number of trays in the second-stage rectification tower is 40-100, preferably 68.
所述的再沸器为电加热器或气体蒸发塔釜液体的换热器。The reboiler is an electric heater or a heat exchanger for the liquid in the bottom of the gas evaporation tower.
所述的高纯气/液氧抽口设在距第二级精馏塔塔釜2～10块塔板的高度，优选距塔釜5块塔板的高度。The high-purity gas/liquid oxygen outlet is set at a height of 2 to 10 trays from the bottom of the second-stage rectification column, preferably at a height of 5 trays from the bottom of the column.
所述的高纯气/液氧抽口设在第二级精馏塔塔釜。The high-purity gas/liquid oxygen extraction port is located in the bottom of the second-stage rectification tower.
一种生产高纯氧及氪氙浓缩物装置的使用方法，其特征在于，该方法包括以下步骤：A method for producing high-purity oxygen and krypton-xenon concentrate device, characterized in that the method comprises the following steps:
(1)将原料经原料进料口导入至第一级精馏塔中进行精馏处理，控制第一级精馏塔的温度为-126～-164℃，压力为1.5～3bar，在塔釜得到氪氙浓缩物，在塔顶得到去除氪、氙及碳氢化合物的氧气或液氧；(1) The raw material is introduced into the first-stage rectification tower through the raw material inlet for rectification treatment, and the temperature of the first-stage rectification tower is controlled to be -126～-164°C and the pressure is 1.5～3bar. Get krypton-xenon concentrate, and get oxygen or liquid oxygen to remove krypton, xenon and hydrocarbons at the top of the tower;
(2)塔顶得到的氧气或液氧进入第二级精馏塔继续精馏，控制第二级精馏塔的温度为-170～-175℃，压力为2～5bar，在高纯气/液氧抽口得到高纯液氧或高纯气氧，塔顶得到氧氩混合物；(2) The oxygen or liquid oxygen obtained at the top of the tower enters the second-stage rectification tower to continue rectification. The liquid oxygen pump port can obtain high-purity liquid oxygen or high-purity gas oxygen, and the top of the tower can obtain a mixture of oxygen and argon;
(3)氮气进入第一级精馏塔塔釜再沸器液化成液氮，液氮经节流阀节流至低压进入第一级精馏塔及第二级精馏塔的塔顶冷凝蒸发器，蒸发成气氮，未被蒸发的液氮作为液氮产品从第一级精馏塔中输出。(3) Nitrogen enters the reboiler of the first-stage rectification tower to be liquefied into liquid nitrogen, and the liquid nitrogen is throttled to a low pressure by the throttle valve and enters the top of the first-stage rectification tower and the second-stage rectification tower to condense and evaporate The liquid nitrogen that has not been evaporated is output from the first-stage rectifying tower as a liquid nitrogen product.
所述的原料包括含氪氙混合物的原料液氧或含氪氙混合物且经换热器预冷至接近饱和状态的低温气氧，所述的原料液氧为连接空分设备的工业液氧或经浓缩并脱除甲烷等高沸点组份的液氧。The raw material includes raw material liquid oxygen containing a krypton-xenon mixture or low-temperature gas oxygen containing a krypton-xenon mixture that is precooled to a state close to saturation through a heat exchanger, and the raw material liquid oxygen is industrial liquid oxygen connected to an air separation plant or Concentrate and remove the liquid oxygen of high boiling point components such as methane.
所述的氪氙浓缩物中氪氙含量为原料中氪氙含量的3～20倍，优选10倍。The krypton-xenon content in the krypton-xenon concentrate is 3 to 20 times, preferably 10 times, the krypton-xenon content in the raw material.
所述的高纯液氧或高纯气氧中氧气纯度达到99.99v/v％-99.9997v/v％。The oxygen purity in the high-purity liquid oxygen or high-purity gas oxygen reaches 99.99v/v%-99.9997v/v%.
与现有技术相比，本发明具有以下优点：Compared with the prior art, the present invention has the following advantages:
(1)可实现氪氙混合物和高纯氧的同时回收，其中高纯氧的回收率高，可以达到90％以上；(1) Simultaneous recovery of krypton-xenon mixture and high-purity oxygen can be realized, and the recovery rate of high-purity oxygen is high, which can reach more than 90%;
(2)高纯氧产品气形式多样，生产的气体产品可以是气体，也可生产液体产品进入液体储槽贮存；(2) There are various forms of high-purity oxygen product gas, and the gas products produced can be gas, and liquid products can also be produced and stored in liquid storage tanks;
(3)设置两只精馏塔，可同时生产氪氙浓缩物以及高纯氧产品。通过逐级精馏，第一级精馏塔底部生产的贫氪氙液或者粗氪氙液，已经脱除掉原料气中的高沸点组分(Kr、Xe、C1～C3、CF4、C2F6、SF6等)，塔顶排放的氧气中仅含微量的Ar和N2，最终获得纯度高于99.999％的高纯氧产品，其中各种杂质含量均低于GB/T14599-2008高纯氧的技术指标；(3) Set up two rectification towers, which can simultaneously produce krypton-xenon concentrate and high-purity oxygen products. Through step-by-step rectification, the krypton-xenon-poor liquid or crude krypton-xenon liquid produced at the bottom of the first-stage rectification tower has removed the high boiling point components (Kr, Xe, C 1 ~ C 3 , CF 4 , C 2 F 6 , SF 6 , etc.), the oxygen discharged from the top of the tower contains only a small amount of Ar and N 2 , and finally obtains a high-purity oxygen product with a purity higher than 99.999%, and the content of various impurities is lower than GB/T14599 -2008 high-purity oxygen technical indicators;
(4)应用范围广，在用户设置了液氧、液氮低温贮槽后，本发明装置可脱离空气分离装置，独立运行。(4) The application range is wide. After the user sets up liquid oxygen and liquid nitrogen cryogenic storage tanks, the device of the present invention can be separated from the air separation device and run independently.
附图说明Description of drawings
图1为实施例1中本发明的结构示意图；Fig. 1 is the structural representation of the present invention in embodiment 1;
图2为实施例2中本发明的结构示意图；Fig. 2 is the structural representation of the present invention in embodiment 2;
图3为实施例3中本发明的结构示意图；Fig. 3 is the structural representation of the present invention in embodiment 3;
图4为实施例4中本发明的结构示意图。Fig. 4 is a schematic structural diagram of the present invention in embodiment 4.
图中，1为第一级精馏塔、2为第二级精馏塔、3为原料、4为低温氮气、5为液氮、6为节流阀、7为液氮、8为氧气、9为氮气、10为液氮、13为液氮、14为氮气、15为高纯液氧、16为液氧、17为氧氩混合物、18为再沸器、19为氪氙浓缩物、20为冷凝蒸发器、21为再沸器、22为冷凝蒸发器。In the figure, 1 is the first-stage rectification tower, 2 is the second-stage rectification tower, 3 is raw material, 4 is low-temperature nitrogen, 5 is liquid nitrogen, 6 is a throttle valve, 7 is liquid nitrogen, 8 is oxygen, 9 is nitrogen, 10 is liquid nitrogen, 13 is liquid nitrogen, 14 is nitrogen, 15 is high-purity liquid oxygen, 16 is liquid oxygen, 17 is oxygen-argon mixture, 18 is reboiler, 19 is krypton xenon concentrate, 20 21 is a condensing evaporator, 21 is a reboiler, and 22 is a condensing evaporator.
具体实施方式Detailed ways
下面结合附图和具体实施例对本发明进行详细说明。The present invention will be described in detail below in conjunction with the accompanying drawings and specific embodiments.
实施例1Example 1
一种生产高纯氧及氪氙浓缩物的装置，其结构如图1所示，原料液氧产品3以1000Nm3/h送入第一级精馏塔1之中，塔内操作压力在2bar，设置10块塔板，塔底得到200Nm3/h贫氪氙液，氪、氙、甲烷等高沸点组分初次洗涤进入贫氪氙液中，其中氪氙约600ppm，甲烷约200ppm，其余杂质含量约20ppm，顶排放的氧气8中几乎不含氪氙等高沸点组分，塔底流体得到贫氪氙液，进入第二级精馏塔2内再次精馏。贫氪氙塔底部流体采用氮气加热，温度降至饱和点的流体氮气4，经过再沸器21及节流阀6之后分离成以气液两相，得到液氮5，液氮7及液氮13分别进入两个塔顶的冷凝蒸发器20及22中作为冷源，多余的液氮通过管线排出进入储槽，液氮蒸发使上升的氧气冷凝成液氧回流塔内进行精馏，液氮被蒸发得到的氮气9及氮气14，在塔釜得到氪氙浓缩物19。A device for producing high-purity oxygen and krypton-xenon concentrate. Its structure is shown in Figure 1. The raw liquid oxygen product 3 is sent to the first-stage rectification tower 1 at 1000Nm 3 /h, and the operating pressure in the tower is 2bar. , set up 10 trays, and get 200Nm 3 /h krypton-xenon-poor liquid at the bottom of the tower, and the high-boiling components such as krypton, xenon, and methane are washed into the krypton-xenon-poor liquid for the first time, of which krypton-xenon is about 600ppm, methane is about 200ppm, and other impurities The content is about 20ppm, and the oxygen 8 discharged from the top almost does not contain high-boiling components such as krypton and xenon. The fluid at the bottom of the krypton-xenon tower is heated with nitrogen, and the fluid nitrogen 4 whose temperature drops to the saturation point is separated into gas-liquid two-phase after passing through the
氧气流线8进入第二级精馏塔2的中上部位置，距离冷凝蒸发器6块塔板位置，第二级精馏塔2底部再沸器18采用电加热器，产生精馏所需的上升氧气，冷源采用经过节流阀6之后的液氮13，冷却上升的氧气产生回流液氧建立精馏工况。第二级精馏塔2操作压力3bar，设置68块塔板，高纯氧(液氧)抽口位于距离塔釜5块位置，得到纯度大于99.999％的高纯液氧15，其中氩的体积含量小于2ppm，总烃含量小于0.5ppm，底部排出含有氪氙、甲烷等高沸点杂质的液氧16，塔顶得到氧氩混合物17。Oxygen flow line 8 enters the middle and upper part of the second-stage rectification tower 2, 6 tray positions away from the condensing evaporator, and the
实施例2Example 2
一种生产高纯氧及氪氙浓缩物的装置，其结构如图2所示，与实施例1的区别是进入第二级精馏塔2的氧气流线8为第一级精馏塔1顶部冷凝蒸发器冷凝的液氧。A device for producing high-purity oxygen and krypton-xenon concentrate, its structure is shown in Figure 2, the difference from Example 1 is that the oxygen flow line 8 entering the second-stage rectification tower 2 is the first-stage rectification tower 1 Liquid oxygen condensed by the top condensing evaporator.
实施例3Example 3
一种生产高纯氧及氪氙浓缩物的装置，其结构如图3所示，与实施例1的区别是进入第一级精馏塔1的塔釜再沸器为电加热器，进入第一级精馏塔1的冷凝蒸发器20的液氮7及第二级精馏塔2的冷凝蒸发器22的液氮13为外部液氮5提供，而不是实施例1第一级精馏塔1的塔釜再沸器冷凝的液氮。A device for producing high-purity oxygen and krypton-xenon concentrates, the structure of which is shown in Figure 3. The difference from Example 1 is that the reboiler entering the first-stage rectification tower 1 is an electric heater, and the reboiler entering the second stage The liquid nitrogen 7 of the
实施例4Example 4
一种生产高纯氧及氪氙浓缩物的装置，其结构如图4所示，与实施例3的区别是进入第二级精馏塔2的氧气流线8为第一级精馏塔1顶部冷凝蒸发器冷凝的液氧。A device for producing high-purity oxygen and krypton-xenon concentrate, its structure is shown in Figure 4, the difference from Example 3 is that the oxygen flow line 8 entering the second-stage rectification tower 2 is the first-stage rectification tower 1 Liquid oxygen condensed by the top condensing evaporator.
实施例5Example 5
一种生产高纯氧及氪氙浓缩物的装置，该装置包括第一级精馏塔及第二级精馏塔，的第一级精馏塔内设置8块塔板，该第一级精馏塔塔侧的管道上设置原料进料口，原料进料口设在距第一级精馏塔塔釜的一块塔板的高度，塔顶设置冷凝蒸发器，塔釜设置气体蒸发塔釜液体的换热器，第二级精馏塔中部与第一级精馏塔的上部经管道连接，该第二级精馏塔内设置40块塔板，塔顶设置冷凝蒸发器，塔釜设置气体蒸发塔釜液体的换热器，塔侧设置高纯气/液氧抽口，高纯气/液氧抽口设在距第二级精馏塔塔釜2块塔板的高度，第一级精馏塔塔釜的再沸器经节流阀与管道与第一级精馏塔及第二级精馏塔塔顶的冷凝蒸发器连接。A device for producing high-purity oxygen and krypton-xenon concentrates. The device includes a first-stage rectification tower and a second-stage rectification tower. Eight trays are arranged in the first-stage rectification tower. The first-stage rectification tower The pipeline on the side of the distillation tower is provided with a raw material feed port, which is set at the height of a plate from the first stage distillation tower tank, a condensing evaporator is set at the top of the tower, and a gas evaporation tower tank liquid is set at the tower tank The middle part of the second-stage rectification tower is connected with the upper part of the first-stage rectification tower through pipelines, 40 trays are arranged in the second-stage rectification tower, a condensing evaporator is arranged on the top of the tower, and a gas The heat exchanger for evaporating the liquid in the bottom of the distillation column is equipped with a high-purity gas/liquid oxygen outlet on the side of the tower, and the high-purity gas/liquid oxygen outlet is set at the height of 2 trays from the bottom of the second-stage distillation column The reboiler in the bottom of the rectification column is connected with the condensing evaporator at the top of the first-stage rectification column and the second-stage rectification column through a throttle valve and a pipeline.
生产高纯氧及氪氙浓缩物装置的使用方法包括以下步骤：The method of using the device for producing high-purity oxygen and krypton-xenon concentrate comprises the following steps:
(1)将浓缩并脱除甲烷等高沸点组份并含氪氙混合物的液氧经进料口导入至第一级精馏塔中进行精馏处理，控制第一级精馏塔的温度为-126℃，压力为1.5bar，在塔釜得到氪氙浓缩物，氪氙浓缩物中氪氙含量为原料中氪氙含量的10倍，在塔顶得到去除氪、氙及碳氢化合物的氧气；(1) Concentrating and removing high boiling point components such as methane and containing liquid oxygen containing a mixture of krypton and xenon is introduced into the first-stage rectification tower through the feed port for rectification treatment, and the temperature of the first-stage rectification tower is controlled to be -126°C, pressure 1.5bar, krypton-xenon concentrate is obtained in the tower kettle, the content of krypton-xenon in the krypton-xenon concentrate is 10 times the content of krypton-xenon in the raw material, and the oxygen that removes krypton, xenon and hydrocarbons is obtained at the top of the tower ;
(2)塔顶得到的氧气进入第二级精馏塔继续精馏，控制第二级精馏塔的温度为-170℃，压力为2bar，在高纯气/液氧抽口得到高纯液氧，高纯液氧或高纯气氧中氧气纯度达到99.99v/v％，塔顶得到氧氩混合物。(2) The oxygen obtained at the top of the tower enters the second-stage rectification tower to continue rectification. The temperature of the second-stage rectification tower is controlled at -170°C, the pressure is 2bar, and high-purity liquid is obtained at the high-purity gas/liquid oxygen outlet. Oxygen, high-purity liquid oxygen or high-purity gas oxygen has a purity of 99.99v/v%, and a mixture of oxygen and argon is obtained at the top of the tower.
(3)氮气进入第一级精馏塔塔釜再沸器液化成液氮，液氮经节流阀节流至低压进入第一级精馏塔及第二级精馏塔的塔顶冷凝蒸发器，蒸发成气氮，未被蒸发的液氮作为液氮产品从第一级精馏塔中输出。(3) Nitrogen enters the reboiler of the first-stage rectification tower to be liquefied into liquid nitrogen, and the liquid nitrogen is throttled to a low pressure by the throttle valve and enters the top of the first-stage rectification tower and the second-stage rectification tower to condense and evaporate The liquid nitrogen that has not been evaporated is output from the first-stage rectifying tower as a liquid nitrogen product.
实施例6Example 6
一种生产高纯氧及氪氙浓缩物的装置，该装置包括第一级精馏塔及第二级精馏塔，所述的第一级精馏塔内设置20块塔板，该第一级精馏塔塔侧的管道上设置原料进料口，原料进料口设在距第一级精馏塔塔釜的5块塔板的高度。塔顶设置冷凝蒸发器，塔釜设置再沸器，第二级精馏塔中部与第一级精馏塔的上部经管道连接，该第二级精馏塔内设置100块塔板，塔顶设置冷凝蒸发器，塔釜设置再沸器，塔釜设置高纯气/液氧抽口，第一级精馏塔塔釜的再沸器经节流阀与管道与第一级精馏塔及第二级精馏塔塔顶的冷凝蒸发器连接。A device for producing high-purity oxygen and krypton-xenon concentrates, the device includes a first-stage rectification tower and a second-stage rectification tower, and 20 trays are arranged in the first-stage rectification tower. The pipeline on the side of the stage rectification tower is provided with a raw material feed port, and the raw material feed port is set at a height of 5 trays away from the bottom of the first stage rectification tower. A condensing evaporator is set on the top of the tower, and a reboiler is set in the bottom of the tower. The middle part of the second-stage rectification tower is connected to the upper part of the first-stage rectification tower through pipelines. There are 100 trays in the second-stage rectification tower. A condensing evaporator is installed, a reboiler is installed in the bottom of the tower, and a high-purity gas/liquid oxygen suction port is installed in the bottom of the tower. The condensing evaporator at the top of the second-stage rectifying column is connected.
生产高纯氧及氪氙浓缩物装置的使用方法包括以下步骤：The method of using the device for producing high-purity oxygen and krypton-xenon concentrate comprises the following steps:
(1)将浓缩并脱除甲烷等高沸点组份并含氪氙混合物的液氧经进料口导入至第一级精馏塔中进行精馏处理，控制第一级精馏塔的温度为-164℃，压力为3bar，在塔釜得到氪氙浓缩物，氪氙浓缩物中氪氙含量为原料中氪氙含量的3倍，在塔顶得到去除氪、氙及碳氢化合物的液氧；(1) Concentrating and removing high boiling point components such as methane and containing liquid oxygen containing a mixture of krypton and xenon is introduced into the first-stage rectification tower through the feed port for rectification treatment, and the temperature of the first-stage rectification tower is controlled to be -164°C, pressure 3bar, krypton-xenon concentrate is obtained in the tower kettle, the content of krypton-xenon in the krypton-xenon concentrate is three times the content of krypton-xenon in the raw material, and liquid oxygen that removes krypton, xenon and hydrocarbons is obtained at the top of the tower ;
(2)塔顶得到的液氧进入第二级精馏塔继续精馏，控制第二级精馏塔的温度为-175℃，压力为5bar，在塔釜的高纯气/液氧抽口得到高纯气氧，高纯气氧中氧气纯度达到99.9997v/v％，塔顶得到氧氩混合物；(2) The liquid oxygen obtained at the top of the tower enters the second-stage rectification tower to continue rectification. The temperature of the second-stage rectification tower is controlled at -175°C and the pressure is 5bar. Obtain high-purity gas oxygen, the purity of oxygen in high-purity gas oxygen reaches 99.9997v/v%, and a mixture of oxygen and argon is obtained at the top of the tower;
(3)氮气进入第一级精馏塔塔釜再沸器液化成液氮，液氮经节流阀节流至低压进入第一级精馏塔及第二级精馏塔的塔顶冷凝蒸发器，蒸发成气氮，未被蒸发的液氮作为液氮产品从第一级精馏塔中输出。(3) Nitrogen enters the reboiler of the first-stage rectification tower to be liquefied into liquid nitrogen, and the liquid nitrogen is throttled to a low pressure by the throttle valve and enters the top of the first-stage rectification tower and the second-stage rectification tower to condense and evaporate The liquid nitrogen that has not been evaporated is output from the first-stage rectifying tower as a liquid nitrogen product.
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