A production device and production process for producing ultra-pure krypton-xenon using a krypton-xenon getter

Abstract

The present invention belongs to a production device and production process for producing ultra-pure krypton and xenon by using a krypton-xenon getter; it includes a crude krypton-xenon gas pipeline, the crude krypton-xenon gas pipeline is connected to the inlet of a krypton-xenon separation tower, the bottom liquid phase outlet of the krypton-xenon separation tower is connected to the inlet of a high-purity xenon tower, and the bottom liquid phase outlet of the high-purity xenon tower is sequentially connected to a xenon gas vaporizer, a xenon gas getter, and a xenon gas membrane compressor and then connected to a xenon gas manifold; the gas phase outlet at the top of the krypton-xenon separation tower is connected to the tube side of a first top condenser and then to a first gas-liquid separator, the gas phase outlet of the first gas-liquid separator is connected to the inlet of a high-purity krypton tower, the gas phase outlet at the top of the high-purity krypton tower is connected to the tube side of a second top condenser and then to a second gas-liquid separator, and the second liquid phase outlet of the second gas-liquid separator is sequentially connected to a krypton gas vaporizer, a krypton gas getter, and a krypton gas membrane compressor and then connected to a krypton gas manifold; it has the characteristics of reducing the floor area, lowering the energy consumption, and improving the purity of krypton and xenon products at the same time.

Description

Technical Field

[0001] The present invention belongs to the technical field of krypton-xenon gas purification, and particularly relates to a production device and a production process for producing ultra-high purity krypton-xenon by using a krypton-xenon getter. Background Art

[0002] Krypton and xenon exist in the air at very low concentrations. Specifically, krypton and xenon exist in the atmosphere at about 1.14 ppm and 0.087 ppm respectively; and both krypton and xenon are widely used in the gas for the electronics and electric light source industries. With the in-depth development of fields such as the semiconductor industry, aerospace, and scientific research, the purity requirements for krypton-xenon gas products are getting higher and higher. Currently, conventional krypton-xenon purification devices are all realized by rectifying in a rectification column. For example, the patent number is 200910056397.5, and the patent name is: A method for preparing pure krypton and pure xenon by full rectification. In this technical solution, a lean krypton-xenon concentrate is used as a raw material and rectified through seven rectification columns to prepare pure krypton and pure xenon, and the purity of the obtained pure krypton and pure xenon is 99.999%. Based on the above content, it can be seen that using the traditional rectification form to prepare pure krypton and pure xenon has the defects of large equipment floor area, high energy consumption, and low purity, which cannot be applied to modern semiconductor industries, aerospace, scientific research and other fields. Summary of the Invention

[0003] The purpose of the present invention is to overcome the defects in the prior art, and provide a production device and a production process for producing ultra-high purity krypton-xenon by using a krypton-xenon getter, which cooperate a rectification column with a krypton-xenon getter to reduce the floor area, lower the energy consumption, and improve the product purity of krypton-xenon, so as to meet the requirements of modern semiconductor industries, aerospace, and scientific research fields.

[0004] The purpose of the present invention is achieved as follows:

[0005] A production device for producing ultra-high purity krypton-xenon by using a krypton-xenon getter includes a crude krypton-xenon gas pipeline, the crude krypton-xenon gas pipeline is connected to the inlet of a krypton-xenon separation column, the bottom liquid phase outlet of the krypton-xenon separation column is connected to the inlet of a high-purity xenon column, and the bottom liquid phase outlet of the high-purity xenon column is sequentially connected to a xenon gas vaporizer, a xenon gas getter, and a xenon gas membrane compressor and then connected to a xenon gas manifold; the gas phase outlet at the top of the krypton-xenon separation column is connected to the tube side of a first top condenser and then connected to a first gas-liquid separator, the gas phase outlet of the first gas-liquid separator is connected to the inlet of a high-purity krypton column, the gas phase outlet at the top of the high-purity krypton column is connected to the tube side of a second top condenser and then connected to a second gas-liquid separator, and the second liquid phase outlet of the second gas-liquid separator is sequentially connected to a krypton gas vaporizer, a krypton gas getter, and a krypton gas membrane compressor and then connected to a krypton gas manifold.

[0006] Preferably, electric heaters for the krypton-xenon separation column bottom, the high-purity krypton column bottom, and the high-purity xenon column are respectively provided at the inner bottoms of the krypton-xenon separation column, the high-purity krypton column, and the high-purity xenon column.

[0007] Preferably, the crude krypton-xenon gas pipeline is connected to the inlet of the krypton-xenon separation column through a first regulating valve, the first inlet of the main heat exchanger of the main heat exchanger, and the first outlet of the main heat exchanger.

[0008] Preferably, the liquid phase outlet of the first gas-liquid separator is connected to the reflux port of the upper part of the krypton-xenon separation column.

[0009] Preferably, the gas phase outlet at the top of the second gas-liquid separator is connected to the recovery unit through a third regulating valve, the second inlet of the main heat exchanger of the main heat exchanger, and the second outlet of the main heat exchanger; the first liquid phase outlet of the second gas-liquid separator is connected to the reflux port of the upper part of the high-purity krypton column through a fourth regulating valve; a fifth regulating valve is provided between the second liquid phase outlet of the second gas-liquid separator and the krypton gas vaporizer.

[0010] Preferably, the gas phase outlet at the top of the high-purity xenon column is connected to the reflux port of the upper part of the high-purity xenon column provided through the tube side of the third top condenser.

[0011] Preferably, it further includes a liquid nitrogen storage tank. The second outlet of the liquid nitrogen storage tank is connected to the first shell side inlet of the third top condenser through an eighth regulating valve; the first outlet of the liquid nitrogen storage tank is connected to the shell side inlet of the first top condenser through a first three-way joint and a sixth regulating valve. The shell side gas phase outlet of the first top condenser is connected to the second shell side inlet of the third top condenser through a second three-way joint and an eleventh regulating valve. The third end of the first three-way joint is connected to the third shell side inlet of the second top condenser through a seventh regulating valve. The third end of the second three-way joint is connected to the fourth shell side inlet of the second top condenser through a tenth regulating valve.

[0012] Preferably, the shell side gas phase outlets of the second top condenser and the third top condenser are respectively connected to the third inlet of the main heat exchanger of the main heat exchanger through pipelines, and the third outlet of the main heat exchanger is connected to the regenerated gas storage tank.

[0013] Preferably, a second regulating valve is provided between the shell side gas phase outlet of the second top condenser and the third inlet of the main heat exchanger of the main heat exchanger, and a ninth regulating valve is provided between the shell side gas phase outlet of the third top condenser and the third inlet of the main heat exchanger of the main heat exchanger.

[0014] The present invention also provides a production process of a production device for producing ultra-high purity krypton-xenon by using a krypton-xenon getter, including the following steps:

[0015] Step 1: The crude krypton-xenon gas from the crude krypton-xenon gas pipeline passes through the first regulating valve and then enters the krypton-xenon separation column through the first inlet and the first outlet of the main heat exchanger. It is rectified by the krypton-xenon separation column bottom electric heater and the first top condenser, which provide heat and cold respectively. The temperature of the crude krypton-xenon gas is 20 - 30°C, the pressure is 0.4 Mpa, the flow rate is 10 Nm 3 / h, the gas phase fraction is 1, and the krypton-xenon content is 95 - 99%;

[0016] Step 2: The crude krypton-xenon gas entering the krypton-xenon separation column in Step 1 is rectified and purified once. The gas phase after rectification and purification passes through the gas phase outlet at the top of the krypton-xenon separation column and the tube side of the first top condenser and enters the first gas-liquid separator for gas-liquid separation. The liquid phase after gas-liquid separation enters the krypton-xenon separation column through the separation column reflux port for re-rectification and purification. The gas phase after gas-liquid separation enters the high-purity krypton column through the gas phase outlet of the first gas-liquid separator; the liquid phase temperature of the first gas-liquid separator is -105.2 - -106.5°C, and the molar fraction of krypton is 90 - 95%; the gas phase temperature of the first gas-liquid separator is -105.2 - -106.5°C, and the molar fraction of krypton is 99.9 - 99.95%;

[0017] Step 3: After the gas phase outlet of the first gas-liquid separator in Step 2 enters the high-purity krypton column, it is rectified by the high-purity krypton column bottom electric heater and the second top condenser, which provide heat and cold respectively. The gas phase after rectification passes through the gas phase outlet at the top of the high-purity krypton column and the tube side of the second top condenser and enters the second gas-liquid separator for gas-liquid separation. A part of the liquid phase after gas-liquid separation is refluxed to the high-purity krypton column through the fourth regulating valve and the high-purity krypton column reflux port for re-rectification; another part of the liquid phase after gas-liquid separation is successively transported to the krypton gas manifold through the fifth regulating valve, the krypton gas vaporizer, the krypton gas aspirator, and the krypton gas membrane compressor; the liquid phase temperature after gas-liquid separation in the second gas-liquid separator is -135 - -138°C, and the molar fraction of krypton is 99.995 - 99.999%; the temperature at the outlet of the krypton gas aspirator is 20 - 25°C, and the molar fraction of krypton transported to the krypton gas manifold is 99.9995 - 99.9999%;

[0018] Step 4: The gas phase after gas-liquid separation in the second gas-liquid separator in Step 3 enters the recovery unit through the third regulating valve, the second inlet and the second outlet of the main heat exchanger; the gas phase temperature at the second outlet of the main heat exchanger is 35 - 40°C, and the molar fraction of krypton is 99.9 - 99.95%;

[0019] Step Five: The liquid phase rectified in the krypton-xenon separation column in Step Two enters the high-purity xenon column through the bottom liquid outlet of the krypton-xenon separation column, and is rectified by providing heat and cold through the electric heater at the bottom of the high-purity xenon column and the third top condenser. The rectified liquid phase is transported to the xenon gas manifold through the bottom liquid outlet of the high-purity xenon column, the xenon gas vaporizer, the xenon gas aspirator, and the xenon gas membrane compressor; the liquid phase temperature at the bottom liquid outlet of the high-purity xenon column is -80 to -82 °C, and the xenon mole fraction is 99.5 to 99.9%; the outlet temperature of the xenon gas aspirator is 20 to 25 °C, and the xenon mole fraction is 99.9997 to 99.9999%;

[0020] Step Six: The gas phase at the top of the high-purity xenon column in Step Five exchanges heat through the tube side of the third top condenser and enters the high-purity xenon column through the reflux port of the high-purity xenon column for re-rectification;

[0021] Step Seven: The liquid nitrogen in the liquid nitrogen storage tank enters the first three-way through the first outlet of the liquid nitrogen storage tank. Part of the liquid nitrogen enters the shell side of the first top condenser through the sixth regulating valve and the shell side inlet of the first top condenser; the other part of the liquid nitrogen enters the shell side of the second top condenser through the seventh regulating valve and the third shell side inlet; the temperature of the liquid nitrogen entering the shell side of the first top condenser through the sixth regulating valve is -174 to -176 °C, and the flow rate is 15 to 25 Nm 3 / h; the temperature of the liquid nitrogen entering the shell side of the second top condenser through the seventh regulating valve is -174 to -176 °C, and the flow rate is 10 to 15 Nm 3 / h;

[0022] Step Eight: The liquid nitrogen in the liquid nitrogen storage tank enters the shell side of the third top condenser through the second outlet of the liquid nitrogen storage tank and the first shell side inlet. The temperature of the liquid nitrogen entering the shell side of the third top condenser through the first shell side inlet is -174 to -176 °C, and the flow rate is 5 to 10 Nm 3 / h;

[0023] Step Nine: The gas phase at the shell side gas outlet of the first top condenser in Step Seven enters the second three-way. Part of the gas phase enters the shell side of the third top condenser through the eleventh regulating valve and the second shell side inlet; the other part of the gas phase enters the shell side of the second top condenser through the tenth regulating valve and the fourth shell side inlet; the temperature of the gas phase at the shell side gas outlet of the first top condenser is -174 to -176 °C, and the flow rate is 10 to 25 Nm 3 / h; the temperature of the gas phase entering the shell side of the third top condenser through the second shell side inlet is -174 to -176 °C, and the flow rate is 5 to 10 Nm 3 / h;

[0024] Step Ten: The gas phase from the shell-side gas phase outlet of the second top condenser and the gas phase from the shell-side gas phase outlet of the third top condenser in Step Nine enter the third inlet of the main heat exchanger, and the gas phase from the third outlet of the main heat exchanger enters the regeneration gas storage tank; the temperature of the gas phase from the third outlet of the main heat exchanger is 35-40°C, and the pressure is 0.65-0.70 MPa.

[0025] A production device and production process for producing ultra-pure krypton and xenon using a krypton-xenon getter, made according to the above solution, by using gas-liquid mixed nitrogen to provide a refrigeration process and utilizing the working principle of the krypton-xenon getter to meet the rectification and purification process for stably producing krypton and xenon products with a purity of not less than 99.9995% each. Compared with traditional process technologies, the present invention has the following advantages: 1. High product purity, meeting the use requirements of the semiconductor industry, aerospace, and scientific research; 2. Simple device process flow. After the krypton gas and xenon gas from the high-purity krypton tower and high-purity xenon tower respectively pass through the corresponding vaporizers, ultra-pure krypton gas and ultra-pure xenon gas can be obtained; 3. The evaporated nitrogen of the first top condenser of the present invention can provide part of the cold energy required during the production process for the second top condenser and the third top condenser, maximizing the energy utilization; 4. The present invention is respectively provided with a krypton gas vaporizer and a xenon gas vaporizer behind the high-purity krypton tower and the high-purity xenon tower. After being fully vaporized, they enter the krypton gas getter and the xenon gas getter, reducing the volume and floor area of the krypton gas getter and the xenon gas getter; 5. The present invention designs the filling manifolds for krypton gas and xenon gas together, with a comprehensive device design. Description of the Drawings

[0026] Figure 1 It is a schematic structural diagram of the present invention. Detailed Embodiments

[0027] For a clearer understanding of the technical features, objectives, and effects of the present invention, the specific embodiments of the present invention are now described with reference to the accompanying drawings. The same reference numerals in each figure represent the same components. To make the drawings concise, only the parts related to the invention are schematically shown in each figure, and they do not represent their actual structure as products.

[0028] As Figure 1As shown in the figure, the present invention relates to a production device and production process for producing ultra-pure krypton and xenon using a krypton-xenon getter. Among them, the production device includes a crude krypton-xenon gas pipeline 22, and the crude krypton-xenon gas pipeline 22 is connected to the inlet of a krypton-xenon separation tower 2. The bottom liquid phase outlet of the krypton-xenon separation tower 2 is connected to the inlet of a high-purity xenon tower 4. The bottom liquid phase outlet of the high-purity xenon tower 4 is sequentially connected to a xenon gas vaporizer 14, a xenon gas getter 18, and a xenon gas membrane compressor 19 and then connected to a xenon gas manifold 20; the gas phase outlet at the top of the krypton-xenon separation tower 2 is connected to the tube side of a first top condenser 9 and then connected to a first gas-liquid separator 8. The gas phase outlet of the first gas-liquid separator 8 is connected to the inlet of a high-purity krypton tower 3. The gas phase outlet at the top of the high-purity krypton tower 3 is connected to the tube side of a second top condenser 10 and then connected to a second gas-liquid separator 38. The second liquid phase outlet of the second gas-liquid separator 38 is sequentially connected to a krypton gas vaporizer 13, a krypton gas getter 15, and a krypton gas membrane compressor 16 and then connected to a krypton gas manifold 17. The present invention uses a mixture of crude krypton and xenon as raw materials, allowing it to enter the krypton-xenon separation tower 2 for rectification separation. By utilizing the different boiling points, xenon becomes the liquid phase and krypton becomes the gas phase, thereby achieving the separation of the two; on this basis, the high-purity xenon tower 4 is used to purify xenon, and in combination with the xenon gas vaporizer 14, the xenon gas getter 18, and the xenon gas membrane compressor 19, the xenon gas is further purified to a mole fraction of 99.9997 - 99.9999%; at the same time, the high-purity krypton tower 3 is used to purify krypton, and in combination with the krypton gas vaporizer 13, the krypton gas getter 15, and the krypton gas membrane compressor 16, the krypton gas is further purified to a mole fraction of 99.9995 - 99.9999%; at the same time, by using the xenon gas manifold 20 and the krypton gas manifold 17, direct filling of storage tanks or transport tank trucks can be achieved.

[0029] Furthermore, a krypton-xenon separation tower bottom electric heater 5, a high-purity krypton tower bottom electric heater 6, and a high-purity xenon tower electric heater 7 are respectively provided at the inner bottoms of the krypton-xenon separation tower 2, the high-purity krypton tower 3, and the high-purity xenon tower 4. In the present invention, the krypton-xenon separation tower 2, the high-purity krypton tower 3, and the high-purity xenon tower 4 are respectively provided with heat by the krypton-xenon separation tower bottom electric heater 5, the high-purity krypton tower bottom electric heater 6, and the high-purity xenon tower electric heater 7.

[0030] Furthermore, the crude krypton-xenon gas pipeline 22 is connected to the inlet of the krypton-xenon separation tower 2 through a first regulating valve 21, the first inlet 35 of the main heat exchanger of the main heat exchanger 1, and the first outlet 39 of the main heat exchanger.

[0031] Furthermore, the liquid phase outlet of the first gas-liquid separator 8 is connected to the separation tower reflux port 49 at the upper part of the krypton-xenon separation tower 2.

[0032] Further, the gas phase outlet at the top of the second gas-liquid separator 38 is connected to the recovery unit 34 through the third regulating valve 23, the second inlet 36 of the main heat exchanger of the main heat exchanger 1, and the second outlet 40 of the main heat exchanger; the first liquid phase outlet of the second gas-liquid separator 38 is connected to the reflux port 51 at the upper part of the high-purity krypton column 3 through the fourth regulating valve 24; a fifth regulating valve 25 is provided between the second liquid phase outlet of the second gas-liquid separator 38 and the krypton gas vaporizer 13.

[0033] Further, the gas phase outlet at the top of the high-purity xenon column 4 is connected to the reflux port 50 provided at the upper part of the high-purity xenon column 4 through the tube side of the third top condenser 11.

[0034] Further, it further includes a liquid nitrogen storage tank 12, and the second outlet 48 of the liquid nitrogen storage tank 12 is connected to the first shell side inlet 45 of the third top condenser 11 through the eighth regulating valve 28;

[0035] The first outlet 26 of the liquid nitrogen storage tank 12 is connected to the shell side inlet of the first top condenser 9 through the first three-way joint 43 and the sixth regulating valve 52. The shell side gas phase outlet of the first top condenser 9 is connected to the second shell side inlet 44 of the third top condenser 11 through the second three-way joint 42 and the eleventh regulating valve 31. The third end of the first three-way joint 43 is connected to the third shell side inlet 47 of the second top condenser 10 through the seventh regulating valve 27. The third end of the second three-way joint 42 is connected to the fourth shell side inlet 46 of the second top condenser 10 through the tenth regulating valve 30.

[0036] Further, the shell side gas phase outlets of the second top condenser 10 and the third top condenser 11 are respectively connected to the third inlet 37 of the main heat exchanger of the main heat exchanger 1 through pipelines, and the main heat exchanger third outlet 41 is connected to the regeneration gas storage tank 29.

[0037] Further, a second regulating valve 32 is provided between the shell side gas phase outlet of the second top condenser 10 and the third inlet 37 of the main heat exchanger of the main heat exchanger 1, and a ninth regulating valve 33 is provided between the shell side gas phase outlet of the third top condenser 11 and the third inlet 37 of the main heat exchanger of the main heat exchanger 1.

[0038] The present invention also claims a production process of a production device for producing ultra-high purity krypton-xenon by using a krypton-xenon getter, including the following steps:

[0039] Step 1: The crude krypton-xenon gas from the crude krypton-xenon gas pipeline 22 passes through the first regulating valve 21 and then enters the krypton-xenon separation column 2 through the first inlet 35 and the first outlet 39 of the main heat exchanger. It is rectified by the heat and cold provided by the krypton-xenon separation column bottom electric heater 5 and the first top condenser 9 respectively. The temperature of the crude krypton-xenon gas: 20 - 30 °C, pressure: 0.4 Mpa, flow rate: 10 Nm3 / h, the gas fraction is: 1, and the krypton-xenon content is: 95-99%;

[0040] Step 2: Subject the crude krypton-xenon gas entering the krypton-xenon separation column 2 in Step 1 to primary rectification and purification. The gas phase after rectification and purification enters the first gas-liquid separator 8 through the gas phase outlet at the top of the krypton-xenon separation column 2 and the tube side of the first top condenser 9 for gas-liquid separation. The liquid phase after gas-liquid separation enters the krypton-xenon separation column 2 through the separation column reflux port 49 for secondary rectification and purification. The gas phase after gas-liquid separation enters the high-purity krypton column 3 through the gas phase outlet of the first gas-liquid separator 8; the liquid phase temperature of the first gas-liquid separator 8 is: -105.2 to -106.5 °C, and the mole fraction of krypton is: 90-95%; the gas phase temperature of the first gas-liquid separator 8 is: -105.2 to -106.5 °C, and the mole fraction of krypton is: 99.9-99.95%;

[0041] Step 3: After the gas phase outlet of the first gas-liquid separator 8 described in Step 2 enters the high-purity krypton column 3, rectification is carried out by providing heat and cold through the high-purity krypton column bottom electric heater 6 and the second top condenser 10. The gas phase after rectification enters the second gas-liquid separator 38 through the gas phase outlet at the top of the high-purity krypton column 3 and the tube side of the second top condenser 10 for gas-liquid separation. A part of the liquid phase after gas-liquid separation is refluxed to the high-purity krypton column 3 through the fourth regulating valve 24 and the high-purity krypton column reflux port 51 for secondary rectification; another part of the liquid phase after gas-liquid separation is successively transported to the krypton gas manifold 17 through the fifth regulating valve 25, the krypton gas vaporizer 13, the krypton gas aspirator 15, and the krypton gas membrane compressor 16; the liquid phase temperature after gas-liquid separation in the second gas-liquid separator 38 is: -135 to -138 °C, and the mole fraction of krypton is: 99.995-99.999%; the temperature at the outlet of the krypton gas aspirator 15 is: 20-25 °C, and the mole fraction of krypton transported to the krypton gas manifold 17 is: 99.9995-99.9999%;

[0042] Step 4: The gas phase after gas-liquid separation in the second gas-liquid separator 38 in Step 3 enters the recovery unit 34 through the third regulating valve 23, the second inlet 36 of the main heat exchanger of the main heat exchanger 1, and the second outlet 40 of the main heat exchanger; the gas phase temperature at the outlet of the second outlet 40 of the main heat exchanger is 35-40 °C, and the mole fraction of krypton is: 99.9-99.95%;

[0043] Step Five: The liquid phase rectified by the krypton-xenon separation column 2 in Step Two enters the high-purity xenon column 4 through the bottom liquid outlet of the krypton-xenon separation column 2, and is rectified by providing heat and cold through the bottom liquid-phase electric heater 7 and the third top condenser 11 of the high-purity xenon column. The rectified liquid phase is transported into the xenon gas manifold 20 through the bottom liquid outlet of the high-purity xenon column 4, the xenon gas vaporizer 14, the xenon gas aspirator 18, and the xenon gas membrane compressor 19; the liquid temperature at the bottom liquid outlet of the high-purity xenon column 4 is -80 to -82 °C, and the xenon mole fraction is 99.5 to 99.9%; the outlet temperature of the xenon gas aspirator 18 is 20 to 25 °C, and the xenon mole fraction is 99.9997 to 99.9999%;

[0044] Step Six: The gas phase at the top of the high-purity xenon column 4 in Step Five exchanges heat through the tube side of the third top condenser 11 and enters the high-purity xenon column 4 through the reflux port 50 of the high-purity xenon column for re-rectification;

[0045] Step Seven: The liquid nitrogen in the liquid nitrogen storage tank 12 enters the first three-way valve 43 through the first outlet 49 of the liquid nitrogen storage tank. Part of the liquid nitrogen enters the shell side of the first top condenser 9 through the sixth regulating valve 52 and the shell side inlet of the first top condenser 9; another part of the liquid nitrogen enters the shell side of the second top condenser 10 through the seventh regulating valve 27 and the third shell side inlet 47; the temperature of the liquid nitrogen entering the shell side of the first top condenser 9 through the sixth regulating valve 26 is -174 to -176 °C, and the flow rate is 15 to 25 Nm 3 / h; the temperature of the liquid nitrogen entering the shell side of the second top condenser 10 through the seventh regulating valve 27 is -174 to -176 °C, and the flow rate is 10 to 15 Nm 3 / h;

[0046] Step Eight: The liquid nitrogen in the liquid nitrogen storage tank 12 enters the shell side of the third top condenser 11 through the second outlet 48 of the liquid nitrogen storage tank and the first shell side inlet 45. The temperature of the liquid nitrogen entering the shell side of the third top condenser 11 through the first shell side inlet 45 is -174 to -176 °C, and the flow rate is 5 to 10 Nm 3 / h;

[0047] Step Nine: The gas phase at the shell side gas outlet of the first top condenser 9 in Step Seven enters the second three-way valve 42. Part of the gas phase enters the shell side of the third top condenser 11 through the eleventh regulating valve 31 and the second shell side inlet 44; another part of the gas phase enters the shell side of the second top condenser 10 through the tenth regulating valve 30 and the fourth shell side inlet 46; the temperature of the gas phase at the shell side gas outlet of the first top condenser 9 is -174 to -176 °C, and the flow rate is 10 to 25 Nm 3 / h; The gas phase temperature entering the shell side of the third top condenser 11 through the second shell side inlet 44 is: -174 to -176 °C, and the flow rate is 5 to 10 Nm 3 / h;

[0048] Step Ten: The gas phase at the gas phase outlet of the shell side of the second top condenser 10 and the gas phase at the gas phase outlet of the shell side of the third top condenser 11 in Step Nine enter the third inlet 37 of the main heat exchanger, and the gas phase exiting from the third outlet 41 of the main heat exchanger enters the regeneration gas storage tank 29; the gas phase temperature at the third outlet 41 of the main heat exchanger is 35 to 40 °C, and the pressure is 0.65 to 0.70 MPa.

[0049] The present invention purifies the crude krypton-xenon mixed gas. Specifically, it adopts a gas-liquid mixed nitrogen refrigeration and krypton-xenon getter adsorption process to rectify and adsorb and purify krypton and xenon, obtaining a production device and a production process with the purity of krypton-xenon products not less than 99.9995%. Among them, the quality of ultra-pure krypton and xenon products is higher than the quality indexes of the national standards GB / T 5829-2006 "Krypton Gas" ≥99.999% and GB / T 5828-2006 "Xenon Gas" ≥99.9995%; the advantages of the process method of the present invention are as follows: 1. The product purity is high, meeting the use requirements of the semiconductor industry, aerospace, and scientific research; 2. The device process flow is simple. After the krypton gas and xenon gas exiting the high-purity krypton column and the high-purity xenon column are vaporized by the corresponding vaporizers respectively, ultra-pure krypton gas and ultra-pure xenon gas can be obtained; 3. The evaporated nitrogen gas of the first top condenser of the present invention can provide part of the cold energy required in the production process for the second top condenser and the third top condenser, maximizing the energy utilization; 4. The present invention is respectively provided with a krypton gas vaporizer and a xenon gas vaporizer behind the high-purity krypton column and the high-purity xenon column. After being fully vaporized, they enter the krypton gas getter and the xenon gas getter, reducing the volume and floor area of the krypton gas getter and the xenon gas getter; 5. The present invention designs the filling manifolds for krypton gas and xenon gas together, and the device design is comprehensive.

[0050] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. All other embodiments obtained by those of ordinary skill in the art within the scope of the present invention without making creative efforts shall fall within the protection scope of the present invention.

[0051] Example 1

[0052] A production device for producing ultra-pure krypton-xenon using a krypton-xenon getter, comprising a crude krypton-xenon gas pipeline 22, the crude krypton-xenon gas pipeline 22 is connected to the inlet of a krypton-xenon separation tower 2, the bottom liquid phase outlet of the krypton-xenon separation tower 2 is connected to the inlet of a high-purity xenon tower 4, and the bottom liquid phase outlet of the high-purity xenon tower 4 is sequentially connected to a xenon gas vaporizer 14, a xenon gas getter 18 and a xenon gas membrane compressor 19 and then to a xenon gas manifold 20; the gas phase outlet at the top of the krypton-xenon separation tower 2 is connected to the tube side of a first top condenser 9 and then to a first gas-liquid separator 8, the gas phase outlet of the first gas-liquid separator 8 is connected to the inlet of a high-purity krypton tower 3, the gas phase outlet at the top of the high-purity krypton tower 3 is connected to the tube side of a second top condenser 10 and then to a second gas-liquid separator 38, and the second liquid phase outlet of the second gas-liquid separator 38 is sequentially connected to a krypton gas vaporizer 13, a krypton gas getter 15 and a krypton gas membrane compressor 16 and then to a krypton gas manifold 17. At the inner bottom of the krypton-xenon separation tower 2, the high-purity krypton tower 3 and the high-purity xenon tower 4, there are respectively provided a krypton-xenon separation tower bottom electric heater 5, a high-purity krypton tower bottom electric heater 6 and a high-purity xenon tower electric heater 7. The crude krypton-xenon gas pipeline 22 is connected to the inlet of the krypton-xenon separation tower 2 through a first regulating valve 21, the first main heat exchanger inlet 35 and the first main heat exchanger outlet 39 of a main heat exchanger 1. The liquid phase outlet of the first gas-liquid separator 8 is connected to the separation tower reflux port 49 at the upper part of the krypton-xenon separation tower 2. The gas phase outlet at the top of the second gas-liquid separator 38 is connected to a recovery device 34 through a third regulating valve 23, the second main heat exchanger inlet 36 and the second main heat exchanger outlet 40 of the main heat exchanger 1; the first liquid phase outlet of the second gas-liquid separator 38 is connected to the high-purity krypton tower reflux port 51 at the upper part of the high-purity krypton tower 3 through a fourth regulating valve 24; a fifth regulating valve 25 is provided between the second liquid phase outlet of the second gas-liquid separator 38 and the krypton gas vaporizer 13. The gas phase outlet at the top of the high-purity xenon tower 4 is connected to the high-purity xenon tower reflux port 50 provided at the upper part of the high-purity xenon tower 4 through the tube side of a third top condenser 11. It further includes a liquid nitrogen storage tank 12, the second liquid nitrogen storage tank outlet 48 of the liquid nitrogen storage tank 12 is connected to the first shell side inlet 45 of the third top condenser 11 through an eighth regulating valve 28; the first liquid nitrogen storage tank outlet 26 of the liquid nitrogen storage tank 12 is connected to the shell side inlet of the first top condenser 9 through a first three-way joint 43 and a sixth regulating valve 52, the shell side gas phase outlet of the first top condenser 9 is connected to the second shell side inlet 44 of the third top condenser 11 through a second three-way joint 42 and an eleventh regulating valve 31, the third end of the first three-way joint 43 is connected to the third shell side inlet 47 of the second top condenser 10 through a seventh regulating valve 27, and the third end of the second three-way joint 42 is connected to the fourth shell side inlet 46 of the second top condenser 10 through a tenth regulating valve 30. The shell side gas phase outlets of the second top condenser 10 and the third top condenser 11 are respectively connected to the third main heat exchanger inlet 37 of the main heat exchanger 1 through pipelines, and the main heat exchanger third outlet 41 is connected to a regenerated gas storage tank 29.A second regulating valve 32 is provided between the shell-side gas phase outlet of the second top condenser 10 and the third inlet 37 of the main heat exchanger of the main heat exchanger 1, and a ninth regulating valve 33 is provided between the shell-side gas phase outlet of the third top condenser 11 and the third inlet 37 of the main heat exchanger of the main heat exchanger 1.

[0053] A production process of a production device for producing ultra-pure krypton and xenon using a krypton-xenon getter includes the following steps:

[0054] Step 1: The crude krypton-xenon gas from the crude krypton-xenon gas pipeline 22 passes through the first regulating valve 21 and then enters the krypton-xenon separation tower 2 through the first inlet 35 and the first outlet 39 of the main heat exchanger, and is rectified by the krypton-xenon separation tower bottom electric heater 5 and the first top condenser 9 to provide heat and cold respectively. The temperature of the crude krypton-xenon gas is 20 - 30 °C, the pressure is 0.4 Mpa, the flow rate is 10 Nm 3 / h, the gas phase fraction is 1, and the krypton-xenon content is 95 - 99%;

[0055] Step 2: The crude krypton-xenon gas entering the krypton-xenon separation tower 2 in Step 1 is rectified and purified once. The gas phase after rectification and purification passes through the gas phase outlet at the top of the krypton-xenon separation tower 2 and the tube side of the first top condenser 9 and enters the first gas-liquid separator 8 for gas-liquid separation. The liquid phase after gas-liquid separation enters the krypton-xenon separation tower 2 through the separation tower reflux port 49 for re-rectification and purification, and the gas phase after gas-liquid separation enters the high-purity krypton tower 3 through the gas phase outlet of the first gas-liquid separator 8. The liquid phase temperature of the first gas-liquid separator 8 is -105.2 - -106.5 °C, and the molar fraction of krypton is 90%; the gas phase temperature of the first gas-liquid separator 8 is -105.2 - -106.5 °C, and the molar fraction of krypton is 99.9%;

[0056] Step 3: After the gas phase outlet of the first gas-liquid separator 8 described in Step 2 enters the high-purity krypton tower 3, it is rectified by the high-purity krypton tower bottom electric heater 6 and the second top condenser 10 to provide heat and cold. The gas phase after rectification passes through the gas phase outlet at the top of the high-purity krypton tower 3 and the tube side of the second top condenser 10 and enters the second gas-liquid separator 38 for gas-liquid separation. A part of the liquid phase after gas-liquid separation is refluxed to the high-purity krypton tower 3 through the fourth regulating valve 24 and the high-purity krypton tower reflux port 51 for re-rectification; another part of the liquid phase after gas-liquid separation is sequentially transported to the krypton gas manifold 17 through the fifth regulating valve 25, the krypton gas vaporizer 13, the krypton gas getter 15, and the krypton gas membrane compressor 16. The liquid phase temperature after gas-liquid separation in the second gas-liquid separator 38 is -135 - -138 °C, and the molar fraction of krypton is 99.995%; the temperature at the outlet of the krypton gas getter 15 is 20 - 25 °C, and the molar fraction of krypton transported to the krypton gas manifold 17 is 99.9995%;

[0057] Step 4: The gas phase after gas-liquid separation by the second gas-liquid separator 38 in Step 3 enters the recovery unit 34 through the third regulating valve 23, the second inlet 36 of the main heat exchanger of the main heat exchanger 1, and the second outlet 40 of the main heat exchanger; the temperature of the gas phase at the outlet of the second outlet 40 of the main heat exchanger is 35-40 °C, and the mole fraction of krypton is 99.9%;

[0058] Step 5: The liquid phase rectified by the krypton-xenon separation column 2 in Step 2 enters the high-purity xenon column 4 through the bottom liquid outlet of the krypton-xenon separation column 2, and is rectified by providing heat and cold through the high-purity xenon column bottom electric heater 7 and the third top condenser 11. The rectified liquid phase is transported to the xenon gas manifold 20 through the bottom liquid outlet of the high-purity xenon column 4, the xenon gas vaporizer 14, the xenon gas aspirator 18, and the xenon gas membrane compressor 19; the temperature of the liquid phase at the bottom liquid outlet of the high-purity xenon column 4 is -80 to -82 °C, and the mole fraction of xenon is 99.5%; the outlet temperature of the xenon gas aspirator 18 is 20-25 °C, and the mole fraction of xenon is 99.9997%;

[0059] Step 6: The gas phase at the top of the high-purity xenon column 4 in Step 5 is heat-exchanged through the tube side of the third top condenser 11 and enters the high-purity xenon column 4 through the high-purity xenon column reflux port 50 for re-rectification;

[0060] Step 7: The liquid nitrogen in the liquid nitrogen storage tank 12 enters the first three-way valve 43 through the first outlet 49 of the liquid nitrogen storage tank. Part of the liquid nitrogen enters the shell side of the first top condenser 9 through the sixth regulating valve 52 and the shell side inlet of the first top condenser 9; another part of the liquid nitrogen enters the shell side of the second top condenser 10 through the seventh regulating valve 27 and the third shell side inlet 47; the temperature of the liquid nitrogen entering the shell side of the first top condenser 9 through the sixth regulating valve 26 is -174 to -176 °C, and the flow rate is 15 Nm 3 / h; the temperature of the liquid nitrogen entering the shell side of the second top condenser 10 through the seventh regulating valve 27 is -174 to -176 °C, and the flow rate is 10 Nm 3 / h;

[0061] Step 8: The liquid nitrogen in the liquid nitrogen storage tank 12 enters the shell side of the third top condenser 11 through the second outlet 48 of the liquid nitrogen storage tank and the first shell side inlet 45. The temperature of the liquid nitrogen entering the shell side of the third top condenser 11 through the first shell side inlet 45 is -174 to -176 °C, and the flow rate is 5 Nm 3 / h;

[0062] Step Nine: The gas phase at the shell side gas outlet of the first top condenser 9 in Step Seven enters the second three-way valve 42. A part of the gas phase enters the shell side of the third top condenser 11 through the eleventh regulating valve 31 and the second shell side inlet 44; another part of the gas phase enters the shell side of the second top condenser 10 through the tenth regulating valve 30 and the fourth shell side inlet 46; the temperature of the gas phase at the shell side gas outlet of the first top condenser 9 is: -174 to -176 °C, and the flow rate is 10 Nm 3 / h; the temperature of the gas phase entering the shell side of the third top condenser 11 through the second shell side inlet 44 is: -174 to -176 °C, and the flow rate is 5 Nm 3 / h;

[0063] Step Ten: The gas phase at the shell side gas outlet of the second top condenser 10 and the gas phase at the shell side gas outlet of the third top condenser 11 in Step Nine enter the third inlet 37 of the main heat exchanger. The gas phase exiting from the third outlet 41 of the main heat exchanger enters the regenerated gas storage tank 29; the temperature of the gas phase exiting from the third outlet 41 of the main heat exchanger is 35 to 40 °C, and the pressure is 0.65 to 0.70 MPa.

[0064] Example 2

[0065] A production device for producing ultra-pure krypton and xenon using a krypton-xenon getter, comprising a crude krypton-xenon gas pipeline 22, the crude krypton-xenon gas pipeline 22 is connected to the inlet of a krypton-xenon separation tower 2, the bottom liquid phase outlet of the krypton-xenon separation tower 2 is connected to the inlet of a high-purity xenon tower 4, and the bottom liquid phase outlet of the high-purity xenon tower 4 is successively connected to a xenon gas vaporizer 14, a xenon gas getter 18 and a xenon gas membrane compressor 19 and then connected to a xenon gas manifold 20; the gas phase outlet at the top of the krypton-xenon separation tower 2 is connected to the tube side of a first top condenser 9 and then connected to a first gas-liquid separator 8, the gas phase outlet of the first gas-liquid separator 8 is connected to the inlet of a high-purity krypton tower 3, the gas phase outlet at the top of the high-purity krypton tower 3 is connected to the tube side of a second top condenser 10 and then connected to a second gas-liquid separator 38, and the second liquid phase outlet of the second gas-liquid separator 38 is successively connected to a krypton gas vaporizer 13, a krypton gas getter 15 and a krypton gas membrane compressor 16 and then connected to a krypton gas manifold 17. Electric heaters for the bottom of the krypton-xenon separation tower kettle 5, the high-purity krypton tower kettle 6 and the high-purity xenon tower 7 are respectively provided at the inner bottoms of the krypton-xenon separation tower 2, the high-purity krypton tower 3 and the high-purity xenon tower 4. The crude krypton-xenon gas pipeline 22 is connected to the inlet of the krypton-xenon separation tower 2 through a first regulating valve 21, the first inlet 35 of the main heat exchanger of the main heat exchanger 1 and the first outlet 39 of the main heat exchanger. The liquid phase outlet of the first gas-liquid separator 8 is connected to the separation tower reflux port 49 at the upper part of the krypton-xenon separation tower 2. The gas phase outlet at the top of the second gas-liquid separator 38 is connected to a recovery device 34 through a third regulating valve 23, the second inlet 36 of the main heat exchanger of the main heat exchanger 1 and the second outlet 40 of the main heat exchanger; the first liquid phase outlet of the second gas-liquid separator 38 is connected to the high-purity krypton tower reflux port 51 at the upper part of the high-purity krypton tower 3 through a fourth regulating valve 24; a fifth regulating valve 25 is provided between the second liquid phase outlet of the second gas-liquid separator 38 and the krypton gas vaporizer 13. The gas phase outlet at the top of the high-purity xenon tower 4 is connected to the high-purity xenon tower reflux port 50 provided at the upper part of the high-purity xenon tower 4 through the tube side of a third top condenser 11. It further includes a liquid nitrogen storage tank 12, the second outlet 48 of the liquid nitrogen storage tank 12 is connected to the first shell side inlet 45 of the third top condenser 11 through an eighth regulating valve 28; the first outlet 26 of the liquid nitrogen storage tank 12 is connected to the shell side inlet of the first top condenser 9 through a first three-way joint 43 and a sixth regulating valve 52, the shell side gas phase outlet of the first top condenser 9 is connected to the second shell side inlet 44 of the third top condenser 11 through a second three-way joint 42 and an eleventh regulating valve 31, the third end of the first three-way joint 43 is connected to the third shell side inlet 47 of the second top condenser 10 through a seventh regulating valve 27, and the third end of the second three-way joint 42 is connected to the fourth shell side inlet 46 of the second top condenser 10 through a tenth regulating valve 30. The shell side gas phase outlets of the second top condenser 10 and the third top condenser 11 are respectively connected to the third inlet 37 of the main heat exchanger of the main heat exchanger 1 through pipelines, and the main heat exchanger third outlet 41 is connected to a regeneration gas storage tank 29.A second regulating valve 32 is provided between the shell-side gas phase outlet of the second top condenser 10 and the third inlet 37 of the main heat exchanger of the main heat exchanger 1, and a ninth regulating valve 33 is provided between the shell-side gas phase outlet of the third top condenser 11 and the third inlet 37 of the main heat exchanger of the main heat exchanger 1.

[0066] A production process of a production device for producing ultra-pure krypton and xenon using a krypton-xenon getter includes the following steps:

[0067] Step 1: The crude krypton-xenon gas from the crude krypton-xenon gas pipeline 22 passes through the first regulating valve 21 and then enters the krypton-xenon separation tower 2 through the first inlet 35 and the first outlet 39 of the main heat exchanger, and is rectified by the krypton-xenon separation tower bottom electric heater 5 and the first top condenser 9 to provide heat and cold respectively. The temperature of the crude krypton-xenon gas is 20 - 30 °C, the pressure is 0.4 Mpa, the flow rate is 10 Nm 3 / h, the gas phase fraction is 1, and the krypton-xenon content is 95 - 99%;

[0068] Step 2: The crude krypton-xenon gas entering the krypton-xenon separation tower 2 in Step 1 is rectified and purified once. The gas phase after rectification and purification passes through the gas phase outlet at the top of the krypton-xenon separation tower 2 and the tube side of the first top condenser 9 and enters the first gas-liquid separator 8 for gas-liquid separation. The liquid phase after gas-liquid separation enters the krypton-xenon separation tower 2 through the separation tower reflux port 49 for re-rectification and purification, and the gas phase after gas-liquid separation enters the high-purity krypton tower 3 through the gas phase outlet of the first gas-liquid separator 8. The liquid phase temperature of the first gas-liquid separator 8 is -105.2 - -106.5 °C, and the molar fraction of krypton is 95%; the gas phase temperature of the first gas-liquid separator 8 is -105.2 - -106.5 °C, and the molar fraction of krypton is 99.95%;

[0069] Step 3: After the gas phase outlet of the first gas-liquid separator 8 described in Step 2 enters the high-purity krypton tower 3, it is rectified by the high-purity krypton tower bottom electric heater 6 and the second top condenser 10 to provide heat and cold. The gas phase after rectification passes through the gas phase outlet at the top of the high-purity krypton tower 3 and the tube side of the second top condenser 10 and enters the second gas-liquid separator 38 for gas-liquid separation. A part of the liquid phase after gas-liquid separation is refluxed to the high-purity krypton tower 3 through the fourth regulating valve 24 and the high-purity krypton tower reflux port 51 for re-rectification; another part of the liquid phase after gas-liquid separation is sequentially transported to the krypton gas manifold 17 through the fifth regulating valve 25, the krypton gas vaporizer 13, the krypton gas getter 15, and the krypton gas membrane compressor 16. The liquid phase temperature after gas-liquid separation in the second gas-liquid separator 38 is -135 - -138 °C, and the molar fraction of krypton is 99.999%; the temperature at the outlet of the krypton gas getter 15 is 20 - 25 °C, and the molar fraction of krypton transported to the krypton gas manifold 17 is 99.9999%;

[0070] Step 4: The gas phase after gas-liquid separation by the second gas-liquid separator 38 in Step 3 enters the recovery unit 34 through the third regulating valve 23, the second inlet 36 of the main heat exchanger of the main heat exchanger 1, and the second outlet 40 of the main heat exchanger; the temperature of the gas phase at the second outlet 40 of the main heat exchanger is 35-40 °C, and the molar fraction of krypton is 99.95%;

[0071] Step 5: The liquid phase rectified by the krypton-xenon separation column 2 in Step 2 enters the high-purity xenon column 4 through the bottom liquid outlet of the krypton-xenon separation column 2, and is rectified by providing heat and cold through the high-purity xenon column bottom electric heater 7 and the third top condenser 11. The rectified liquid phase is transported to the xenon manifold 20 through the bottom liquid outlet of the high-purity xenon column 4, the xenon vaporizer 14, the xenon aspirator 18, and the xenon membrane compressor 19; the temperature of the liquid phase at the bottom liquid outlet of the high-purity xenon column 4 is -80 to -82 °C, and the molar fraction of xenon is 99.9%; the outlet temperature of the xenon aspirator 18 is 20-25 °C, and the molar fraction of xenon is 99.9999%;

[0072] Step 6: The gas phase at the top of the high-purity xenon column 4 in Step 5 is heat-exchanged through the tube side of the third top condenser 11 and enters the high-purity xenon column 4 through the high-purity xenon column reflux port 50 for re-rectification;

[0073] Step 7: The liquid nitrogen in the liquid nitrogen storage tank 12 enters the first three-way 43 through the first outlet 49 of the liquid nitrogen storage tank. Part of the liquid nitrogen enters the shell side of the first top condenser 9 through the sixth regulating valve 52 and the shell side inlet of the first top condenser 9; another part of the liquid nitrogen enters the shell side of the second top condenser 10 through the seventh regulating valve 27 and the third shell side inlet 47; the temperature of the liquid nitrogen entering the shell side of the first top condenser 9 through the sixth regulating valve 26 is -174 to -176 °C, and the flow rate is 25 Nm 3 / h; the temperature of the liquid nitrogen entering the shell side of the second top condenser 10 through the seventh regulating valve 27 is -174 to -176 °C, and the flow rate is 15 Nm 3 / h;

[0074] Step 8: The liquid nitrogen in the liquid nitrogen storage tank 12 enters the shell side of the third top condenser 11 through the second outlet 48 of the liquid nitrogen storage tank and the first shell side inlet 45. The temperature of the liquid nitrogen entering the shell side of the third top condenser 11 through the first shell side inlet 45 is -174 to -176 °C, and the flow rate is 10 Nm 3 / h;

[0075] Step Nine: The gas phase at the shell-side gas phase outlet of the first top condenser 9 in Step Seven enters the second three-way valve 42. A part of the gas phase enters the shell side of the third top condenser 11 through the eleventh regulating valve 31 and the second shell-side inlet 44; another part of the gas phase enters the shell side of the second top condenser 10 through the tenth regulating valve 30 and the fourth shell-side inlet 46; the temperature of the gas phase at the shell-side gas phase outlet of the first top condenser 9 is: -174 to -176 °C, and the flow rate is 25 Nm 3 / h; the temperature of the gas phase entering the shell side of the third top condenser 11 through the second shell-side inlet 44 is: -174 to -176 °C, and the flow rate is 10 Nm 3 / h;

[0076] Step Ten: The gas phase at the shell-side gas phase outlet of the second top condenser 10 and the gas phase at the shell-side gas phase outlet of the third top condenser 11 in Step Nine enter the third inlet 37 of the main heat exchanger. The gas phase exiting from the third outlet 41 of the main heat exchanger enters the regenerated gas storage tank 29; the temperature of the gas phase exiting from the third outlet 41 of the main heat exchanger is 35 to 40 °C, and the pressure is 0.65 to 0.70 MPa.

[0077] Example 3

[0078] A production device for producing ultra-pure krypton-xenon by using a krypton-xenon getter, comprising a crude krypton-xenon gas pipeline 22, the crude krypton-xenon gas pipeline 22 being connected to the inlet of a krypton-xenon separation tower 2, the bottom liquid phase outlet of the krypton-xenon separation tower 2 being connected to the inlet of a high-purity xenon tower 4, the bottom liquid phase outlet of the high-purity xenon tower 4 being sequentially connected to a xenon gas vaporizer 14, a xenon gas getter 18 and a xenon gas membrane compressor 19 and then connected to a xenon gas manifold 20; the gas phase outlet at the top of the krypton-xenon separation tower 2 is connected to the tube side of a first top condenser 9 and then connected to a first gas-liquid separator 8, the gas phase outlet of the first gas-liquid separator 8 being connected to the inlet of a high-purity krypton tower 3, the gas phase outlet at the top of the high-purity krypton tower 3 is connected to the tube side of a second top condenser 10 and then connected to a second gas-liquid separator 38, the second liquid phase outlet of the second gas-liquid separator 38 being sequentially connected to a krypton gas vaporizer 13, a krypton gas getter 15 and a krypton gas membrane compressor 16 and then connected to a krypton gas manifold 17. Electric heaters 5 for the bottom of the krypton-xenon separation tower, 6 for the bottom of the high-purity krypton tower and 7 for the high-purity xenon tower are respectively provided at the inner bottoms of the krypton-xenon separation tower 2, the high-purity krypton tower 3 and the high-purity xenon tower 4. The crude krypton-xenon gas pipeline 22 is connected to the inlet of the krypton-xenon separation tower 2 through a first regulating valve 21, the first inlet 35 and the first outlet 39 of the main heat exchanger 1 of the main heat exchanger. The liquid phase outlet of the first gas-liquid separator 8 is connected to the separation tower reflux port 49 at the upper part of the krypton-xenon separation tower 2. The gas phase outlet at the top of the second gas-liquid separator 38 is connected to a recovery device 34 through a third regulating valve 23, the second inlet 36 and the second outlet 40 of the main heat exchanger 1 of the main heat exchanger; the first liquid phase outlet of the second gas-liquid separator 38 is connected to the high-purity krypton tower reflux port 51 at the upper part of the high-purity krypton tower 3 through a fourth regulating valve 24; a fifth regulating valve 25 is provided between the second liquid phase outlet of the second gas-liquid separator 38 and the krypton gas vaporizer 13. The gas phase outlet at the top of the high-purity xenon tower 4 is connected to the high-purity xenon tower reflux port 50 provided at the upper part of the high-purity xenon tower 4 through the tube side of a third top condenser 11. It further comprises a liquid nitrogen storage tank 12, the second outlet 48 of the liquid nitrogen storage tank 12 being connected to the first shell side inlet 45 of the third top condenser 11 through an eighth regulating valve 28; the first outlet 26 of the liquid nitrogen storage tank 12 being connected to the shell side inlet of the first top condenser 9 through a first three-way joint 43 and a sixth regulating valve 52, the shell side gas phase outlet of the first top condenser 9 being connected to the second shell side inlet 44 of the third top condenser 11 through a second three-way joint 42 and an eleventh regulating valve 31, the third end of the first three-way joint 43 being connected to the third shell side inlet 47 of the second top condenser 10 through a seventh regulating valve 27, the third end of the second three-way joint 42 being connected to the fourth shell side inlet 46 of the second top condenser 10 through a tenth regulating valve 30. The shell side gas phase outlets of the second top condenser 10 and the third top condenser 11 are respectively connected to the third inlet 37 of the main heat exchanger 1 of the main heat exchanger through pipelines, and the third outlet 41 of the main heat exchanger is connected to a regeneration gas storage tank 29.A second regulating valve 32 is provided between the shell-side gas phase outlet of the second top condenser 10 and the third inlet 37 of the main heat exchanger of the main heat exchanger 1, and a ninth regulating valve 33 is provided between the shell-side gas phase outlet of the third top condenser 11 and the third inlet 37 of the main heat exchanger of the main heat exchanger 1.

[0079] A production process of a production device for producing ultra-pure krypton and xenon using a krypton-xenon getter includes the following steps:

[0080] Step 1: The crude krypton-xenon gas from the crude krypton-xenon gas pipeline 22 passes through the first regulating valve 21 and then enters the krypton-xenon separation tower 2 through the first inlet 35 and the first outlet 39 of the main heat exchanger, and is rectified by the krypton-xenon separation tower bottom electric heater 5 and the first top condenser 9 to provide heat and cold respectively. The temperature of the crude krypton-xenon gas is 20 - 30 °C, the pressure is 0.4 Mpa, the flow rate is 10 Nm 3 / h, the gas phase fraction is 1, and the krypton-xenon content is 95 - 99%;

[0081] Step 2: The crude krypton-xenon gas entering the krypton-xenon separation tower 2 in Step 1 is rectified and purified once. The gas phase after rectification and purification enters the first gas-liquid separator 8 through the gas phase outlet at the top of the krypton-xenon separation tower 2 and the tube side of the first top condenser 9 for gas-liquid separation. The liquid phase after gas-liquid separation enters the krypton-xenon separation tower 2 through the separation tower reflux port 49 for re-rectification and purification, and the gas phase after gas-liquid separation enters the high-purity krypton tower 3 through the gas phase outlet of the first gas-liquid separator 8; the liquid phase temperature of the first gas-liquid separator 8 is -105.2 - -106.5 °C, and the molar fraction of krypton is 90 - 95%; the gas phase temperature of the first gas-liquid separator 8 is -105.2 - -106.5 °C, and the molar fraction of krypton is 99.92%;

[0082] Step 3: After the gas phase outlet of the first gas-liquid separator 8 described in Step 2 enters the high-purity krypton tower 3, it is rectified by the high-purity krypton tower bottom electric heater 6 and the second top condenser 10 to provide heat and cold. The gas phase after rectification enters the second gas-liquid separator 38 through the gas phase outlet at the top of the high-purity krypton tower 3 and the tube side of the second top condenser 10 for gas-liquid separation. A part of the liquid phase after gas-liquid separation is refluxed to the high-purity krypton tower 3 through the fourth regulating valve 24 and the high-purity krypton tower reflux port 51 for re-rectification; another part of the liquid phase after gas-liquid separation is successively transported to the krypton gas manifold 17 through the fifth regulating valve 25, the krypton gas vaporizer 13, the krypton gas getter 15, and the krypton gas membrane compressor 16; the liquid phase temperature after gas-liquid separation in the second gas-liquid separator is -135 - -138 °C, and the molar fraction of krypton is 99.997%; the temperature at the outlet of the krypton gas getter 15 is 20 - 25 °C, and the molar fraction of krypton transported to the krypton gas manifold 17 is 99.9998%;

[0083] Step 4: The gas phase after gas-liquid separation by the second gas-liquid separator 38 in Step 3 enters the recovery unit 34 through the third regulating valve 23, the second inlet 36 of the main heat exchanger of the main heat exchanger 1, and the second outlet 40 of the main heat exchanger; the temperature of the gas phase at the outlet of the second outlet 40 of the main heat exchanger is 35-40 °C, and the molar fraction of krypton is 99.92%;

[0084] Step 5: The liquid phase rectified by the krypton-xenon separation column 2 in Step 2 enters the high-purity xenon column 4 through the bottom liquid outlet of the krypton-xenon separation column 2, and is rectified by providing heat and cold through the high-purity xenon column bottom electric heater 7 and the third top condenser 11. The rectified liquid phase is transported into the xenon gas manifold 20 through the bottom liquid outlet of the high-purity xenon column 4, the xenon gas vaporizer 14, the xenon gas aspirator 18, and the xenon gas membrane compressor 19; the temperature of the liquid phase at the bottom liquid outlet of the high-purity xenon column 4 is -80 to -82 °C, and the molar fraction of xenon is 99.7%; the outlet temperature of the xenon gas aspirator 18 is 20-25 °C, and the molar fraction of xenon is 99.9998%;

[0085] Step 6: The gas phase at the top of the high-purity xenon column 4 in Step 5 is heat-exchanged through the tube side of the third top condenser 11 and enters the high-purity xenon column 4 through the high-purity xenon column reflux port 50 for re-rectification;

[0086] Step 7: The liquid nitrogen in the liquid nitrogen storage tank 12 enters the first three-way 43 through the first outlet 49 of the liquid nitrogen storage tank. Part of the liquid nitrogen enters the shell side of the first top condenser 9 through the sixth regulating valve 52 and the shell side inlet of the first top condenser 9; another part of the liquid nitrogen enters the shell side of the second top condenser 10 through the seventh regulating valve 27 and the third shell side inlet 47; the temperature of the liquid nitrogen entering the shell side of the first top condenser 9 through the sixth regulating valve 26 is -174 to -176 °C, and the flow rate is 20 Nm 3 / h; the temperature of the liquid nitrogen entering the shell side of the second top condenser 10 through the seventh regulating valve 27 is -174 to -176 °C, and the flow rate is 12 Nm 3 / h;

[0087] Step 8: The liquid nitrogen in the liquid nitrogen storage tank 12 enters the shell side of the third top condenser 11 through the second outlet 48 of the liquid nitrogen storage tank and the first shell side inlet 45. The temperature of the liquid nitrogen entering the shell side of the third top condenser 11 through the first shell side inlet 45 is -174 to -176 °C, and the flow rate is 7 Nm 3 / h;

[0088] Step Nine: The gas phase at the shell-side gas outlet of the first top condenser 9 in Step Seven enters the second three-way valve 42. A part of the gas phase enters the shell side of the third top condenser 11 through the eleven-way regulating valve 31 and the second shell-side inlet 44; another part of the gas phase enters the shell side of the second top condenser 10 through the tenth regulating valve 30 and the fourth shell-side inlet 46; the temperature of the gas phase at the shell-side gas outlet of the first top condenser 9 is: -174 to -176 °C, and the flow rate is 17 Nm 3 / h; the temperature of the gas phase entering the shell side of the third top condenser 11 through the second shell-side inlet 44 is: -174 to -176 °C, and the flow rate is 8 Nm 3 / h;

[0089] Step Ten: The gas phase at the shell-side gas outlet of the second top condenser 10 and the gas phase at the shell-side gas outlet of the third top condenser 11 in Step Nine enter the third inlet 37 of the main heat exchanger. The gas phase exiting from the third outlet 41 of the main heat exchanger enters the regenerated gas storage tank 29; the temperature of the gas phase exiting from the third outlet 41 of the main heat exchanger is 35 to 40 °C, and the pressure is 0.65 to 0.70 MPa.

[0090] In the description of the present invention, it should be noted that unless otherwise clearly specified and defined, terms such as "connection" and "connection" should be understood in a broad sense. For example, it can be a fixed connection, an integral connection, or a detachable connection; it can also be the communication inside two components; it can be directly connected or indirectly connected through an intermediate medium. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances. The above examples are only specific descriptions of the feasible implementation modes of the present invention, and they are not intended to limit the protection scope of the present invention. All equivalent implementation modes, changes, and modifications made without departing from the technical spirit of the present invention should be included within the protection scope of the present invention.

Claims

1. A production device for producing ultra-pure krypton-xenon by using a krypton-xenon getter, comprising a crude krypton-xenon gas pipeline (22), characterized in that: The crude krypton-xenon gas pipeline (22) is connected to the inlet of the krypton-xenon separation column (2). The bottom liquid phase outlet of the krypton-xenon separation column (2) is connected to the inlet of the high-purity xenon column (4). The bottom liquid phase outlet of the high-purity xenon column (4) is successively connected to the xenon gas vaporizer (14), the xenon gas aspirator (18), and the xenon gas membrane compressor (19) and then connected to the xenon gas manifold (20). The gas phase outlet at the top of the krypton-xenon separation column (2) is connected to the first gas-liquid separator (8) through the tube side of the first top condenser (9). The gas phase outlet of the first gas-liquid separator (8) is connected to the inlet of the high-purity krypton column (3). The gas phase outlet at the top of the high-purity krypton column (3) is connected to the second gas-liquid separator (38) through the tube side of the second top condenser (10). The second liquid phase outlet of the second gas-liquid separator (38) is successively connected to the krypton gas vaporizer (13), the krypton gas aspirator (15), and the krypton gas membrane compressor (16) and then connected to the krypton gas manifold (17). The inner bottoms of the krypton-xenon separation column (2), the high-purity krypton column (3), and the high-purity xenon column (4) are respectively provided with a krypton-xenon separation column bottom electric heater (5), a high-purity krypton column bottom electric heater (6), and a high-purity xenon column electric heater (7). The crude krypton-xenon gas pipeline (22) is connected to the inlet of the krypton-xenon separation column (2) through the first regulating valve (21), the first inlet (35) of the main heat exchanger of the main heat exchanger (1), and the first outlet (39) of the main heat exchanger.

2. The production device for producing ultra-pure krypton-xenon by using a krypton-xenon getter, according to claim 1, is characterized in that: The liquid phase outlet of the first gas-liquid separator (8) is connected to the separation column reflux port (49) at the upper part of the krypton-xenon separation column (2).

3. The production device for producing ultra-pure krypton-xenon by using a krypton-xenon getter as claimed in claim 1, characterized in that: The gas phase outlet at the top of the second gas-liquid separator (38) is connected to the recovery unit (34) through the third regulating valve (23), the second inlet (36) of the main heat exchanger of the main heat exchanger (1), and the second outlet (40) of the main heat exchanger. The first liquid phase outlet of the second gas-liquid separator (38) is connected to the high-purity krypton column reflux port (51) at the upper part of the high-purity krypton column (3) through the fourth regulating valve (24). A fifth regulating valve (25) is provided between the second liquid phase outlet of the second gas-liquid separator (38) and the krypton gas vaporizer (13).

4. A production device for producing ultra-pure krypton-xenon using a krypton-xenon getter, characterized in that: The gas phase outlet at the top of the high-purity xenon column (4) is connected to the high-purity xenon column reflux port (50) provided at the upper part of the high-purity xenon column (4) through the tube side of the third top condenser (11).

5. A production device for producing ultra-pure krypton-xenon using a krypton-xenon getter, characterized in that: It further includes a liquid nitrogen storage tank (12). The second outlet (48) of the liquid nitrogen storage tank (12) is connected to the first shell side inlet (45) of the third top condenser (11) through the eighth regulating valve (28). The first outlet (26) of the liquid nitrogen storage tank (12) is connected to the shell side inlet of the first top condenser (9) through the first three-way joint (43) and the sixth regulating valve (52). The shell side gas phase outlet of the first top condenser (9) is connected to the second shell side inlet (44) of the third top condenser (11) through the second three-way joint (42) and the eleventh regulating valve (31). The third end of the first three-way valve (43) is connected to the third shell-side inlet (47) of the second top condenser (10) through the seventh regulating valve (27), and the third end of the second three-way valve (42) is connected to the fourth shell-side inlet (46) of the second top condenser (10) through the tenth regulating valve (30).

6. The production device for producing ultra-pure krypton-xenon by using a krypton-xenon getter according to claim 5, characterized in that: The shell-side gas-phase outlets of the second top condenser (10) and the third top condenser (11) are respectively connected to the third main heat exchanger inlet (37) of the main heat exchanger (1) through pipelines, and the third main heat exchanger outlet (41) is connected to the regenerated gas storage tank (29).

7. The production device for producing ultra-pure krypton-xenon by using a krypton-xenon getter according to claim 6, characterized in that: A second regulating valve (32) is provided between the shell-side gas-phase outlet of the second top condenser (10) and the third main heat exchanger inlet (37) of the main heat exchanger (1), and a ninth regulating valve (33) is provided between the shell-side gas-phase outlet of the third top condenser (11) and the third main heat exchanger inlet (37) of the main heat exchanger (1).

8. A production process of a production device for producing ultra-pure krypton-xenon using a krypton-xenon getter, characterized in that: This production process includes the following steps: Step 1: The crude krypton-xenon gas from the crude krypton-xenon gas pipeline (22) passes through the first regulating valve (21) and then enters the krypton-xenon separation column (2) through the first inlet (35) and the first outlet (39) of the main heat exchanger, and is rectified by the krypton-xenon separation column bottom electric heater (5) and the first top condenser (9) to provide heat and cold respectively. The temperature of the crude krypton-xenon gas is 20 - 30 °C, the pressure is 0.4 Mpa, the flow rate is 10 Nm 3 / h, the gas phase fraction is 1, and the krypton-xenon content is 95 - 99%; Step two: The crude krypton-xenon gas entering the krypton-xenon separation column (2) in step one is subjected to primary rectification and purification. The gas phase after rectification and purification enters the first gas-liquid separator (8) through the gas-phase outlet at the top of the krypton-xenon separation column (2) and the tube side of the first top condenser (9) for gas-liquid separation. The liquid phase after gas-liquid separation enters the krypton-xenon separation column (2) through the separation column reflux port (49) for secondary rectification and purification, and the gas phase after gas-liquid separation enters the high-purity krypton column (3) through the gas-phase outlet of the first gas-liquid separator (8); the liquid phase temperature of the first gas-liquid separator (8): -105.2 to -106.5 °C, krypton mole fraction: 90 to 95%; The gas phase temperature of the first gas-liquid separator (8) is: -105.2 to -106.5 °C, krypton mole fraction: 99.9 to 99.95%; Step three: After the gas-phase outlet of the first gas-liquid separator (8) described in step two enters the high-purity krypton column (3), it is rectified by the high-purity krypton column kettle electric heater (6) and the second top condenser (10) to provide heat and cold. The gas phase after rectification enters the second gas-liquid separator (38) through the gas-phase outlet at the top of the high-purity krypton column (3) and the tube side of the second top condenser (10) for gas-liquid separation. A part of the liquid phase after gas-liquid separation is refluxed to the high-purity krypton column (3) through the fourth regulating valve (24) and the high-purity krypton column reflux port (51) for secondary rectification; another part of the liquid phase after gas-liquid separation is successively transported to the krypton gas manifold (17) through the fifth regulating valve (25), the krypton gas vaporizer (13), the krypton gas aspirator (15) and the krypton gas membrane compressor (16); the liquid phase temperature after gas-liquid separation in the second gas-liquid separator (38): -135 to -138 °C, krypton mole fraction: 99.995 to 99.999%; the temperature at the outlet of the krypton gas aspirator (15) is: 20 to 25 °C, and the krypton mole fraction of the krypton gas transported to the krypton gas manifold (17): 99.9995 to 99.9999%; Step 4: The gas phase after gas-liquid separation by the second gas-liquid separator (38) in Step 3 enters the recovery unit (34) through the third regulating valve (23), the second inlet (36) of the main heat exchanger of the main heat exchanger (1), and the second outlet (40) of the main heat exchanger; the temperature of the gas phase at the outlet of the second outlet (40) of the main heat exchanger is 35 - 40 °C, and the mole fraction of krypton is 99.9 - 99.95%; Step 5: The liquid phase rectified by the krypton-xenon separation column (2) in Step 2 enters the high-purity xenon column (4) through the bottom liquid outlet of the krypton-xenon separation column (2), and is rectified by providing heat and cold through the high-purity xenon column bottom electric heater (7) and the third top condenser (11). The rectified liquid phase is transported to the xenon gas manifold (20) through the bottom liquid outlet of the high-purity xenon column (4), the xenon gas vaporizer (14), the xenon gas aspirator (18), and the xenon gas membrane compressor (19); the temperature of the liquid phase at the bottom liquid outlet of the high-purity xenon column (4) is -80 - 82 °C, and the mole fraction of xenon is 99.5 - 99.9%; the outlet temperature of the xenon gas aspirator (18) is 20 - 25 °C, and the mole fraction of xenon is 99.9997 - 99.9999%; Step 6: The gas phase at the top of the high-purity xenon column (4) in Step 5 exchanges heat through the tube side of the third top condenser (11) and enters the high-purity xenon column (4) through the high-purity xenon column reflux port (50) for re-rectification; Step Seven: The liquid nitrogen in the liquid nitrogen storage tank (12) enters the first three-way valve (43) through the first outlet (26) of the liquid nitrogen storage tank. Part of the liquid nitrogen enters the shell side of the first top condenser (9) through the sixth regulating valve (52) and the shell side inlet of the first top condenser (9); another part of the liquid nitrogen enters the shell side of the second top condenser (10) through the seventh regulating valve (27) and the third shell side inlet (47); the temperature of the liquid nitrogen entering the shell side of the first top condenser (9) through the sixth regulating valve (52) is: -174 to -176 °C, and the flow rate is 15 to 25 Nm 3 / h; the temperature of the liquid nitrogen entering the shell side of the second top condenser (10) through the seventh regulating valve (27) is: -174 to -176 °C, and the flow rate is 10 to 15 Nm 3 / h; Step Eight: The liquid nitrogen in the liquid nitrogen storage tank (12) enters the shell side of the third top condenser (11) through the second outlet (48) of the liquid nitrogen storage tank and the first shell side inlet (45). The temperature of the liquid nitrogen entering the shell side of the third top condenser (11) through the first shell side inlet (45) is -174 to -176 °C, and the flow rate is 5 to 10 Nm 3 / h; Step Nine: The gas phase at the shell-side gas outlet of the first top condenser (9) in Step Seven enters the second three-way (42). A part of the gas phase enters the shell side of the third top condenser (11) through the eleventh regulating valve (31) and the second shell-side inlet (44); another part of the gas phase enters the shell side of the second top condenser (10) through the tenth regulating valve (30) and the fourth shell-side inlet (46); the temperature of the gas phase at the shell-side gas outlet of the first top condenser (9) is: -174 to -176 °C, and the flow rate is 10 to 25 Nm 3 / h; the temperature of the gas phase entering the shell side of the third top condenser (11) through the second shell-side inlet (44) is: -174 to -176 °C, and the flow rate is 5 to 10 Nm 3 / h; Step 10: The gas phase at the shell side gas outlet of the second top condenser (10) and the gas phase at the shell side gas outlet of the third top condenser (11) in Step 9 enter the third inlet (37) of the main heat exchanger, and the gas phase at the outlet of the third outlet (41) of the main heat exchanger enters the regeneration gas storage tank (29); the temperature of the gas phase at the outlet of the third outlet (41) of the main heat exchanger is 35 - 40 °C, and the pressure is 0.65 - 0.70 MPa.

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