Multi-productization high-purity helium purification method

By combining cryogenic freezing with multi-stage adsorption, the problem of separating high-purity helium using traditional methods has been solved, achieving efficient helium purification and neon recovery, meeting the high-purity requirements of the semiconductor industry, and ensuring stable equipment operation and high recovery rate.

CN121341969APending Publication Date: 2026-01-16VACREE TECH
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Patent Information

Application Number
CN202511625552.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-11-07
Publication Date
2026-01-16

AI Technical Summary

Technical Problem

Traditional methods are difficult to effectively separate and purify high-purity helium, especially to meet the semiconductor industry's requirement of helium purity ≥99.9999%, and also suffer from problems such as complex equipment, high energy consumption, and low impurity separation efficiency.

Method used

A method combining low-temperature freezing and multi-stage adsorption is adopted. High-boiling-point gases and neon are removed through the first adsorption tank and the second adsorption tank, respectively. The solidification and separation of neon is achieved by utilizing the temperature difference. The continuous production of helium is achieved by monitoring and automatically controlling the neon in the freezing tank.

Benefits of technology

It achieves the purification of high-purity helium, meeting the requirements of the semiconductor industry, increasing the helium recovery rate to 98%, and achieving a purity of 99.99% for the by-product neon gas, while ensuring stable operation of the equipment and low maintenance costs.

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Abstract

The invention discloses a multi-productization high-purity helium purification method which comprises the following steps: S1, cooling helium feed gas containing neon gas and high-boiling-point gas to a first temperature interval, and adsorbing and removing liquefied high-boiling-point gas through a first adsorption tank to obtain helium mixed gas without the high-boiling-point gas; s2, the helium mixed gas with the high-boiling-point gas removed is cooled to a second temperature interval, neon is solidified and separated in the freezing tank, and unliquefied helium containing a trace amount of neon is output; s3, unliquefied helium containing trace neon is introduced into a second adsorption tank to adsorb residual neon, and a high-purity helium product is obtained; and S4, the solidified neon gas in the freezing tank is heated and gasified, and the recycled pure neon gas is output. According to the invention, a purification method of low-temperature freezing and multi-stage adsorption is adopted, so that the obtained product gas meets the requirement of ultra-pure helium and can also meet the use requirement of helium in the semiconductor industry, the working stages of the adsorption tank and the freezing tank can be automatically switched, and automatic control and continuous production are realized.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of helium purification, and in particular to a multi-product high-purity helium purification method. BACKGROUND

[0002] As a non-renewable rare gas, helium is widely used in semiconductor manufacturing (lithography gas), low-temperature superconducting (MRI, particle accelerator), space propulsion (coolant) and optical fiber production fields. Due to the high concentration of global helium resources (dominated by the United States and Qatar), China's dependence on foreign countries has been over 90% for a long time, and self-controllable helium extraction technology is urgently needed to ensure the safety of the supply chain.

[0003] At present, the semiconductor industry requires helium purity ≥ 99.9999%, and the traditional process is difficult to stabilize and meet the standards. According to the "Pure Helium, High-purity Helium and Ultra-pure Helium" GB / T4844-2011, the neon content in high-purity helium (99.999%) is <4ppm, and the neon content in ultra-pure helium (99.9999%) is <1ppm. If this standard is met, the de-neon process needs to be considered. However, neon (Ne) has a very low boiling point (-246.08°C), and its boiling point is close to that of helium (He), hydrogen (H2) and other light gases. The traditional low-temperature rectification method has high energy consumption and complex equipment; the traditional adsorption method (such as molecular sieve) has low selectivity for neon, and is easily disturbed by other components (such as N2, CH4); the traditional membrane separation method has low separation efficiency due to the small molecular dynamics diameter of neon (about 2.75Å). Moreover, in the industrial production process, the impurities of the raw gas are unstable, which leads to the freezing of trace high-boiling-point gas impurities (nitrogen, oxygen) at -258°C, affecting the continuous operation of the equipment. SUMMARY

[0004] To solve the technical problems in the background art, the present application provides a multi-product high-purity helium purification method.

[0005] The multi-product high-purity helium purification method provided by the present application comprises the following steps: S1, cooling the helium raw gas containing neon gas and high-boiling-point gas to a first temperature interval, adsorbing and removing liquefied high-boiling-point gas through a first adsorption tank, and obtaining helium gas mixed gas from which high-boiling-point gas is removed; S2, cooling the helium gas mixed gas from which high-boiling-point gas is removed to a second temperature interval, the second temperature interval being lower than the solidification temperature of neon gas and higher than the liquefaction temperature of helium gas, so that neon gas is solidified and separated in the freezing tank, and unliquefied helium gas containing trace neon gas is output; S3, passing the unliquefied helium gas containing trace neon gas into a second adsorption tank to adsorb residual neon gas, and obtaining high-purity helium gas product; S4, warming up the solidified neon gas in the freezing tank to gasify, and outputting recycled pure neon gas.

[0006] Preferably, the cold energy supply of the helium raw gas to the first temperature interval is dynamically switched by the control module, wherein: when the temperature sensor in the freezing tank detects that the temperature is higher than the critical temperature of neon solidification, the external liquid nitrogen is used to provide cold energy; when the temperature sensor in the freezing tank detects that the temperature reaches the second temperature interval and the helium flow sensor at the output end of the second adsorption tank detects a stable flow, the cold energy of the high-purity helium product is switched to the cooling link to realize the cold energy circulation supply.

[0007] Preferably, the cold energy of the high-purity helium product is transferred in the following order: first flows through the cooling flow channel connected with the freezing tank to pre-cool the helium mixed gas to be introduced into the freezing tank; and then flows through the cooling flow channel connected with the inlet of the first adsorption tank to pre-cool the helium raw gas.

[0008] Preferably, before S1, the method further comprises: introducing a circulating gas with the same components as the high-purity helium product into a closed circulating pipeline, wherein the first adsorption tank, the freezing tank and the second adsorption tank are sequentially connected in series in the circulating pipeline; and the external cold source continuously acts on the circulating gas until the temperature in the first adsorption tank is stably maintained in the first temperature interval and the temperature in the freezing tank is stably maintained at the lower limit of the second temperature interval.

[0009] Preferably, the circulating pipeline comprises an external pipeline section and a main pipeline section, wherein the first adsorption tank, the freezing tank and the second adsorption tank are connected in series on the main pipeline section, the storage tank and the booster pump for driving the circulating gas to circulate in the circulating pipeline are arranged on the external pipeline section, and the gas injection unit for injecting the circulating gas into the buffer tank is additionally provided on the storage tank.

[0010] Preferably, the working stages of the first adsorption tank and the second adsorption tank include a purification stage and an activation stage, and the first adsorption tank and the second adsorption tank periodically enter the purification stage and the activation stage, wherein the purification stage is a stage of adsorbing and removing liquefied high-boiling gas by the first adsorption tank and a stage of adsorbing residual neon by the second adsorption tank, and the activation stage is a stage of releasing high-boiling gas by the first adsorption tank and a stage of releasing residual neon by the second adsorption tank.

[0011] Preferably, S4 specifically comprises: monitoring the filling state of the solidified neon by the multi-point temperature sensor array distributed along the axial direction of the freezing tank in cooperation with the pressure sensor; when the sensor data calculated by the control module shows that the filling volume ratio of the solidified neon in the tank reaches a preset threshold, the following linkage operations are triggered: the solidified neon in the current freezing tank is warmed and gasified for recovery, and the recovered pure neon gas is output; and the working stages of the first adsorption tank and the second adsorption tank are switched synchronously, and the working stages are specifically the purification stage or the activation stage.

[0012] Preferably, the activation stage specifically comprises: releasing pressure in the first / second adsorption canister to normal pressure, releasing and transferring the gas in the first / second adsorption canister to mix with the raw gas in S1 to normal pressure; warming up and vacuumizing the first / second adsorption canister to desorb the high-boiling gas / residual neon gas.

[0013] Preferably, when the frozen canister in the purification stage is determined by the sensor array and the control module to reach a preset threshold of the solidified neon gas filling volume ratio, the following operations are triggered synchronously: the frozen canister in the current purification stage enters the activation stage for neon gas recovery, the frozen canister in the current activation stage enters the preparation stage, the frozen canister in the current preparation stage enters the purification stage; the first adsorption canister in the current purification stage enters the activation stage for high-boiling gas release, the first adsorption canister in the current activation stage enters the preparation stage, the first adsorption canister in the current preparation stage enters the purification stage; the second adsorption canister in the current purification stage enters the activation stage for residual neon gas release, the second adsorption canister in the current activation stage enters the preparation stage, the second adsorption canister in the current preparation stage enters the purification stage; the purification stage performs gas adsorption separation, the activation stage performs adsorbent regeneration and gas release; the preparation stage is a transition state for switching to the purification stage after the activation is completed.

[0014] In the present application, the purification method of low-temperature freezing + multi-stage adsorption is adopted, so that the obtained product gas meets the requirements of ultrapure helium gas, and also meets the requirements of helium gas used in the semiconductor industry; at the same time, the accumulation height of the solid neon gas in the frozen canister is monitored to realize automatic control of the warming and gasification of the solid neon gas in the frozen canister and automatic switching of the working stages of the two adsorption canisters, so as to ensure continuous production; the process uses the warming and gasification process of the solid neon gas as the time point for judging the switching of the adsorption canister from the purification stage to the activation stage, so that the structure design is simple, the maintenance cost is low, and the inaccurate time point judgment caused by the peak shape change of different impurities and concentrations can be avoided. The present application also sets the first adsorption canister before low-temperature freezing to remove high-boiling impurities, so as to avoid the freezing blockage in the later stage and ensure stable operation of the equipment; by setting multiple high-purity helium recovery and utilization interfaces, the helium recovery rate can be increased to 98%, and the purity of the byproduct neon gas can reach 99.99%, meeting the requirements of neon gas used in the semiconductor industry. BRIEF DESCRIPTION OF DRAWINGS

[0015] Figure 1 The flow chart of the multi-product high-purity helium purification method proposed in the present application; Figure 2 The system diagram of the multi-product high-purity helium purification method proposed in the present application. DETAILED DESCRIPTION

[0016] The helium raw gas component is known to contain 0-1000 ppm of neon, 0-10 ppm of hydrogen, and 0-1000 ppm of nitrogen, oxygen, and methane three impurities, the raw gas pressure is 1.0-1.5 MPa, and the raw gas flow is 10-100 N / m³. The first adsorption tank 1 and the second adsorption tank 3 are both filled with adsorbents, which are activated carbon + molecular sieve combination.

[0017] Referring to Figure 2 , the application provides a multi-product high-purity helium purification system, which comprises a first adsorption tank 1, a cold head heat exchanger 6, and a freezing tank 2 connected in series, wherein the cold head heat exchanger 6 is connected with a refrigerator 7 for providing a cold source for the cold head heat exchanger 6, the first adsorption tank 1 is connected with a three-channel first plate heat exchanger 4: liquid nitrogen enters through the a inlet of the first plate heat exchanger 4, the nitrogen gas after heat exchange is discharged through the a outlet of the first plate heat exchanger 4, the helium raw gas enters through the b inlet of the first plate heat exchanger 4, the helium raw gas after heat exchange is discharged through the b outlet of the first plate heat exchanger 4, and the low-temperature high-purity helium product enters the first plate heat exchanger 4 from the c inlet and exchanges heat with the helium raw gas, and the normal-temperature high-purity helium product after heat exchange is discharged from the c outlet of the first plate heat exchanger 4; the first adsorption tank 1 is connected with a second plate heat exchanger 5: the helium gas mixture after removal of high-boiling-point gas enters the a inlet of the second plate heat exchanger 5, the gas after cooling is discharged through the a outlet of the second plate heat exchanger 5, and the low-temperature high-purity helium product discharged from the second adsorption tank 3 enters the b inlet of the second plate heat exchanger 5 and exchanges heat with the helium gas mixture after removal of high-boiling-point gas, and the low-temperature high-purity helium product after heat exchange is discharged from the b outlet of the second plate heat exchanger 5. The first plate heat exchanger 4 and the second plate heat exchanger 5 can make full use of the cold carried in the high-purity helium product obtained in the purification process, and reduce the power consumption of the refrigerator 7.

[0018] Among them, the pipeline where the first adsorption tank 1, the freezing tank 2 and the second adsorption tank 3 are located forms a main pipeline section of a circulating loop, the circulating pipeline further comprises an external pipeline end, a storage tank 8 and a booster pump for driving the circulating gas to flow in the circulating pipeline are arranged on the external pipeline section, the storage tank 8 is in communication with the high-purity helium inlet and can be used to introduce high-purity helium into the circulating loop for precooling the system before production.

[0019] Based on the above system, referring to Figure 1 , the application provides a multi-product high-purity helium purification method, which comprises the following three processes: Precooling process: Liquid nitrogen enters the a inlet of the first plate heat exchanger 4 from the liquid nitrogen inlet, and high-purity helium gas enters the storage tank 8 from the high-purity helium gas inlet as a circulating gas, which is then pumped into the main pipeline section connected to the helium raw gas by the booster pump, and then flows into the b inlet of the first plate heat exchanger 4 to exchange heat with the liquid nitrogen, and then sequentially passes through the first adsorption tank 1, the second plate heat exchanger 5, the cold head heat exchanger 6, the freezing tank 2, the second adsorption tank 3, the second plate heat exchanger 5, and then returns to the storage tank 8 from the first plate heat exchanger 4 for circulation cooling. In this process, the external cold source (liquid nitrogen and refrigerator 7) continuously acts on the circulating gas until the temperature in the first adsorption tank 1 is stably maintained in the first temperature interval and the temperature in the freezing tank 2 is stably maintained in the lower limit of the second temperature interval (i.e. -258℃~-255℃).

[0020] When the temperature decreases, the gas pressure will gradually decrease due to the principle of thermal expansion and contraction of gas. At this time, high-purity helium gas needs to be supplemented into the circulation loop. This process can ensure the production plan by precooling and cooling.

[0021] Purification process: S1: When the gas is first introduced, the helium raw gas containing neon gas and high-boiling-point gas is introduced into the b inlet of the first plate heat exchanger 4, and at the same time, liquid nitrogen enters the a inlet of the first plate heat exchanger 4 from the liquid nitrogen inlet; at this time, the raw gas and the liquid nitrogen exchange heat in the first plate heat exchanger 4, and the helium raw gas is cooled to the first temperature interval (-190℃~-185℃), and the liquid nitrogen after heat exchange is discharged through the nitrogen gas outlet at 20℃~25℃, and then the helium raw gas enters the first adsorption tank 1 for adsorption. This process mainly adsorbs and removes high-boiling-point impurities (such as nitrogen, oxygen, methane, carbon dioxide, etc.) in the helium raw gas to avoid freezing and blocking of high-boiling-point impurities in the raw gas at the temperature of -253℃ in the later stage.

[0022] S2, the helium gas mixture from which the high-boiling-point gas is removed is discharged from the first adsorption tank 1 into the second plate heat exchanger 5, and exchanges heat with the high-purity helium gas product (the first gas is cooled and exchanged with the high-purity helium gas in the precooling process), and the helium gas mixture is cooled to -248℃~-243℃ and discharged from the a outlet of the second plate heat exchanger 5, and then enters the cold head heat exchanger 6, which is made of red copper and has good heat conduction effect, so that the cold quantity of the refrigerator 7 can be quickly transferred to the cold head heat exchanger 6 to quickly cool the internal flowing gas, so that the temperature of the helium gas mixture can quickly reach the second temperature interval (i.e. -258℃~-255℃), which is lower than the solidification temperature of neon gas and higher than the liquefaction temperature of helium gas. At this time, the neon gas is solidified and separated in the freezing tank 2, and the solidified neon solid is deposited at the bottom, and the unliquefied helium gas containing a small amount of neon gas is output.

[0023] To ensure that high-boiling point gas impurities do not enter the second plate heat exchanger 5, the first adsorption tank 1 outlet gas is analyzed and detected by a chromatograph before the helium mixed gas is introduced into the first adsorption tank 1. If the first adsorption tank 1 outlet gas does not meet the requirement that the sum of nitrogen, oxygen, methane and other impurities is ≤1 ppm, it indicates that the first adsorption tank 1 outlet gas is not pure, and the part of the impure gas is returned to the front end through a pipeline for recycling; if the first adsorption tank 1 outlet gas meets the requirement that the sum of nitrogen, oxygen, methane and other impurities is ≤1 ppm, the gas in the first adsorption tank 1 is allowed to enter the second plate heat exchanger 5. This ensures that high-boiling point impurity gases do not enter the pipeline and cause freezing and plugging.

[0024] S3, the un-solidified / liquefied gas is transported to the second adsorption tank 3 through the cold tank 2 outlet for further adsorption of trace amounts of unfrozen neon gas. After adsorption, the neon gas in the helium gas is ≤1 ppm, and other impurities are all ≤0.1 ppm, meeting the requirements of ultrapure helium, and obtaining high-purity helium gas products; the high-purity helium gas products can meet the requirements of the semiconductor industry for helium gas use; Then, the obtained high-purity helium gas products are sequentially transported to the filling area through the second plate heat exchanger 5, the first plate heat exchanger 4 and the product gas outlet; in this process, the liquid nitrogen input is adjusted and controlled, and the temperature is controlled in the interval of -190°C to -185°C, so as to ensure that the product gas outlet temperature is in the temperature interval of 20°C to 25°C.

[0025] In the above process, the cold energy of the obtained high-purity helium gas products is distributed in the following order: first flows through the second plate heat exchanger 5 connected with the cold tank 2 to pre-cool the helium mixed gas to be introduced into the cold tank 2; and then flows through the first plate heat exchanger 4 connected with the first adsorption tank 1 inlet to pre-cool the helium raw gas, so as to effectively utilize the product gas cold energy and reduce the power consumption of the refrigerator 7.

[0026] The cooling of the helium raw gas to the first temperature interval is realized by the first plate heat exchanger 4, wherein the cold source of the first plate heat exchanger 4 includes liquid nitrogen and low-temperature high-purity helium gas products + liquid nitrogen, and the two cold sources are dynamically switched by a control module: in the pre-cooling process, the liquid nitrogen is used as the cold source of the first plate heat exchanger 4, at this time the temperature sensor in the cold tank 2 detects that the temperature is higher than the neon solidification critical temperature; when the temperature sensor in the cold tank 2 detects that the temperature reaches the second temperature interval and the helium flow sensor at the output end of the second adsorption tank 3 detects a stable flow, the cold energy of the high-purity helium gas products is switched to the first plate heat exchanger 4 to realize cold energy circulation supply. By using the cold energy carried by the high-purity helium gas products as the cold source of the first plate heat exchanger 4, the cold energy utilization rate can be improved while the consumption of liquid nitrogen is reduced.

[0027] Activation process: The filling state of the solidified neon gas is monitored by a multi-point temperature sensor array distributed along the axis of the freezing tank 2 in cooperation with a pressure sensor; when the sensor data is calculated by the control module to reach a preset threshold of the filling volume ratio of the solidified neon gas in the tank, the following linkage operation is triggered: S41, the solidified neon gas in the current freezing tank 2 is warmed and gasified for recovery, and the recovered pure neon gas is output; specifically, when the pressure in the freezing tank 2 is released to 0.01 MPa, the remaining gas is extracted and vented to ensure that the internal neon purity reaches 99.9%; when the pressure in the freezing tank 2 is extracted to 0.09 MPa, the heater is heated to -243 DEG C, so that the solid neon in the freezing tank 2 becomes gas, and then the gas is heated and warmed to be transported to the neon filling area, and 99.99% neon gas can be obtained.

[0028] Since the freezing tank 2 is filled with part of the unliquefied helium gas carrying un-solidified neon gas, if the solidified neon gas in the freezing tank 2 is directly heated and gasified, the purity of the neon gas will be affected by the part of the gas; since the part of the gas contains helium, in order to recycle the part of the helium, the part of the unliquefied helium gas is directly heated and warmed, and then returned to the front end under the adsorption of the vacuum pump to be mixed into the helium raw gas for recycling.

[0029] S42, the working stages of the first adsorption tank 1 and the second adsorption tank 3 are synchronously switched, and the first adsorption tank 1 and the second adsorption tank 3 are switched from the above purification stage of the purification process to the following activation stage, specifically: the first adsorption tank 1 and the second adsorption tank 3 are released to normal pressure, and the gas discharged in the release process contains helium, so as to recover the part of the helium, the part of the release gas is heated and warmed, and then introduced into the helium raw gas pipeline to be mixed with the helium raw gas; After the first adsorption tank 1 and the second adsorption tank 3 are released to normal pressure, the first adsorption tank 1 and the second adsorption tank 3 are heated and warmed to 50 DEG C and extracted to a negative pressure of 0.09 MPa, so as to desorb the high-boiling-point gas adsorbed in the first adsorption tank 1 in the purification process and the residual neon gas adsorbed in the second adsorption tank 3 in the purification process.

[0030] The present application sets up multiple helium recovery pipelines in the above activation process, so that the helium recovery rate can be increased to 98%, and the purity of the byproduct neon gas can reach 99.99%, which meets the use of neon gas in the semiconductor industry.

[0031] The switching of the above purification process to the activation process is automatically controlled in the following manner: three groups of the freezing tank 2, the first adsorption tank 1 and the second adsorption tank 3 are arranged and connected in parallel in a circulating loop in a switchable manner, wherein the three groups of the freezing tank 2, the first adsorption tank 1 and the second adsorption tank 3 each have three modes of a purification phase, an activation phase and a preparation phase; the purification phase performs gas adsorption separation, the activation phase performs adsorbent regeneration and gas release; and the preparation phase is a transition state after the completion of the activation for switching to the purification phase.

[0032] When the freezing tank 2 in the purification phase is determined by the sensor array and the control module that the solidified neon gas filling volume ratio reaches a preset threshold value, the following operations are triggered synchronously: (1) Freezing tank 2 switching: the freezing tank 2 in the current purification phase is switched into the activation phase for neon gas recovery, the freezing tank 2 in the current activation phase is switched into the preparation phase, and the freezing tank 2 in the current preparation phase is switched into the purification phase; (2) First adsorption tank 1 switching: the first adsorption tank 1 in the current purification phase is switched into the activation phase for high-boiling-point gas release, the first adsorption tank 1 in the current activation phase is switched into the preparation phase, and the first adsorption tank 1 in the current preparation phase is switched into the purification phase; (3) Second adsorption tank 3 switching: the second adsorption tank 3 in the current purification phase is switched into the activation phase for residual neon gas release, the second adsorption tank 3 in the current activation phase is switched into the preparation phase, and the second adsorption tank 3 in the current preparation phase is switched into the purification phase.

[0033] With the above control scheme, the present application can determine the solidified neon gas filling volume ratio in the freezing tank 2 through the sensor array and the control module, and then determine the time point of switching from the purification to the activation phase, so as to realize automatic switching control, and the rotation of the three phases can also ensure the continuous performance of the helium purification process and the yield.

[0034] The above only describes the preferred embodiments of the present application, but the protection scope of the present application is not limited thereto, and any person skilled in the art can make equivalent replacements or changes to the technical solutions and the inventive concept of the present application within the technical range disclosed by the present application, which should be covered within the protection scope of the present application.

Claims

1. A method for purifying high-purity helium gas for multiple products, characterized by, The method comprises the following steps: S1, cooling the helium raw gas containing neon gas and high-boiling gas to a first temperature range, removing the liquefied high-boiling gas by a first adsorption tank, and obtaining the helium mixed gas from which the high-boiling gas is removed; S2, cooling the helium mixed gas from which the high-boiling gas is removed to a second temperature range, the second temperature range being lower than the solidification temperature of neon gas and higher than the liquefaction temperature of helium gas, solidifying and separating the neon gas in a freezing tank, and outputting the unliquefied helium gas containing trace neon gas; S3, passing the unliquefied helium gas containing trace neon gas into a second adsorption tank to adsorb the residual neon gas, and obtaining the high-purity helium gas product; S4, warming and gasifying the solidified neon gas in the freezing tank, and outputting the recovered pure neon gas.

2. The multi-product high-purity helium purification process of claim 1, wherein, The cold energy supply for cooling the helium raw gas to the first temperature range is dynamically switched by a control module, wherein when the temperature sensor in the freezing tank detects that the temperature is higher than the critical solidification temperature of neon gas, external liquid nitrogen is used to provide cold energy; when the temperature sensor in the freezing tank detects that the temperature reaches the second temperature range and the helium flow sensor at the output end of the second adsorption tank detects a stable flow, the cold energy of the high-purity helium gas product is branched off to the cooling link to realize cold energy circulation supply.

3. The multi-product high-purity helium purification process of claim 1, wherein, The cold energy branching of the high-purity helium gas product is transferred in the following order: first flowing through the cooling flow channel connected with the freezing tank to precool the helium mixed gas to be introduced into the freezing tank; and then flowing through the cooling flow channel connected with the inlet of the first adsorption tank to precool the helium raw gas.

4. The multi-product high-purity helium purification process of claim 1, wherein, Before S1, the method further comprises the following steps: passing the circulating gas with the same components as the high-purity helium gas product into a closed circulating pipeline, sequentially connecting the first adsorption tank, the freezing tank and the second adsorption tank in the circulating pipeline; and continuously acting on the circulating gas by an external cold source until the temperature in the first adsorption tank is stably maintained at the first temperature range and the temperature in the freezing tank is stably maintained at the lower limit of the second temperature range.

5. The multi-product high-purity helium purification process of claim 4, wherein, The circulating pipeline comprises an external pipeline section and a main pipeline section, the first adsorption tank, the freezing tank and the second adsorption tank are connected in series on the main pipeline section, a storage tank and a booster pump for driving the circulating gas to circulate in the circulating pipeline are arranged on the external pipeline section, and a gas injection unit for injecting the circulating gas into the buffer tank is further arranged on the storage tank.

6. The multiproduct high-purity helium purification process of claim 1, wherein, The working stages of the first adsorption tank and the second adsorption tank include a purification stage and an activation stage, the first adsorption tank and the second adsorption tank periodically enter the purification stage and the activation stage, the purification stage is the stage of removing the liquefied high-boiling gas by the first adsorption tank and the stage of adsorbing the residual neon gas by the second adsorption tank, and the activation stage is the stage of releasing the high-boiling gas by the first adsorption tank and the stage of releasing the residual neon gas by the second adsorption tank.

7. The multiproduct high-purity helium purification process of claim 6, wherein, S4 specifically comprises the following steps: monitoring the filling state of the solidified neon gas by a multi-point temperature sensor array distributed along the axial direction of the freezing tank in cooperation with a pressure sensor; when the filling volume ratio of the solidified neon gas in the tank calculated by the sensor data through the control module reaches a preset threshold, the following linkage operations are triggered: warming and gasifying the solidified neon gas in the current freezing tank to recover the pure neon gas; and synchronously switching the working stages of the first adsorption tank and the second adsorption tank, the working stages being specifically the purification stage or the activation stage.

8. The multiproduct high-purity helium purification process of claim 7, wherein, The activation stage specifically includes: releasing pressure in the first / second adsorption tank to normal pressure, releasing and transferring the gas in the first / second adsorption tank to mix with the raw gas in S1, and warming up and vacuumizing the first / second adsorption tank to desorb high-boiling gas / residual neon.

9. The multiproduct high-purity helium purification process of claim 7, wherein, When the frozen tank in the purification stage is determined by the sensor array and the control module to reach a preset threshold of the solidified neon gas filling volume ratio, the following operations are triggered synchronously: the frozen tank in the current purification stage enters the activation stage for neon gas recovery, the frozen tank in the current activation stage enters the preparation stage, the frozen tank in the current preparation stage enters the purification stage; the first adsorption tank in the current purification stage enters the activation stage for high-boiling gas release, the first adsorption tank in the current activation stage enters the preparation stage, the first adsorption tank in the current preparation stage enters the purification stage; the second adsorption tank in the current purification stage enters the activation stage for residual neon gas release, the second adsorption tank in the current activation stage enters the preparation stage, and the second adsorption tank in the current preparation stage enters the purification stage; the purification stage performs gas adsorption separation, the activation stage performs adsorbent regeneration and gas release; the preparation stage is a transition state for switching to the purification stage after the activation is completed.

Citation Information

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