Cryogenic adsorption device and adsorption regeneration method thereof

Abstract

The application discloses a kind of cryogenic adsorption devices and its adsorption regeneration method, it is characterized in that, including cover 1, shell 2, upper envelope 3, low temperature adsorber 4, space I between shell and inner part, special channel II, special channel II's outer cylinder body 5, lower envelope 6, raw gas inlet pipeline 7, support plate 8, outer regeneration gas inlet pipeline 9, ultra-pure product outlet pipeline 10, specific outer regeneration channel. By cryogenic adsorption device can produce 6N level and above ultra-pure product;Device structure is simple, compact, save outer regeneration gas and precooling low temperature liquid consumption;Greatly improve the heat utilization rate of outer regeneration gas, reduce the use amount of ultra-pure product during regeneration, improve the yield of ultra-pure product, especially suitable in large-scale purification device;Simultaneously using different temperature low temperature gas gradually precooling low temperature adsorber, effectively reduce the stress generated by alternating load, control stress in allowable range, ensure the safe operation of equipment.

Description

TECHNICAL FIELD

[0001] The present application relates to an adsorption device, in particular to a deep low-temperature adsorption device and an adsorption regeneration method thereof. BACKGROUND

[0002] Special gases such as helium, neon, argon, hydrogen, etc. are widely used in aerospace, medical, metallurgy, semiconductor, reactor, superconducting manufacturing fields, which are strategic resources related to national defense security. The purity of the gas in these fields is required to be higher and higher, usually 5N level, even 6N level and above.

[0003] In the conventional low-temperature purification device, the low-temperature adsorber is usually wrapped with an electric heating belt for heating and regeneration. First, there is a risk of electric shock. Second, when the processing scale is large, multiple low-temperature adsorbers need to be used in series or parallel, and the structure of the wrapped electric heating belt is complex. Third, in order to ensure the yield of the product, it is impossible to use a large amount of ultra-pure product as a regeneration gas. Fourth, the existing integrated equipment from normal temperature condensation to low temperature (such as CN103848398 patent) has a complex structure, and the consumption of regeneration gas and pre-cooling low-temperature liquid is large. The existing device does not set a specific external regeneration channel, and due to the large space cross-sectional area, the heat utilization rate of the external regeneration gas is very low. Therefore, a specific external regeneration channel is needed, and an auxiliary regeneration method is used to heat the low-temperature adsorber externally to improve the heat utilization rate of the external regeneration gas, reduce the use amount of ultra-pure product during regeneration, improve the yield of ultra-pure product, and be suitable for large-scale purification devices. SUMMARY

[0004] The purpose of the present application is to provide a deep low-temperature adsorption device and an adsorption regeneration method thereof, to solve the problems of low heat utilization rate of regeneration gas, large consumption of regeneration gas and pre-cooling low-temperature liquid in the prior art.

[0005] The present application is implemented by the following technical scheme: a deep low-temperature adsorption device, characterized in that it comprises a cover 1, a shell 2, an upper sealing cylinder 3, a low-temperature adsorber 4, a space I between the shell and the inner part, a special channel II, an outer cylinder body 5 of the special channel II, a lower sealing cylinder 6, a raw gas inlet pipeline 7, a support plate 8, an external regeneration gas inlet pipeline 9, an ultra-pure product outlet pipeline 10, and a specific external regeneration channel. The cover 1 and the shell 2 form a closed container. The upper sealing cylinder 3 is connected with the cover 1 and the outer cylinder body 5 of the special channel II. The outer cylinder body 5 of the special channel II is connected with the sealing cylinder 3, the low-temperature adsorber 4, the lower sealing cylinder 6, and the support plate 8. The raw gas inlet pipeline 7 is connected with the cover 1 and the low-temperature adsorber 4. The external regeneration gas inlet pipeline 9 is connected with the cover 1. The ultra-pure product outlet pipeline 10 is connected with the cover 1 and the low-temperature adsorber 4. The adsorbent loading port D① is connected with the cover 1.

[0006] Further, the special channel II is a narrow channel formed between the outer cylinder 5 of the special channel II and the cylinder of the low-temperature adsorber 4, for the passage of the regeneration gas; and the specific outer regeneration channel is a channel composed of the outer regeneration gas inlet pipeline 9, the lower sealing cylinder 6, the special channel II, the upper sealing cylinder 3, and the outer regeneration gas outlet pipeline.

[0007] Further, the upper sealing cylinder 3 includes cylinder segments and transverse sealing plates, which seal the space between the upper part of the low-temperature adsorber and the cover 1, forming a channel at the outer regeneration gas outlet; and the lower sealing cylinder 6 includes cylinder segments and transverse sealing plates, which cover the outlet of the outer regeneration gas inlet pipeline 9.

[0008] Further, the low-temperature adsorber 4 is fixed in the outer cylinder 5 of the special channel II, and is filled with adsorbent inside; the adsorbent loading port D① of the low-temperature adsorber 4 leads out of the cover 1, and when the low-temperature adsorption device is in the adsorption process, most of the space I between the shell and the inner part is filled with low-temperature liquid, and the low-temperature adsorber is immersed in the low-temperature liquid.

[0009] Further, the raw material gas inlet pipeline 7 is provided with cooling coils, and when the low-temperature adsorption device is adsorbing, it is immersed in the low-temperature liquid, and the lower part is connected with the low-temperature adsorber inlet.

[0010] Further, the cover 1 is a flat cover connected by flanges or an oval, butterfly-shaped end cover; and the cylinder of the shell 2 and the lower end cover are a multi-layer vacuum insulation or vacuum powder insulation Dewar structure or a single-layer structure with external insulation.

[0011] Further, a deep low-temperature adsorption regeneration method comprises the following steps:

[0012] The low-temperature adsorption method G1: the pre-cooled raw material gas is introduced from the raw material gas inlet B①, and after being cooled by the coils of the raw material gas inlet pipeline, it enters the low-temperature adsorber; the low-temperature adsorber adsorbs impurities, and the ultra-pure product flows out from the outlet B②;

[0013] The low-temperature liquid discharge method G2: at the beginning of the regeneration of the low-temperature adsorption device, 0.3~0.6MPa low-temperature gas is introduced from the outer regeneration gas inlet A②, and the low-temperature liquid in the space I is discharged from the low-temperature liquid inlet and outlet E to the low-temperature liquid storage tank by pressure difference;

[0014] The outer regeneration method G3: the outer regeneration gas is introduced from the outer regeneration gas inlet A②, passes through the specific outer regeneration channel, and is heated in the low-temperature adsorber shell to rapidly heat the low-temperature adsorber and desorb the impurities in the bed, and then is discharged from the outer regeneration gas outlet A①;

[0015] The pressure relief method G4: the high-purity gas is released from the raw material gas inlet B① to relieve the pressure, and the discharged high-purity gas is recycled in the recycling system to prepare for the further regeneration of the low-temperature adsorber bed;

[0016] Ultrapure product gas regeneration method G5: Hot ultrapure product gas at a certain pressure is introduced from the ultrapure product outlet B②, passes through the low temperature adsorber bed to remove impurities, and is then discharged from the raw material gas inlet B① to the recovery system for recycling.

[0017] Vacuuming method G6: Evacuate from the raw material gas inlet B①, reduce the pressure inside the low-temperature adsorber to 2~20kPaA, and discharge the extracted gas.

[0018] Low-temperature gas precooling method G7: Low-temperature external regeneration gas at different temperatures is introduced from external regeneration gas inlet A②, and discharged from external regeneration gas outlet A① through a specific external regeneration channel, gradually precooling the internal components such as the low-temperature adsorber to -145~-200℃;

[0019] Cryogenic liquid cooling method G8: Cryogenic liquid is introduced from the cryogenic liquid inlet and outlet E. The cryogenic liquid cools the pre-cooled internal components and shell of the cryogenic adsorber to the cryogenic liquid temperature and fills the liquid level to the set height. The cryogenic liquid vapor is discharged from the external regeneration gas outlet A①.

[0020] Pressure boosting method G9: Introduce ultrapure product gas through port B② to slowly increase the pressure inside the low-temperature adsorber to the adsorption pressure.

[0021] Furthermore, the cryogenic liquid can be liquid nitrogen, liquid argon, liquid air, liquid neon, liquid helium, or other media; the raw material gas has a pressure of 2~20MPa, a temperature of -145~-243℃, and an impurity content of less than 7.5%.

[0022] Furthermore, the external regeneration gas temperature of the external regeneration method G3 is -100~120℃, and the pressure is 0.2~0.5MPa.

[0023] Furthermore, the regenerated ultrapure gas temperature in the ultrapure product gas regeneration method G5 is -100~120℃, and the pressure is 0.1~0.3MPa.

[0024] The beneficial effects of this invention are as follows: The low-temperature adsorption device can produce ultrapure products of grade 6N and above; the device has a simple and compact structure, saving on the consumption of external regeneration gas and pre-cooling cryogenic liquid; the above-mentioned regeneration method, due to the existence of a dedicated external regeneration channel, greatly improves the heat utilization rate of the external regeneration gas, reduces the amount of ultrapure product used during regeneration, and increases the yield of ultrapure products, making it particularly suitable for large-scale purification devices; simultaneously, the use of cryogenic gases at different temperatures to gradually pre-cool the cryogenic adsorber effectively reduces the stress generated by alternating loads, keeping the stress within an allowable range and ensuring the safe operation of the equipment. Attached Figure Description

[0025] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. The drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on the structures shown in these drawings without creative effort.

[0026] Figure 1 A schematic diagram of a cryogenic adsorption device;

[0027] In the diagram, 1-cap, 2-shell, 3-upper sealing cylinder, 4-low temperature adsorber, 5-outer cylinder of dedicated channel II, 6-lower sealing cylinder, 7-raw material gas inlet pipe, 8-support plate, 9-external regenerated gas inlet pipe, 10-ultra-pure outlet pipe. Detailed Implementation

[0028] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. The components of the embodiments of the present invention described and shown in the accompanying drawings can generally be arranged and designed in various different configurations.

[0029] Therefore, the following detailed description of the embodiments of the invention provided in the accompanying drawings is not intended to limit the scope of the claimed invention, but merely to illustrate selected embodiments of the invention. All other embodiments obtained by those skilled in the art based on the embodiments of the invention without inventive effort are within the scope of protection of the invention.

[0030] like Figure 1 As shown, a cryogenic adsorption device includes a cap 1, a shell 2, an upper sealing cylinder 3, a cryogenic adsorber 4, a space I between the shell and the internal components, a dedicated channel II, an outer cylinder 5 of the dedicated channel II, a lower sealing cylinder 6, a raw material gas inlet pipe 7, a support plate 8, an external regeneration gas inlet pipe 9, an ultrapure product outlet pipe 10, and a specific external regeneration channel.

[0031] The cap 1 and shell 2 form a closed container; the upper sealing cylinder 3 is connected to the cap 1 and the upper end of the outer cylinder 5 of the dedicated channel II; the lower sealing cylinder 6 is connected to the lower end of the outer cylinder 5 of the dedicated channel II; a low-temperature adsorber 4 is connected inside the outer cylinder 5 of the dedicated channel II, and a support plate 8 is connected to the outer wall of the outer cylinder 5 of the dedicated channel II; the raw material gas inlet pipe 7 is connected to the cap 1 and the low-temperature adsorber 4, and a cooling coil is connected in the middle of the raw material gas inlet pipe 7; the external regeneration gas inlet pipe 9 is connected to the cap 1, and the external regeneration gas inlet pipe 9 is L-shaped, with its outlet near the lower part of the low-temperature adsorber 4, located inside the lower sealing cylinder 6; the ultrapure product outlet pipe 10 The system is connected to the cap 1 and the low-temperature adsorber 4; the adsorbent loading port D① is connected to the cap 1 and the low-temperature adsorber 4, and the unloading port D② is connected to the lower end of the low-temperature adsorber 4; the ultrapure product outlet B② is connected to the cap 1 and the low-temperature adsorber 4; the external regeneration gas outlet A①, external regeneration gas inlet A②, raw material gas inlet B①, ultrapure product outlet B②, low-temperature liquid evaporation gas outlet C, and loading port D① are all led out from the cap; the low-temperature liquid inlet and outlet E are located at the bottom of the low-temperature adsorption device shell 2; the dedicated channel II is a narrow channel formed between the outer cylinder 5 of the dedicated channel II and the cylinder of the low-temperature adsorber 4, for the regeneration gas to pass through, so as to improve the heat utilization rate and heat transfer efficiency. The specific external regeneration channel is a channel composed of the external regeneration gas inlet pipe 9, the lower cap 6, the dedicated channel II, the upper cap 3, and the external regeneration gas outlet pipe, which regulates the flow path of the external regeneration gas to improve the heat utilization rate and heat transfer efficiency.

[0032] In this specific embodiment, a cryogenic adsorption regeneration method for obtaining ultrapure helium products at liquid nitrogen temperature using liquid nitrogen as the cryogenic liquid and nitrogen as the external regeneration gas includes the following process steps:

[0033] During the adsorption process, the pre-cooled front-end unit, at a pressure of 2-20 MPa, is pre-cooled to -190~-195℃. The feed gas enters through feed gas inlet B①, is cooled by the coil in the feed gas inlet pipe, and then enters the cryogenic adsorber. Impurities are adsorbed, and the ultrapure product flows out from outlet B②. The heat of adsorption causes the temperature of the cryogenic adsorber, immersed in liquid nitrogen, to rise, causing the liquid nitrogen to evaporate. The evaporated nitrogen gas flows out through a dedicated channel II and the cryogenic liquid evaporated gas outlet C. The cryogenic liquid inlet and outlet E are used to replenish liquid nitrogen. When the impurity content of the ultrapure product reaches the set value or the adsorption time reaches the set time, adsorption must be stopped (applicable to intermittent operation) or switched to another cryogenic adsorption unit with complete regeneration (including heating regeneration, pre-cooling, and pressurization) (applicable to continuous operation).

[0034] During the regeneration process of the cryogenic adsorption unit, the cryogenic liquid discharge method G2 is first performed. Cryogenic nitrogen gas at 0.3~0.6 MPa is introduced through port A②, forcing the liquid nitrogen out through port E to the cryogenic liquid storage tank. Simultaneously, the depressurization method G4 is performed, reducing the pressure inside the cryogenic adsorber to 0.02~0.05 MPa through the raw material gas inlet B①. The released high-purity gas is then recycled to the recovery system. After the cryogenic liquid is completely discharged, the external regeneration method G3 begins. Nitrogen gas at 80~120℃ is introduced through port A②, passing through a specific external regeneration channel and exiting through port A①. Simultaneously with external regeneration method G3, the ultrapure product gas regeneration method G5 is performed. Ultrapure product gas at 0.1~0.3 MPa and 80~120℃ is introduced through port B②, passing through the cryogenic adsorber bed and exiting through port B① to the recovery system. After these two regeneration methods are completed, the cryogenic... The adsorber will contain only trace amounts of impurities. Next, the cryogenic gas precooling method G7 begins, where nitrogen gas at different temperatures is gradually introduced through a specific external regeneration channel from port A② and discharged from port A①, precooling the internal components of the cryogenic adsorber to -145~-150℃. During this period, the vacuuming method G6 begins when the precooling reaches approximately 60℃, evacuating the system from port B①. The extracted gas is then recycled to the recovery system, and the pressure is evacuated to 2~20 kPaA. After the nitrogen precooling is completed, the cryogenic liquid cooling method G8 begins, where liquid nitrogen is introduced from port E to cool the cryogenic adsorber and its internal components to -190~-195℃. Simultaneously, the pressurization method G9 begins, where ultrapure product gas is introduced from port B② to slowly increase the pressure inside the cryogenic adsorber to the adsorption pressure at a rate of 0.1~0.3 MPa / min. At this point, the cryogenic adsorption device has completed regeneration and is ready for switching or shutdown.

[0035] According to the above method, this invention can obtain ultrapure products with a purity of 6N or higher through low-temperature adsorption (at temperatures of -190 to -195°C). The device has a simple and compact structure, saving on the consumption of external regeneration gas and pre-cooling cryogenic liquid. When two or more cryogenic adsorption devices are used in parallel or series, the devices can be freely switched, enabling continuous production, which is particularly suitable for large-scale cryogenic purification devices. The auxiliary regeneration method using external heating of the cryogenic adsorber greatly improves the heat utilization rate of the external regeneration gas, reduces the amount of ultrapure product used during regeneration, and increases the yield of ultrapure product. At the same time, the gradual pre-cooling of the cryogenic adsorber with cryogenic gases at different temperatures effectively reduces the stress generated by alternating loads, keeping the stress within the allowable range and ensuring the safe operation of the equipment.

[0036] The above embodiments describe the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely illustrative of the principles of the invention. Modifications and variations made by those skilled in the art without departing from the spirit and scope of the invention should be within the protection scope of the appended claims.

Claims

1. A cryo-pumping device, characterized by, The application relates to a low-temperature adsorption device and a method thereof, and belongs to the field of adsorption technology.

2. A cryosorption apparatus according to claim 1, wherein The device comprises a device shell and an internal adsorption device and matched pipelines, wherein the device shell comprises a cover (1) and a shell (2), the internal adsorption device and the matched pipelines comprise an upper sealing cylinder (3), a low-temperature adsorber (4), a space I between the shell and the internal components, a special channel II, an outer cylinder body (5) of the special channel II, a lower sealing cylinder (6), a raw material gas inlet pipeline (7), an outer regeneration gas inlet pipeline (9), an ultrapure product outlet pipeline (10) and a special outer regeneration channel.

3. The apparatus of claim 1, wherein the apparatus is a cryosorption apparatus. The cover (1) and the shell (2) constitute a closed container.

4. The apparatus of claim 1, wherein the apparatus is a cryosorption apparatus. The upper sealing cylinder (3) is connected with the cover (1) and the outer cylinder body (5) of the special channel II.

5. The apparatus of claim 1 wherein, The outer cylinder body (5) of the special channel II is connected with the upper sealing cylinder (3), the low-temperature adsorber (4), the lower sealing cylinder (6) and a supporting plate (8).

6. A method of cryoadsorption regeneration, implemented on a cryoadsorption apparatus according to any one of claims 1-5, characterized in that, The raw material gas inlet pipeline (7) is connected with the cover (1) and the low-temperature adsorber (4). The outer regeneration gas inlet pipeline (9) is connected with the cover (1). The ultrapure product outlet pipeline (10) is connected with the cover (1) and the low-temperature adsorber (4). The special outer regeneration channel is formed by the outer regeneration gas inlet pipeline (9), the lower sealing cylinder (6), the special channel II, the upper sealing cylinder (3) and an outer regeneration gas outlet pipeline. The upper sealing cylinder (3) comprises a cylinder section and a transverse sealing plate, and the space between the upper part of the low-temperature adsorber and the cover (1) is sealed to form a channel at the outer regeneration gas outlet. The lower sealing cylinder (6) comprises a cylinder section and a transverse sealing plate, and the outer regeneration gas inlet pipeline (9) is covered. The low-temperature adsorber (4) is fixed in the outer cylinder body (5) of the special channel II, and is filled with adsorbents. The raw material gas inlet pipeline (7) is provided with a cooling coil, and is immersed in the low-temperature liquid during the adsorption of the low-temperature adsorption device. The cover (1) is a flat cover or an oval cover or a butterfly cover which is connected through flanges. The shell (2) is a multi-layer vacuum insulation or vacuum powder insulation Dewar structure or a single-layer structure with external insulation. The application further discloses a low-temperature adsorption method. The low-temperature adsorption method G1 comprises the following steps: the pre-cooled raw material gas is introduced from a raw material gas inlet B1, is cooled through the cooling coil of the raw material gas inlet pipeline and then is introduced into the low-temperature adsorber, the low-temperature adsorber adsorbs impurities, and the ultrapure product flows out from an outlet B2; The low-temperature liquid discharge method G2 comprises the following steps: 0.3-0.6 MPa low-temperature gas is introduced from an outer regeneration gas inlet A2 in the regeneration starting stage of the low-temperature adsorption device, and the low-temperature liquid in the space I is discharged to a low-temperature liquid storage tank through the low-temperature liquid inlet and outlet E by pressure difference; External regeneration method G3: External regeneration gas is introduced from the external regeneration gas inlet A②, passes through the specific external regeneration channel, is heated by the low-temperature adsorber shell to rapidly heat the low-temperature adsorber and desorb the impurities in the bed, and is then discharged from the external regeneration gas outlet A①; Pressure relief method G4: High-purity gas is discharged from the raw material gas inlet B①, and the discharged high-purity gas is recovered in the recovery system to prepare for further regeneration of the low-temperature adsorber bed by the ultra-pure product; Ultra-pure product gas regeneration method G5: Hot ultra-pure product gas is introduced from the ultra-pure product outlet B②, passes through the low-temperature adsorber bed, desorbs the impurities, and is then discharged from the raw material gas inlet B① to the recovery system for recovery; Vacuum method G6: The raw material gas inlet B① is evacuated to reduce the pressure in the low-temperature adsorber to 2~20kPaA, and the extracted gas is discharged; Low-temperature gas precooling method G7: Low-temperature external regeneration gas at different temperatures is introduced from the external regeneration gas inlet A②, passes through the specific external regeneration channel, and is discharged from the external regeneration gas outlet A① to gradually precool the low-temperature adsorber to -145~-200℃; Low-temperature liquid cooling method G8: Low-temperature liquid is introduced from the low-temperature liquid inlet and outlet E, the low-temperature liquid cools the pre-cooled low-temperature adsorber and shell to the temperature of the low-temperature liquid, and the liquid level is filled to a set height, and the low-temperature liquid vapor is discharged from the external regeneration gas outlet A①; Pressure increasing method G9: Ultra-pure product gas is introduced from B② to slowly increase the pressure in the low-temperature adsorber to the adsorption pressure.

7. A method of cryoadsorption regeneration as claimed in claim 6, wherein, The low-temperature liquid is liquid nitrogen, liquid argon, liquid air, liquid neon, or liquid helium; the raw material gas pressure is 2~20MPa, and the temperature is -145~-243℃.

8. A method of cryoadsorption regeneration as claimed in claim 6, wherein, The external regeneration gas temperature of the external regeneration method G3 is -100~120℃, and the pressure is 0.2~0.5MPa.

9. A method of cryoadsorption regeneration as claimed in claim 6, wherein, The regeneration ultra-pure gas temperature of the ultra-pure product gas regeneration method G5 is -100~120℃, and the pressure is 0.1~0.3MPa.

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