A high-purity nitrogen production device and preparation method thereof

Abstract

The invention discloses a high-purity nitrogen production equipment and a preparation method thereof, comprising: a nitrogen production mechanism and a purification mechanism, wherein the nitrogen production mechanism comprises: a first adsorption tower, a second adsorption tower, a carbon molecular sieve, and a one-way filtering structure; the purification mechanism comprises a first deoxidation tower, a second deoxidation tower, a cooler, a first purification tower, and a second purification tower, and further comprises: a middle heating structure, comprising a first fixed clamp seat, a second fixed clamp seat, a heating frame, and a one-way hole, wherein a catalyst is arranged on the inner side of the first fixed clamp seat and the second fixed clamp seat and on the outer side of the heating frame, a circulating supply structure, comprising a feed guide seat, a heat medium feed pipe, a catalyst supply pipeline, and a catalyst circulation pipe; and a circulating material guide structure, comprising a material pocket tray, a material holding cavity, a material blocking slope, and a rotating component. The invention can improve the purity of nitrogen, which is 20% higher than the output of the traditional method.

Description

Technical Field

[0001] The invention relates to a nitrogen production device, in particular to a high-purity nitrogen production device and a preparation method thereof. Background Art

[0002] Pressure swing adsorption (PSA for short) is a new gas separation technology. Taking adsorbent molecular sieves as an example, its principle is to separate gas mixtures by utilizing the difference in the "adsorption" properties of molecular sieves to different gas molecules. PSA nitrogen generator uses carbon molecular sieves as adsorbents and compressed air as raw materials. It uses pressure swing adsorption technology to separate the oxygen in it to obtain nitrogen. It is an automated device. After the nitrogen is prepared, the nitrogen composition has reached 99.9%, but it cannot be put into use directly. The nitrogen needs to be purified. In the purification stage, purification mechanisms are generally used for purification. As a highly efficient gas purification mechanism, the purification mechanism has a wide range of application environments. Whether it is electronics, chemical or pharmaceutical industries, high-purity nitrogen is required to ensure product quality and production safety. In industrial production, equipment is required to provide nitrogen continuously and stably to meet production needs.

[0003] However, in the process of nitrogen production, the following problems were found: 1. The valve action of the traditional PSA nitrogen generator is generally synchronous up and down in the pressure equalization stage. The instantaneous atmospheric flow has a greater impact on the molecular sieve filler, and the air flow speed and air flow cannot be controlled. If the air flow speed is fast, it will cause great damage to the carbon molecules, resulting in poor nitrogen purification effect. When the raw air enters the adsorption tower, if there are impurities in the raw air, it is easy to block the molecular sieve. However, if a simple filtering structure is set, it will be reintegrated into the tower body when the molecular sieve is regenerated; 2. The traditional purification mechanism needs to go through preheating-heating-deoxygenation-heat exchange- The water cooling-waste gas removal process is cumbersome and complex in structure. It is too wasteful in an environment where the gas consumption is small but continuous. The existing deoxygenation tower directly sets the catalyst in the deoxygenation tower, and uses a heater to heat the entire deoxygenation tower, so that the catalyst reacts with ordinary nitrogen at a certain temperature to generate carbon dioxide, which simplifies the entire deoxygenation step. However, since the hot end of the heater and the catalyst are not located in the same place, it is easy to cause incomplete reaction between nitrogen and catalyst, so that the oxygen in the nitrogen cannot be completely reacted, the purity of the nitrogen is reduced, and the purity of the purified nitrogen cannot reach ≥99.999%. Summary of the invention

[0004] The present invention provides a high-purity nitrogen production equipment and a preparation method thereof, which can absorb the air pressure inside the barrel, make the air pressure rise more stably, effectively ensure the stability of the molecular sieve filler in the tower, improve the purity of nitrogen, and achieve an output 20% higher than that of the traditional method. At the same time, the air entering the molecular sieve can be relatively pure, and the tower body will not be polluted even in the regeneration stage. At the same time, the heat source can be set in the carrier of the catalyst, so that the descending general nitrogen can be fully reacted at the position of the catalyst, and the trace oxygen entrained in the nitrogen can completely react with the carbon in the catalyst to generate carbon dioxide. When the catalyst needs to be replaced, the catalyst can be more conveniently extracted and a new catalyst can be pumped in, so that the catalyst can be evenly distributed in the deoxidation tower, which can effectively solve the above problems.

[0005] The present invention is achieved in that:

[0006] A high-purity nitrogen production equipment comprises: a nitrogen production mechanism and a purification mechanism, wherein the nitrogen production mechanism comprises a first adsorption tower and a second adsorption tower, wherein the first adsorption tower and the second adsorption tower are both provided with a carbon molecular sieve, wherein the lower end of the carbon molecular sieve is provided with a one-way filtering structure, and when gas passes into the first adsorption tower or the second adsorption tower from bottom to top, the one-way filtering structure filters the gas, and extracts the filtered material on the filtering structure before regeneration under normal pressure;

[0007] The first adsorption tower and the second adsorption tower are respectively connected with a first air inlet branch pipe and a second air inlet branch pipe, the first air inlet branch pipe and the second air inlet branch pipe are connected with an air inlet input pipe, the first air inlet branch pipe and the second air inlet branch pipe are respectively provided with a first air inlet valve and a second air inlet valve, the tops of the first adsorption tower and the second adsorption tower are respectively connected with an output pipe through a first air outlet branch pipe and a second air outlet branch pipe, the first air outlet branch pipe and the second air outlet branch pipe are respectively connected with a first air outlet valve and a second air outlet valve, a pressure equalizing valve is connected between the first air outlet branch pipe and the second air outlet branch pipe, the first adsorption tower and the second adsorption tower are respectively connected with a first middle pressure equalizing valve and a second middle pressure equalizing valve on the side, the first adsorption tower and the second adsorption tower are connected with a first lower pressure equalizing valve and a second lower pressure equalizing valve at the lower ends, a nitrogen gas storage tank is connected to the output pipe, and a pressure stabilizing valve and a flow meter are connected to the gas outlet end of the nitrogen gas storage tank;

[0008] The purification mechanism comprises a first deoxygenation tower connected to a nitrogen gas storage tank, the first deoxygenation tower is connected to a second deoxygenation tower and is filled with a catalyst, the second deoxygenation tower is connected to a cooler through a pipeline, the cooler connects the first purification tower and the second purification tower, the first purification tower and the second purification tower are connected to a finished nitrogen outlet, and the purification mechanism also includes:

[0009] The middle heating structure comprises a first fixing clamp seat fixed at the middle position of the first deoxidation tower, a second fixing clamp seat is arranged below the first fixing clamp seat, the first fixing clamp seat and the second fixing clamp seat are arranged at an interval and symmetrically with each other, a heating frame is arranged in the interval between the first fixing clamp seat and the second fixing clamp seat, one-way holes are opened on the outer sides of the first fixing clamp seat and the second fixing clamp seat, and the catalyst is arranged on the inner sides of the first fixing clamp seat and the second fixing clamp seat and on the outer side of the heating frame;

[0010] The circulating supply structure comprises a feed guide seat arranged on one side of the heating frame, a heat medium feed pipe communicating with the interior of the heating frame is arranged on the inner side of the feed guide seat, a catalyst supply pipeline communicating with the first fixed clamp seat and the second fixed clamp seat is arranged at the upper end of the heat medium feed pipe, and a catalyst circulation pipe is arranged at the lower end of the other side of the heating frame;

[0011] The circulating material guiding structure comprises a material pocket tray arranged below the heating frame, a plurality of movable material holding cavities are arranged at the bottom of the material pocket tray, a material blocking slope is arranged on the outer side of the middle part of the heating frame, and a rotating component is arranged on one side of the heating frame. When the catalyst enters the gap between the first fixed clamp seat and the second fixed clamp seat through the catalyst supply pipeline and is distributed to the gap between the material pocket tray, the material holding cavity and the material blocking slope, when the catalyst reaches the use cycle, the catalyst on the heating frame is shaken downward by the rotating component, and the used catalyst is extracted through the catalyst circulation pipe.

[0012] As a further improvement, the one-way filtration structure includes an annular disk located below the carbon molecular sieve and fixedly connected to the inner walls of the first adsorption tower and the second adsorption tower. A filter element is provided on the inner side of the annular disk, and a reflection element is provided at the lower end of the filter element. The end of the reflection element is connected to the outside world.

[0013] As a further improvement, the annular disk includes an upper mounting frame for mounting the filter element, the lower end of the upper mounting frame is connected to a lower mounting frame, and an anti-separation member is arranged on the inner side of the lower mounting frame.

[0014] As a further improvement, the filter element includes a filter plate connected to the inner side of the upper mounting frame, the filter plate is provided with a plurality of filter holes, a filter membrane is fixedly connected to the inner side of the filter holes, and a plurality of adsorption columns are provided below the filter membrane.

[0015] As a further improvement, the anti-separation member includes a connecting plate connected to the lower mounting frame, the connecting plate is provided with through holes staggered with the filter holes, and suction pipes are arranged directly below the filter holes, and all the suction pipes are connected to an external discharge pipe.

[0016] As a further improvement, the first fixed clamp seat includes a circular portion fixedly connected to the inner wall of the first deoxidation tower, the inner side of the circular portion is connected to an arched outer convex portion, and the outer sides of the circular portion and the outer convex portion are both provided with one-way holes, and the heating frame includes a transverse axis section arranged on the circulation supply structure, and a plurality of V-shaped contact sections are connected to the outer peripheral surface of the transverse axis section, and the V-shaped contact section is communicated with the transverse axis section.

[0017] As a further improvement, the material-blocking slope is a plurality of circular protrusions, and the material-blocking slopes are arranged at intervals, and the nitrogen passing through the outer protrusion reacts with the catalyst in the material-blocking slope at the position of the V-shaped contact section.

[0018] As a further improvement, the material holding cavity includes a plurality of conical holes opened on the material pocket tray, an elastic bag is arranged inside the conical hole, and a spring fixedly connected to the second fixing clamp seat is arranged at the bottom of the elastic bag.

[0019] As a further improvement, the rotating assembly includes a driving member connected to the outside of the heating frame, one side of the driving member is provided with an outer sealing sleeve connected to the end of the heating frame, the inner side of the outer sealing sleeve is provided with a heat medium discharge pipe communicated with the heating frame, the driving member includes a fixed gear fixedly connected to the outside of the heating frame, a moving gear is meshed above the fixed gear, and the moving gear is driven by a motor.

[0020] The present invention also provides a high-purity nitrogen production method, comprising the above-mentioned high-purity nitrogen production equipment, comprising the following steps:

[0021] S1: The first adsorption tower adsorbs, and the second adsorption tower does not adsorb: compressed air enters the first adsorption tower from the only opened air inlet input pipe through the first air inlet valve on the first air inlet branch pipe for pressure boost pre-adsorption, and the nitrogen production process begins, that is, the first air outlet valve on the first air outlet branch pipe is opened to transport the finished nitrogen into the nitrogen gas storage tank, and then the finished nitrogen is transported through the upper bypass valve to analyze and purge the second adsorption tower, and the impurities are discharged to the atmosphere through the second lower pressure equalizing valve and then through the muffler;

[0022] S2: Step-by-step pressure equalization: After the first adsorption tower has worked for 40 seconds, the carbon molecular sieve approaches saturation and enters the 3s upper flow-limiting pressure equalization process. First, all valves are closed and only the pressure equalizing valve is opened to enter the upper flow-limiting pressure equalization process. After 3 seconds, the second air intake valve and the first middle pressure equalizing valve are opened to enter the upper middle inequality pressure equalization. The high-pressure semi-finished nitrogen in the first adsorption tower passes through the second air intake valve, the pressure equalizing valve, and the first middle pressure equalizing valve to enter the second adsorption tower, so that the gas pressure of the two adsorption towers is consistent. The pressure equalization is completed after 2 seconds;

[0023] S3: adsorption in the second adsorption tower and desorption in the first adsorption tower: open the second air inlet valve and the air inlet input pipe to allow compressed air to enter the second adsorption tower and start adsorption. Open the second air outlet valve to send nitrogen into the nitrogen gas storage tank. At the same time, open the bypass valve and the first lower pressure equalizing valve to discharge the impurities in the first adsorption tower into the atmosphere until the second adsorption tower completes adsorption and close all valves to start pressure equalization operation.

[0024] S4: Repeat the above steps to continuously produce nitrogen;

[0025] S5: The nitrogen obtained in S4 is introduced into the first deoxidation tower to react with the catalyst at 300° C., and the oxygen in the nitrogen reacts with the carbon to generate carbon dioxide;

[0026] S6: The nitrogen and the generated gas are passed into a cooler for cooling. After cooling, the gas is passed into a first purification tower and a second purification tower to adsorb carbon dioxide and water to obtain high-purity clean nitrogen with a purity of ≥99.999%.

[0027] The beneficial effects of the present invention are:

[0028] The present invention adopts a pressure swing adsorption method to prepare nitrogen, adopts a carbon molecular sieve as an adsorbent, and connects two towers in parallel to alternately perform a nitrogen preparation method of pressurized adsorption and normal pressure regeneration, so that one tower can prepare while the other tower regenerates, so that the entire nitrogen preparation process is carried out continuously, and in the process of preparation, a balanced pressure state is always maintained, which reduces the burden on the molecular sieve and enables the molecular sieve to be used for a long time and stably.

[0029] When air enters the adsorption tower, if the air carries a part of oil or other impurities, it will directly affect the screening effect of the molecular sieve and cannot be regenerated. Therefore, the present invention sets a one-way filtering structure at the lower end of the molecular sieve. Before the air is about to contact the molecular sieve in the tower body, the oil and impurities in the air are first blocked in the one-way filtering structure, and the blocked impurities are immediately removed after the air passes through. In this process, the normal circulation of the gas will not be hindered, so that the purity of the incoming air can be guaranteed, thereby improving the purification effect of the molecular sieve on the air, thereby indirectly improving the purity of the nitrogen.

[0030] The present invention is adopted in stages. First, the upper bypass valve is opened, and there is a certain initial pressure on the top. After the gas enters, the first middle pressure equalizing valve and the second middle pressure equalizing valve are opened to achieve better pressure stabilization and flow limiting effects, which effectively ensure the stability of the molecular sieve filling material in the tower and improve the nitrogen purity at the same time, which is 20% higher than the output of the traditional method.

[0031] The existing nitrogen purification directly heats the general nitrogen and the catalyst under high temperature conditions in the equipment, but the hot end of this step is not always in the same place as the catalyst, which leads to incomplete reaction between the general nitrogen and the catalyst, and further leads to the inability to completely remove the oxygen in the general nitrogen. Therefore, the present invention forms a space for loading the catalyst through the first fixed clamp seat and the second fixed clamp seat through an additional middle heating structure, and directly arranges a heating rack between the first fixed clamp seat and the second fixed clamp seat. On the one hand, the catalyst can be evenly distributed between the first fixed clamp seat and the second fixed clamp seat, and can evenly contact the catalyst when the nitrogen is input from the first fixed clamp seat. At the same time, because the catalyst is directly dispersed on the outside of the heating rack, it is exactly at the optimal temperature when the catalyst contacts the nitrogen, so that the complete reaction of the nitrogen and the catalyst can be achieved. At this stage, the oxygen in the nitrogen completely forms carbon dioxide with the carbon in the catalyst, thereby improving the purity of the nitrogen, and the purity of the nitrogen is ≥99.999%.

[0032] The entire first fixing clamp seat and the second fixing clamp seat are not of a regular shape. In order to adapt to the shape of the heating rack and increase the contact area between the heating rack and the nitrogen as much as possible, the first fixing clamp seat of the present invention includes a circular ring portion and an outer convex portion, so that it can have a relatively uniform plane to accommodate the catalyst and an inclined surface to contact the nitrogen in advance. Correspondingly, the catalyst can be held at the inner bottom of the second fixing clamp seat, thereby improving the efficiency and completeness of the overall reaction.

[0033] Traditional heating structures are often spring tube structures or columnar structures, but in fact this arrangement is not only not conducive to contact with the gas, but also not conducive to the attachment of the catalyst thereto. Therefore, the heating rack of the present invention includes a transverse transverse axis section to ensure the heating of the transverse section and the overall heat medium circulation, and a V-shaped contact section is also provided. The annular arrangement of the V-shaped contact section on the transverse axis section not only increases the contact with nitrogen on multiple surfaces, but also the V-shaped contact section can serve as a catalyst bearing surface, so that the catalyst falls on the V-shaped contact section after being blown in, and has more possibilities of contact with nitrogen.

[0034] However, relatively speaking, the entire V-shaped contact section is still relatively smooth, and the catalyst may not be able to stay on the V-shaped contact section. Therefore, the barrier slope of the present invention is a plurality of circular protrusions, forming small partitions, allowing the catalyst to stay between two protrusions, thereby improving the reaction efficiency at this location.

[0035] Since the direction of vacuuming is the same as the direction of nitrogen entry, it is not feasible to set up a one-way valve structure. However, since the vacuuming stage adopts a negative pressure method, compared with the top pressure of nitrogen entry, the impact on the one-way structure is not that great. Therefore, the present invention provides a one-way valve plate on the one-way hole. When the positive pressure of nitrogen entry is applied, the one-way valve plate will be opened to allow the gas to flow normally. When the catalyst is extracted by negative pressure, although the one-way valve plate will be partially affected, it will not be fully opened. Even if it is partially opened, it can reduce the gap connecting to the outside, thereby not affecting the extraction of the catalyst.

[0036] The material holding chamber is used to hold the catalyst, but if it is directly set as a solid structure, it is difficult to extract the catalyst particles inside. Therefore, the present invention arranges an elastic bag and a spring inside the material holding chamber. When the catalyst enters, pressure can be applied to the elastic bag and the spring to form temporary storage. When negative pressure suction is generated, it can also be deformed in time to discharge the catalyst in time, completing the circulation of a new catalyst.

[0037] In order to allow the used catalyst on the V-shaped contact section to fall off completely, the present invention arranges a driving member on the outside of the heating frame, which drives the entire heating frame to rotate, and seals the matching gap between the heating frame and the heat medium discharge pipe through a sealing sleeve to prevent heat medium leakage, while not affecting the driving member to drive the heating frame to rotate.

[0038] During the use of the catalyst, after a period of use, the carbon content contained therein will gradually decrease until it contains no carbon at all. Therefore, the catalyst needs to be replaced after a period of use. However, since the catalyst has been installed between the first fixed clamp seat and the second fixed clamp seat, it is relatively difficult to replace the catalyst. Therefore, in this case, a circulating material guiding structure is set up on the basis of the middle heating structure. When the catalyst enters the first fixed clamp seat and the second fixed clamp seat, it will be irregularly distributed on the inner side of the material pocket tray, the material holding cavity, the material blocking slope, and the second fixed clamp seat. After use, the catalyst on the heating rack is thrown down by rotating the assembly, so that all the catalyst falls down to the material pocket tray, the material holding cavity, and the second fixed clamp seat, and then the entire tower body is evacuated through the catalyst circulation pipe to extract all the catalyst, and then the new catalyst is injected into the catalyst through the catalyst supply pipeline to replace the catalyst. BRIEF DESCRIPTION OF THE DRAWINGS

[0039] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for use in the embodiments will be briefly introduced below. It should be understood that the following drawings only show certain embodiments of the present invention and therefore should not be regarded as limiting the scope. For ordinary technicians in this field, other related drawings can be obtained based on these drawings without paying creative work.

[0040] Figure 1 It is a structural schematic diagram of the present invention.

[0041] Figure 2 It is a schematic diagram of the three-dimensional structure of the nitrogen production equipment of the present invention.

[0042] Figure 3 The present invention Figure 2 Schematic diagram of the front view structure.

[0043] Figure 4 It is a structural schematic diagram of the first adsorption tower of the present invention.

[0044] Figure 5 The present invention Figure 4 Schematic diagram of the top view structure.

[0045] Figure 6 The present invention Figure 5 Cross-section view at AA in the middle.

[0046] Figure 7 It is a structural schematic diagram of the filter element of the present invention.

[0047] Figure 8 It is a structural schematic diagram of the anti-separation component of the present invention.

[0048] Fig. 9 It is a structural schematic diagram of the purification mechanism of the present invention.

[0049] Fig.10 It is a structural schematic diagram of the first deoxidation tower of the present invention.

[0050] Fig.11 The present invention Fig.10 Schematic diagram of the top view structure.

[0051] Fig.12 The present invention Fig.11 Cross-section view at the middle BB.

[0052] Fig.13 It is a structural schematic diagram of the first fixing clamp seat of the present invention.

[0053] Fig.14 It is a structural schematic diagram of the material pocket tray of the present invention (first viewing angle).

[0054] Fig.15 It is a schematic structural diagram of the material pocket tray of the present invention (second viewing angle).

[0055] Fig.16 It is a structural schematic diagram of the circulating material guiding structure of the present invention (first viewing angle).

[0056] Fig.17 It is a structural schematic diagram of the circulating material guiding structure of the present invention (second viewing angle).

[0057] In the figure:

[0058] The first adsorption tower 1, the first air inlet branch pipe 101, the air inlet input pipe 102, the first air outlet branch pipe 103, the output pipe 104, the first middle equalizing pressure valve 105, the first lower equalizing pressure valve 106, the second adsorption tower 2, the second air inlet branch pipe 201, the second air outlet branch pipe 202, the second middle equalizing pressure valve 203, the second lower equalizing pressure valve 204, the equalizing valve 3, the annular disk 401, the upper mounting frame 4011, the lower mounting frame 4012, the filter element 402, the filter plate 4021, the filter hole 4022, the filter membrane 4023, the adsorption column 4024, the anti-separation element 403, the connecting disk 4031, the through hole 4032, the suction pipe 4033, the external exhaust pipe 4034, the nitrogen storage tank 5, the muffler 6, the bypass valve 7, the first Deoxidation tower 10, second deoxidation tower 20, cooler 30, first purification tower 40, second purification tower 50, first fixed clamp seat 61, annular portion 611, outer convex portion 612, second fixed clamp seat 62, heating frame 63, transverse axis section 631, V-shaped contact section 632, one-way hole 64, feed guide seat 71, heat medium feed pipe 72, catalyst supply pipeline 73, catalyst circulation pipe 74, side bend conduit 741, lower guide pipe 742, material tray 81, material holding cavity 82, tapered hole 821, elastic bag 822, spring 823, material blocking slope 83, rotating assembly 84, driving member 841, fixed gear 8411, moving gear 8412, motor 8413, outer sealing sleeve 842, heat medium discharge pipe 843. DETAILED DESCRIPTION

[0059] In order to make the embodiments of the present invention, all belong to the scope of protection of the present invention. Therefore, the following detailed description of the embodiments of the present invention provided in the accompanying drawings is not intended to limit the scope of the invention claimed for protection, but merely represents the selected embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work belong to the scope of protection of the present invention.

[0060] In the description of the present invention, the terms "first" and "second" are only used for descriptive purposes and cannot be understood as referring to the purpose, technical solutions and advantages of the methods. To be more clear, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work indicate or imply relative importance or implicitly indicate the number of indicated technical features. Therefore, the features defined as "first" and "second" may explicitly or implicitly include one or more of the features. In the description of the present invention, the meaning of "multiple" is two or more, unless otherwise clearly and specifically defined.

[0061] Reference Figure 1 to Figure 17As shown, a high-purity nitrogen production equipment comprises: a nitrogen production mechanism and a purification mechanism, wherein the nitrogen production mechanism comprises a first adsorption tower 1 and a second adsorption tower 2, wherein the first adsorption tower 1 and the second adsorption tower 2 are both provided with carbon molecular sieves, and the lower end of the carbon molecular sieve is provided with a one-way filtering structure, and when the gas passes into the first adsorption tower 1 or the second adsorption tower 2 from bottom to top, the one-way filtering structure filters the gas, and extracts the filtered material on the filtering structure before regeneration under normal pressure; the first adsorption tower 1 and the second adsorption tower 2 are respectively connected with a first air intake branch pipe 101 and a second air intake branch pipe 201, the first air intake branch pipe 101 and the second air intake branch pipe 201 are connected with an air intake input pipe 102, and the first air intake branch pipe 101 and the second air intake branch pipe 201 are connected with an air intake input pipe 102, and the first air intake branch pipe 101 and the second air intake branch pipe 201 are connected with an air intake input pipe 102. The first adsorption tower 1 and the second adsorption tower 2 are respectively provided with a first air inlet valve and a second air inlet valve, the tops of the first adsorption tower 1 and the second adsorption tower 2 are respectively connected to the output pipe 104 through the first air outlet branch pipe 103 and the second air outlet branch pipe 202, the first air outlet branch pipe 103 and the second air outlet branch pipe 202 are respectively connected to the first air outlet valve and the second air outlet valve, a pressure equalizing valve 3 is connected between the first air outlet branch pipe 103 and the second air outlet branch pipe 202, the first adsorption tower 1 and the second adsorption tower 2 are respectively connected to the side with a first middle pressure equalizing valve 105 and a second middle pressure equalizing valve 203, the lower ends of the first adsorption tower 1 and the second adsorption tower 2 are connected with a first lower pressure equalizing valve 106 and a second lower pressure equalizing valve 204, and the output pipe 104 is connected to a nitrogen storage The gas tank 5 is connected to a pressure regulating valve and a flow meter at the gas outlet of the nitrogen gas storage tank 5; the purification mechanism includes a first deoxidation tower 10 connected to the nitrogen gas storage tank 5, the first deoxidation tower 10 is connected to the second deoxidation tower 20 and is filled with a catalyst, the second deoxidation tower 20 is connected to a cooler 30 through a pipeline, the cooler 30 is connected to the first purification tower 40 and the second purification tower 50, the first purification tower 40 and the second purification tower 50 are connected to a finished nitrogen outlet, and also includes: a middle heating structure, including a first fixed clamp seat 61 fixed to the middle position of the first deoxidation tower 10, a second fixed clamp seat 62 is arranged below the first fixed clamp seat 61, and the first fixed clamp seat 61 and the second fixed clamp seat 62 are arranged at intervals. And they are symmetrical to each other, a heating frame 63 is arranged in the interval between the first fixing clamp seat 61 and the second fixing clamp seat 62, and one-way holes 64 are opened on the outer sides of the first fixing clamp seat 61 and the second fixing clamp seat 62, and the catalyst is arranged on the inner sides of the first fixing clamp seat 61 and the second fixing clamp seat 62 and the outer side of the heating frame 63; a circulating supply structure comprises a feed guide seat 71 arranged on one side of the heating frame 63, a heat medium feed pipe 72 communicating with the inside of the heating frame 63 is arranged on the inner side of the feed guide seat 71, a catalyst supply pipeline 73 communicating with the interval between the first fixing clamp seat 61 and the second fixing clamp seat 62 is arranged on the upper end of the heat medium feed pipe 72, and a catalyst circulation pipe 74 is arranged on the lower end of the other side of the heating frame 63;The circulating material guiding structure includes a material pan 81 arranged below the heating frame 63, a plurality of movable material holding cavities 82 are arranged at the bottom of the material pan 81, a material blocking slope 83 is arranged on the outer side of the middle of the heating frame 63, and a rotating assembly 84 is arranged on one side of the heating frame 63. When the catalyst enters the interval between the first fixed clamp seat 61 and the second fixed clamp seat 62 through the catalyst supply pipeline 73 and is distributed to the interval between the material pan 81, the material holding cavity 82, and the material blocking slope 83, when the catalyst reaches the use cycle, the catalyst on the heating frame 63 is shaken downward by the rotating assembly 84, and the used catalyst is extracted through the catalyst circulation pipe 74. ;

[0062] In this embodiment, the output pipe 104 is connected to a nitrogen gas storage tank 5 , and the gas outlet end of the nitrogen gas storage tank 5 is connected to a pressure regulating valve and a flow meter, and the generated nitrogen is directly introduced into the nitrogen gas storage tank 5 for storage.

[0063] In order to prevent the sound of the pressure-equalizing exhausted gas from being too loud, the first lower pressure-equalizing valve 106 and the second lower pressure-equalizing valve 204 are both connected to the muffler 6 .

[0064] Furthermore, a bypass valve 7 connected in parallel with the pressure equalizing valve 3 is provided between the first gas outlet branch pipe 103 and the second gas outlet branch pipe 202 .

[0065] In the whole nitrogen production process, the valve is controlled in stages. The upper bypass valve 7 is opened first, and there is a certain initial pressure at the top. After the gas enters, the first middle pressure equalizing valve 105 and the second middle pressure equalizing valve 203 are opened to achieve better pressure stabilization and flow limiting, effectively ensuring the stability of the molecular sieve filling material in the tower, and improving the nitrogen purity. The output is 20% higher than the traditional method. The overall work flow is divided into several parts, namely:

[0066] ①. The first adsorption tower 1 adsorbs, and the second adsorption tower 2 does not adsorb; compressed air enters the first adsorption tower 1 from the only opened air inlet input pipe 102 through the first air inlet valve on the first air inlet branch pipe 101 for pressure increase and pre-adsorption, and the nitrogen production process begins, that is, the first air outlet valve on the first air outlet branch pipe 103 is opened to transport the finished nitrogen into the nitrogen gas storage tank 5, and then the finished nitrogen is transported through the upper bypass valve 7 to the second adsorption tower 2 for analysis and purge, and the impurities are discharged to the atmosphere through the second lower pressure equalizing valve 204 and then through the muffler 6; ②. Step-by-step pressure equalization; After the first adsorption tower 1 has worked for 40 seconds, the carbon molecular sieve approaches saturation, and first enters the upper flow limiting pressure equalization process of about 3 seconds. First, all valves are closed and only the pressure equalizing valve 3 is opened to enter the upper flow limiting pressure equalization process. After 3 seconds, the second air inlet valve and the first middle pressure equalizing valve 105 are opened to enter the upper middle inequality pressure equalization, and the first adsorption tower 1 The high-pressure semi-finished nitrogen in the second adsorption tower 2 passes through the second air inlet valve, the pressure equalizing valve 3, and the first middle pressure equalizing valve 105 to make the air pressure of the two adsorption towers consistent (pressure is about 3-4KG), and the pressure equalization is completed in about 2 seconds; ③. The second adsorption tower 2 adsorbs, and the first adsorption tower 1 desorbs; open the second air inlet valve and the air inlet input pipe 102 to allow compressed air to enter the second adsorption tower 2 and start adsorption. The second air outlet valve is opened to send nitrogen into the nitrogen storage tank 5. At the same time, the impurities in the first adsorption tower 1 are discharged into the atmosphere by opening the bypass valve 7 and the first lower pressure equalizing valve 106 until the second adsorption tower 2 completes the adsorption, and all valves are closed to enter the pressure equalization operation; ④. Repeat the above steps to continuously produce nitrogen.

[0067] This embodiment adopts a pressure swing adsorption method to produce nitrogen, uses a carbon molecular sieve as an adsorbent, and connects two towers in parallel to alternately perform a nitrogen production method of pressurized adsorption and normal pressure regeneration, so that one tower can produce while the other tower is regenerating, so that the entire nitrogen production process is carried out continuously, and in the process of production, it is always kept in a state of equal pressure, which reduces the burden on the molecular sieve and allows the molecular sieve to be used for a long time and stably.

[0068] When air enters the adsorption tower, if the air carries a part of oil or other impurities, it will directly affect the screening effect of the molecular sieve and cannot be regenerated. Therefore, the present invention sets a one-way filtering structure at the lower end of the molecular sieve. Before the air is about to contact the molecular sieve in the tower body, the oil and impurities in the air are first blocked in the one-way filtering structure, and the blocked impurities are immediately removed after the air passes through. In this process, the normal circulation of the gas will not be hindered, so that the purity of the incoming air can be guaranteed, thereby improving the purification effect of the molecular sieve on the air, thereby indirectly improving the purity of the nitrogen.

[0069] Among them, the one-way filtration structure includes an annular disk 401 located below the carbon molecular sieve and fixedly connected to the inner walls of the first adsorption tower 1 and the second adsorption tower 2. A filter element 402 is arranged on the inner side of the annular disk 401. A reflection element 403 is arranged at the lower end of the filter element 402. The end of the reflection element 403 is connected to the outside world. After each air enters, the filter element 402 will filter, and after each filtration, the reflection element 403 will quickly reflect the substances adhered to the reflection element 403, so that the filter element 402 will not re-incorporate this part of impurities into the tower body when the molecular sieve is regenerated.

[0070] During the entire filtering and anti-separation process, the positions of the filter element 402 and the anti-separation element 403 are fixed and are both through the annular disk 401. Therefore, the annular disk 401 includes an upper mounting frame 4011 for mounting the filter element 402, and the lower end of the upper mounting frame 4011 is connected to a lower mounting frame 4012, and the anti-separation element 403 is arranged on the inner side of the lower mounting frame 4012.

[0071] During filtering, filtering is performed through two parts. Specifically, the filter element 402 includes a filter plate 4021 connected to the inner side of the upper mounting frame 4011, and a plurality of filter holes 4022 are arranged on the filter plate 4021. A filter membrane 4023 is fixedly connected to the inner side of the filter holes 4022, and a plurality of adsorption columns 4024 are arranged under the filter membrane 4023. The adsorption columns 4024 are used to adsorb the granular structure, and the filter membrane 4023 is used to filter and adsorb gaseous and liquid impurities such as oil stains.

[0072] After each filtration, the anti-separation is quickly performed. The anti-separation member 403 includes a connecting plate 4031 connected to the lower mounting frame 4012. The connecting plate 4031 is provided with a through hole 4032 staggered from the filter hole 4022. A suction pipe 4033 is arranged directly below the filter hole 4022. All the suction pipes 4033 are connected to an external discharge pipe 4034. The suction pipe 4033 is located below the filter hole 4022. The impurities dripping and the impurities in the filter hole 4022 can be quickly taken away during extraction, and the staggered through holes 4032 can ensure normal air inflow and normal pressure regeneration without blocking the flow path.

[0073] The prepared nitrogen needs to be purified before it can be put into use, otherwise it will contain oxygen and water vapor impurities.

[0074] In the process of nitrogen purification, the general nitrogen (purity ≥99.9%) produced by the nitrogen production system directly enters the middle heating structure inside the deoxygenation tower and is heated to about 300°C. Under the catalytic action of the catalyst, trace oxygen in the nitrogen reacts with carbon to generate carbon dioxide. After being cooled to a lower temperature by the cooler 30, it is processed by the specially designed first purification tower 40 and the second purification tower 50 (using molecular sieves with strong carbon dioxide adsorption capacity to shorten the operation switching cycle of the adsorption dryer and increase the amount of carbon dioxide adsorption while ensuring nitrogen consumption) to remove carbon dioxide and trace moisture, and then pass through the purity analysis device to obtain high-purity clean nitrogen with a purity ≥99.999%.

[0075] The existing nitrogen purification directly heats the general nitrogen and the catalyst under high temperature conditions in the equipment, but the hot end of this step is not always in the same place as the catalyst, which leads to incomplete reaction between the general nitrogen and the catalyst, and further leads to the inability to completely remove the oxygen in the general nitrogen. Therefore, the present invention forms a space for loading the catalyst through the first fixed clamp seat 61 and the second fixed clamp seat 62 through the additional middle heating structure, and directly sets a heating rack 63 between the first fixed clamp seat 61 and the second fixed clamp seat 62. On the one hand, the catalyst can be evenly distributed between the first fixed clamp seat 61 and the second fixed clamp seat 62, so that the nitrogen can be evenly contacted with the catalyst when it is input from the first fixed clamp seat 61. At the same time, because the catalyst is directly dispersed on the outside of the heating rack 63, it is exactly located at the optimal temperature when the catalyst contacts the nitrogen, so that the complete reaction of the nitrogen and the catalyst can be achieved. At this stage, the oxygen in the nitrogen completely forms carbon dioxide with the carbon in the catalyst, thereby improving the purity of the nitrogen, and the purity of the nitrogen is ≥99.999%.

[0076] The entire first fixing clamp seat 61 and the second fixing clamp seat 62 are not of a regular shape. In order to adapt to the shape of the heating rack 63 and increase the contact area between the heating rack 63 and the nitrogen as much as possible, the first fixing clamp seat 61 of the present embodiment includes a circular portion 611 fixed to the inner wall of the first deoxidation tower 10, and the inner side of the circular portion 611 is connected to an arched outer convex portion 612, and the outer sides of the circular portion 611 and the outer convex portion 612 are both provided with a one-way hole 64, wherein the first fixing clamp seat 61 includes the circular portion 611 and the outer convex portion 612, so that it can have a relatively uniform plane to accommodate the catalyst, and also has an inclined surface to contact the nitrogen in advance, and correspondingly, the catalyst can be held at the inner bottom of the second fixing clamp seat 62, thereby improving the efficiency and completeness of the overall reaction.

[0077] Traditional heating structures are often spring tube structures or columnar structures, but in fact this arrangement is not only not conducive to contact with the gas, but also not conducive to the attachment of the catalyst thereto. Therefore, the heating rack 63 of this embodiment includes a transverse axis section 631 arranged on the circulation supply structure, and a plurality of V-shaped contact sections 632 are connected to the outer peripheral surface of the transverse axis section 631, and the V-shaped contact section 632 is communicated with the transverse axis section 631. The heating rack 63 includes a transverse transverse axis section 631 to ensure the heating of the transverse section and the overall heat medium circulation, and a V-shaped contact section 632 is also arranged. The annular arrangement of the V-shaped contact section 632 on the transverse axis section 631 not only increases the contact with nitrogen on multiple surfaces, but also the V-shaped contact section 632 can serve as a catalyst bearing surface, so that the catalyst falls on the V-shaped contact section 632 after being blown in, and has more contact possibilities with nitrogen. In this embodiment, six groups of V-shaped contact sections 632 are arranged, and can also be arranged in four or five groups, etc.

[0078] However, relatively speaking, the entire V-shaped contact section 632 is still relatively smooth, and the catalyst may not be able to stay on the V-shaped contact section 632. Therefore, in this embodiment, the material blocking slope 83 is a plurality of circular protrusions, and the material blocking slopes 83 are arranged at intervals. The nitrogen through the outer protrusion 612 reacts with the catalyst in the material blocking slope 83 at the position of the V-shaped contact section 632, and small partitions are formed between the material blocking slopes 83, allowing the catalyst to stay between the two protrusions, thereby improving the reaction efficiency at this position. In other embodiments, the material blocking slope 83 can also be a concave structure, which can be directly used to carry catalyst particles and react directly inside.

[0079] Since the direction of vacuuming is the same as the direction of nitrogen entry, it is not feasible to set up a one-way valve structure. However, since negative pressure is used in the vacuuming stage, the impact on the one-way structure is not that great compared to the top pressure applied when nitrogen enters. Therefore, the one-way hole 64 of this embodiment includes a through hole connecting the inside and outside of the first fixed clamp seat 61, and a one-way valve plate is provided on the side of the through hole facing the inside of the first fixed clamp seat 61. By providing a one-way valve plate on the one-way hole 64, when positive pressure is applied when nitrogen enters, the one-way valve plate will be opened to allow the gas to flow normally. When the catalyst is extracted under negative pressure, although the one-way valve plate will be partially affected, it will not be fully opened. Even if it is partially opened, the gap connecting to the outside can be reduced, thereby not affecting the extraction of the catalyst.

[0080] The catalyst circulation pipe 74 is not arranged at the upper end like the catalyst supply pipe 73, but is arranged at the lower end, and is intended to be rotated at a certain angle. Specifically, the catalyst circulation pipe 74 includes a side bend conduit 741 inserted laterally into the second fixed clamp seat 62, and a lower lead pipe 742 is arranged on the outer side of the side bend conduit 741. After the side bend conduit 741 changes direction, the liquid is discharged externally through the lower lead pipe 742.

[0081] During the use of the catalyst, after a period of use, the carbon content contained therein will gradually decrease until it is completely carbon-free. Therefore, the catalyst needs to be replaced after a period of use. However, since the catalyst has been installed between the first fixed clamp seat 61 and the second fixed clamp seat 62, it is relatively difficult to replace the catalyst. Therefore, in this case, a circulating material guiding structure is set up on the basis of the middle heating structure. When the catalyst is introduced into the first fixed clamp seat 61 and the second fixed clamp seat 62, it will be irregularly distributed on the inner side of the material pocket plate 81, the material holding cavity 82, the material blocking slope 83, and the second fixed clamp seat 62. After use, the catalyst on the heating frame 63 is thrown down by the rotating component 84, so that all the catalyst falls down to the material pocket plate 81, the material holding cavity 82, and the second fixed clamp seat 62, and then the entire tower body is evacuated through the catalyst circulation pipe 74 to extract all the catalyst, and then the new catalyst is injected into the catalyst through the catalyst supply pipeline 73 to replace the catalyst.

[0082] Since the entire heating rack 63 needs to rotate, the material tray 81 cannot be directly set on the heating rack 63. Therefore, the material tray 81 of this embodiment is located above the second fixed clamp seat 62, and the general nitrogen entering through the one-way hole 64 on the annular portion 611 directly reacts with the catalyst in the material tray 81 under the heating of the heating rack 63.

[0083] The material holding chamber 82 is used to hold the catalyst, but if it is directly set as a solid structure, it is difficult to extract the catalyst particles inside. Therefore, the material holding chamber 82 of this embodiment includes a plurality of conical holes 821 opened on the material pocket tray 81, and an elastic bag 822 is arranged inside the conical hole 821. The bottom of the elastic bag 822 is provided with a spring 823 fixed to the second fixed clamp seat 62. By arranging the elastic bag 822 and the spring 823 inside the material holding chamber 82, when the catalyst enters, pressure can be applied to the elastic bag 822 and the spring 823 to form temporary storage, and when negative pressure suction is generated, it can also be deformed in time to discharge the catalyst in time, thereby completing the circulation of the new catalyst.

[0084] In order to allow the used catalyst on the V-shaped contact section 632 to completely fall off, the present invention sets a driving member 841 on the outer side of the heating frame 63, and the rotating assembly 84 includes a driving member 841 connected to the outer side of the heating frame 63, and one side of the driving member 841 is provided with an outer sealing sleeve 842 connected to the end of the heating frame 63, and the inner side of the outer sealing sleeve 842 is provided with a heat medium discharge pipe 843 communicated with the heating frame 63. The driving member 841 drives the entire heating frame 63 to rotate, and the sealing sleeve 842 seals the fitting gap between the heating frame 63 and the heat medium discharge pipe 843 to prevent leakage of heat medium, while not affecting the driving member 841 to drive the heating frame 63 to rotate.

[0085] The driving member 841 of this embodiment includes a fixed gear 8411 fixedly connected to the outside of the heating frame 63, and a movable gear 8412 is meshed above the fixed gear 8411. The movable gear 8412 is driven by a motor 8413. The movable gear 8412 is driven to rotate by the external motor 8413, thereby rotating the fixed gear 8411 and the heating frame 63 connected to the fixed gear 8411, thereby achieving a better material replacement effect.

[0086] Another embodiment of the present invention further provides a high-purity nitrogen production method, comprising the above-mentioned high-purity nitrogen production equipment, comprising the following steps:

[0087] S1: The first adsorption tower 1 adsorbs, and the second adsorption tower 2 does not adsorb: the compressed air enters the first adsorption tower 1 from the only opened air inlet input pipe 102 through the first air inlet valve on the first air inlet branch pipe 101 to increase the pressure for pre-adsorption, and the nitrogen production process begins, that is, the first air outlet valve on the first air outlet branch pipe 103 is opened to transport the finished nitrogen into the nitrogen gas storage tank 5, and then the finished nitrogen is transported through the upper bypass valve 7 to analyze and purge the second adsorption tower 2, and the impurities are discharged to the atmosphere through the second lower pressure equalizing valve 204 and then through the muffler 6;

[0088] S2: Step-by-step pressure equalization: After the first adsorption tower 1 has worked for 40 seconds, the carbon molecular sieve approaches saturation and enters the upper flow-limiting pressure equalization process for 3 seconds. First, all valves are closed and only the pressure equalizing valve 3 is opened to enter the upper flow-limiting pressure equalization process. After 3 seconds, the second air intake valve and the first middle pressure equalizing valve 105 are opened to enter the upper middle inequality pressure equalization. The high-pressure semi-finished nitrogen in the first adsorption tower 1 enters the second adsorption tower 2 through the second air intake valve, the pressure equalizing valve 3, and the first middle pressure equalizing valve 105, so that the air pressure of the two adsorption towers is consistent, and the pressure equalization is completed after 2 seconds;

[0089] S3: The second adsorption tower 2 adsorbs, and the first adsorption tower 1 desorbs: the second air inlet valve and the air inlet input pipe 102 are opened to allow compressed air to enter the second adsorption tower 2, and the adsorption work is started. The second air outlet valve is opened to send nitrogen into the nitrogen gas storage tank 5. At the same time, the impurities in the first adsorption tower 1 are discharged into the atmosphere by opening the bypass valve 7 and the first lower pressure equalizing valve 106 until the second adsorption tower 2 completes the adsorption, and all valves are closed to enter the pressure equalizing operation;

[0090] S4: Repeat the above steps to continuously produce nitrogen;

[0091] S5: The nitrogen obtained in S4 is introduced into the first deoxidation tower 10 to react with the catalyst at 300° C., and the oxygen in the nitrogen reacts with the carbon to generate carbon dioxide;

[0092] S6: The nitrogen and the generated gas are passed into the cooler 30 for cooling. The cooled gas is passed into the first purification tower 40 and the second purification tower 50 to adsorb carbon dioxide and water, thereby obtaining high-purity clean nitrogen with a purity of ≥99.999%.

[0093] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A high-purity nitrogen production equipment, characterized in that: include: A nitrogen production mechanism and a purification mechanism, the nitrogen production mechanism comprising a first adsorption tower (1) and a second adsorption tower (2), the first adsorption tower (1) and the second adsorption tower (2) are both provided with a carbon molecular sieve, a one-way filter structure is provided at the lower end of the carbon molecular sieve, when the gas passes into the first adsorption tower (1) or the second adsorption tower (2) from bottom to top, the one-way filter structure filters the gas, and the filtered matter on the filter structure is extracted before regeneration at normal pressure; The first adsorption tower (1) and the second adsorption tower (2) are respectively connected to a first air inlet branch pipe (101) and a second air inlet branch pipe (201); the first air inlet branch pipe (101) and the second air inlet branch pipe (201) are connected to an air inlet input pipe (102); the first air inlet branch pipe (101) and the second air inlet branch pipe (201) are respectively provided with a first air inlet valve and a second air inlet valve; the tops of the first adsorption tower (1) and the second adsorption tower (2) are respectively connected to an output pipe (104) via a first air outlet branch pipe (103) and a second air outlet branch pipe (202); the first air outlet branch pipe (103) and the second air outlet branch pipe (201) are respectively connected to an output pipe (104) via a first air outlet branch pipe (103) and a second air outlet branch pipe (202); 202), a first gas outlet valve and a second gas outlet valve are respectively connected to the first gas outlet branch pipe (103) and the second gas outlet branch pipe (202), a pressure equalizing valve (3) is connected between the first gas outlet branch pipe (103) and the second gas outlet branch pipe (202), a first middle pressure equalizing valve (105) and a second middle pressure equalizing valve (203) are respectively connected to the sides of the first adsorption tower (1) and the second adsorption tower (2), a first lower pressure equalizing valve (106) and a second lower pressure equalizing valve (204) are connected to the lower ends of the first adsorption tower (1) and the second adsorption tower (2), a nitrogen gas storage tank (5) is connected to the output pipe (104), and a pressure stabilizing valve and a flow meter are connected to the gas outlet end of the nitrogen gas storage tank (5); The purification mechanism comprises a first deoxidation tower (10) connected to a nitrogen storage tank (5); the first deoxidation tower (10) is connected to a second deoxidation tower (20) and is filled with a catalyst; the second deoxidation tower (20) is connected to a cooler (30) via a pipeline; the cooler (30) is connected to the first purification tower (40) and the second purification tower (50); the first purification tower (40) and the second purification tower (50) are connected to a finished nitrogen outlet; the purification mechanism further comprises: A middle heating structure comprises a first fixing clamp seat (61) fixed at the middle position of the first deoxidation tower (10); a second fixing clamp seat (62) is arranged below the first fixing clamp seat (61); the first fixing clamp seat (61) and the second fixing clamp seat (62) are arranged at an interval and symmetrically with each other; a heating frame (63) is arranged in the interval between the first fixing clamp seat (61) and the second fixing clamp seat (62); one-way holes (64) are provided on the outer sides of the first fixing clamp seat (61) and the second fixing clamp seat (62); the catalyst is arranged on the inner sides of the first fixing clamp seat (61), the second fixing clamp seat (62) and the outer side of the heating frame (63); A circulating supply structure, comprising a feed guide seat (71) arranged on one side of a heating frame (63), a heat medium feed pipe (72) communicating with the interior of the heating frame (63) being arranged on the inner side of the feed guide seat (71), a catalyst supply pipeline (73) communicating with the first fixed clamp seat (61) and the second fixed clamp seat (62) being arranged at the upper end of the heat medium feed pipe (72), and a catalyst circulation pipe (74) being arranged at the lower end of the other side of the heating frame (63); The circulating material guiding structure comprises a material collecting tray (81) arranged below a heating frame (63); a plurality of movable material containing cavities (82) are arranged at the bottom of the material collecting tray (81); a material blocking slope (83) is arranged on the outer side of the middle part of the heating frame (63); and a rotating assembly (84) is arranged on one side of the heating frame (63). When the catalyst enters the gap between the first fixed clamp seat (61) and the second fixed clamp seat (62) through a catalyst supply pipeline (73) and is distributed to the gap between the material collecting tray (81), the material containing cavities (82) and the material blocking slope (83), when the catalyst reaches the end of the use cycle, the catalyst on the heating frame (63) is shaken downward by the rotating assembly (84), and the used catalyst is extracted through the catalyst circulation pipe (74).

2. A high-purity nitrogen production equipment according to claim 1, characterized in that: The one-way filtering structure comprises an annular disk (401) located below the carbon molecular sieve and fixedly connected to the inner walls of the first adsorption tower (1) and the second adsorption tower (2); a filter element (402) is arranged on the inner side of the annular disk (401); a return element (403) is arranged at the lower end of the filter element (402); and the end of the return element (403) is connected to the outside.

3. A high-purity nitrogen production equipment according to claim 2, characterized in that: The annular disk (401) comprises an upper mounting frame (4011) for mounting a filter element (402); a lower mounting frame (4012) is connected to the lower end of the upper mounting frame (4011); and a de-separation element (403) is provided on the inner side of the lower mounting frame (4012).

4. A high-purity nitrogen production equipment according to claim 3, characterized in that: The filter element (402) comprises a filter plate (4021) connected to the inner side of an upper mounting frame (4011), a plurality of filter holes (4022) being provided on the filter plate (4021), a filter membrane (4023) being fixedly connected to the inner side of the filter hole (4022), and a plurality of adsorption columns (4024) being provided below the filter membrane (4023).

5. A high-purity nitrogen production equipment according to claim 3, characterized in that: The anti-separation member (403) comprises a connecting plate (4031) connected to the lower mounting frame (4012); the connecting plate (4031) is provided with a through hole (4032) staggered with the filter hole (4022); a suction pipe (4033) is arranged directly below the filter hole (4022); and all the suction pipes (4033) are connected to an external discharge pipe (4034).

6. A high-purity nitrogen production equipment according to claim 1, characterized in that: The first fixing clamp seat (61) comprises a circular portion (611) fixedly connected to the inner wall of the first deoxidation tower (10); the inner side of the circular portion (611) is connected to an arched outer convex portion (612); the outer sides of the circular portion (611) and the outer convex portion (612) are both provided with one-way holes (64); the heating frame (63) comprises a transverse axis section (631) provided on the circulation supply structure; the outer peripheral surface of the transverse axis section (631) is connected to a plurality of V-shaped contact sections (632); the V-shaped contact sections (632) are in communication with the transverse axis section (631).

7. A high-purity nitrogen production equipment according to claim 6, characterized in that: The material blocking slope (83) is a plurality of circular protrusions, and the material blocking slopes (83) are arranged at intervals, and the nitrogen passing through the outer protrusion (612) reacts with the catalyst in the material blocking slope (83) at the position of the V-shaped contact section (632).

8. A high-purity nitrogen production equipment according to claim 7, characterized in that: The material holding cavity (82) comprises a plurality of conical holes (821) formed on the material pocket tray (81), an elastic bag (822) being arranged inside the conical holes (821), and a spring (823) fixedly connected to the second fixing clamp seat (62) being arranged at the bottom of the elastic bag (822).

9. A high-purity nitrogen production equipment according to claim 8, characterized in that: The rotating assembly (84) comprises a driving member (841) sleeved on the outside of the heating frame (63); an outer sealing sleeve (842) sleeved on the end of the heating frame (63) is provided on one side of the driving member (841); a heat medium discharge pipe (843) in communication with the heating frame (63) is provided on the inner side of the outer sealing sleeve (842); the driving member (841) comprises a fixed gear (8411) fixedly connected to the outside of the heating frame (63); a movable gear (8412) is meshed on the upper side of the fixed gear (8411); and the movable gear (8412) is driven by a motor (8413).

10. A high-purity nitrogen production method, comprising the high-purity nitrogen production equipment according to any one of claims 1 to 9, characterized in that: The following steps are included: S1: The first adsorption tower (1) adsorbs, and the second adsorption tower (2) does not adsorb: compressed air enters the first adsorption tower (1) from the only opened air inlet input pipe (102) through the first air inlet valve on the first air inlet branch pipe (101) to increase the pressure for pre-adsorption, and the nitrogen production process begins, that is, the first air outlet valve on the first air outlet branch pipe (103) is opened to transport the finished nitrogen into the nitrogen storage tank (5), and then the finished nitrogen is transported through the upper bypass valve (7) to analyze and purge the second adsorption tower (2), and the impurities are discharged to the atmosphere through the second lower pressure equalizing valve (204) and the silencer (6); S2: Step-by-step pressure equalization: After the first adsorption tower (1) has been operating for 40 seconds, the carbon molecular sieve approaches saturation and enters the upper flow limiting pressure equalization process for 3 seconds. First, all valves are closed and only the pressure equalization valve (3) is opened to enter the upper flow limiting pressure equalization process. After 3 seconds, the second air inlet valve and the first middle pressure equalization valve (105) are opened to enter the upper middle inequality pressure equalization process. The high-pressure semi-finished nitrogen in the first adsorption tower (1) enters the second adsorption tower (2) through the second air inlet valve, the pressure equalization valve (3) and the first middle pressure equalization valve (105), so that the gas pressure of the two adsorption towers is consistent. The pressure equalization is completed after 2 seconds. S3: The second adsorption tower (2) adsorbs and the first adsorption tower (1) desorbs: the second air inlet valve and the air inlet input pipe (102) are opened to allow compressed air to enter the second adsorption tower (2) and start adsorption. The second air outlet valve is opened to send nitrogen into the nitrogen storage tank (5). At the same time, the impurities in the first adsorption tower (1) are discharged into the atmosphere by opening the bypass valve (7) and the first lower pressure equalizing valve (106) until the second adsorption tower (2) completes adsorption and all valves are closed to start pressure equalization operation. S4: Repeat the above steps to continuously produce nitrogen; S5: the nitrogen obtained in S4 is introduced into the first deoxidation tower (10) to react with the catalyst at 300°C, and the oxygen in the nitrogen reacts with the carbon to generate carbon dioxide; S6: The nitrogen and the generated gas are passed into a cooler (30) for cooling. The cooled gas is passed into a first purification tower (40) and a second purification tower (50) to adsorb carbon dioxide and water, thereby obtaining high-purity clean nitrogen with a purity of ≥99.999%.

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