Molecular sieve regeneration column and regeneration method thereof

Abstract

The invention discloses a molecular sieve regeneration column and a regeneration method thereof, the molecular sieve regeneration column comprises: a furnace tube, the furnace tube comprises a hollow space enclosed by a tube body, the upper end part of the tube body is provided with a hydrogen inlet, and the lower end part of the tube body is provided with a hydrogen outlet; the shell is coaxially arranged on the periphery of the outer side wall of the pipe body; the heating pipe is attached to the periphery of the pipe body, is arranged in an interlayer space between the shell and the outer side wall of the pipe body and is used for heating the pipe body; the heat conduction frame is arranged in the hollow space of the furnace tube, the heat conduction frame is used for filling a molecular sieve, the heat conduction frame comprises an axial connecting rod and at least two layers of heat conduction nets, the axial connecting rod vertically penetrates through the centers of the heat conduction nets and is fixedly connected with the heat conduction nets, and the heat conduction nets are provided with vertically-hollowed-out hole channels. The heat conduction frame is arranged in the molecular sieve regeneration column and can quickly transfer heat of the heating pipe into the furnace pipe, so that the radial temperature difference is reduced, the defect of poor heat conduction of the molecular sieve is overcome, and the regeneration period is shortened.

Description

Technical Field

[0001] The invention relates to a molecular sieve regeneration column and a regeneration method thereof. Background Art

[0002] Green hydrogen can help achieve the goal of carbon neutrality. The use of new energy sources such as wind power and photovoltaics to electrolyze water to produce green hydrogen is pollution-free and carbon-free throughout the process, which fully meets the requirements of carbon neutrality. The impurities in the electrolysis of water to produce hydrogen only contain oxygen and water. To obtain high-purity hydrogen, the impurities must be removed. Molecular sieves are a key link in hydrogen dehumidification, but the dehumidification function of the molecular sieve fails after the molecular sieve is saturated with water. If the dehumidification function of the molecular sieve is to be activated, it must be regenerated. The traditional regeneration method of molecular sieves is to purge with hot nitrogen for several hours, and then purge with cold nitrogen for several hours, and the molecular sieve is regenerated. However, traditional molecular sieve regeneration equipment is bulky and takes a long time to regenerate, making it difficult to meet the requirements for further efficiency improvement. Summary of the invention

[0003] In order to overcome the problems of low integration of molecular sieve regeneration equipment and long molecular sieve regeneration time in the prior art, the present invention provides a molecular sieve regeneration column and a regeneration method thereof. The molecular sieve regeneration column of the present invention occupies less space, which is conducive to system integration; since the hydrogen generated by the system is used as the regeneration gas, the need for nitrogen in the traditional method is overcome, so that the molecular sieve regeneration column has the advantages of stronger environmental adaptability and the like.

[0004] The present invention solves the above technical problems through the following technical solutions:

[0005] A molecular sieve regeneration column, comprising:

[0006] A furnace tube, the furnace tube comprising a hollow space enclosed by a tube body, an upper end of the tube body being provided with a hydrogen inlet, and a lower end of the tube body being provided with a hydrogen outlet;

[0007] A shell, the shell being coaxially arranged on the periphery of the outer side wall of the tube body;

[0008] A heating tube, which is attached to the outer periphery of the tube body and placed in the interlayer space between the shell and the outer side wall of the tube body, and is used to heat the tube body;

[0009] A heat-conducting frame is arranged in the hollow space of the tube body, the heat-conducting frame is used to fill the molecular sieve, the heat-conducting frame includes an axial connecting rod and at least two layers of heat-conducting mesh, the axial connecting rod vertically passes through the center of the heat-conducting mesh and is fixedly connected to the heat-conducting mesh, the heat-conducting mesh has upper and lower hollow channels, and the diameter of the heat-conducting mesh does not exceed the inner diameter of the tube body.

[0010] In this technical solution, the heating tube of the molecular sieve regeneration column is arranged outside the molecular sieve for external heating, and a heat-conducting frame is arranged inside the tube body to cooperate with the heating tube. The heat-conducting frame can quickly transfer the heat of the external heating tube to the furnace tube, accelerate the conduction of heat to the core of the furnace tube, and reduce the radial temperature gradient, thereby overcoming the disadvantage of poor thermal conductivity of the molecular sieve, thereby improving the regeneration effect and shortening the regeneration cycle. In addition, in this technical solution, preferably, the heat-conducting network is 7 layers.

[0011] Preferably, the heat-conducting frame is further provided with a plurality of axial conduits, the axial conduits vertically passing through the channels of the heat-conducting net and fixedly connected to the heat-conducting net, the axial conduits being used to place thermocouples, and the thermocouples being used to detect the temperature of the molecular sieve.

[0012] In the present technical solution, preferably, three axial catheters are provided.

[0013] Preferably, the lengths of the axial conduits are different from each other; preferably, the lengths of the three axial conduits are equidistantly distributed, and the temperatures of the molecular sieves in the upper, middle and lower regions inside the furnace tube can be detected separately in order to perform heating monitoring.

[0014] Preferably, the holes of the heat-conducting net are in the shape of a circle, a triangle, a fan, or a quadrilateral.

[0015] Preferably, the heat-conducting net, the axial conduit and the axial connecting rod are all made of stainless steel. In this technical solution, the heat-conducting net, the axial conduit and the axial connecting rod are made of stainless steel, which is beneficial to heat transfer.

[0016] Preferably, the molecular sieve regeneration column also includes an insulation layer, which is coaxially arranged on the periphery of the outer wall of the tube body and placed in the interlayer space between the shell and the outer wall of the tube body; the heating tube is integrated into the inner wall of the insulation layer.

[0017] In this technical solution, the molecular sieve regeneration column is provided with an insulation layer for heat preservation to prevent heat loss from the heating tube, thereby improving the heating efficiency; at the same time, the heating tube is integrated into the inner wall of the insulation layer, which is an integrated design and can increase the integration of the molecular sieve regeneration column.

[0018] Preferably, the heating tubes are equidistantly arranged along the circumference of the inner wall of the insulation layer. In the present technical solution, the equidistantly arranged heating tubes can improve the uniformity of heating, ensure that the molecular sieves at different positions can be heated synchronously, improve heating efficiency, and shorten regeneration time.

[0019] Preferably, the length of the heating tube is the same as the height of the insulation layer; in the present technical solution, the length of the heating tube is equal to the height of the insulation layer, which can maximize the use of the space on the inner wall of the insulation layer, save space, improve the utilization rate per unit area, and is conducive to the integration of the molecular sieve regeneration column.

[0020] Preferably, a thermocouple is also attached to the inner wall of the thermal insulation layer, and the thermocouple is used to detect the temperature of the tube body;

[0021] Preferably, the insulation layer is formed by two semi-cylindrical structures buckled on the periphery of the outer wall of the tube body, and the buckled seams of the insulation layer correspond to each other. In this technical solution, the insulation layer is a split design for easy assembly.

[0022] Preferably, the molecular sieve regeneration column further comprises a cooling tube, which is coaxially arranged on the periphery of the outer wall of the tube body and is placed between the heating tube and the outer wall of the tube body. The cooling tube is forced to cool down by water cooling to shorten the cooling time and the regeneration cycle.

[0023] Preferably, a water inlet is provided at one end of the cooling pipe, a water outlet is provided at the other end of the cooling pipe, and the cooling medium is water.

[0024] Preferably, the cooling pipe is formed by two water pipes which are distributed in an S shape along the axial direction of the pipe body and have a semicircular structure along the circumference of the pipe body, which are buckled on the periphery of the outer wall of the pipe body, and the positions of the buckled joints of the two water pipes correspond to each other; in the present technical solution, the cooling pipe is a split design for easy installation, and is designed to be S-shaped, which can increase the flow path of the cooling water, thereby increasing the relative cooling time of the cooling water, thereby taking away more heat and improving the cooling effect.

[0025] Preferably, the shell is a semi-cylindrical shell, and a plurality of heat dissipation holes are provided on the shell; in the present technical solution, the heat dissipation holes are rectangular grids, which play a role in heat dissipation, accelerate heat discharge and shorten the cooling period during the cooling process of the molecular sieve.

[0026] Preferably, the two ends of the tube body are sealed by flanges. In this technical solution, the ends of the tube body are sealed by flanges by bolts to improve air tightness.

[0027] A molecular sieve regeneration method, the molecular sieve regeneration method is implemented using the molecular sieve regeneration column as described above; the molecular sieve regeneration method comprises the following steps:

[0028] Fill the molecular sieve and the heat-conducting balls into the heat-conducting frame, test the air tightness of the molecular sieve regeneration column, and proceed to step S1 after the air tightness reaches a preset standard;

[0029] S1, start the heating tube, heat the temperature inside the tube body to a first preset temperature and maintain it at the first preset temperature, and pass hydrogen into the tube body while heating the tube body, the hydrogen enters the tube body from the hydrogen inlet, flows through the molecular sieve on the heat-conducting frame, and then flows out from the hydrogen outlet; in this technical solution, preferably, the hydrogen source is provided from a PEM water electrolysis hydrogen generator, that is, the hydrogen inlet of the molecular sieve regeneration column is connected to the hydrogen generator;

[0030] S2. When it is detected that the temperature of the hydrogen flowing out of the hydrogen outlet reaches a second preset temperature, the heating tube is turned off, the hydrogen continues to be introduced into the tube body, and cooling water is connected to the cooling tube;

[0031] S3. When it is detected that the temperature of the molecular sieve drops to a third preset temperature, the introduction of the hydrogen into the tube body is stopped, and the introduction of the cooling water is stopped and the cooling water in the cooling tube is drained.

[0032] The particle size of the molecular sieve is 1.6mm-5mm, preferably 2mm; the particle size of the heat conductive ball is 1mm-3mm, preferably 1.5mm;

[0033] The volume ratio of the molecular sieve to the heat conductive ball is 10:3-10:1, preferably 10:2;

[0034] The first preset temperature is 250°C-400°C, preferably 350°C;

[0035] The second preset temperature is 150°C-200°C, preferably 180°C;

[0036] The third preset temperature is 20°C-40°C, preferably 20°C.

[0037] On the basis of being in accordance with the common sense in the art, the above-mentioned preferred conditions can be arbitrarily combined to obtain the preferred embodiments of the present invention.

[0038] The reagents and raw materials used in the present invention are commercially available.

[0039] The positive and progressive effect of the present invention is that the present invention provides a molecular sieve regeneration column, which has a columnar structure, a heating tube is arranged outside the furnace tube of the molecular sieve regeneration column, and a heat-conducting frame is arranged inside the furnace tube. The heat-conducting frame can quickly transfer the heat of the external heating tube to the furnace tube, accelerate the conduction of heat to the core of the furnace tube, and reduce the radial temperature gradient, thereby overcoming the disadvantage of poor thermal conductivity of the molecular sieve, thereby improving the regeneration effect and shortening the regeneration cycle. Since the heating tube and the furnace tube are integrated together, the occupied space is reduced, which is conducive to system integration; at the same time, hydrogen is introduced as regeneration gas through the hydrogen inlet to purge the molecular sieve, so as to replace the demand for nitrogen in the traditional method, so that the molecular sieve regeneration column has stronger environmental adaptability. BRIEF DESCRIPTION OF THE DRAWINGS

[0040] Figure 1 This is an exploded view of the molecular sieve regeneration column of Example 1 of the present invention.

[0041] Figure 2 Schematic diagram of the furnace tube of Example 1 of the present invention.

[0042] Figure 3 Schematic diagram of a heat conducting frame according to Embodiment 1 of the present invention.

[0043] Figure 4 This is a schematic diagram of the shell of Example 1 of the present invention.

[0044] Figure 5 This is a schematic diagram of the interior of the thermal insulation layer of Example 1 of the present invention.

[0045] Figure 6 This is a schematic diagram of a cooling tube according to Example 1 of the present invention.

[0046] Figure 7 This is a cross-sectional view of the molecular sieve regeneration column of Example 1 of the present invention.

[0047] Figure 8 This is an overall view of the molecular sieve regeneration column of Example 1 of the present invention.

[0048] Description of reference numerals:

[0049] Furnace tube 1, flange 11, screw 12, nut 13, hydrogen inlet 14, furnace tube cavity 15;

[0050] Shell 2, heat dissipation holes 21;

[0051] Heating tube 3;

[0052] Heat conducting frame 4, heat conducting net 41, axial connecting rod 42, axial conduit 43;

[0053] Insulation layer 5;

[0054] Cooling pipe 6, water inlet 61, water outlet 62. DETAILED DESCRIPTION

[0055] The present invention is further described below by way of examples, but the present invention is not limited to the scope of the examples. The experimental methods in the following examples without specifying specific conditions are carried out according to conventional methods and conditions, or selected according to the product specifications.

[0056] Example 1

[0057] This embodiment provides a molecular sieve regeneration column, such as Figure 1-4As shown, the molecular sieve regeneration column includes a furnace tube 1, a shell 2, a heating tube 3, and a heat-conducting frame 4, wherein the furnace tube 1 includes a hollow space formed by a tube body, a hydrogen inlet 14 is provided at the upper end of the tube body, and a hydrogen outlet is provided at the lower end of the tube body (not shown in the figure, the hydrogen inlet 14 is a through hole on the flange 11 at the end of the tube body). The shell 2 is coaxially arranged on the periphery of the outer wall of the tube body. The heating tube 3 is attached to the outer periphery of the tube body and is placed in the interlayer space between the shell 2 and the outer wall of the tube body for heating the tube body. The heat-conducting frame 4 is arranged in the hollow space of the tube body, and the heat-conducting frame 4 is used to fill the molecular sieve. The heat-conducting frame 4 includes an axial connecting rod 42 and at least two layers of heat-conducting nets 41, and the axial connecting rod 42 vertically passes through the center of the heat-conducting net 41 and is fixedly connected to the heat-conducting net 41. The heat-conducting net 41 has a hollow channel up and down, and the diameter of the heat-conducting net 41 does not exceed the inner diameter of the tube body.

[0058] In this embodiment, the heat-conducting net 41 has a total of 7 layers. The heating tube 3 of the molecular sieve regeneration column is arranged on the outside of the furnace tube 1 for external heating. A heat-conducting frame 4 is arranged inside the tube body of the furnace tube 1 to cooperate with the heating tube 3. The heat-conducting frame 4 can quickly transfer the heat of the external heating tube 3 to the furnace tube 1, accelerate the conduction of heat to the core of the furnace tube 1, and reduce the radial temperature gradient, thereby overcoming the disadvantage of poor thermal conductivity of the molecular sieve, thereby improving the regeneration effect and shortening the regeneration cycle.

[0059] The heat-conducting frame 4 is also provided with three axial conduits 43, which vertically pass through the 41 channels of the heat-conducting network and are fixedly connected to the heat-conducting network 41. The axial conduits 43 are used to place thermocouples, which are used to detect the temperature of the molecular sieve. Among them, the lengths of the axial conduits 43 are different from each other; in this embodiment, the lengths of the three axial conduits 43 are equidistantly distributed, and the temperatures of the molecular sieves in the upper, middle and lower areas of the furnace tube 1 can be detected in the furnace tube 1 respectively for heating monitoring. In other embodiments, different numbers of axial conduits 43 can be set as needed. The volume of the heat-conducting frame 4 accounts for less than 10% of the furnace tube cavity 15.

[0060] In this embodiment, the pores of the heat-conducting net 41 are quadrilateral and can allow at least part of the molecular sieve to pass through. In other embodiments, the pores of the heat-conducting net 41 can be circular, triangular, or fan-shaped.

[0061] The heat conducting net 41, the axial conduit 43 and the axial connecting rod 42 are all made of stainless steel. In this embodiment, the structure made of stainless steel is conducive to heat transfer. In other embodiments, other materials that are conducive to heat conduction can also be used to make the structure.

[0062] like Figure 5 As shown, the molecular sieve regeneration column also includes an insulation layer 5, which is coaxially arranged on the periphery of the outer wall of the tube body and is placed in the interlayer space between the shell 2 and the outer wall of the tube body; the heating tube 3 is integrated into the inner wall of the insulation layer 5.

[0063] In this embodiment, the molecular sieve regeneration column is provided with an insulation layer 5 for heat preservation to prevent heat loss of the heating tube 3, thereby improving the heating efficiency; at the same time, the heating tube 3 is integrated into the inner wall of the insulation layer 5, which is an integrated design and can increase the integration of the molecular sieve regeneration column.

[0064] The heating tubes 3 are equidistantly arranged along the circumference of the inner wall of the insulation layer 5. In this embodiment, the heating tubes 3 are equidistantly arranged to improve the uniformity of heating, ensure that the molecular sieves at different positions can be heated synchronously, improve the heating efficiency, and shorten the regeneration time.

[0065] The length of the heating tube 3 is the same as the height of the insulation layer 5; in this embodiment, such an arrangement can maximize the use of the space on the inner wall of the insulation layer 5, save space, improve the utilization rate per unit area, and is beneficial to the integrity of the molecular sieve regeneration column.

[0066] The inner wall of the insulation layer 5 is also provided with a thermocouple, which is used to detect the temperature of the tube body. During the molecular sieve regeneration process, the thermocouple on the inner wall of the insulation layer 5 can monitor the heating temperature in real time. Further, the molecular sieve regeneration column can perform corresponding operations according to whether the temperature is too high or too low, such as increasing the heating power, or stopping heating when the temperature is over-temperature;

[0067] The insulation layer 5 is formed by two semi-cylindrical structures buckled on the outer periphery of the outer wall of the tube body, and the buckled seams of the insulation layer 5 correspond to each other. In this embodiment, the insulation layer 5 is a split design, which is easy to assemble and maintain.

[0068] like Figure 6-7 As shown, the molecular sieve regeneration column also includes a cooling tube 6, which is coaxially arranged on the periphery of the outer wall of the tube body, and the cooling tube 6 is placed between the heating tube 3 and the outer wall of the tube body. In this embodiment, water cooling of the cooling tube 6 is used to force cooling to shorten the cooling time and regeneration cycle.

[0069] A water inlet 61 is provided at one end of the cooling pipe 6, and a water outlet 62 is provided at the other end of the cooling pipe. The cooling medium is water.

[0070] The cooling pipe 6 is formed by two water pipes which are distributed in an S shape along the axial direction of the pipe body and have a semicircular structure along the circumference of the pipe body and are buckled on the outer periphery of the outer wall of the pipe body, and the buckled joints of the two water pipes correspond to each other;

[0071] In this embodiment, the cooling pipe 6 is a split design for easy installation and maintenance, and is designed in an S shape, which can improve the flow path of the cooling water, thereby increasing the relative cooling time of the cooling water, thereby taking away more heat and improving the cooling effect.

[0072] like Figure 8The shell 2 is a semi-cylindrical shell, and a plurality of rectangular heat dissipation holes 21 are provided on the shell 2. In the embodiment, the heat dissipation holes 21 are rectangular grids, which play a role in heat dissipation, accelerate heat dissipation during the cooling process of the molecular sieve, and shorten the cooling period. In other embodiments, the heat dissipation holes 21 are other shapes, such as circular.

[0073] The two ends of the tube body are sealed by flanges 11. In this embodiment, the ends of the tube body are sealed by screws 12 and nuts 14 to improve air tightness. The sealing material between the flanges 11 is one of graphite and tetrafluoroethylene. The furnace tube 1 and the flange 11 are made of 316L stainless steel.

[0074] This embodiment also provides a molecular sieve regeneration method, which is implemented using the molecular sieve regeneration column as described above; the molecular sieve regeneration method comprises the following steps:

[0075] Molecular sieves and thermal conductive balls are filled into the furnace tube cavity 15, and then the air tightness of the molecular sieve regeneration column is tested. After the air tightness reaches the preset standard, step S1 is performed; wherein the molecular sieve is one of 5A, 13X, and PSA-H2, and the thermal conductive balls are stainless steel balls; the dispersed thermal conductive balls can form a discontinuous thermal conductive network to promote heat conduction.

[0076] S1. Start the heating tube, and heat the temperature inside the tube to 350°C in 30 minutes and keep it at 350°C for 3 hours. While heating the tube, introduce hydrogen into the tube. The hydrogen enters the tube from the hydrogen inlet 14, flows through the molecular sieve on the heat-conducting frame 4, and then flows out from the hydrogen outlet. In this embodiment, the hydrogen source is provided by the PEM water electrolysis hydrogen generator, that is, the hydrogen inlet 14 of the molecular sieve regeneration column is connected to the hydrogen generator; during the heating process, the molecular sieve is quickly heated to 350°C under the support of the heat-conducting ball and the heat-conducting frame 4.

[0077] S2. When it is detected that the temperature of the hydrogen flowing out of the hydrogen outlet reaches 180°C, the heating tube is turned off, and hydrogen continues to be introduced into the tube body, and cooling water is connected to the cooling tube.

[0078] S3, when it is detected that the temperature of the molecular sieve drops to 20°C, stop introducing hydrogen into the tube body, stop introducing cooling water and drain the cooling water in the cooling tube. In this step, it takes 1 hour for the molecular sieve to drop from 350°C to 20°C, that is, when the molecular sieve drops to 20°C, the molecular sieve regeneration is complete.

[0079] In this embodiment, the molecular sieve uses aluminosilicate 5A molecular sieve with a particle size of 3mm-5mm, and the thermal conductive balls use 304 stainless steel balls with a particle size of 1mm and 2mm; the volume ratio of the molecular sieve to the thermal conductive ball is V 5A :V SUS3041mm :V SUS3042mm =20:2:1.

[0080] The traditional molecular sieve regeneration process, such as the molecular sieve regeneration time set in SY / T0076-2008 (Natural Gas Dehydration Design Specifications), is:

[0081] Heating time: 4.5h;

[0082] Cooling time: 3h;

[0083] Standby and switching time: 0.5h;

[0084] The total time is 8h.

[0085] By using the molecular sieve regeneration column provided in this embodiment in combination with the above method, the heating time and the cooling time are greatly shortened, and there is no need to switch equipment. The total time consumed for molecular sieve regeneration is only 4.5 hours, and the molecular sieve regeneration time is greatly shortened.

[0086] Example 2

[0087] This embodiment provides a molecular sieve regeneration method. The steps of the molecular sieve regeneration method of this embodiment are mostly the same as those of Example 1, except that:

[0088] The first preset temperature of this embodiment is 350°C, the second preset temperature is 180°C, and the third preset temperature is 30°C. The time for heating to 350°C is 0.5h, the time for heat preservation is 4h, the time for cooling from 350°C to 30°C is 1.5h, and the total regeneration period is 6h.

[0089] The molecular sieve of this embodiment uses aluminosilicate 5A molecular sieve with a particle size of 2 mm, and the thermal conductive balls use 304 stainless steel balls with a particle size of 1.5 mm; the volume ratio of the molecular sieve to the thermal conductive balls is 10:1.

[0090] Example 3

[0091] This embodiment provides a molecular sieve regeneration method. The steps of the molecular sieve regeneration method of this embodiment are mostly the same as those of Example 1, except that:

[0092] The first preset temperature of this embodiment is 300°C; the second preset temperature is 150°C; the third preset temperature is 20°C, wherein the time for heating to 300°C is 0.5h, the insulation time is 3h, the time for cooling from 300°C to 20°C is 1.5h, and the total regeneration cycle is 5h.

[0093] The molecular sieve of this embodiment uses aluminosilicate 5A molecular sieve with a particle size of 3 mm, and the thermal conductive balls use 304 stainless steel balls with a particle size of 2 mm; the volume ratio of the molecular sieve to the thermal conductive balls is 10:2.

[0094] Example 4

[0095] This embodiment provides a molecular sieve regeneration method. The steps of the molecular sieve regeneration method of this embodiment are mostly the same as those of Example 1, except that:

[0096] In this embodiment, the first preset temperature is 300°C, the second preset temperature is 150°C, and the third preset temperature is 20°C. The time for heating to 300°C is 0.5h, the time for keeping warm is 4h, the time for cooling from 300°C to 20°C is 0.5h, and the total regeneration period is 5h.

[0097] The molecular sieve of this embodiment uses aluminosilicate 5A molecular sieve with a particle size of 1.6 mm, and the thermal conductive balls use 304 stainless steel balls with a particle size of 1 mm; the volume ratio of the molecular sieve to the thermal conductive balls is 10:3.

[0098] Example 5

[0099] This embodiment provides a molecular sieve regeneration method. The steps of the molecular sieve regeneration method of this embodiment are mostly the same as those of Example 1, except that:

[0100] The first preset temperature of this embodiment is 380°C, the second preset temperature is 200°C, and the third preset temperature is 35°C. The time for heating to 380°C is 1 hour, the time for keeping warm is 3 hours, the time for cooling from 380°C to 35°C is 1.5 hours, and the total regeneration period is 5.5 hours.

[0101] The molecular sieve of this embodiment uses aluminosilicate 5A molecular sieve with a particle size of 5 mm, and the thermal conductive balls use 304 stainless steel balls with a particle size of 2 mm; the volume ratio of the molecular sieve to the thermal conductive balls is 10:1.

[0102] Although the specific embodiments of the present invention are described above, it should be understood by those skilled in the art that this is only for illustration and the protection scope of the present invention is defined by the appended claims. Those skilled in the art may make various changes or modifications to these embodiments without departing from the principles and essence of the present invention, but these changes and modifications all fall within the protection scope of the present invention.

Claims

1. A molecular sieve regeneration column, characterized in that: The molecular sieve regeneration column comprises: A furnace tube, the furnace tube comprising a hollow space enclosed by a tube body, an upper end of the tube body being provided with a hydrogen inlet, and a lower end of the tube body being provided with a hydrogen outlet; A shell, the shell being coaxially arranged on the periphery of the outer side wall of the tube body; A heating tube, which is attached to the outer periphery of the tube body and placed in the interlayer space between the shell and the outer side wall of the tube body, and is used to heat the tube body; A heat-conducting frame is arranged in the hollow space of the furnace tube, and is used to fill the molecular sieve. The heat-conducting frame includes an axial connecting rod and at least two layers of heat-conducting meshes. The axial connecting rod vertically passes through the center of the heat-conducting mesh and is fixedly connected to the heat-conducting mesh. The heat-conducting mesh has upper and lower hollow channels, and the diameter of the heat-conducting mesh does not exceed the inner diameter of the tube body.

2. The molecular sieve regeneration column according to claim 1, characterized in that: The heat-conducting frame is also provided with a plurality of axial conduits, which vertically pass through the holes of the heat-conducting net and are fixedly connected to the heat-conducting net. The axial conduits are used to place thermocouples, which are used to detect the temperature of the molecular sieve.

3. The molecular sieve regeneration column according to claim 2, characterized in that: The lengths of the axial conduits are different from each other; And / or, the channels of the heat-conducting network are one of circular, triangular, fan-shaped, and quadrilateral; And / or, the heat conducting network, the axial conduit and the axial connecting rod are all made of stainless steel.

4. The molecular sieve regeneration column according to claim 1, characterized in that: The molecular sieve regeneration column further comprises a heat-insulating layer, which is coaxially arranged on the periphery of the outer side wall of the tube body, and the heat-insulating layer is placed in the interlayer space between the shell and the outer side wall of the tube body; The heating pipe is integrated with the inner wall of the thermal insulation layer.

5. The molecular sieve regeneration column according to claim 4, characterized in that: The heating pipes are arranged equidistantly along the circumference of the inner side wall of the thermal insulation layer; And / or, the length of the heating tube is the same as the height of the insulation layer; And / or, a thermocouple is also attached to the inner wall of the thermal insulation layer, and the thermocouple is used to detect the temperature of the tube body; And / or, the thermal insulation layer is formed by two semi-cylindrical structures buckled on the periphery of the outer side wall of the tube body, and the buckled seams of the thermal insulation layer correspond to each other.

6. The molecular sieve regeneration column according to claim 4, characterized in that: The molecular sieve regeneration column further comprises a cooling tube, which is coaxially arranged at the periphery of the outer side wall of the tube body and is placed between the heating tube and the outer side wall of the tube body.

7. The molecular sieve regeneration column according to claim 6, characterized in that: One end of the cooling pipe is provided with a water inlet, and the other end of the cooling pipe is provided with a water outlet. And / or, the cooling pipe is formed by two water pipes distributed in an S-shape along the axial direction of the pipe body and in a semicircular structure along the circumference of the pipe body, which are buckled on the periphery of the outer wall of the pipe body, and the buckled joints of the two water pipes correspond to each other; And / or, the housing is provided with a plurality of heat dissipation holes; And / or, two ends of the tube body are sealed by flanges.

8. A molecular sieve regeneration method, characterized in that: The molecular sieve regeneration method is implemented using the molecular sieve regeneration column according to any one of claims 1 to 7; the molecular sieve regeneration method comprises the following steps: S1, starting the heating tube, heating the temperature inside the tube body to a first preset temperature and maintaining it at the first preset temperature, while heating the tube body, passing hydrogen into the tube body, the hydrogen entering the tube body from the hydrogen inlet, flowing through the molecular sieve on the heat conducting frame, and then flowing out from the hydrogen outlet; S2. When it is detected that the temperature of the hydrogen flowing out of the hydrogen outlet reaches a second preset temperature, the heating tube is turned off, and the hydrogen continues to be introduced into the tube body; S3. When it is detected that the temperature of the molecular sieve drops to a third preset temperature, stop introducing the hydrogen into the tube body.

9. The molecular sieve regeneration method according to claim 8, characterized in that: Before step S1, the method further includes: filling the molecular sieve and the heat-conducting balls into the heat-conducting frame, testing the air tightness of the molecular sieve regeneration column, and performing step S1 after the air tightness reaches a preset standard; And / or, step S2 further includes: connecting cooling water to a cooling pipe when it is detected that the temperature of the hydrogen flowing out of the hydrogen outlet reaches a second preset temperature; And / or, step S3 further includes: when it is detected that the temperature of the molecular sieve drops to a third preset temperature, stopping the introduction of the cooling water and draining the cooling water in the cooling pipe.

10. The molecular sieve regeneration method according to claim 9, characterized in that: The particle size of the molecular sieve is 1.6mm-5mm, preferably 2mm; the particle size of the thermal conductive ball is 1mm-3mm, preferably 1.5mm; And / or, the volume ratio of the molecular sieve to the thermally conductive balls is 10:3-10:1, preferably 10:2; And / or, the first preset temperature is 250°C-400°C, preferably 350°C; And / or, the second preset temperature is 150°C-200°C, preferably 180°C; And / or, the third preset temperature is 20°C-40°C, preferably 20°C.

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