Purification system for separating feed gas in 13C stable isotope by low-temperature rectification method

Abstract

The invention discloses a purification system for separating feed gas in 13C stable isotope by a low-temperature rectification method, and belongs to the technical field of low-temperature rectification, the purification system comprises a feed gas tank, a normal-temperature adsorption device, a low-temperature adsorption device and a refrigerant supply device, a motor is mounted at the top end of the normal-temperature adsorption tank, and a support frame is mounted in the normal-temperature adsorption tank; the rotating shaft rotates between the top wall of the normal-temperature adsorption tank and the supporting frame and is connected with the motor, the spiral blade is installed on the lower portion of the rotating shaft, the top end of the normal-temperature adsorption tank is provided with a filler funnel, and the bottom end of the normal-temperature adsorption tank is provided with a discharging port. And the refrigerant supply device is communicated with the top end of the low-temperature adsorption device. New adsorption materials are added to the top end of the normal-temperature adsorption tank, the spiral blades convey the waste adsorption materials to the bottom end of the normal-temperature adsorption tank through rotation of the rotating shaft, uninterrupted updating of the adsorption materials is achieved, and the purification effect of feed gas is guaranteed.

Description

Technical Field

[0001] The present invention belongs to the technical field of cryogenic distillation, and in particular relates to a cryogenic distillation separation method. 13 Purification system for raw gas containing C stable isotopes. Background Art

[0002] 13 C is one of the main isomorphs of carbon. 13 C is mainly used in the fields of medical testing and scientific research. 13 C is used to detect the presence of Helicobacter pylori in the stomach by taking a 13 C urea capsule, and then blow air to detect the ratio of carbon 13 to carbon 12 in the breath sample (δ value), which can determine whether it is infected with Helicobacter pylori; in the field of scientific research, 13 C is used as an isotope marker to study the metabolic pathways and regulatory mechanisms of organisms, or to synthesize 13 C-labeled biomacromolecules.

[0003] 13 The production methods of C include gas diffusion, thermal diffusion, chemical exchange, laser and cryogenic distillation, and cryogenic distillation is the main method of industrial production. 13 C raw gas, and the main impurities in industrial CO raw gas are O2, H2O, CO2 and Ar. In the prior art, there are processes such as room temperature adsorption and low temperature adsorption for the purification of CO raw gas. Whether in the room temperature adsorption or low temperature adsorption process, the adsorption performance of the adsorption material decreases after long-term use, and the adsorption material needs to be replaced or desorbed, otherwise it will affect the purification effect of the CO raw gas. Summary of the invention

[0004] In view of this, the present invention provides a cryogenic distillation separation method 13 The purification system of raw gas containing C stable isotopes is used to solve the above problems.

[0005] In order to achieve the above object, the present invention adopts the following technical solution:

[0006] A cryogenic distillation method for separation 13A purification system for raw gas in C stable isotopes, comprising: a raw gas tank, a normal temperature adsorption device, a low temperature adsorption device and a refrigerant providing device, wherein the normal temperature adsorption device comprises a normal temperature adsorption tank, a motor, a rotating shaft, a support frame and a spiral blade, wherein the motor is mounted at the top of the normal temperature adsorption tank, the support frame is mounted at the inner bottom end of the normal temperature adsorption tank, the rotating shaft is rotatably connected between the top wall of the normal temperature adsorption tank and the support frame, the top end of the rotating shaft is fixedly connected to the output end of the motor, the spiral blade is mounted at the bottom of the rotating shaft, a filling funnel is provided at the top of the normal temperature adsorption tank, a discharge port is provided at the bottom end of the normal temperature adsorption tank, the raw gas tank is communicated with the lower part of the normal temperature adsorption tank through a pipeline, the low temperature adsorption device is communicated with the upper part of the normal temperature adsorption tank through a pipeline, the low temperature adsorption device is communicated with a low temperature distillation device, and the refrigerant providing device is communicated with the top of the low temperature adsorption device.

[0007] Furthermore, the room temperature adsorption device also includes a stirring rod, and a plurality of stirring rods are distributed in the middle and upper parts of the rotating shaft.

[0008] Furthermore, the filling funnel and the discharge port are both provided with sealing covers, and the sealing covers are used to prevent air impurities from entering the normal temperature adsorption tank.

[0009] Furthermore, a flow meter is provided on the connecting pipeline between the raw gas tank and the normal temperature adsorption tank.

[0010] Furthermore, the low-temperature adsorption device includes a low-temperature adsorption tank, fins, capillary tubes, a capillary tube air inlet branching device, a capillary tube air outlet branching device and an air outlet pipe, the fins are installed in the low-temperature adsorption tank, and multiple capillary tubes are distributed on the fins. The refrigerant providing device passes through the top of the low-temperature adsorption tank and is connected with the capillary tube air inlet branching device. The tops of multiple capillary tubes are connected with the capillary tube air inlet branching device, and the bottoms are connected with the capillary tube air outlet branching device. The capillary tube air outlet branching device is connected with the air outlet pipe, and the air outlet pipe passes through the bottom end of the low-temperature adsorption tank, and the normal temperature adsorption tank is connected with the bottom end of the low-temperature adsorption tank.

[0011] Furthermore, the plurality of fins are arranged circumferentially, and the capillary tubes are arranged on one side of the fins.

[0012] Furthermore, the low-temperature adsorption device is provided in plurality, and the tops of the plurality of low-temperature adsorption devices are all connected to the refrigerant providing device, and the bottoms are all connected to the upper part of the normal temperature adsorption tank.

[0013] The beneficial effects of the present invention are:

[0014] The present invention adds new adsorption material to the top of the normal temperature adsorption tank, and the motor drives the rotating shaft to rotate, so that the spiral blades at the bottom of the rotating shaft continuously move the adsorption material downward, so that the adsorption material is continuously updated, thereby ensuring the purification effect of the raw gas; when the adsorption material is not added or discharged, the motor drives the rotating shaft to rotate, and the rotating shaft drives the stirring rod to rotate, so that the adsorption material is continuously rolled, thereby increasing the contact opportunity with the impurity gas in the CO raw gas, and preventing the contact position between the adsorption materials from failing to adsorb the impurities in the raw gas; the filling funnel and the discharge hole at the top of the normal temperature adsorption tank are provided with a sealing cover, so as to prevent the external gas from mixing when the adsorption material is not updated. into the raw gas; the refrigerant supply device disperses the refrigerant into multiple thin tubes through the thin tube air inlet distribution device, and the thin tubes are distributed on the fins, which increases the refrigeration effect of the fins and prevents the fins from having a temperature at the position contacting the refrigerant that is different from the temperature at the far end due to heat conduction; the fins are distributed circumferentially and thin tubes are arranged on one side, which increases the contact area between the fins and the adsorption material and improves the effect of low-temperature adsorption of impurities in the raw gas; multiple low-temperature adsorption devices are set, and during the production process, the adsorption material in one of the low-temperature adsorption tanks is replaced, and the other low-temperature adsorption devices continue the low-temperature adsorption work, thereby achieving the effect of replacing the adsorption material without affecting the production. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on the provided drawings without paying creative work.

[0016] Figure 1 It is a cryogenic distillation separation 13 Schematic diagram of the purification system of raw gas containing C stable isotopes;

[0017] Figure 2 yes Figure 1 Sectional view of AA in the middle;

[0018] Among them, in the figure:

[0019] 10-raw gas tank, 21-normal temperature adsorption tank, 211-filling funnel, 212-discharge port, 213-sealing cover, 22-motor, 23-rotating shaft, 24-support frame, 25-stirring rod, 26-spiral blade, 30-low temperature adsorption device, 31-low temperature adsorption tank, 32-fin, 33-thin tube, 34-thin tube air inlet branch pipe device, 35-thin tube air outlet branch pipe device, 36-outlet pipe, 40-refrigerant supply device, 50-flow meter. DETAILED DESCRIPTION

[0020] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only 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 are within the scope of protection of the present invention.

[0021] Example 1

[0022] Refer to the attached Figure 1-2 As shown, the present invention provides a cryogenic distillation separation method 13 The purification system of raw gas in C stable isotope comprises: raw gas tank 10, room temperature adsorption device, low temperature adsorption device 30 and refrigerant providing device 40, the raw gas tank 10 is used to contain CO raw gas, the room temperature adsorption device comprises room temperature adsorption tank 21, motor 22, rotating shaft 23, supporting frame 24 and spiral blade 26, the room temperature adsorption tank 21 is filled with adsorption material, the adsorption material can be common coconut shell activated carbon, the motor 22 is installed at the top of the room temperature adsorption tank 21, the supporting frame 24 is installed at the inner bottom of the room temperature adsorption tank 21, the rotating shaft 23 is between the top wall of the room temperature adsorption tank 21 and the supporting frame 24 Rotationally connected, the top of the rotating shaft 23 is fixedly connected to the output end of the motor 22, the spiral blade 26 is installed at the lower part of the rotating shaft 23, the top of the normal temperature adsorption tank 21 is provided with a filling funnel 211, the bottom of the normal temperature adsorption tank 21 is provided with a discharge port 212, the raw gas tank 10 is connected with the lower part of the normal temperature adsorption tank 21 through a pipeline, the low-temperature adsorption device 30 is connected with the upper part of the normal temperature adsorption tank 21 through a pipeline, the low-temperature adsorption device 30 is connected with the low-temperature distillation equipment, the refrigerant providing device 40 is connected with the top of the low-temperature adsorption device 30, and the refrigerant providing device 40 can be a liquid nitrogen tank or a liquid nitrogen production equipment. When the adsorption material in the normal temperature adsorption tank 21 needs to be replaced, the filling funnel 211 at the top is opened, new adsorption material is added to the normal temperature adsorption tank 21, the motor 22 switch and the discharge port 212 at the bottom are turned on, the motor 22 drives the rotating shaft 23 to rotate, and the rotating shaft 23 drives the spiral blade 26 at the bottom to continuously move the adsorption material downward, and the old adsorption material is discharged through the discharge port 212, so that the adsorption material is continuously updated, ensuring the purification effect of the raw gas. After passing through the normal temperature adsorption tank 21 and the low temperature adsorption device 30, the CO raw gas enters the low temperature distillation equipment.

[0023] The room temperature adsorption device also includes a stirring rod 25, and a plurality of stirring rods 25 are distributed in the middle and upper parts of the rotating shaft 23; when the adsorption material is not added or discharged, the motor 22 drives the rotating shaft 23 to rotate, and the rotation drives the stirring rod 25 to rotate, so that the adsorption material continuously rolls, increasing the contact opportunity with the impurity gas in the CO raw gas, and preventing the adsorption material from being unable to adsorb impurities in the raw gas due to the contact position.

[0024] The packing hopper 211 and the discharge port 212 are both provided with sealing covers 213. When the adsorption material in the normal temperature adsorption tank 21 is not replaced, the sealing cover 213 seals the packing hopper 211 and the discharge port 212 to prevent air impurities from entering the normal temperature adsorption tank 21. When the adsorption material is replaced, a small amount of gas in the raw gas tank 10 enters the normal temperature adsorption tank 21 to prevent air impurities from entering the normal temperature adsorption tank 21 when the sealing covers 213 of the packing hopper 211 and the discharge port 212 are opened.

[0025] A flow meter 50 is provided on the connecting pipeline between the raw gas tank 10 and the normal temperature adsorption tank 21 for counting the flow rate of the CO raw gas entering the normal temperature adsorption tank 21 .

[0026] The low-temperature adsorption device 30 includes a low-temperature adsorption tank 31, fins 32, capillary tubes 33, capillary tube air inlet branch pipes 34, capillary tube air outlet branch pipes 35 and an air outlet pipe 36. The fins 32 are installed in the low-temperature adsorption tank 31. At the same time, the low-temperature adsorption material is filled in the low-temperature adsorption tank 31. The refrigerant providing device 40 provides refrigerant for the low-temperature adsorption device 30. The low-temperature adsorption material, combined with the low-temperature environment provided by the refrigerant, adsorbs Ar in the CO raw gas. A plurality of capillary tubes 33 are distributed on the fins 32, the refrigerant providing device 40 passes through the top end of the low-temperature adsorption tank 31 and is connected with the capillary tube air inlet branching device 34, the top ends of the plurality of capillary tubes 33 are connected with the capillary tube air inlet branching device 34, the bottom ends are connected with the capillary tube air outlet branching device 35, and the capillary tube air outlet branching device 35 is connected with the air outlet pipe 36; the function of the capillary tube air inlet branching device 34 is to connect the pipeline of the refrigerant providing device 40 entering the low-temperature adsorption tank 31 with the plurality of capillary tubes 33, the function of the capillary tube air outlet branching device 35 is to gather the outlets of the plurality of capillary tubes 33 and connect them with the air outlet pipe 36; the air outlet pipe 36 passes through the bottom end of the low-temperature adsorption tank 31, and the normal temperature adsorption tank 21 is connected with the bottom end of the low-temperature adsorption tank 31. The refrigerant supply device 40 distributes the refrigerant into a plurality of thin tubes 33 through the thin tube air inlet distribution device 34. The thin tubes 33 are distributed on the fins 32, which increases the cooling effect of the fins 32 and prevents the fins 32 from having a different temperature at the position where the refrigerant contacts due to heat conduction than at the far end. Figure 2 The number of fins 32 is four, which can be set to multiple according to actual needs. The multiple fins 32 are distributed circumferentially and a thin tube 33 is arranged on one side, which increases the contact area between the fin 32 and the adsorption material and improves the effect of low-temperature adsorption of impurities in the raw gas.

[0027] There are multiple cryogenic adsorption devices 30, the tops of which are connected to the refrigerant supply device 40 through a multi-way valve, and the bottoms are connected to the upper part of the normal temperature adsorption tank 21 through a multi-way valve. During the production process, the cryogenic adsorption material in one of the cryogenic adsorption tanks 31 is replaced, and the other cryogenic adsorption devices 30 continue the cryogenic adsorption work, so that the replacement of the cryogenic adsorption material does not affect the production, and the production efficiency is improved.

[0028] In this specification, each embodiment is described in a progressive manner, and each embodiment focuses on the differences from other embodiments. The same or similar parts between the embodiments can be referred to each other. For the device disclosed in the embodiment, since it corresponds to the method disclosed in the embodiment, the description is relatively simple, and the relevant parts can be referred to the method part.

[0029] The above description of the disclosed embodiments enables one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to the embodiments shown herein, but rather to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A cryogenic distillation separation 13 The system for purifying raw gas containing C stable isotopes is characterized in that: include: A raw gas tank (10), a normal temperature adsorption device, a low temperature adsorption device (30) and a refrigerant supply device (40), wherein the normal temperature adsorption device comprises a normal temperature adsorption tank (21), a motor (22), a rotating shaft (23), a support frame (24) and a spiral blade (26), wherein the motor (22) is mounted on the top end of the normal temperature adsorption tank (21), the support frame (24) is mounted on the inner bottom end of the normal temperature adsorption tank (21), the rotating shaft (23) is rotatably connected between the top wall of the normal temperature adsorption tank (21) and the support frame (24), and the top end of the rotating shaft (23) is connected to the motor (22). The output end is fixedly connected, the spiral blade (26) is installed at the lower part of the rotating shaft (23), the top end of the normal temperature adsorption tank (21) is provided with a filling funnel (211), the bottom end of the normal temperature adsorption tank (21) is provided with a discharge port (212), the raw gas tank (10) is connected to the lower part of the normal temperature adsorption tank (21) through a pipeline, the low temperature adsorption device (30) is connected to the upper part of the normal temperature adsorption tank (21) through a pipeline, the low temperature adsorption device (30) is connected to the low temperature distillation equipment, and the refrigerant providing device (40) is connected to the top of the low temperature adsorption device (30).

2. A cryogenic distillation separation according to claim 1 13 The system for purifying raw gas containing C stable isotopes is characterized in that: The room temperature adsorption device further comprises a stirring rod (25), wherein a plurality of stirring rods (25) are distributed in the middle and upper parts of the rotating shaft (23).

3. A cryogenic distillation separation according to claim 1 13 The system for purifying raw gas containing C stable isotopes is characterized in that: The filling funnel (211) and the discharge port (212) are both provided with a sealing cover (213), and the sealing cover (213) is used to prevent air impurities from entering the normal temperature adsorption tank (21).

4. A cryogenic distillation separation according to claim 1 13 The system for purifying raw gas containing C stable isotopes is characterized in that: A flow meter (50) is provided on the communication pipeline between the raw gas tank (10) and the normal temperature adsorption tank (21).

5. A cryogenic distillation separation according to claim 1 13 The system for purifying raw gas containing C stable isotopes is characterized in that: The low-temperature adsorption device (30) comprises a low-temperature adsorption tank (31), fins (32), capillary tubes (33), a capillary tube air inlet branching device (34), a capillary tube air outlet branching device (35) and an air outlet pipe (36). The fins (32) are installed in the low-temperature adsorption tank (31), and a plurality of capillary tubes (33) are distributed on the fins (32). The refrigerant supply device (40) passes through the top end of the low-temperature adsorption tank (31) and is connected to the capillary tube air inlet branching device (34). The top ends of the plurality of capillary tubes (33) are connected to the capillary tube air inlet branching device (34), and the bottom ends are connected to the capillary tube air outlet branching device (35). The capillary tube air outlet branching device (35) is connected to the air outlet pipe (36). The air outlet pipe (36) passes through the bottom end of the low-temperature adsorption tank (31), and the normal temperature adsorption tank (21) is connected to the bottom end of the low-temperature adsorption tank (31).

6. A cryogenic distillation separation method according to claim 5 13 The system for purifying raw gas containing C stable isotopes is characterized in that: The plurality of fins (32) are arranged in a circumferential direction, and the capillary tubes (33) are arranged on one side of the fins (32).

7. A cryogenic distillation separation method according to claim 5 13 The system for purifying raw gas containing C stable isotopes is characterized in that: The low-temperature adsorption device (30) is provided in plurality, and the top ends of the plurality of low-temperature adsorption devices (30) are all connected to the refrigerant supply device (40), and the bottom ends are all connected to the upper end of the normal temperature adsorption tank (21).

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