Reactor for removing hydrogen isotope from helium-3 gas and use method thereof

Abstract

The reactor comprises a sealed reactor shell and a heating electric furnace, the sealed reactor shell is located in the heating electric furnace, a gas outlet pipe and a gas inlet pipe are installed at the top end and the bottom end of the heating electric furnace respectively, and the gas outlet pipe is welded to the top of the sealed reactor shell and led out from the top of the sealed reactor shell; the gas inlet pipe is welded to the bottom of the sealed reactor shell and is introduced from the bottom of the sealed reactor shell; and an air outlet sintering filter plate and an air inlet sintering filter plate are respectively arranged at the positions close to the top and the bottom in the sealed reactor shell. According to the utility model, the reactor has a relatively long gas circulation path while having a good heating effect, and the heating and cooling operations are simple and convenient.

Description

Technical Field

[0001] The invention relates to the field of gas production technology, and more particularly to a reactor for removing hydrogen isotopes from helium-3 gas. Background Art

[0002] Helium-3 gas can generally be used to make proportional counter tubes, nuclear magnetic resonance and other fields. Helium reserves are scarce and expensive. As a helium-poor country, my country mainly relies on imports for its annual helium consumption.

[0003] Due to the inert chemical properties of helium, a variety of impurity removal methods can be used, such as the getter method, uranium chip purification method, and activated carbon method for removing oxygen, nitrogen, and water vapor; and the uranium chip adsorption method, palladium tube purification method, activated carbon method, and catalytic oxidation method for removing hydrogen.

[0004] The above purification methods require a dedicated reactor. The structure of the reactor will affect the purification efficiency. For example, the uranium powder purification method can remove hydrogen from helium-3 gas. The reaction formula is 2U+3H2=2UH3. Using copper oxide to remove hydrogen is very economical. The reaction principle is that hydrogen reduces copper oxide at high temperature to generate water and pure copper: CuO+H2=H2O+Cu. The generated water is adsorbed by the molecular sieve to achieve the effect of removing hydrogen isotopes.

[0005] The CuO device used in the traditional helium-3 purification process is a straight-cylinder design with no internal flow-guiding structure. This design makes the gas flow path shorter, so that the gas cannot fully react with copper oxide, resulting in a low purification rate. Another design method uses a serpentine coil as the CuO column shell. Although this method makes the gas flow path longer, the manufacturing process is complicated. The spiral structure of the circular tube will also have many heating empty areas during heating, poor thermal uniformity, and will also generate a lot of waste heat. It is necessary to design a reactor filled with CuO filler and improve its structure so that it has a good heating effect and a longer gas flow path.

[0006] The heating reactor structure described in this patent can be applied to heating gas-solid reactions in different fields, and the reactor filled with CuO filler can be used to remove hydrogen isotopes from gases in other fields. Summary of the invention

[0007] The purpose of the present invention is to design a reactor for removing hydrogen isotope gas from helium in a gas production process and describe a method of use. The heating reactor described in this patent can be applied to heating gas-solid reactions in different fields. It also has the characteristics of simple operation.

[0008] The technical scheme of the present invention is as follows: a reactor for removing hydrogen isotopes from helium-3 gas, comprising a sealed reactor shell and a heating furnace, wherein the sealed reactor shell is located inside the heating furnace, and an outlet pipe and an inlet pipe are respectively installed at the top and bottom of the heating furnace, wherein the outlet pipe is welded to the top of the sealed reactor shell and is led out from the top of the sealed reactor shell; the inlet pipe is welded to the bottom of the sealed reactor shell and is introduced from the bottom of the sealed reactor shell; an outlet sintered filter plate and an inlet sintered filter plate are respectively installed near the top and the bottom of the sealed reactor shell;

[0009] A spiral guide plate is welded inside the sealed reactor shell, and CuO particle filler is loaded along the spiral guide plate;

[0010] An armored thermocouple is inserted and installed through the armored thermocouple installation hole on the side of the heating electric furnace, and the armored thermocouple contacts the side surface of the sealed reactor shell.

[0011] When the heating furnace is closed, it completely wraps around the sealed reactor shell, causing the sealed reactor shell to heat up.

[0012] The heating electric furnace has a split structure.

[0013] A method for using a reactor for removing hydrogen isotopes from helium-3 gas comprises the following steps:

[0014] S1: Loading the CuO particle filler into the sealed reactor shell along the spiral guide plate, and vibrating it to fill the sealed reactor shell;

[0015] S2: Connect the power supply to heat up the heating furnace, and the temperature is fed back through the armored thermocouple. The temperature of the entire reactor is raised to 400-500°C, and the outlet pipe is connected to the vacuum system for evacuation;

[0016] S3: Reactor leak detection: After stopping the thermal degassing of the reactor and evacuating it, connect it to the leak detection system for leak detection;

[0017] S4: oxygen regeneration: after the reactor passes the leak detection, the heating furnace is continuously heated to maintain the temperature at 400-500°C, the air inlet pipe is connected to the oxygen bottle, oxygen is filled into the reactor, and after the CuO particle filler reacts fully with the oxygen, the vacuum system is continued to be used for vacuuming;

[0018] S5: The heating electric furnace is heated and maintained at a temperature of 400-500°C, the gas to be purified is introduced through the air inlet pipe, and the purified gas is discharged through the air outlet pipe.

[0019] S8: After the reactor is heated, it is allowed to stand and cool down, or the heating furnace can be removed to quickly cool it down. In S1, the CuO particle filler is in a granular form with a particle size of 0.2mm-3mm.

[0020] In S1, gas circulation is ensured and filler is prevented from pulverizing.

[0021] In the S2, the vacuum is evacuated to a degree of vacuum less than 5 Pa.

[0022] In S3, the leakage rate is less than 1.0×10 10 Pa·m 3 / s means qualified.

[0023] In S5, a gas circulation pump is used to circulate and purify the gas; the flow rate is controlled to be 1 to 15 L / min.

[0024] It also includes S7: after the purification task is completed, the device is thermally exhausted, and the temperature of the filler in the sealed reactor shell is monitored by a thermocouple to make the temperature of the filler in the sealed reactor shell reach the set temperature. At the same time, a vacuum system is used to evacuate the air outlet until the vacuum degree is less than 5Pa.

[0025] The remarkable effects of the present invention are:

[0026] 1) The overall design of the reactor ensures that the reactor has a good heating effect while having a long gas flow path, and the heating and cooling operations are simple.

[0027] 2) The flow-guiding structure design achieves the increase of the gas diffusion path in a limited space without affecting the gas fluidity, so that the gas to be purified has more complete contact with the copper oxide filler, thereby improving the purification efficiency.

[0028] 3) After the reactor has been used many times and its reduction reaction capacity has decreased, it is heated and oxygen is continuously introduced to regenerate the copper oxide filler in the copper oxide reactor so that it can be recycled.

[0029] 4) The circulating pressure is controlled to be 1.3-2atm, and the gas to be purified at a flow rate of 1-10L / min passes through the high-temperature reactor. Helium containing 0.5% hydrogen isotope gas can be purified to a hydrogen isotope gas of ≤0.01% within 1 hour. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] Figure 1 Schematic diagram of a reactor for removing hydrogen isotopes from helium-3 gas.

[0031] In the figure: 1—air outlet pipe; 2—sintered filter plate at the air outlet; 3—spiral guide plate; 4—sealed reactor shell; 5—armored thermocouple mounting hole; 6—heating electric furnace; 7—sintered filter plate at the air inlet; 8—air inlet pipe; 9—CuO particle filler. DETAILED DESCRIPTION

[0032] Many specific details are described in the following description to facilitate a full understanding of the present application. However, the present application can be implemented in many other ways than those described herein, and those skilled in the art can make similar generalizations without violating the connotation of the present application, so the present application is not limited by the specific implementation disclosed below.

[0033] The terms used in one or more embodiments of the present application are only for the purpose of describing specific embodiments, and are not intended to limit one or more embodiments of the present application. The singular forms of "a", "said" and "the" used in one or more embodiments of the present application and the appended claims are also intended to include plural forms, unless the context clearly indicates other meanings. It should also be understood that the term "and / or" used in one or more embodiments of the present application refers to and includes any or all possible combinations of one or more associated listed items.

[0034] It should be understood that, although the terms first, second, etc. may be used to describe various information in one or more embodiments of the present application, such information should not be limited to these terms. These terms are only used to distinguish the same type of information from each other. For example, without departing from the scope of one or more embodiments of the present application, the first may also be referred to as the second, and similarly, the second may also be referred to as the first.

[0035] A reactor for removing hydrogen isotopes from helium-3 gas comprises an outlet pipe 1, an outlet sintered filter plate 2, a spiral guide plate 3, a sealed reactor shell 4, an armored thermocouple mounting hole 5, a heating electric furnace 6, an inlet sintered filter plate 7, an inlet pipe 8, and a CuO particle filler 9.

[0036] The sealed reactor shell 4 is located inside the heating furnace 6. When the heating furnace 6 is closed, it completely wraps the sealed reactor shell 4 to heat up the sealed reactor shell 4. The heating furnace 6 is a split structure. An air outlet pipe 1 and an air inlet pipe 8 are installed at the top and bottom of the heating furnace 6, respectively. The air outlet pipe 1 is welded to the top of the sealed reactor shell 4 and is led out from the top of the sealed reactor shell 4. The air inlet pipe 8 is welded to the bottom of the sealed reactor shell 4 and is introduced from the bottom of the sealed reactor shell 4. An air outlet sintered filter plate 2 and an air inlet sintered filter plate 7 are installed near the top and bottom of the sealed reactor shell 4, respectively. The intake air is filtered through the air inlet sintered filter plate 7, and the outlet air is filtered through the air outlet sintered filter plate 2. A spiral guide plate 3 is welded inside the sealed reactor shell 4, and CuO particle filler 9 is loaded along the spiral guide plate 3.

[0037] An armored thermocouple is inserted and installed through the armored thermocouple installation hole 5 on the side of the heating furnace 6, and the armored thermocouple contacts the side surface of the sealed reactor shell 4, so that the armored thermocouple measures the temperature of the outer wall of the sealed reactor shell 4;

[0038] A method for using a reactor for removing hydrogen isotopes from helium-3 gas comprises the following steps:

[0039] 1) The CuO particle filler 9 is loaded into the sealed reactor shell 4 along the spiral guide plate 3 and vibrated to fill the sealed reactor shell 4. However, the filler should be prevented from pulverizing during the process. The CuO particle filler 9 is in the form of particles with a particle size of 0.2mm-3mm. Particles of any shape can be used as long as the gas flow is ensured.

[0040] 2) Assemble the whole set of separate heating reactor, connect the power supply to heat the heater, and feed back the temperature signal to the control system through the armored thermocouple to achieve temperature control. The temperature is raised to 400-500°C. The outlet pipe 1 is connected to the vacuum system for evacuation. The purpose of this process is to exhaust the impurity gas adsorbed in the micropores of the CuO particle filler and evacuate it to a vacuum degree of <5Pa.

[0041] 3) Reactor leak detection: After stopping the thermal degassing of the reactor and evacuating the air, observe the vacuum gauge for 5 minutes. If the pressure rises to more than 10Pa, it means it is unqualified; connect to the leak detection system for leak detection, and the leakage rate is less than 1.0×10 10 Pa·m 3 / s.

[0042] 4) Perform oxygen regeneration: After the reactor passes the leak detection test, heat it to 400-500°C through the heating furnace 6, connect the air inlet pipe 8 to the oxygen cylinder, slowly open the oxygen cylinder pressure regulating valve, and slowly fill the reactor with oxygen until the pressure of the oxygen increases significantly, indicating that the CuO and oxygen in the reactor have reacted fully, and the oxidation regeneration is considered qualified. Close the charging valve, open the outlet valve, and continue to use the vacuum system to evacuate.

[0043] 5) The reactor is preheated before use, and the preheating temperature is 400-500°C. The purpose of preheating is to make the temperature of the filler in the sealed reactor shell 4 uniform. After the preheating is completed, the gas to be purified is introduced through the inlet pipe 8, the flow rate and the gas pressure in the reactor are controlled, and the purified gas is discharged from the outlet pipe 1.

[0044] 6) In order to achieve better purification effect, a gas circulation pump can be used to circulate the gas for purification. The flow rate is controlled to be 1 to 15 L / min.

[0045] 7) After the purification task is completed, the device is thermally exhausted. Even if the heater is heated up, the temperature of the filler in the sealed reactor shell 4 is monitored by a thermocouple and fed back to the control system in real time. The control system then feeds back to the heater to control the heating power so that the temperature of the filler in the sealed reactor shell 4 reaches the set temperature. While heating, the vacuum system is used to evacuate the air from the air outlet 1, generally evacuating to a vacuum degree of <5Pa.

[0046] 8) After the reactor is heated, it is allowed to stand to cool down, or the heating furnace 6 can be removed to cool it down quickly.

[0047] Application examples:

[0048] According to the above steps, the test was carried out on the purification test of helium-4 gas with a hydrogen content of 0.3%. The performance was compared using a traditional copper oxide column without a guide structure and a copper oxide column with a guide structure. The purification time was 1 hour. The results are shown in the following table. It can be seen that the copper oxide column with a guide structure has a better purification effect.

[0049] The above description is only a preferred embodiment of this patent and is not intended to limit this patent. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of this patent should be included in the scope of protection of this patent.

[0050] It should be noted that, for the above-mentioned method embodiments, for the sake of simplicity of description, they are all expressed as a series of action combinations, but those skilled in the art should be aware that the present application is not limited by the described action sequence, because according to the present application, certain steps can be performed in other sequences or simultaneously. Secondly, those skilled in the art should also be aware that the embodiments described in the specification are all preferred embodiments, and the actions and modules involved are not necessarily required by the present application.

[0051] In the above embodiments, the description of each embodiment has its own emphasis. For parts that are not described in detail in a certain embodiment, reference can be made to the relevant descriptions of other embodiments.

[0052] The preferred embodiments of the present application disclosed above are only used to help explain the present application. The optional embodiments do not describe all the details in detail, nor do they limit the invention to the specific implementation methods described. Obviously, many modifications and changes can be made according to the content of the present application. The present application selects and specifically describes these embodiments in order to better explain the principles and practical applications of the present application, so that those skilled in the art can understand and use the present application well.

Claims

1. A reactor for removing hydrogen isotopes from helium-3 gas, characterized in that: The invention comprises a sealed reactor shell (4) and a heating furnace (6), wherein the sealed reactor shell (4) is located inside the heating furnace (6), and an air outlet pipe (1) and an air inlet pipe (8) are respectively installed at the top and bottom of the heating furnace (6); the air outlet pipe (1) is welded to the top of the sealed reactor shell (4) and is led out from the top of the sealed reactor shell (4); the air inlet pipe (8) is welded to the bottom of the sealed reactor shell (4) and is led from the bottom of the sealed reactor shell (4); and an air outlet sintered filter plate (2) and an air inlet sintered filter plate (7) are respectively installed near the top and the bottom of the sealed reactor shell (4); A spiral guide plate (3) is welded inside the sealed reactor shell (4), and a CuO particle filler (9) is loaded along the spiral guide plate (3); An armored thermocouple is inserted and installed through the armored thermocouple installation hole (5) on the side of the heating electric furnace (6), and the armored thermocouple contacts the side surface of the sealed reactor shell (4).

2. A reactor for removing hydrogen isotopes from helium-3 gas according to claim 1, characterized in that: When the heating electric furnace (6) is closed, it completely wraps the sealed reactor shell (4) to increase the temperature of the sealed reactor shell (4).

3. A reactor for removing hydrogen isotopes from helium-3 gas according to claim 1, characterized in that: The heating electric furnace (6) is of split structure.

4. A method for using a reactor for removing hydrogen isotopes from helium-3 gas, using the reactor for removing hydrogen isotopes from helium-3 gas as claimed in claim 1, characterized in that: The following steps are involved: S1: Loading the CuO particle filler (9) into the sealed reactor shell (4) along the spiral guide plate (3), and vibrating the filler to fill the sealed reactor shell (4); S2: Connecting the power supply to heat the heating furnace (6), feeding back the temperature through the armored thermocouple, heating the entire reactor to 400-500° C., and connecting the gas outlet pipe (1) to the vacuum system for evacuation; S3: Reactor leak detection: After stopping the thermal degassing of the reactor and evacuating it, connect it to the leak detection system for leak detection; S4: regeneration by oxygen: after the reactor passes the leak detection, the heating furnace (6) is continuously heated to maintain the temperature at 400-500°C, the air inlet pipe (8) is connected to the oxygen bottle, oxygen is filled into the reactor, and after the CuO particle filler (9) reacts fully with the oxygen, the vacuum system is continued to be used for vacuuming; S5: The heating electric furnace (6) is heated and maintained at a temperature of 400-500° C. The gas to be purified is introduced through the gas inlet pipe (8), and the purified gas is discharged through the gas outlet pipe (1); S8: After the reactor is heated, it is allowed to stand to cool down. Alternatively, the heating furnace (6) may be removed to allow the reactor to cool down quickly.

5. The method for using a reactor for removing hydrogen isotopes from helium-3 gas according to claim 4, characterized in that: In the S1, the CuO particle filler (9) is in a granular form with a particle size of 0.2 mm to 3 mm.

6. The method for using a reactor for removing hydrogen isotopes from helium-3 gas according to claim 5, characterized in that: In S1, gas circulation is ensured and filler is prevented from pulverizing.

7. The method for using a reactor for removing hydrogen isotopes from helium-3 gas according to claim 4, characterized in that: In the S2, the vacuum is evacuated to a degree of vacuum less than 5 Pa.

8. The method for using a reactor for removing hydrogen isotopes from helium-3 gas according to claim 4, characterized in that: In S3, the leakage rate is less than 1.0×10 10 Pa·m 3 / s means qualified.

9. The method for using a reactor for removing hydrogen isotopes from helium-3 gas according to claim 4, characterized in that: In S5, a gas circulation pump is used to circulate and purify the gas; the flow rate is controlled to be 1 to 15 L / min.

10. The method for using a reactor for removing hydrogen isotopes from helium-3 gas according to claim 4, characterized in that: The process also includes S7: after the purification is completed, the device is thermally exhausted, and the temperature of the filler in the sealed reactor shell (4) is monitored by a thermocouple to make the temperature of the filler in the sealed reactor shell (4) reach a set temperature. At the same time, a vacuum is drawn from the gas outlet (1) using a vacuum system until the vacuum degree is less than 5 Pa.

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