A heat treatment controllable atmosphere preparation device and a preparation method thereof

Abstract

This invention discloses a controllable atmosphere preparation device for heat treatment, comprising: a methanol tank equipped with a first connecting component; a heat recovery unit connected to the methanol tank via the first connecting component; and a methanol evaporator connected to the heat recovery unit via a second pipe. This invention relates to the field of methanol atmosphere preparation technology. By setting a multi-stage pyrolysis structure, this invention enables methanol and liquid ammonia to fully complete the pyrolysis reaction. Combined with a pre-set catalyst and alumina molecular sieve, it ensures both sufficient pyrolysis and uniform reaction temperature, allowing for complete decomposition and the production of a controllable atmosphere with a dew point meeting requirements. Compared to traditional drip-feed preparation methods, this method completes the methanol pyrolysis within the device before introducing it into the heat treatment furnace, eliminating the need for pyrolysis within the furnace. This significantly reduces the difficulty of controlling process parameters within the furnace, prevents workpiece oxidation and decarburization, and reduces the amount of controllable atmosphere required.

Description

Technical Field

[0001] This invention relates to the field of methanol atmosphere preparation technology, specifically to a heat treatment controllable atmosphere preparation device and its preparation method. Background Technology

[0002] Methanol atmosphere is a protective atmosphere formed by mixing nitrogen and methanol. It is mainly used for atmosphere control in high-temperature processes. By adjusting the amount of enriched gas (pure nitrogen) and air introduced, the carbon potential can be controlled, achieving precise control of the carbon potential. It is widely used in high-temperature and heat treatment protective atmospheres, such as quenching, carburizing, carbonitriding and other processes.

[0003] Currently, the preparation of methanol atmospheres in existing technologies typically employs two common methods: one is to directly drip liquid methanol into the heat treatment furnace for high-temperature pyrolysis; the other is to premix methanol with nitrogen to form a so-called nitrogen-methanol atmosphere, which is then introduced into the furnace. While these methods are relatively simple to operate and require lower initial equipment investment, they have a significant drawback: because they employ a drip-feed atmosphere for carburizing, critical process parameters, such as the flow rate of the dripping liquid and the furnace temperature, must be controlled with extreme precision and stability throughout the process. Deviations or improper control of these parameters can easily lead to carbon deposits or the precipitation of network carbides on the workpiece surface, severely impacting the final performance and quality of the workpiece. Furthermore, this process characteristic limits the gas production per unit time, resulting in relatively low capacity, thus failing to meet the stringent requirements of modern continuous, large-scale batch production models for high efficiency and stable output. Summary of the Invention

[0004] To address the shortcomings of existing technologies, this invention provides a heat treatment controllable atmosphere preparation device and method, which solves the problem that in the preparation of methanol atmosphere in existing technologies, liquid methanol is directly dripped into the heat treatment furnace for high-temperature cracking or pre-mixed with nitrogen. This requires extremely precise and stable control of key process parameters, which limits the amount of gas produced per unit time and results in relatively low production capacity.

[0005] To achieve the above objectives, the present invention provides the following technical solution: a heat treatment controllable atmosphere preparation apparatus, comprising: A methanol tank, wherein the methanol tank is equipped with a first communication component.

[0006] A heat recovery unit, which is connected to the methanol tank via the first communication component.

[0007] A methanol evaporator is connected to the heat recovery unit via a second pipe. A heating element is installed at the top of the methanol evaporator and is configured to preheat and evaporate the methanol flowing into the heat recovery unit.

[0008] A packing mechanism connected to the heat recovery unit and the methanol evaporator, the packing mechanism being configured to form a feed channel for the heat treatment feedstock to flow to the heat recovery unit and the methanol evaporator.

[0009] A pyrolysis mechanism, which is connected to the methanol evaporator.

[0010] In some embodiments, the filling mechanism includes a liquid ammonia tank, a liquid ammonia radiator, a pair of material filling pipes, an eighth pipe, and a second connecting assembly.

[0011] The liquid ammonia tank is connected to the liquid ammonia radiator via the second connecting assembly, and the liquid ammonia radiator is connected to the heat recovery unit via the fourth pipe. The liquid ammonia radiator is used to dissipate heat from the liquid ammonia. A pair of material filling pipes are respectively disposed on the heat recovery unit and the methanol evaporator. The eighth pipe is connected to the methanol evaporator and is configured to provide a channel for nitrogen to flow into the methanol evaporator. A one-way valve and a control valve are installed on the eighth pipe, and a one-way valve is installed on the fourth pipe.

[0012] In some embodiments, the second connection component includes a third pipe and a liquid ammonia shut-off valve.

[0013] The two ends of the third pipeline are connected to the liquid ammonia tank and the liquid ammonia radiator, respectively. The liquid ammonia shut-off valve is configured on the third pipeline to enable it to flow or block. A control valve and a check valve are installed on the third pipeline.

[0014] In some embodiments, the pyrolysis mechanism includes a fifth pipe, a liquid ammonia evaporation coil, a pyrolysis furnace, a controlled atmosphere coil, a pair of first pyrolysis tanks, a connecting pipe, a second heater, a second pyrolysis tank, a third pyrolysis tank, a third connecting assembly, and a heat dissipation assembly.

[0015] The second and third pyrolysis tanks are respectively fixed to the methanol evaporator and the heat recovery unit. One end of the fifth pipe is connected to the liquid ammonia evaporation coil, and the other end passes through the heat recovery unit and the second pyrolysis tank and is arranged in a spiral shape inside the second pyrolysis tank. The end of the liquid ammonia evaporation coil away from the fifth pipe is connected to the pyrolysis furnace. A pair of first pyrolysis tanks and liquid ammonia evaporation coils are both arranged inside the pyrolysis furnace. A pair of first pyrolysis tanks are connected to the second and third pyrolysis tanks respectively through the third connecting assembly. One end of the controllable atmosphere coil passes through the heat recovery unit and the second pyrolysis tank and is arranged in a spiral shape inside the second pyrolysis tank. The other end of the controllable atmosphere coil is connected to a heat dissipation assembly. A pair of first pyrolysis tanks are connected to each other through the connecting pipe. The second heater is arranged inside the pyrolysis furnace and is used to heat the pyrolysis furnace.

[0016] In some embodiments, the third connection component includes a sixth pipe and a seventh pipe.

[0017] The sixth pipe is connected to the heat recovery unit and one of the first pyrolysis tanks at both ends, and the seventh pipe is connected to the methanol evaporator and another of the first pyrolysis tanks at both ends.

[0018] In some embodiments, the heat dissipation assembly includes a controlled atmosphere radiator and a tenth conduit.

[0019] The air inlet and exhaust outlet of the controlled atmosphere radiator are connected to the controlled atmosphere coil and the tenth pipe, respectively, and the controlled atmosphere radiator is configured to dissipate heat from the controlled atmosphere. A one-way valve is installed on the tenth pipe.

[0020] In some embodiments, a catalytic mechanism is also included, which includes a plurality of alumina pipes, a plurality of catalyst pipes, and a drain pipe.

[0021] Multiple alumina pipes and multiple catalyst pipes are arranged in the first pyrolysis tank, the second pyrolysis tank and the third pyrolysis tank, and the material filling pipe is connected to the corresponding catalyst pipe. The multiple alumina pipes are filled with alumina molecular sieves. The drain pipe is installed in the methanol evaporator and passes through the methanol evaporator and is connected to the third pyrolysis tank.

[0022] In some embodiments, the heating assembly includes a first heater and a thermocouple.

[0023] The first heater and the thermocouple are fixedly connected to the second pyrolysis vessel, and the first heater is used to heat the second pyrolysis vessel.

[0024] In some embodiments, the first connection assembly includes a first pipe, a methanol shut-off valve, a methanol pump, and a ninth pipe.

[0025] The first pipeline is connected to the methanol tank and the second pyrolysis tank at both ends, respectively. The methanol shut-off valve and the methanol pump are configured in the first pipeline. The methanol shut-off valve and the methanol pump are used to control the flow of methanol. The first pipeline is equipped with a control valve and a check valve. The ninth pipeline is connected to the pyrolysis furnace and the heat recovery unit, respectively.

[0026] A method for preparing a heat treatment controllable atmosphere preparation apparatus, the method being used to prepare a heat treatment controllable atmosphere in the apparatus, the method comprising the following steps: S1. Raw material preparation: The methanol is transported through the methanol tank via the first connecting component, so that the methanol is delivered at a rate of 0.5-1.0 m³ / min. 3 A flow rate of [amount] m³ / h enters the heat recovery unit, while simultaneously, liquid ammonia is transported from the liquid ammonia tank through the third pipeline. The liquid ammonia shut-off valve and control valve are opened to control the liquid ammonia flow rate at 0.3-0.6 m³ / h. 3 / h enters the liquid ammonia radiator.

[0027] S2. Preheating and Evaporation: The methanol in the heat recovery unit absorbs waste heat to 80-100°C through the controllable atmosphere coil, and then enters the methanol evaporator through the second pipe. The first heater is started to heat the methanol to 150-200°C, causing it to evaporate into a gaseous state. At the same time, nitrogen is introduced into the methanol evaporator through the eighth pipe, with the nitrogen flow rate being 5-10% of the total gas volume.

[0028] S3. Cracking reaction: Gaseous methanol enters the first cracking tank in the cracking furnace through the ninth pipe. Liquid ammonia enters the liquid ammonia evaporation coil of the heat recovery unit through the fourth pipe and evaporates into gaseous state. It is then introduced into the first cracking tank. The second heater is started to raise the temperature of the cracking tank to 350-450℃. The cracking reaction is carried out under the action of the catalyst. The reaction time is controlled at 20-30 minutes.

[0029] S4. Atmosphere treatment: The pyrolysis mixture enters the controlled atmosphere coil of the heat recovery unit and exchanges heat with the methanol and liquid ammonia to be heated, reducing the temperature to 150-200℃. Then it enters the controlled atmosphere radiator for further cooling to 80-100℃. During this period, the alumina molecular sieve dries the mixture to remove moisture to a dew point ≤-40℃.

[0030] S5. Atmosphere Output: The treated controllable atmosphere is discharged into the target heat treatment furnace through the tenth pipe. The output pressure is adjusted to 0.1-0.3MPa by the control valve to complete the preparation operation.

[0031] This invention provides a controllable atmosphere preparation apparatus and method for heat treatment, which has the following beneficial effects: This invention, by setting up a pyrolysis structure, enables methanol and liquid ammonia to fully complete the pyrolysis reaction. Combined with a packing mechanism, it ensures both thorough pyrolysis and uniform reaction temperature, facilitating complete decomposition and yielding a controllable atmosphere with the required dew point. Compared to traditional drip-feed preparation methods, this method completes methanol pyrolysis within the device before introducing it into the heat treatment furnace, eliminating the need for furnace-based pyrolysis. This significantly reduces the difficulty of controlling furnace process parameters, prevents workpiece oxidation and decarburization, reduces the amount of controllable atmosphere required, and allows for stable and continuous production of qualified controllable atmosphere gas with a higher gas output per unit time, meeting the demands of modern continuous batch production. Furthermore, by incorporating a heat recovery unit, the residual heat from the high-temperature controllable atmosphere after pyrolysis is used to preheat the raw materials methanol and liquid ammonia, fully recovering and utilizing the residual heat after the reaction, reducing overall energy consumption and production costs. Attached Figure Description

[0032] Figure 1 This is a schematic diagram of the structure of the present invention.

[0033] Figure 2 For the present invention Figure 1 The main view in the text.

[0034] Figure 3 For the present invention Figure 1 The top view in the image.

[0035] Figure 4 For the present invention Figure 1 A side view of the plane.

[0036] Figure 5 For the present invention Figure 1 The planar sectional view.

[0037] Figure 6 For the present invention Figure 1 A partial structural planar sectional view.

[0038] Figure 7 For the present invention Figure 1 A partial structural planar sectional view.

[0039] In the diagram: 1. Methanol tank; 2. First pipeline; 3. Methanol shut-off valve; 4. Methanol pump; 5. Heat recovery unit; 6. Methanol evaporator; 7. Second pipeline; 8. Liquid ammonia tank; 9. Third pipeline; 10. Liquid ammonia shut-off valve; 11. Liquid ammonia radiator; 12. Fourth pipeline; 13. Fifth pipeline; 14. Liquid ammonia evaporation coil; 15. Cracking furnace; 16. First cracking vessel; 17. Connecting pipe; 18. Second heater; 19. Alumina pipeline; 20. Catalyst pipeline; 21. Material filling pipe; 22. Sixth pipeline; 23. Seventh pipeline; 24. Eighth pipeline; 25. Drain pipe; 26. First heater; 27. Thermocouple; 28. Controlled atmosphere coil; 29. ​​Controlled atmosphere radiator; 30. Tenth pipeline; 31. Second cracking vessel; 32. Third cracking vessel; 33. Ninth pipeline. Detailed Implementation

[0040] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0041] Example 1 Please see Figure 1-7 The present invention provides a technical solution: a heat treatment controllable atmosphere preparation apparatus, comprising: Methanol tank 1, which is equipped with a first connecting component.

[0042] Heat recovery unit 5 is connected to methanol tank 1 via a first connecting component.

[0043] Methanol evaporator 6 is connected to heat recovery unit 5 via a second pipe 7. A heating component is installed at the top of methanol evaporator 6, which is configured to preheat and evaporate the methanol flowing into heat recovery unit 5.

[0044] The packing mechanism is connected to the heat recovery unit 5 and the methanol evaporator 6. The packing mechanism is configured to form a feed channel for the heat treatment raw materials to flow to the heat recovery unit 5 and the methanol evaporator 6.

[0045] The cracking mechanism is connected to the methanol evaporator 6.

[0046] Methanol tank 1 stores methanol. Through the first connecting component, the methanol inside the methanol tank 1 can be discharged into the heat recovery unit for preliminary preheating reaction. Then, through the second pipe 7, it is discharged into the methanol evaporator 6 for further reaction. The packing mechanism can discharge alumina molecular sieves and catalysts into designated positions to assist the subsequent reaction and ensure that the cracking operation proceeds normally.

[0047] By setting up a cracking structure, methanol and liquid ammonia can fully complete the cracking reaction. With the pre-set catalyst and alumina molecular sieve, not only can the cracking be fully guaranteed, but a controllable atmosphere with the required dew point can also be obtained. Compared with the traditional drip-feed preparation method, this method completes the cracking of methanol in the device before it is introduced into the heat treatment furnace, eliminating the need for the cracking reaction to be completed in the furnace. This greatly reduces the difficulty of controlling the process parameters in the furnace, prevents oxidation and decarburization of the workpiece, and reduces the amount of controllable atmosphere used. At the same time, the device can stably and continuously produce qualified controllable atmosphere gas with a higher gas output per unit time, which can meet the needs of modern continuous batch production. By setting up a heat recovery unit 5, the waste heat of the high-temperature controllable atmosphere after cracking is used to preheat the raw materials methanol and liquid ammonia, which can fully recover and utilize the waste heat after the reaction, reduce the overall energy consumption of the process, and reduce the preparation cost.

[0048] like Figure 1-5 As shown, in this embodiment, the filling mechanism is further configured to include a liquid ammonia tank 8, a liquid ammonia radiator 11, a pair of material filling pipes 21, an eighth pipe 24, and a second connecting assembly.

[0049] The liquid ammonia tank 8 is connected to the liquid ammonia radiator 11 via the second connecting assembly, and the liquid ammonia radiator 11 is connected to the heat recovery unit 5 via the fourth pipe 12. The liquid ammonia radiator 11 is used to dissipate heat from the liquid ammonia. A pair of material filling pipes 21 are respectively configured on the heat recovery unit 5 and the methanol evaporator 6. The eighth pipe 24 is connected to the methanol evaporator 6 and is configured to provide a channel for nitrogen to flow into the methanol evaporator 6. A check valve and a control valve are installed on the eighth pipe 24, and a check valve is installed on the fourth pipe 12.

[0050] The liquid ammonia tank 8 stores liquid ammonia. The liquid ammonia can be discharged into the liquid ammonia radiator 11 through the second connecting component to dissipate heat. After turning into a gaseous state, it is discharged into the heat recovery unit 5 through the fourth pipe 12. At the same time, the eighth pipe 24 can introduce nitrogen into the methanol evaporator 6 to form the basic feed passage of raw materials and meet the basic raw material supply requirements for the preparation atmosphere.

[0051] like Figure 1-4 As shown, in this embodiment, the second connecting component is further configured to include a third pipe 9 and a liquid ammonia shut-off valve 10.

[0052] The two ends of the third pipe 9 are connected to the liquid ammonia tank 8 and the liquid ammonia radiator 11, respectively. The liquid ammonia shut-off valve 10 is configured on the third pipe 9 to form a flow or blockage state. A control valve and a check valve are installed on the third pipe 9.

[0053] The liquid ammonia shut-off valve 10 can control the on / off state of liquid ammonia in the third pipeline 9. In conjunction with the control valve, the flow rate of liquid ammonia can be precisely adjusted. The one-way valve can prevent backflow of liquid ammonia and ensure that the feeding process is stable and controllable. The liquid ammonia radiator 11 evaporates the liquid ammonia to form gaseous ammonia, which meets the raw material ratio requirements for atmosphere preparation.

[0054] like Figure 1-7 As shown, in this embodiment, the pyrolysis mechanism is further configured to include a fifth pipe 13, a liquid ammonia evaporation coil 14, a pyrolysis furnace 15, a controllable atmosphere coil 28, a pair of first pyrolysis tanks 16, a connecting pipe 17, a second heater 18, a second pyrolysis tank 31, a third pyrolysis tank 32, a third connecting assembly, and a heat dissipation assembly.

[0055] The second cracking tank 31 and the third cracking tank 32 are respectively fixed in the methanol evaporator 6 and the heat recovery unit 5. One end of the fifth pipe 13 is connected to the liquid ammonia evaporation coil 14, and the other end passes through the heat recovery unit 5 and the second cracking tank 31 and is arranged in a spiral shape in the second cracking tank 31. The end of the liquid ammonia evaporation coil 14 away from the fifth pipe 13 is connected to the cracking furnace 15. A pair of first cracking tanks 16 and the liquid ammonia evaporation coil 14 are both arranged in the cracking furnace 15. The pair of first cracking tanks 16 are connected to the second cracking tank 31 and the third cracking tank 32 respectively through the third connecting component. One end of the controllable atmosphere coil 28 passes through the heat recovery unit 5 and the second cracking tank 31 and is arranged in a spiral shape in the second cracking tank 31. The other end of the controllable atmosphere coil 28 is connected to a heat dissipation component. The pair of first cracking tanks 16 are connected by a connecting pipe 17. The second heater 18 is arranged in the cracking furnace 15 and is used to heat the cracking furnace 15.

[0056] The first cracking tank 16 is located inside the cracking furnace 15. The second heater 18 provides a stable heating temperature to the cracking furnace 15. Liquid ammonia enters the cracking furnace 15 through the liquid ammonia evaporation coil 14, and the liquid ammonia can be heated and evaporated using the temperature inside the cracking furnace 15. Then, it enters the cracking tank to complete the cracking. Methanol enters the first cracking tank 16 after preheating. After passing through the first cracking tank 16, the second cracking tank 31, and the third cracking tank 32 in sequence, the resulting controlled atmosphere is sent to the controlled atmosphere coil 28. Finally, it is cooled and output through the heat dissipation component. The multi-stage cracking combined with sufficient heat recovery and utilization can make the cracking reaction of methanol and liquid ammonia more complete, stabilize the cracking efficiency of the raw materials, and thus increase the output of the controlled atmosphere. The second heater 18 can be electrically heated.

[0057] like Figure 1-6 As shown, in this embodiment, the third connecting component is further configured to include a sixth pipe 22 and a seventh pipe 23.

[0058] The two ends of the sixth pipe 22 are connected to the heat recovery unit 5 and a first cracking tank 16, respectively, and the two ends of the seventh pipe 23 are connected to the methanol evaporator 6 and another first cracking tank 16, respectively.

[0059] Two feed paths are formed by the sixth pipe 22 and the seventh pipe 23, respectively, to send the raw materials that have been heated by the heat recovery unit 5 and the methanol evaporated by the methanol evaporator 6 into two different first cracking tanks 16, ensuring that each raw material can be fed independently, avoiding mixing and interference between different raw materials during the transportation stage, and ensuring the orderly progress of the cracking reaction.

[0060] like Figure 1-4 As shown, in this embodiment, the heat dissipation assembly is further configured to include a controllable atmosphere radiator 29 and a tenth conduit 30.

[0061] The air inlet and exhaust outlet of the controlled atmosphere radiator 29 are connected to the controlled atmosphere coil 28 and the tenth pipe 30, respectively, and the controlled atmosphere radiator 29 is configured to dissipate heat from the controlled atmosphere. A one-way valve is installed on the tenth pipe 30.

[0062] The controlled atmosphere radiator 29 can rapidly cool the prepared controlled atmosphere, ensuring that the output controlled atmosphere meets the temperature requirements for subsequent use. The one-way valve on the tenth pipe 30 can prevent gas backflow, ensure the stability of the output process, and avoid gas pressure fluctuations affecting the stability of atmosphere preparation. The controlled atmosphere radiator 29 can be composed of a condenser, a fan, and other supporting structures to achieve heat dissipation.

[0063] like Figure 3-7 As shown, this embodiment is further configured to include a catalytic mechanism, which includes multiple alumina pipes 19, multiple catalyst pipes 20, and a drain pipe 25.

[0064] Multiple alumina pipes 19 and multiple catalyst pipes 20 are arranged in the first cracking tank 16, the second cracking tank 31 and the third cracking tank 32, and the material filling pipe 21 is connected to the corresponding catalyst pipe 20. The multiple alumina pipes 19 are filled with alumina molecular sieves. The drain pipe 25 is installed in the methanol evaporator 6 and passes through the methanol evaporator 6 and is connected to the third cracking tank 32.

[0065] The material filling pipe 21 can be fitted with a cap to improve its performance, or it can be directly connected to an external feeding structure. The catalyst pipe 20 can be filled with catalyst, such as nickel-based cracking catalyst. Alumina molecular sieves and catalysts are filled in their respective pipes, which can fully contact the raw materials during the multi-stage cracking process, reduce the cracking activation energy of methanol and ammonia, improve the cracking reaction rate and raw material conversion rate, and avoid the problem of incomplete reaction. The drain pipe 25 can drain the condensate generated in the third cracking pipe to maintain stable pipeline pressure.

[0066] like Figure 1-5 As shown, in this embodiment, the heating assembly is further configured to include a first heater 26 and a thermocouple 27.

[0067] The first heater 26 and the thermocouple 27 are fixedly connected to the second pyrolysis vessel 31. The first heater 26 is used to heat the second pyrolysis vessel 31.

[0068] The first heater 26 can continuously heat the second pyrolysis vessel 31 to maintain the reaction temperature inside the second pyrolysis vessel 31. In conjunction with the thermocouple, the temperature inside the vessel can be monitored in real time, which allows the operator to adjust the heating power according to the actual pyrolysis needs, ensuring that the pyrolysis reaction is always within a suitable temperature range and improving the stability of the reaction. The first heater 26 can be electrically heated.

[0069] like Figure 1-5 As shown, in this embodiment, the first connecting component is further configured to include a first pipe 2, a methanol shut-off valve 3, a methanol pump 4, and a ninth pipe 33.

[0070] The two ends of the first pipeline 2 are connected to the methanol tank 1 and the second cracking tank 31, respectively. The methanol shut-off valve 3 and the methanol pump 4 are configured in the first pipeline 2. The methanol shut-off valve 3 and the methanol pump 4 are used to control the flow of methanol. The first pipeline 2 is equipped with a control valve and a check valve. The ninth pipeline 33 is connected to the cracking furnace 15 and the heat recovery unit 5, respectively.

[0071] The methanol shut-off valve 3 controls the flow of methanol in the first pipeline 2, and together with the methanol pump 4, it provides stable power for methanol delivery and precisely regulates the methanol flow rate. The one-way valve also prevents methanol backflow, ensuring a stable and controllable methanol delivery process and providing a stable raw material supply for the entire atmosphere preparation process. Through the cooperation of these components, the device can prepare a controlled atmosphere through multi-stage pyrolysis, making overall process parameter control easier, the pyrolysis reaction more complete, and the gas production per unit time steadily increased, meeting the needs of large-scale batch production.

[0072] The ninth pipe 33 is configured to send the excess waste heat collected by the heat recovery unit 5 into the pyrolysis furnace 15 to recover and utilize the waste heat generated inside the device, reduce the power consumption of the second heater 18, reduce the overall energy consumption, and at the same time make the heat distribution inside the device more reasonable and improve the thermal energy utilization rate.

[0073] Please see Figure 1-7 A method for preparing a heat treatment controllable atmosphere preparation apparatus, the method being used to prepare a heat treatment controllable atmosphere in the apparatus, the method comprising the following steps: S1. Raw material preparation: Methanol is transported through methanol tank 1 via the first connecting component, so that the methanol flows at a rate of 0.5-1.0 m³ / min. 3A flow rate of [amount] m³ / h enters the heat recovery unit 5, while simultaneously, liquid ammonia is transported from the liquid ammonia tank through the third pipeline. The liquid ammonia shut-off valve and control valve are opened to control the liquid ammonia flow rate at 0.3-0.6 m³ / h. 3 / h enters the liquid ammonia radiator 11.

[0074] S2. Preheating and Evaporation: The methanol in the heat recovery unit 5 absorbs waste heat to 80-100°C through the controlled atmosphere coil 28, and then enters the methanol evaporator 6 through the second pipe 7. The first heater 26 is started to heat the methanol to 150-200°C, causing it to evaporate into a gaseous state. At the same time, nitrogen is introduced into the methanol evaporator 6 through the eighth pipe 24, with the nitrogen flow rate being 5-10% of the total gas volume.

[0075] S3. Cracking reaction: Gaseous methanol enters the first cracking tank 16 in the cracking furnace 15 through the ninth pipe 33. Liquid ammonia enters the liquid ammonia evaporation coil 14 of the heat recovery unit 5 through the fourth pipe 12 and evaporates into gaseous state. It is then introduced into the first cracking tank 16. The second heater 18 is started to raise the temperature of the cracking tank to 350-450℃. The cracking reaction is carried out under the action of the catalyst. The reaction time is controlled at 20-30 minutes.

[0076] S4. Atmosphere treatment: The pyrolysis mixture enters the controlled atmosphere coil 28 of the heat recovery unit 5 and exchanges heat with the methanol and liquid ammonia to be heated, reducing the temperature to 150-200℃. Then it enters the controlled atmosphere radiator 29 for further cooling to 80-100℃. During this period, the alumina molecular sieve dries the mixture to remove moisture to a dew point ≤-40℃.

[0077] S5. Atmosphere Output: The treated controllable atmosphere is discharged into the target heat treatment furnace through the tenth pipe 30. The output pressure is adjusted to 0.1-0.3MPa by the control valve to complete the preparation operation.

[0078] The following describes a specific embodiment of this application with reference to the accompanying drawings: When this device is needed, the components can be assembled according to the assembly process as shown in the drawings, ensuring that the bolts are tightened and the welding is firm. Then, the circuit and control devices are connected, and after checking that all interfaces are correct, the power is turned on for testing to ensure that the current detection, position feedback and other functions are normal. The control devices are then installed in appropriate positions. Before operation, all structures are cleaned. Afterwards, the first pipe 2 can discharge the methanol in the methanol tank 1 to the heat recovery unit 5 through the methanol shut-off valve 3 and the methanol pump 4. The methanol undergoes a preliminary reaction in the alumina molecular sieve in the second cracking tank 31 inside the heat recovery unit 5, and flows into the second cracking tank 31 inside the methanol evaporator 6 through the second pipe 7. At the same time, the first heater 26 and the thermocouple 27 work to preheat the methanol. After the methanol has been preheated, it enters the first cracking tank 16 inside the cracking furnace 15 through the sixth pipe 22. Meanwhile, the liquid ammonia inside the liquid ammonia tank 8 enters the liquid ammonia radiator 11 through the third pipe 9, and then enters the liquid ammonia evaporation coil inside the heat recovery unit 5 through the fourth pipe 12. 13. After absorbing residual heat, the methanol evaporates into a gaseous state and then enters the liquid ammonia evaporation coil 14 in the cracking furnace 15 for further heating. After that, it is introduced into the first cracking tank 16 to participate in the cracking reaction. The eighth pipe 24 can add a certain amount of nitrogen to the methanol evaporator 6 according to production needs and mix it with the cracked raw materials. At this time, the second heater 18 will also heat the entire cracking furnace 15, so that the methanol in the first cracking tank 16 will be further heated and cracked. The alumina molecular sieve filled inside the alumina pipe 19 dries the atmosphere in each cracking tank and absorbs excess moisture in the atmosphere. The catalyst pipe 20 can add the corresponding catalyst according to needs to promote the cracking reaction of methanol and liquid ammonia. After cracking, the controlled atmosphere obtained enters the controlled atmosphere radiator 29 through the controlled atmosphere coil 28. When the controlled atmosphere coil 28 flows, it transfers its own heat to the methanol and liquid ammonia to be heated in the heat recovery unit 5 to complete the heat recovery and utilization. Finally, the cooled controlled atmosphere is discharged into the target heat treatment furnace through the tenth pipe 30, thus completing the preparation of the controlled atmosphere.

[0079] Example 2 Unlike Embodiment 1, in this embodiment, the heat recovery unit 5, the methanol evaporator 6, and the outer wall of the cracking furnace 15 are all provided with a heat insulation layer.

[0080] The insulation layer uses aluminum silicate insulation cotton with a thickness of 20-30mm, which can effectively isolate the heat exchange between the inside of the device and the outside, reduce the heat loss of the device, further maintain the stable temperature required for the reaction, reduce the continuous energy consumption of the heater, improve the overall thermal energy utilization rate, and also prevent the outer wall temperature of the equipment from being too high and causing burns to the operators, thus improving the safety performance of the device.

[0081] Example 3 Unlike Example 1, in this example, the catalyst is replaced by a palladium-based cracking catalyst instead of a nickel-based cracking catalyst. The palladium-based cracking catalyst is filled with 80%-90% of the nickel-based cracking catalyst. Within the same reaction temperature range, the palladium-based cracking catalyst can further reduce the cracking activation energy of methanol and liquid ammonia, increase the cracking reaction rate, and shorten the residence time of the raw materials in the cracking tank. Under the premise of maintaining the same gas production, the overall volume of the cracking tank can be appropriately reduced, thereby reducing the overall footprint and manufacturing cost of the device. At the same time, the palladium-based cracking catalyst has stronger resistance to poisoning and a longer service life, which can reduce the frequency of catalyst replacement and reduce the maintenance cost of long-term use.

[0082] It should be noted that, in this document, relational terms such as "first" and "second" are used merely to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or apparatus. Without further limitations, the phrase "comprising an element defined as..." does not exclude the presence of other identical elements in the process, method, article, or apparatus that includes the element.

[0083] It is worth noting that all standard parts used in this invention can be purchased from the market, and irregularly shaped parts can be customized according to the description and drawings. The specific connection methods of each part all adopt conventional methods such as bolts, rivets, and welding that are mature in the prior art. The models of electrical structure equipment involved can be selected according to the user's needs, as long as they meet the requirements of this application. In addition, the circuit connection adopts conventional connection methods in the prior art. The supporting electrical structures such as the control, current detection, position feedback, predicted voltage synchronization and parameter adjustment of the electrical equipment are all existing technologies, such as PLC controllers and module structures, so they will not be described in detail here.

[0084] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A controllable atmosphere preparation apparatus for heat treatment, characterized in that, include: A methanol tank (1) is equipped with a first communication component; A heat recovery unit (5) is connected to the methanol tank (1) via the first communication component; A methanol evaporator (6) is connected to the heat recovery unit (5), and the methanol evaporator (6) is equipped with a heating assembly configured to preheat the methanol flowing into the heat recovery unit (5). A packing mechanism connected to the heat recovery unit (5) and the methanol evaporator (6) is configured to form a feed channel for the heat treatment raw materials to flow to the heat recovery unit (5) and the methanol evaporator (6); A pyrolysis mechanism is connected to the methanol evaporator (6).

2. The heat treatment controllable atmosphere preparation apparatus according to claim 1, characterized in that, The filling mechanism includes a liquid ammonia tank (8), a liquid ammonia radiator (11), a pair of material filling pipes (21), an eighth pipe (24), and a second connecting assembly; The liquid ammonia tank (8) is connected to the liquid ammonia radiator (11) via the second connecting assembly, and the liquid ammonia radiator (11) is connected to the heat recovery unit (5). The liquid ammonia radiator (11) is used to dissipate heat from the liquid ammonia. A pair of material filling pipes (21) are respectively disposed on the heat recovery unit (5) and the methanol evaporator (6). The eighth pipe (24) is connected to the methanol evaporator (6) and is configured to provide a channel for nitrogen to flow into the methanol evaporator (6).

3. The heat treatment controllable atmosphere preparation apparatus according to claim 2, characterized in that, The second connection assembly includes a third pipe (9) and a liquid ammonia shut-off valve (10); The two ends of the third pipe (9) are connected to the liquid ammonia tank (8) and the liquid ammonia radiator (11) respectively. The liquid ammonia shut-off valve (10) is configured on the third pipe (9) and makes it either in a flow or interception state.

4. The heat treatment controllable atmosphere preparation apparatus according to claim 1, characterized in that, The pyrolysis mechanism includes a fifth pipe (13), a liquid ammonia evaporation coil (14), a pyrolysis furnace (15), a controllable atmosphere coil (28), a pair of first pyrolysis tanks (16), a connecting pipe (17), a second heater (18), a second pyrolysis tank (31), a third pyrolysis tank (32), a third connecting assembly, and a heat dissipation assembly; The second pyrolysis tank (31) and the third pyrolysis tank (32) are respectively fixed in the methanol evaporator (6) and the heat recovery unit (5). One end of the fifth pipe (13) is connected to the liquid ammonia evaporation coil (14), and the other end passes through the heat recovery unit (5) and the second pyrolysis tank (31) and is arranged in a spiral shape in the second pyrolysis tank (31). The end of the liquid ammonia evaporation coil (14) away from the fifth pipe (13) is connected to the pyrolysis furnace (15). A pair of first pyrolysis tanks (16) and liquid ammonia evaporation coils (14) are both arranged in the pyrolysis furnace (15). The first pyrolysis tank (16) is connected to the second pyrolysis tank (31) and the third pyrolysis tank (32) respectively through the third connecting assembly. One end of the controllable atmosphere coil (28) passes through the heat recovery unit (5) and the second pyrolysis tank (31) and is arranged in a spiral shape inside the second pyrolysis tank (31). The other end of the controllable atmosphere coil (28) is connected to a heat dissipation assembly. A pair of first pyrolysis tanks (16) are connected through the connecting pipe (17). The second heater (18) is disposed inside the pyrolysis furnace (15) and is used to heat the pyrolysis furnace (15).

5. The heat treatment controllable atmosphere preparation apparatus according to claim 4, characterized in that, The third connection component includes a sixth pipe (22) and a seventh pipe (23); The two ends of the sixth pipe (22) are connected to the heat recovery unit (5) and a first pyrolysis tank (16) respectively, and the two ends of the seventh pipe (23) are connected to the methanol evaporator (6) and another first pyrolysis tank (16) respectively.

6. The heat treatment controllable atmosphere preparation apparatus according to claim 4, characterized in that, The heat dissipation assembly includes a controlled atmosphere radiator (29) and a tenth conduit (30). The air inlet and exhaust outlet of the controlled atmosphere radiator (29) are connected to the controlled atmosphere coil (28) and the tenth pipe (30), respectively, and the controlled atmosphere radiator (29) is configured to dissipate heat in a controlled atmosphere.

7. The heat treatment controllable atmosphere preparation apparatus according to claim 2, characterized in that, It also includes a catalytic mechanism, which includes multiple alumina pipes (19), multiple catalyst pipes (20) and a drain pipe (25). Multiple alumina pipes (19) and multiple catalyst pipes (20) are arranged in the first pyrolysis tank (16), the second pyrolysis tank (31) and the third pyrolysis tank (32), and the material filling pipe (21) is connected to the corresponding catalyst pipe (20). The multiple alumina pipes (19) are filled with alumina molecular sieves. The drain pipe (25) is installed in the methanol evaporator (6), and the drain pipe (25) passes through the methanol evaporator (6) and is connected to the third pyrolysis tank (32).

8. The heat treatment controllable atmosphere preparation apparatus according to claim 4, characterized in that, The heating assembly includes a first heater (26) and a thermocouple (27); The first heater (26) and the thermocouple (27) are fixedly connected to the second pyrolysis vessel (31), and the first heater (26) is used to heat the second pyrolysis vessel (31).

9. The heat treatment controllable atmosphere preparation apparatus according to claim 4, characterized in that, The first connecting assembly includes a first pipe (2), a methanol shut-off valve (3), a methanol pump (4), and a ninth pipe (33). The two ends of the first pipeline (2) are connected to the methanol tank (1) and the second cracking tank (31) respectively. The methanol shut-off valve (3) and the methanol pump (4) are configured in the first pipeline (2). The methanol shut-off valve (3) and the methanol pump (4) are used to control the flow of methanol. The ninth pipeline (33) is connected to the cracking furnace (15) and the heat recovery unit (5) respectively.

10. A method for preparing a heat treatment controllable atmosphere preparation apparatus, the method being used to prepare a heat treatment controllable atmosphere for the apparatus according to claims 1-9, characterized in that, The preparation method includes the following steps: S1, raw material preparation: the methanol is transported through the methanol tank (1) via the first communication assembly, so that the methanol enters the heat recovery device (5) at a flow rate of 0.5-1.0 m3 / h, while the heat-treated raw material is filled to the designated position; 3 / h of flow rate, while the heat-treated raw material is filled to the designated position; S2, Preheating and Evaporation: The methanol in the heat recovery unit (5) absorbs residual heat to 80-100°C through the cracking mechanism, and then enters the methanol evaporator (6) to heat the methanol to 150-200°C, causing it to evaporate into a gaseous state. At the same time, nitrogen gas is introduced into the methanol evaporator (6) at a flow rate of 5-10% of the total gas volume. S3, Cracking reaction: Gaseous methanol enters the cracking mechanism, and liquid ammonia enters the heat recovery unit (5) and evaporates into gaseous state. It is then introduced into the cracking mechanism to raise the temperature inside the cracking mechanism to 350-450℃. The cracking reaction is carried out under the action of the raw materials being processed, and the reaction time is controlled at 20-30 minutes. S4. Atmosphere treatment: The pyrolysis mixture enters the heat recovery unit (5) and exchanges heat with the methanol and liquid ammonia to be heated. The temperature drops to 150-200℃ and is then further cooled to 80-100℃. During this period, the mixture is dried to remove moisture to a dew point ≤-40℃. S5. Atmosphere Output: The treated controllable atmosphere is discharged into the target heat treatment furnace. The preparation operation is completed by adjusting the output pressure to 0.1-0.3MPa.

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