Reaction apparatus under inert gas protection

Abstract

This invention provides a reaction apparatus with inert gas protection, belonging to the technical field of chemical production equipment. It includes a reaction vessel, a feeding assembly, an inert gas buffer tank, and a controller. A temperature sensor is installed inside the reaction vessel; the reaction vessel is also equipped with a jacketed circulating cooling regulating valve, which is used to reduce the internal temperature of the reaction vessel. The feeding assembly is located at the top of the reaction vessel and communicates with it; the feeding assembly is used to add raw materials to the reaction vessel. The inert gas buffer tank is connected to both the feeding assembly and the reaction vessel; the inert gas buffer tank provides inert gas to the feeding assembly and the reaction vessel, thereby maintaining a protective atmosphere in both. The controller is communicatively connected to the temperature sensor, the jacketed circulating cooling regulating valve, and the feeding assembly. The addition of raw materials can be completed in a completely closed state, without frequent opening of the reaction system, fully meeting the stringent requirements of highly sensitive chemical reactions for an oxygen-free environment.

Description

Technical Field

[0001] This invention belongs to the technical field of chemical production equipment, and more specifically, relates to a reaction device protected by inert gas. Background Technology

[0002] In many chemical synthesis fields, such as organic synthesis, inorganic material preparation, and organometallic chemical reactions, especially in reactions highly sensitive to oxygen and moisture, experiments and production operations are usually conducted under an inert gas protective atmosphere, such as inert gas or argon, to prevent the oxidation or hydrolysis of reactants or products and to ensure the smooth progress of the reaction and the purity of the product. Traditional inert gas protection methods often rely on temporarily assembled reaction devices, manually setting up gas paths using components such as three-way valves, balloons, and double-row pipes, and repeatedly evacuating and purging the system to achieve protection. The operation process is complex and depends on manual control.

[0003] Existing reaction apparatuses have the following drawbacks: During the feeding process, existing apparatuses typically require frequent system opening and closing for refueling and feeding to control the internal temperature of the reactor. Frequent opening and closing of the system easily introduces air and moisture, disrupting the reaction atmosphere and making it impossible to maintain a stable inert gas protective atmosphere in a completely sealed environment. This makes it difficult to meet the stringent requirements of highly sensitive chemical reactions for an anhydrous and oxygen-free environment. Summary of the Invention

[0004] The purpose of this invention is to provide a reaction device protected by inert gas, which aims to solve the problem that in the prior art, reaction devices usually need to be frequently opened for feeding and replenishing in order to control the temperature inside the reactor during the feeding process.

[0005] To achieve the above objectives, the technical solution adopted by the present invention is: to provide a reaction apparatus protected by an inert gas, comprising: The reactor is equipped with a temperature sensor inside; the reactor is also equipped with a jacketed circulating cooling regulating valve; the temperature sensor is used to detect and output real-time temperature information inside the reactor; the jacketed circulating cooling regulating valve is used to reduce the temperature inside the reactor. A feeding assembly is disposed at the top of the reactor and communicates with the reactor; the feeding assembly is used to feed raw materials into the reactor. An inert gas buffer tank is connected to both the feeding assembly and the reactor; the inert gas buffer tank is used to supply inert gas to the feeding assembly and the reactor, thereby maintaining a protective atmosphere in the feeding assembly and the reactor. The controller is communicatively connected to the temperature sensor, the jacket circulating cooling regulating valve, and the feeding assembly; the controller is configured to: Receive the real-time temperature information; During the feeding process of the feeding component, the feeding speed of the feeding component is adjusted or the jacket circulation cooling regulating valve is adjusted according to the real-time temperature information.

[0006] In one possible implementation, adjusting the feeding speed of the feeding component or adjusting the jacket circulating cooling regulating valve based on the real-time temperature information during the feeding process of the feeding component includes: The rate of temperature rise inside the reactor is calculated based on the real-time temperature information. The temperature rise rate is compared with a rise rate threshold. If the temperature rise rate is higher than the rise rate threshold, the feeding component is controlled to reduce the feeding speed or open the jacket circulation cooling regulating valve; otherwise, the feeding component is controlled to maintain the current feeding speed or not open the jacket circulation cooling regulating valve.

[0007] In one possible implementation, the reactor is further provided with an emergency cooling valve; the controller is communicatively connected to the emergency cooling valve and is configured to: When the real-time temperature information is higher than the temperature safety threshold, the feeding component is controlled to stop feeding and the emergency cooling valve is controlled to open.

[0008] In one possible implementation, a pressure sensor is installed inside the reactor, and an emergency control valve is installed on the reactor; the pressure sensor is configured to detect and output real-time pressure information inside the reactor; the controller is communicatively connected to the pressure sensor and the emergency control valve, and is configured to: Receive the real-time pressure information; The real-time pressure information is compared with the pressure safety threshold. If the real-time pressure information is higher than the safety threshold, the feeding component is controlled to stop feeding and the emergency control valve is controlled to open; otherwise, the feeding component is controlled to continue feeding and the emergency control valve is controlled to close.

[0009] In one possible implementation, a receiving tank and a condenser are also included; the inert gas buffer tank is connected to the receiving tank and is used to provide an inert gas protective atmosphere to the receiving tank; the condenser inlet is connected to the top of the reactor and the outlet is connected to the top of the receiving tank.

[0010] In one possible implementation, the system further includes an exhaust gas buffer module and an exhaust gas absorption module; the exhaust gas buffer module is connected to the receiving tank and is used to condense the exhaust gas discharged from the receiving tank; the exhaust gas absorption module is connected to the exhaust gas buffer module and is used to absorb materials in the exhaust gas that are soluble in water or react with water.

[0011] In one possible implementation, the exhaust gas buffer module includes a first exhaust gas buffer tank and a second exhaust gas buffer tank, with the top of the first exhaust gas buffer tank connected to the receiving tank, and the top of the second exhaust gas buffer tank connected to the top of the first exhaust gas buffer tank.

[0012] In one possible implementation, check valves are provided between the receiving tank and the inert gas buffer tank, between the receiving tank and the first exhaust gas buffer tank, and between the first exhaust gas buffer tank and the second exhaust gas buffer tank.

[0013] In one possible implementation, the exhaust gas absorption module includes a first exhaust gas absorption tower and a second exhaust gas absorption tower; the top of the second exhaust gas buffer tank is connected to the middle of the first exhaust gas absorption tower, and the top of the first exhaust gas absorption tower is connected to the middle of the second exhaust gas absorption tower.

[0014] In one possible implementation, a demister and an exhaust gas fan are also included; the demister is disposed between the second exhaust gas absorption tower and the exhaust gas fan; the input end of the demister is connected to the top of the second exhaust gas absorption tower, and the output end is connected to the exhaust gas fan; the exhaust gas discharged from the second exhaust gas absorption tower is demisted by the demister and then sent to the regenerative thermal oxidizer for treatment by the exhaust gas fan.

[0015] The beneficial effects of the inert gas protected reaction device provided by the present invention are as follows: Compared with the prior art, the inert gas protected reaction device of the present invention completes the raw material addition operation in a completely closed state, without the need to frequently open the reaction system for feeding and adding materials. This fundamentally avoids the problem of air and moisture being introduced into the reaction environment when the system is opened, and can maintain a stable inert gas protective atmosphere in the reaction components and feeding components at all times, fully meeting the stringent requirements of high-sensitivity chemical reactions for an oxygen-free environment.

[0016] The temperature sensor can capture the temperature changes inside the reactor in real time and feed back relevant information. The controller can flexibly adjust the feeding speed of the feeding component according to the real-time temperature, and can also adjust the working status of the jacket circulation cooling regulating valve as needed. This achieves precise control of the temperature inside the reactor during the feeding process, keeping the reaction temperature within a suitable range.

[0017] The intelligent temperature regulation combined with the continuous protection of inert gas ensures that the chemical reaction can proceed smoothly according to the preset process requirements, effectively avoids problems caused by abnormal temperature or damage to the system atmosphere, greatly improves the purity of the reaction products, and significantly enhances the controllability and stability of the entire reaction process.

[0018] The automated operation of feeding and temperature control has replaced the traditional manual control mode, reducing the errors and uncertainties caused by manual operation, lowering the labor costs in the production process, and making the operation process of chemical production simpler and more efficient, adapting to the needs of large-scale industrial production. Attached Figure Description

[0019] To more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0020] Figure 1 A schematic diagram of the structure of the inert gas protected reaction device provided in an embodiment of the present invention; Figure 2 This is a schematic diagram of the control process during the feeding of the inert gas protected reaction device provided in an embodiment of the present invention.

[0021] Explanation of reference numerals in the attached figures: 1. Inert gas buffer tank; 2. Feeding assembly; 3. Reactor; 4. Condenser; 5. Receiving tank; 6. First tail gas buffer tank; 7. Second tail gas buffer tank; 8. First tail gas absorption tower; 9. Second tail gas absorption tower; 10. Demister; 11. Tail gas fan. Detailed Implementation

[0022] To make the technical problems to be solved, the technical solutions, and the beneficial effects of the present invention clearer, the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the present invention and are not intended to limit the present invention.

[0023] Based on the embodiments in this application, all other embodiments obtained by those skilled in the art without inventive effort are within the scope of protection of this application.

[0024] It should be further noted that the accompanying drawings and embodiments of the present invention mainly describe the concept of the present invention. Based on this concept, some specific forms and arrangements of connection relationships, positional relationships, power mechanisms, power supply systems, hydraulic systems and control systems may not be fully described. However, under the premise that those skilled in the art understand the concept of the present invention, they can implement the above-mentioned specific forms and arrangements in a well-known manner.

[0025] When a component is referred to as being "fixed to" or "set on" another component, it can be directly on or indirectly on that other component. When a component is referred to as being "connected to" another component, it can be directly connected to or indirectly connected to that other component.

[0026] In the description of this invention, "a plurality of" means two or more, and "several" means one or more, unless otherwise explicitly specified.

[0027] The directional terms "inner" and "outer" refer to the inner and outer contours of each component itself. The terms "length," "width," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," and "outer" indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on the present invention.

[0028] For ease of description, spatial relative terms such as "above," "on top of," "on the upper surface of," and "above" are used here to describe the spatial positional relationship between a device or feature and other devices or features, as shown in the figure. It should be understood that spatial relative terms are intended to... The invention includes different orientations of the device in use or operation, in addition to those described in the figures. For example, if a device in the figures is inverted, a device described as "above" or "on top of" other devices or structures will be positioned as "below" or "under" other devices or structures. Thus, the exemplary term "above" can include both "above" and "below". The device may also be positioned in other different ways, and the spatial relative descriptions used herein are interpreted accordingly. The terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of indicated technical features. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the invention, "a plurality of" means two or more, and "a number" means one or more, unless otherwise explicitly specified.

[0029] Reference Figures 1 to 2 The inert gas protected reaction apparatus provided by the present invention will now be described. The inert gas protected reaction apparatus includes a reaction vessel 3, a feeding assembly 2, an inert gas buffer tank 1, and a controller.

[0030] A temperature sensor is installed inside the reactor 3; a jacketed circulating cooling regulating valve is also installed in the reactor 3; the temperature sensor detects and outputs real-time temperature information inside the reactor 3; the jacketed circulating cooling regulating valve is used to reduce the temperature inside the reactor 3. A feeding assembly 2 is located at the top of the reactor 3 and communicates with it; the feeding assembly 2 is used to feed raw materials into the reactor 3. An inert gas buffer tank 1 is connected to both the feeding assembly 2 and the reactor 3; the inert gas buffer tank 1 provides inert gas to both the feeding assembly 2 and the reactor 3, thereby maintaining a protective atmosphere in both. A controller is communicatively connected to the temperature sensor, the jacketed circulating cooling regulating valve, and the feeding assembly 2; the controller is configured to: receive real-time temperature information; and adjust the feeding speed of the feeding assembly 2 or regulate the jacketed circulating cooling regulating valve based on the real-time temperature information during the feeding process of the feeding assembly 2.

[0031] In a preferred embodiment, the inert gas buffer tank 1 includes an inert gas inlet switch valve, an inert gas inlet regulating valve, a check valve, a pressure transmitter, and a control switch valve. The inert gas inlet regulating valve automatically adjusts according to the pressure transmitter reading to ensure that the pressure in the inert gas buffer tank 1 remains within a certain range. The feeding assembly 2 is connected to the top of the inert gas buffer tank 1 via a connecting pipe, and the connecting pipe is equipped with a switch valve, a regulating valve, and a pressure transmitter. The inert gas regulating valve of the feeding assembly 2 automatically adjusts according to the pressure transmitter reading to ensure that the pressure inside the feeding assembly 2 remains within a certain range.

[0032] When the pressure in inert gas buffer tank 1 is above the high limit, the control valve automatically opens; when the pressure is below the high limit, the control valve closes. Simultaneously, the inert gas regulating valve in inert gas buffer tank 1 automatically adjusts its opening according to the pressure, ensuring a stable supply of inert gas to the buffer tank. The feeding assembly 2 is connected to the upper part of inert gas buffer tank 1, and the connecting pipeline is equipped with a switch valve, regulating valve, and pressure transmitter. Based on the feeding speed, the opening of the inert gas regulating valve is adjusted to maintain a slightly positive pressure inert gas protective atmosphere in the feeding assembly 2's hopper. The inert gas buffer tank 1 is connected to the lower pipeline of the feeding assembly 2, and is equipped with a switch valve and check valve. In case of difficulty or blockage in feeding the lower part of the feeding assembly 2, it is preferable to close the feeding valve above the reactor 3, open the control valve of the feeding assembly 2, and open the inert gas valve on the pipeline from inert gas buffer tank 1 to the lower part of the feeding assembly 2. This allows gas to clear the feeding end of the feeding assembly 2 without causing inert gas overflow, ensuring the safety of operators.

[0033] The inert gas protected reaction device operates based on a fully sealed inert atmosphere. Relying on the coordinated operation of the reactor 3, feeding assembly 2, inert gas buffer tank 1, and controller, it achieves automated feeding and precise control of the reaction temperature. The overall process is a continuous operation consisting of initial inert atmosphere construction, sealed automated feeding and reaction start-up, and dynamic adaptive temperature control. After the device starts, inert gas is first introduced into the feeding assembly 2 and reactor 3 from the inert gas buffer tank 1 to replace the air inside the assemblies, establishing and maintaining a stable sealed inert protective atmosphere within the feeding assembly 2 and reactor 3. Simultaneously, the temperature sensor initializes and enters real-time monitoring mode, the controller initializes its parameters, establishes communication connections with the temperature sensor, jacket circulating cooling regulating valve, and feeding assembly 2, confirming normal response from each actuator. The jacket circulating cooling regulating valve remains initially closed, and the feeding assembly 2 enters a ready-to-feed state, preparing for the subsequent reaction.

[0034] After the initial preparation is completed, the controller sends a feeding command to the feeding component 2. The feeding component 2 quantitatively feeds the reaction raw materials into the reactor 3 through the connecting channel at the top of the reactor 3. The entire feeding process is kept completely sealed. The inert gas buffer tank 1 continuously replenishes inert gas to the feeding component 2 and the reactor 3 to ensure that the internal inert protective atmosphere is not destroyed. After the raw materials enter the reactor 3, the chemical reaction is started immediately. The internal temperature of the reactor 3 changes dynamically with the reaction process. The temperature sensor continuously detects the real-time temperature inside the reactor 3 and converts the temperature signal into real-time temperature information, which is continuously transmitted to the controller to provide real-time data support for subsequent temperature control.

[0035] During the feeding and reaction process, the controller, as the core control unit, continuously receives real-time temperature information from the temperature sensor. Based on this information, it adaptively adjusts the feeding speed of the feeding component 2 or the working state of the jacket circulating cooling regulating valve to achieve precise control of the internal temperature of the reactor 3. If the real-time temperature inside the reactor 3 is within the preset suitable range and there is no abnormal upward trend, the controller will control the feeding component 2 to maintain the current feeding speed while keeping the jacket circulating cooling regulating valve closed. If the real-time temperature inside the reactor 3 rises with the feeding and reaction, and the temperature change reaches the preset control threshold, the controller will select the corresponding control method according to the process requirements. It may send a speed adjustment command to the feeding component 2 to reduce the feeding speed and slow down the raw material input rate to control the reaction exothermic rate, or send an opening command to the jacket circulating cooling regulating valve to open the regulating valve and put the reactor 3 jacket into circulating cooling mode, thereby reducing the internal temperature of the reactor 3 through jacket heat exchange.

[0036] The entire temperature control process is a dynamic closed-loop operation. The temperature sensor continuously provides real-time temperature information within reactor 3. The controller continuously adjusts the control commands based on real-time temperature changes. The feeding component 2 and the jacketed circulating cooling regulating valve respond and execute precisely according to the controller's commands in real time until the entire feeding process is completed, ensuring that the internal temperature of reactor 3 remains stable within the appropriate range required by the process. All components maintain a closed and interconnected working state throughout the process. The inert gas buffer tank 1 continuously supplies inert gas to the feeding component 2 and reactor 3 to ensure the stability of the protective atmosphere. The controller achieves automated and precise control of feeding and temperature based on real-time temperature data, eliminating the need for manual intervention by opening the reaction system. This fundamentally meets the stringent requirements of highly sensitive chemical reactions for an anhydrous and oxygen-free closed environment, while ensuring the controllability and stability of the reaction process.

[0037] In one possible implementation, during the feeding process of the feeding component 2, the feeding speed of the feeding component 2 is adjusted or the jacket circulation cooling regulating valve is adjusted based on real-time temperature information, including: The rate of temperature rise inside reactor 3 is calculated based on real-time temperature information. The temperature rise rate is compared with the rise rate threshold. If the temperature rise rate is higher than the rise rate threshold, the feeding component 2 is controlled to reduce the feeding speed or open the jacket circulation cooling regulating valve; otherwise, the feeding component 2 is controlled to maintain the current feeding speed or the jacket circulation cooling regulating valve is not opened.

[0038] The controller calculates the rate of temperature rise inside reactor 3 based on real-time temperature information, upgrading the basis for temperature control from a single temperature value to a dynamic rate of change. By comparing the rate of temperature rise with a preset threshold for control decisions, the triggering of feeding speed adjustments and cooling operations becomes more precise and rational, avoiding ineffective control. Maintaining the current feeding speed and closing the cooling valve when the rate of temperature rise does not exceed the threshold ensures the efficiency of the reaction and reduces unnecessary energy consumption. When the rate of temperature rise exceeds the threshold, promptly reducing the feeding speed or opening the cooling valve can quickly suppress abnormal temperature increases, controlling the rate of exothermic reaction from the source. Precise dynamic control ensures that the temperature inside reactor 3 remains stable, avoiding the adverse effects of sudden temperature increases on the reaction system and products. This further improves the stability of the reaction process, ensuring that the chemical reaction always proceeds under controllable process conditions and guaranteeing consistent product quality.

[0039] In a preferred embodiment, the temperature rise rate threshold is set to 2℃ / h, and the temperature rise rate should be stable at 1-2℃ / h. When the temperature rise rate is higher than 2℃ / h, it indicates that the temperature rise rate inside the reactor 3 is too high, and the temperature rise rate inside the reactor 3 should be reduced. This can be achieved by reducing the feeding rate to decrease the heat generated by the reaction or by opening the jacket circulation cooling regulating valve to improve the heat dissipation efficiency of the reactor 3, thereby reducing the rise rate to below 2℃ / h.

[0040] It should be noted that the above-mentioned rate of increase threshold values ​​are illustrative only and not fixed values. They are determined based on the required temperature range and feeding time. For example, if the required temperature range for the reaction is 40-88℃ and the feeding time is 24 hours, then the rate of increase threshold for the internal temperature of reactor 3 should be 2℃ / h. Those skilled in the art can adjust the rate of increase threshold adaptively according to actual production conditions.

[0041] In one possible implementation, the reactor 3 is also equipped with an emergency cooling valve; the controller is communicatively connected to the emergency cooling valve and is configured as follows: When the real-time temperature information is higher than the temperature safety threshold, the feeding component 2 is controlled to stop feeding and the emergency cooling valve is controlled to open.

[0042] The installation of the emergency cooling valve adds an independent emergency protection layer to the temperature control of reactor 3, forming a dual temperature protection system of conventional cooling and emergency cooling. When the temperature inside reactor 3 exceeds the safety threshold, the controller can quickly control the feeding component 2 to stop feeding, fundamentally cutting off the raw material supply to the reaction and slowing down the continuous increase in exothermic reaction. Simultaneously, the controller opens the emergency cooling valve, activating a rapid cooling mechanism to efficiently cool reactor 3 and quickly curb the continued temperature rise. Timely emergency operation effectively reduces the risk of material overflow caused by excessively rapid feeding, significantly improving the safety and reliability of the unit's operation. This allows the unit to have rapid response and emergency handling capabilities in the face of sudden temperature anomalies, adapting to the complex operating conditions in chemical production.

[0043] In one possible implementation, a pressure sensor is installed inside the reactor 3, and an emergency control valve is installed on the reactor 3; the pressure sensor is configured to detect and output real-time pressure information inside the reactor 3; the controller is communicatively connected to the pressure sensor and the emergency control valve, and is configured to: Receive real-time pressure information; The real-time pressure information is compared with the pressure safety threshold. If the real-time pressure information is higher than the safety threshold, the feeding component 2 is controlled to stop feeding and the emergency control valve is controlled to open; otherwise, the feeding component 2 is controlled to continue feeding and the emergency control valve is controlled to close.

[0044] The pressure sensor can detect pressure changes inside reactor 3 in real time and provide accurate pressure information, filling the gap in the device's pressure monitoring of the reaction system and achieving dual parameter monitoring of temperature and pressure. The linkage between the emergency control valve and the controller establishes a dedicated pressure emergency control mechanism for the reaction system, allowing the device to take targeted measures to deal with pressure anomalies.

[0045] When the pressure inside reactor 3 exceeds the safety threshold, the controller promptly stops feeding via the feeding component 2 to prevent further pressure increases caused by continuous raw material input. Simultaneously, the controller opens the emergency control valve to quickly release excess pressure within reactor 3, allowing the system pressure to rapidly return to a safe range. This effectively prevents safety accidents such as reactor 3 leakage, equipment deformation, or even explosions caused by excessive pressure, ensuring the safety of personnel and equipment at the production site. It also prevents disturbances to the reaction system caused by abnormal pressure, avoiding reaction imbalances and product structure damage due to sudden pressure changes, ensuring the normal progress of the reaction. The dual monitoring and control system for temperature and pressure provides more comprehensive control over the device, further enhancing the controllability and stability of the reaction process.

[0046] In one possible implementation, a receiving tank 5 and a condenser 4 are also included; an inert gas buffer tank 1 is connected to the receiving tank 5 to provide an inert gas protective atmosphere to the receiving tank 5; the inlet of the condenser 4 is connected to the top of the reactor 3, and the outlet is connected to the top of the receiving tank 5.

[0047] The upper part of the reactor 3 is connected to the upper part of the condenser 4 through an inlet, and a first switching valve, a second switching valve, and a temperature transmitter are provided between the reactor 3 and the condenser 4. The lower part of the condenser 4 is connected to the upper part of the receiving tank 5; the upper part of the receiving tank 5 is connected to the inert gas buffer tank 1 through a pipeline, and an inert gas switching valve and a check valve are provided in the pipeline between the upper part of the receiving tank 5 and the inert gas buffer tank 1.

[0048] Condenser 4 rapidly condenses the steam discharged from the top of reactor 3, effectively separating reaction products from gaseous materials and improving product collection efficiency. Inert gas buffer tank 1 provides a continuous inert gas protective atmosphere for receiving tank 5, ensuring a consistently anhydrous and oxygen-free environment. This effectively prevents oxidation and hydrolysis of the distillation-separated products within receiving tank 5, guaranteeing that the purity and quality of the products are not negatively affected. The inert gas protection between the distillation separation and reaction stages forms a closed loop, ensuring a stable inert protective atmosphere throughout the entire process from reaction to product collection. The integrated design allows the reaction and distillation operations to be completed within the same sealed device, eliminating the need for material transfer and preventing losses and contamination caused by contact with air during material transfer. This reduces intermediate steps in the process, improves overall production efficiency, and lowers material loss and production costs.

[0049] In one possible implementation, the system further includes an exhaust gas buffer module and an exhaust gas absorption module; the exhaust gas buffer module is connected to the receiving tank 5 and is used to condense the exhaust gas discharged from the receiving tank 5; the exhaust gas absorption module is connected to the exhaust gas buffer module and is used to absorb materials in the exhaust gas that are soluble in water or react with water.

[0050] In one possible implementation, the exhaust gas buffer module includes a first exhaust gas buffer tank 6 and a second exhaust gas buffer tank 7, with the top of the first exhaust gas buffer tank 6 connected to the receiving tank 5, and the top of the second exhaust gas buffer tank 7 connected to the top of the first exhaust gas buffer tank 6.

[0051] In one possible implementation, check valves are provided between the receiving tank 5 and the inert gas buffer tank 1, between the receiving tank 5 and the first tail gas buffer tank 6, and between the first tail gas buffer tank 6 and the second tail gas buffer tank 7.

[0052] In a preferred embodiment, the upper part of the receiving tank 5 is connected to the upper part of the first exhaust gas buffer tank 6 via a pipe, and a check valve is provided on the pipe connecting the upper part of the receiving tank 5 and the upper part of the first exhaust gas buffer tank 6. The upper part of the first exhaust gas buffer tank 6 is connected to the upper part of the second exhaust gas buffer tank 7 via a pipe, and a check valve is provided on the pipe connecting the upper part of the first exhaust gas buffer tank 6 and the upper part of the second exhaust gas buffer tank 7.

[0053] In one possible implementation, the exhaust gas absorption module includes a first exhaust gas absorption tower 8 and a second exhaust gas absorption tower 9; the top of the second exhaust gas buffer tank 7 is connected to the middle of the first exhaust gas absorption tower 8, and the top of the first exhaust gas absorption tower 8 is connected to the middle of the second exhaust gas absorption tower 9.

[0054] In a preferred embodiment, the upper part of the second tail gas buffer tank 7 is connected to the middle part of the first tail gas absorption tower 8, and a differential pressure detector is provided thereon; the upper part of the first tail gas absorption tower 8 is connected to the middle part of the second tail gas absorption tower 9. The first tail gas absorption tower 8 is equipped with a first circulation pump, and the second tail gas absorption tower 9 is equipped with a second circulation pump. Both the first tail gas absorption tower 8 and the second tail gas absorption tower 9 contain absorbent liquid for absorbing tail gas. The first circulation pump sprays the absorbent liquid from the bottom of the first tail gas absorption tower 8 onto the top of the first tail gas absorption tower 8, thereby absorbing substances in the tail gas that are soluble in water, react with water, or react with the effective components in the absorbent liquid. The second circulation pump sprays the absorbent liquid from the bottom of the second tail gas absorption tower 9 onto the top of the second tail gas absorption tower 9, thereby absorbing substances in the tail gas that are soluble in water, react with water, or react with the effective components in the absorbent liquid.

[0055] In one possible implementation, a demister 10 and an exhaust gas fan 11 are also included; the demister 10 is disposed between the second exhaust gas absorption tower 9 and the exhaust gas fan 11; the input end of the demister 10 is connected to the top of the second exhaust gas absorption tower 9, and the output end is connected to the exhaust gas fan 11; the exhaust gas discharged from the second exhaust gas absorption tower 9 is demisted by the demister 10 and then sent to the regenerative thermal oxidizer for treatment by the exhaust gas fan 11.

[0056] The beneficial effects of the inert gas protected reaction device provided by this invention are as follows: Compared with the prior art, the inert gas protected reaction device of this invention completes the addition of raw materials in a completely closed state. The inert gas buffer tank 1 continuously provides inert gas to the feeding component 2 and the reaction vessel 3, maintaining a stable protective atmosphere and completely avoiding the introduction of air and moisture, thus meeting the stringent requirements of high-sensitivity chemical reactions for an anhydrous and oxygen-free environment. The temperature sensor detects the temperature inside the reaction vessel 3 in real time, and the controller adjusts the feeding speed of the feeding component 2 or regulates the jacket circulation cooling regulating valve according to the real-time temperature information. It can also calculate the temperature rise rate and compare it with the threshold to achieve precise control. The emergency cooling valve stops feeding and quickly cools down when the temperature exceeds the safe threshold. The pressure sensor and emergency control switch valve enable timely handling of pressure abnormalities. Multiple controls ensure that the temperature and pressure inside the reaction vessel 3 are always within a safe range, ensuring the smooth progress of the reaction.

[0057] The system is equipped with a condenser 4 and a receiving tank 5 to achieve distillation and separation. The receiving tank 5 is also protected by an inert gas buffer tank 1 to prevent product oxidation and hydrolysis, thereby improving product purity and collection efficiency. The tail gas buffer module performs staged condensation of the tail gas to achieve secondary material recovery. The tail gas absorption module absorbs soluble materials in the tail gas in stages, and a check valve prevents backflow of gas and material, ensuring the normal operation of all components. The demister 10 removes tail gas droplets, and the tail gas fan 11 transports the tail gas to the incinerator for harmless treatment. The entire process integrates reaction, distillation, and tail gas treatment, with automated operation replacing manual control, reducing operational errors, minimizing labor and material losses, improving production efficiency and operational stability, and making it suitable for large-scale industrial production.

[0058] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

[0059] It should be noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the exemplary embodiments according to this application. As used herein, the singular form is intended to include the plural form as well, unless the context clearly indicates otherwise. Furthermore, it should be understood that when the terms "comprising" and / or "including" are used in this specification, they indicate the presence of features, steps, operations, devices, components, and / or combinations thereof.

[0060] Unless otherwise specifically stated, the relative arrangement, numerical expressions, and values ​​of the components and steps described in these embodiments do not limit the scope of this application. It should also be understood that, for ease of description, the dimensions of the various parts shown in the drawings are not drawn to actual scale. Techniques, methods, and devices known to those skilled in the art may not be discussed in detail, but where appropriate, such techniques, methods, and devices should be considered part of the specification. In all examples shown and discussed herein, any specific values ​​should be interpreted as merely exemplary and not as limitations. Therefore, other examples of exemplary embodiments may have different values. It should be noted that similar reference numerals and letters in the following drawings denote similar items; therefore, once an item is defined in one drawing, it need not be further discussed in subsequent drawings.

Claims

1. A reaction apparatus protected by an inert gas, characterized in that, include: The reactor is equipped with a temperature sensor inside; the reactor is also equipped with a jacketed circulating cooling regulating valve; the temperature sensor is used to detect and output real-time temperature information inside the reactor; the jacketed circulating cooling regulating valve is used to reduce the temperature inside the reactor. A feeding assembly is disposed at the top of the reactor and communicates with the reactor; the feeding assembly is used to feed raw materials into the reactor. An inert gas buffer tank is connected to both the feeding assembly and the reactor; the inert gas buffer tank is used to supply inert gas to the feeding assembly and the reactor, thereby maintaining a protective atmosphere in the feeding assembly and the reactor. The controller is communicatively connected to the temperature sensor, the jacket circulating cooling regulating valve, and the feeding assembly; the controller is configured to: Receive the real-time temperature information; During the feeding process of the feeding component, the feeding speed of the feeding component is adjusted or the jacket circulation cooling regulating valve is adjusted according to the real-time temperature information.

2. The inert gas protected reaction apparatus as described in claim 1, characterized in that, During the feeding process of the feeding component, adjusting the feeding speed of the feeding component or adjusting the jacket circulating cooling regulating valve according to the real-time temperature information includes: The rate of temperature rise inside the reactor is calculated based on the real-time temperature information. The temperature rise rate is compared with a rise rate threshold. If the temperature rise rate is higher than the rise rate threshold, the feeding component is controlled to reduce the feeding speed or open the jacket circulation cooling regulating valve; otherwise, the feeding component is controlled to maintain the current feeding speed or not open the jacket circulation cooling regulating valve.

3. The inert gas protected reaction apparatus as described in claim 2, characterized in that, The reactor is also equipped with an emergency cooling valve; the controller is communicatively connected to the emergency cooling valve and is configured to: When the real-time temperature information is higher than the temperature safety threshold, the feeding component is controlled to stop feeding and the emergency cooling valve is controlled to open.

4. The inert gas protected reaction apparatus as described in claim 3, characterized in that, A pressure sensor is installed inside the reactor, and an emergency control valve is installed on the reactor. The pressure sensor is configured to detect and output real-time pressure information inside the reactor. The controller is communicatively connected to the pressure sensor and the emergency control valve, and is configured to: Receive the real-time pressure information; The real-time pressure information is compared with the pressure safety threshold. If the real-time pressure information is higher than the safety threshold, the feeding component is controlled to stop feeding and the emergency control valve is controlled to open; otherwise, the feeding component is controlled to continue feeding and the emergency control valve is controlled to close.

5. The inert gas protected reaction apparatus as described in any one of claims 1 to 4, characterized in that, It also includes a receiving tank and a condenser; the inert gas buffer tank is connected to the receiving tank and is used to provide an inert gas protective atmosphere to the receiving tank; the condenser inlet is connected to the top of the reactor and the outlet is connected to the top of the receiving tank.

6. The inert gas protected reaction apparatus as described in claim 5, characterized in that, It also includes an exhaust gas buffer module and an exhaust gas absorption module; the exhaust gas buffer module is connected to the receiving tank and is used to condense the exhaust gas discharged from the receiving tank; the exhaust gas absorption module is connected to the exhaust gas buffer module and is used to absorb materials in the exhaust gas that are soluble in water and react with water.

7. The inert gas protected reaction apparatus as described in claim 6, characterized in that, The exhaust gas buffer module includes a first exhaust gas buffer tank and a second exhaust gas buffer tank. The top of the first exhaust gas buffer tank is connected to the receiving tank, and the top of the second exhaust gas buffer tank is connected to the top of the first exhaust gas buffer tank.

8. The inert gas protected reaction apparatus as described in claim 7, characterized in that, Check valves are provided between the receiving tank and the inert gas buffer tank, between the receiving tank and the first exhaust gas buffer tank, and between the first exhaust gas buffer tank and the second exhaust gas buffer tank.

9. The inert gas protected reaction apparatus as described in claim 7, characterized in that, The exhaust gas absorption module includes a first exhaust gas absorption tower and a second exhaust gas absorption tower; the top of the second exhaust gas buffer tank is connected to the middle of the first exhaust gas absorption tower, and the top of the first exhaust gas absorption tower is connected to the middle of the second exhaust gas absorption tower.

10. The reaction apparatus under inert gas protection as described in claim 9, characterized in that, It also includes a demister and an exhaust gas fan; the demister is disposed between the second exhaust gas absorption tower and the exhaust gas fan; the input end of the demister is connected to the top of the second exhaust gas absorption tower, and the output end is connected to the exhaust gas fan; The exhaust gas discharged from the second exhaust gas absorption tower is demisted by the demister and then sent to the regenerative thermal oxidizer by the exhaust gas fan.

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