Reaction mixing device for synthesizing isocaprylic acid by oxygen oxidation method

Abstract

The utility model belongs to the technical field of isocaprylic acid synthesis, and particularly relates to a reaction mixing device for synthesizing isocaprylic acid through an oxygen oxidation method. The utility model provides a reaction mixing device for synthesizing isocaprylic acid by an oxygen oxidation method, which comprises a cylindrical reactor main body, a plurality of ultrasonic generator nodes, a raw material feeding pipeline, a gas feeding pipeline, a product discharging pipeline, a waste discharging pipeline, a mechanical stirring device, an exhaust pipeline, an intelligent injection system, a sensor system and a central controller, the ultrasonic technology and the multi-stage intelligent injection system are integrated, so that the solubility of oxygen in a liquid phase is remarkably improved, and the reaction rate is increased.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of isooctanoic acid synthesis, and particularly relates to a reaction mixing device for synthesizing isooctanoic acid by an oxygen oxidation method. BACKGROUND

[0002] The synthesis of isooctanoic acid by an oxygen oxidation method is a chemical process that converts specific precursor substances into isooctanoic acid by using oxygen or air as an oxidizing agent. This production method does not require the use of toxic or harmful oxidizing agents, and is favored in the chemical industry due to its environmental friendliness, high selectivity and high efficiency. Isooctanoic acid, as an important organic compound, has a wide range of applications in plastic plasticizers, perfumes and pharmaceuticals. In order to realize this conversion process, a reaction mixing device is needed that can ensure sufficient contact between oxygen and reactants, and maintain appropriate temperature, pressure and stirring conditions. The design of such devices is crucial to improving reaction rates, product selectivity and the quality of the final product.

[0003] At present, there are various types of reactors on the market for the synthesis of isooctanoic acid by an oxygen oxidation method, including but not limited to stirred tank reactors, fixed bed reactors and fluidized bed reactors. These devices each have unique advantages: stirred tank reactors, with their simple structural design and easy operation, are the preferred choice for laboratory research and small-scale production; fixed bed reactors, due to their high energy utilization efficiency and excellent thermal stability, are widely used in large-scale industrial production; and fluidized bed reactors, with their excellent mass transfer performance and high reaction rate, are particularly suitable for situations that require rapid reactions.

[0004] However, despite the excellent performance of these reactors in their respective application ranges, they each face some challenges and limitations. Although stirred tank reactors perform well in many aspects, one of the main problems they face in practical applications is the low solubility of oxygen in the liquid phase. This is because the interaction between oxygen molecules and water or other organic solvents is weak, resulting in very limited natural solubility of oxygen in these media. Traditional stirring methods can only provide a certain degree of shear force to promote bubble breakage and gas dispersion, but this is far from enough to overcome the problem of low oxygen solubility. Especially when dealing with larger volumes of reactant materials, the effective transfer efficiency of oxygen will be significantly reduced, which not only limits the reaction rate, but also can cause the oxygen concentration in local areas to be too high or too low, thereby triggering unnecessary side reactions or reducing the selectivity of the target product.

[0005] In addition, the lower oxygen solubility also leads to a longer reaction time, increasing energy consumption and production costs. Moreover, due to the uneven distribution of oxygen throughout the reaction system, some areas may overreact, while other areas may not react enough, further affecting the consistency of product quality. Therefore, how to effectively improve the solubility and dispersion of oxygen in the liquid phase is one of the key technical problems to be solved in the improvement process of the stirred tank reactor. Utility content

[0006] To solve the above problems, the present application provides a reaction mixing device for synthesizing iso-octanoic acid by oxygen oxidation method, which significantly improves the solubility of oxygen in the liquid phase by combining ultrasonic technology and multi-stage intelligent injection system, and promotes the reaction rate.

[0007] The present application provides a reaction mixing device for synthesizing iso-octanoic acid by oxygen oxidation method, which includes a cylindrical reactor body as the core container of the entire reaction, providing a closed environment for chemical reactions, ensuring that the reaction proceeds under controlled conditions, preventing external factors from interfering with the reaction process, and facilitating accurate control of temperature, pressure and other parameters. A plurality of ultrasonic generator nodes are distributed longitudinally along the reactor body, each node containing at least one rotatable ultrasonic transducer head and being connected to an external power source and control system through a waterproof cable. These ultrasonic generator nodes increase the solubility of oxygen and promote mass transfer between gas and liquid through cavitation effects generated by ultrasonic waves, significantly improving the solubility of oxygen in the liquid phase, reducing bubble size, and thus improving reaction efficiency and product selectivity. In particular, the ultrasonic transducer head is designed in a conical shape, concentrating ultrasonic energy and enhancing cavitation effects, further improving the solubility of oxygen and promoting effective contact between gas and liquid phase.

[0008] The feed system includes a raw material feed pipeline and a gas feed pipeline, which are respectively connected to the top of the reactor body for introducing iso-octanol raw materials and oxygen or air into the reactor, ensuring uniform distribution of raw materials and gas, ensuring continuous supply of raw materials and gas, reducing operational difficulty and manual intervention, and improving production efficiency. The discharge system includes a product discharge pipeline and a waste discharge pipeline, which are respectively located at the bottom of the reactor body for collecting generated iso-octanoic acid products and discharging waste generated during the reaction, achieving efficient collection of products and timely discharge of waste, reducing product loss and environmental pollution.

[0009] The mechanical stirring device is installed inside the reactor, forming a circulating flow pattern through the stirring paddle, promoting the thorough mixing of liquid and gas, improving the mixing effect of the liquid, promoting the breaking and dispersion of gas bubbles, increasing the contact area between oxygen and liquid phase, and improving the solubility and mass transfer efficiency of oxygen.

[0010] An exhaust pipe is arranged at the top of the reactor to discharge the gas not involved in the reaction, maintain the pressure balance in the reactor, ensure the stable pressure in the reactor, and prevent safety hazards caused by gas accumulation.

[0011] The intelligent injection system is configured with multiple circular micro-hole nozzles per layer. The nozzles are connected to the main gas supply pipeline through flexible pipes, which are provided with valves and flow meters. The micro-hole nozzles generate fine bubbles, increasing the contact area between oxygen and the liquid phase. The flanges and sealing washers ensure tight connection and prevent leakage. The circular micro-hole nozzles have a pore size ranging from 0.1 mm to 0.5 mm. Each injection port is equipped with a small flange connected to the flexible pipe through a sealing washer, which improves the oxygen solubility, reduces oxygen waste, and ensures the safety and stability of the system.

[0012] The flexible pipes are made of high-temperature-resistant, pressure-resistant, and flexible materials such as polytetrafluoroethylene (PTFE). The high-temperature-resistant and pressure-resistant materials ensure reliability in harsh working conditions. The good flexibility facilitates installation and maintenance, prolongs the service life of the equipment, reduces maintenance costs, and improves the reliability and safety of the system.

[0013] The number of ultrasonic generator nodes is 3-5 layers, and 4-6 ultrasonic transmitters are uniformly arranged around the reactor per layer. The multi-level and uniform distribution of ultrasonic generator nodes ensures the generation of a uniform ultrasonic field in the entire reactor, improves the oxygen solubility and mass transfer efficiency, reduces local over-oxidation, and improves the reaction selectivity and product quality.

[0014] The intelligent injection system is configured with 3-5 layers, each layer having 3-5 injection ports arranged in a ring shape to ensure uniform distribution of oxygen in the entire reactor, improve the oxygen solubility, promote effective contact between oxygen and the liquid phase, and improve the reaction efficiency and product selectivity.

[0015] The sensor system includes but is not limited to temperature sensors, oxygen concentration sensors, and pH sensors, which are arranged on the inner wall of the reactor to monitor key parameters such as temperature, oxygen concentration, and pH in real time. The data is fed back to the central controller for adjustment, achieving precise monitoring and control of the reaction process, improving reaction consistency and product quality.

[0016] The central controller integrates ultrasonic power adjustment module, injection port flow control module, and data analysis and processing unit. According to the data feedback from the sensors, the parameters such as ultrasonic power and injection port flow are dynamically adjusted to optimize the reaction conditions. Through intelligent control, the reaction efficiency and product selectivity are improved, and human error is reduced.

[0017] This application significantly improves the solubility of oxygen in the liquid phase and promotes the reaction rate by combining ultrasonic technology with a multi-stage intelligent injection system. The multi-stage intelligent injection system ensures uniform oxygen distribution throughout the reaction system, avoiding localized over-oxidation and improving reaction selectivity and product purity. Automated control, through a central controller and sensor system, enables real-time monitoring and dynamic adjustment of reaction conditions, improving production efficiency and product quality. The user interface provides an intuitive operating platform, facilitating remote access and parameter adjustment by operators, reducing operational complexity. Furthermore, by optimizing reaction conditions, unnecessary energy consumption and byproduct generation are reduced, aligning with the trend of green chemistry. These improvements not only solve the problem of low oxygen solubility in traditional stirred tank reactors but also significantly enhance the overall process efficiency and economy. Attached Figure Description

[0018] Figure 1 A schematic diagram of the reaction mixing apparatus for the synthesis of isooctanoic acid by oxygen oxidation.

[0019] Figure 2 This is a schematic diagram of the stirring device structure of the reaction mixing apparatus for the synthesis of isooctanoic acid by oxygen oxidation.

[0020] Figure 3 This is a schematic diagram of the cooling system structure of the reaction mixing apparatus for the synthesis of isooctanoic acid by oxygen oxidation.

[0021] In the diagram: 1. Reactor body; 21. Ultrasonic transmitter; 71. Raw material feed pipe; 72. Gas feed pipe; 81. Product discharge pipe; 82. Waste discharge pipe; 9. Mechanical stirring device; 10. Exhaust pipe; 31. Micro-orifice nozzle; 32. Flexible pipe; 33. Main gas supply pipe; 4. Sensor system; 5. Central controller; 101. Jacket; 102. Inner coil; 1021. Inner coil outlet; 1022. Inner coil inlet. Detailed Implementation

[0022] like Figures 1-2 As shown, in the reaction mixing apparatus for the synthesis of isooctanoic acid via the oxygen oxidation of isooctyl alcohol, the cylindrical reactor body 1 is made of corrosion-resistant material, ensuring long-term stability and uniform liquid flow. The feeding system includes a raw material feed pipe 71 and a gas feed pipe 72, which introduce reactants into the top of the reactor via pumps and compressors, respectively, ensuring that reactants enter the reaction system as needed and maintaining the continuity and stability of the reaction. The discharge system includes an isooctanoic acid product discharge pipe 81 and a waste discharge pipe 82, located at the bottom of the reactor, facilitating product collection and waste treatment, achieving effective separation and collection of products, and maintaining the cleanliness of the reactor interior.

[0023] The mechanical stirring device 9 is installed inside the reactor, generating shear force through rotating blades to break bubbles and promote gas-liquid contact, thereby enhancing mixing effect and improving oxygen utilization efficiency. The mechanical stirring device 9 adopts double-layer stirring paddles. The upper stirring paddle adopts a turbine-type stirring paddle with blades arranged radially, and 4-6 blades are configured. The turbine-type stirring paddle has strong shear force, can effectively push the liquid to the container wall, and form strong turbulence on the liquid surface, which helps the dispersion and dissolution of gas. The lower stirring paddle adopts a propeller-type stirring paddle with propeller-shaped blades, and 3-5 blades are configured. The propeller-type stirring paddle can generate significant axial thrust to push the liquid upward from the bottom, forming a circulating flow, reducing the dead angle area in the reactor, and ensuring uniform distribution of liquid and gas in the entire reaction system. The stirring paddles are connected to the driving motor through the central shaft. The central shaft is made of high-strength stainless steel or titanium alloy material to ensure sufficient rigidity and corrosion resistance. The central shaft is fixed to the reactor top support frame through the bearing and extends to the reactor bottom for installing the upper and lower stirring paddles. The coupling is placed between the motor and the central shaft, and elastic coupling or diaphragm coupling is used to compensate for the slight deviation between the central shaft and the motor, reduce vibration and noise. The upper stirring paddle is fixed in the middle position of the central shaft by bolts or buckles to ensure its stability and facilitate disassembly and maintenance; the lower stirring paddle is fixed at the lower end of the central shaft by bolts or welding, close to the reactor bottom, to ensure that it can effectively push the liquid at the bottom to flow upward.

[0024] The mechanical stirring device 9 is equipped with a variable frequency motor, which can adjust the stirring speed according to different stages of the reaction process. For example, a higher speed can be set in the initial stage of the reaction to quickly disperse the gas, and the speed can be reduced in the later stage of the reaction to avoid excessive shearing. The central controller 5 adjusts the motor speed in real time according to the data feedback by the sensor to adapt to different mixing needs. In addition, dynamic balance calibration is performed on the stirring paddles during installation to ensure that excessive vibration and noise are not generated during operation. To further reduce vibration transmission to the reactor body 1 structure, a damping pad or spring is installed at the bottom of the reactor.

[0025] The working principle of the double-layer stirring paddle is that the upper turbine-type stirring paddle pushes the liquid towards the container wall, forming a radial flow; the lower propeller-type stirring paddle pushes the liquid upwards from the bottom, forming an axial flow. The two work together to build a complete circulating flow pattern, ensuring uniform distribution of the liquid throughout the reactor. This circulating flow pattern not only improves the mixing effect of the liquid, but also promotes the breaking and dispersion of gas bubbles, increasing the contact area between oxygen and the liquid phase, thereby improving the oxygen solubility and mass transfer efficiency. The high-speed rotating stirring paddle exerts shear force on the gas bubbles, breaking them into smaller bubbles. At the same time, the circulating flow pattern helps to evenly distribute these small bubbles in the liquid, avoiding local over-oxidation. Small bubbles have a larger specific surface area, which can dissolve into the liquid phase faster, thereby increasing the oxygen solubility. In addition, the uniform distribution of bubbles is beneficial to the full contact between reactants, improving the reaction efficiency.

[0026] Temperature sensors and oxygen concentration sensors are installed at different heights inside the reactor to monitor the changes of key parameters in real time. The central controller 5 adjusts the stirring speed and oxygen supply based on the data feedback from the sensors, ensuring the best reaction conditions. For example, a higher stirring speed can be set at the beginning of the reaction to quickly disperse the gas, while the stirring speed is reduced at the later stage of the reaction to avoid excessive shear. This precise control helps to improve the consistency of the reaction and the quality of the product.

[0027] The exhaust pipe 10 is arranged at the top of the reactor to discharge the gas that does not participate in the reaction through the pressure difference, maintain the pressure balance inside the reactor, and prevent overpressure phenomenon.

[0028] Multiple ultrasonic generator nodes are distributed at different heights along the longitudinal direction of the reactor, each node containing at least one rotatable ultrasonic emitter head 21 and connected to the external power supply and control system through waterproof cables. The ultrasonic emitter head 21 adopts a conical design, with the front end gradually narrowing to form a sharp tip, which helps to concentrate energy and improve cavitation effect; the emitter head is connected to the fixed support through a ball joint, which facilitates flexible adjustment of direction. These ultrasonic generators form micro-bubbles through high-frequency vibration, significantly improving the oxygen solubility in the liquid phase and promoting the reaction rate.

[0029] The multi-layer intelligent injection system is equipped with multiple circular micro-hole nozzles 31 on each layer. These nozzles are connected to the main gas supply pipeline 33 through flexible pipes 32, and are provided with valves and flow meters to accurately control the gas supply amount of each injection port. The circular micro-hole nozzles 31 have a pore size range of 0.1mm to 0.5mm, with the specific size determined by experiments; each injection port is equipped with a small flange, which is tightly connected to the flexible pipe 32 through a sealing gasket to prevent leakage. The flexible pipe 32 is made of materials such as polytetrafluoroethylene, which has good flexibility and is resistant to high temperature and pressure, ensuring uniform distribution of oxygen in the entire reaction system, avoiding local over-oxidation, and improving reaction selectivity.

[0030] The sensor system 4 includes temperature sensors, oxygen concentration sensors, and pH value sensors distributed at different positions inside the reactor. Each sensor is connected to the central controller 5 through a waterproof joint to ensure the safety and stability of signal transmission. The central controller 5 is integrated with an ultrasonic power adjustment module, a jet port flow control module, and a data analysis and processing unit, which automatically adjusts the operating parameters according to the sensor data, optimizes the reaction conditions, and improves the oxygen utilization efficiency and reaction rate. The user interface provides a touch screen or computer software interface for the operator to view the running state and make necessary adjustments, allowing remote access and adjustment of various parameters, improving the operation convenience.

[0031] The reaction mixing device provided by the present application also includes a cooling system, which includes a jacket 101 and an inner coil 102. The jacket 101 is arranged outside the reactor body 1 and surrounds the reactor body 1. By introducing a cooling medium such as cooling water or refrigerant into the jacket 101, the heat generated during the reaction process can be effectively absorbed and removed from the outside, thereby controlling the reaction temperature. The jacket 101 shell is made of stainless steel material with good corrosion resistance, ensuring that it will not fail due to chemical corrosion during long-term use. The jacket 101 shell is provided with a cooling medium inlet and a cooling medium outlet for convenient introduction or replacement of the cooling medium. The inner coil 102 is installed inside the reactor and can be a spiral or serpentine pipe. The inner coil 102 is also provided with an inner coil outlet 1021 and an inner coil inlet 1022. The cooling medium is introduced from the inner coil inlet 1022, removes the heat inside the reactor in the pipe, and then exits from the inner coil outlet 1021. The inner coil 102 can directly absorb heat from the inside of the reaction liquid to achieve higher cooling efficiency. The inner coil 102 is also made of stainless steel or other high-temperature and pressure-resistant metal materials to ensure its sufficient strength and stability in high-temperature and high-pressure environments. Through the double cooling mechanism of the jacket 101 and the inner coil 102, a large amount of heat generated during the reaction process can be quickly and effectively removed, maintaining the temperature stability of the reaction system and preventing problems such as side reactions or catalyst deactivation caused by overheating. Stable temperature control helps to reduce the thermal stress damage of the equipment caused by temperature fluctuations, prolongs the service life of the equipment, and reduces maintenance costs.

[0032] In use, first check all components are working properly, ensure that the feed system, exhaust duct 10, sensor system 4 and central controller 5 are in standby state. Then through the feed system to introduce isooctanol and oxygen into the reactor. Mechanical stirring device 9 starts to work, to promote the preliminary mixing of isooctanol and oxygen; ultrasonic generator node starts, increase the solubility of oxygen. Multilayer intelligent injection system uniformly distributes oxygen, ensures the reaction under the best conditions; sensor system 4 real-time monitoring of key parameters, central controller 5 according to feedback data automatically adjusts the operating parameters. Finally through the discharge system to collect the generated isooctanoic acid, discharge waste, stop feeding and stirring, close the ultrasonic generator and injection system, discharge the remaining gas, clean the reactor.

Claims

1. A reaction mixing apparatus for synthesizing isooctanoic acid by oxygen oxidation, characterized in that, The application relates to a reaction mixing device for synthesizing iso-octanoic acid by an oxygen oxidation method, which comprises the following parts: a cylindrical reactor body (1) in which a plurality of ultrasonic generator nodes are longitudinally distributed, each node comprising at least one rotatable ultrasonic emission head (21) and being connected to an external power supply and control system through a waterproof cable; a feeding system comprising a raw material feeding pipeline (71) and a gas feeding pipeline (72) which are respectively connected to the top of the reactor body (1); a discharging system comprising a product discharging pipeline (81) and a waste discharging pipeline (82) which are respectively arranged at the bottom of the reactor body (1); a mechanical stirring device (9) arranged in the reactor; an exhaust pipeline (10) arranged at the top of the reactor; an intelligent spraying system comprising a plurality of circular micro-hole nozzles (31) which are connected to a main gas supply pipeline (33) through flexible pipelines (32) provided with valves and flow meters; a sensor system (4) comprising but not limited to temperature sensors, oxygen concentration sensors and pH value sensors which are arranged on the inner wall of the reactor; and a central controller (5) integrated with an ultrasonic power adjusting module, a spraying port flow control module and a data analysis processing unit.

2. The reaction mixing device for synthesizing iso-octanoic acid by an oxygen oxidation method according to claim 1, wherein the ultrasonic emission head (21) is conical.

3. The reaction mixing device for synthesizing iso-octanoic acid by an oxygen oxidation method according to claim 1, wherein the circular micro-hole nozzle (31) has a pore size ranging from 0.1 mm to 0.5 mm, and each spraying port is provided with a small flange connected to the flexible pipeline (32) through a sealing gasket.

4. The reaction mixing device for synthesizing iso-octanoic acid by an oxygen oxidation method according to claim 1, wherein the flexible pipeline (32) is made of polytetrafluoroethylene.

5. The reaction mixing device for synthesizing iso-octanoic acid by an oxygen oxidation method according to claim 1, wherein the ultrasonic generator nodes are arranged in 3-5 layers, and each layer is uniformly arranged with 4-6 ultrasonic emission heads (21) around the circumference of the reactor.

6. The reaction mixing device for synthesizing iso-octanoic acid by an oxygen oxidation method according to claim 1, wherein the intelligent spraying system is arranged in 3-5 layers, and each layer is arranged with 3-5 micro-hole nozzles (31) which are arranged in a ring shape along the inner wall of the reactor body. ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​

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