A reaction system for organic peroxidation reactions

Abstract

The utility model discloses a kind of reaction systems for organic peroxidation, belong to chemical experiment equipment technical field.It includes reaction unit and stirring unit, reaction unit includes reaction cavity, it is used to accommodate reactant in it, stirring unit inserts reaction cavity, the reactant in reaction cavity is stirred, further include foam collecting unit, the foam collecting unit includes foam collection chamber, foam drainage pipe and foam trapping tank, the foam collection chamber is fixed in reaction cavity inner wall, foam drainage pipe one end communicates foam collection chamber inside, foam drainage pipe other end connects foam trapping tank, wherein, the nozzle of foam drainage pipe is towards the notch of foam trapping tank, reaction end line is set on foam collection chamber.The utility model aims at accurate judgment reaction end.

Description

Technical Field

[0001] This utility model belongs to the field of chemical experimental equipment technology, and more specifically, relates to a reaction system for organic peroxidation reaction. Background Technology

[0002] Peroxide-based initiators (such as benzoyl peroxide and methyl ethyl ketone peroxide) are widely used in polymerization reactions and organic synthesis, where temperature control is extremely critical in synthesis or small-scale experiments. Various temperature-controlled reaction devices exist; for example, Chinese patent application No. 202411723925.9, published on February 14, 2025, discloses a temperature-controlled reactor. This reactor includes a reactor body and a temperature control device. The reactor body comprises an inner shell and a jacket. The inner shell contains reactants, and the jacket is located on the outer surface of the inner shell. The temperature control device includes a receiving cavity for containing a temperature-controlled liquid, which connects to the jacket. The temperature control device drives the temperature-controlled liquid in the receiving cavity to flow into the jacket. A stirring device is installed in the jacket to agitate the temperature-controlled liquid, accelerating its flow within the jacket. This allows the temperature-controlled liquid in the jacket to quickly reach a suitable temperature, thereby changing the temperature of the inner shell to achieve the appropriate temperature. This ensures the reaction within the inner shell can proceed at the optimal temperature, improving processing efficiency and product quality. However, the determination of the reaction endpoint depends on the reaction time.

[0003] However, due to the unique nature of organic peroxidation reactions, the reaction process is influenced by multiple factors, including temperature control precision, ambient temperature, material mixing effects, and the rate of acyl chloride droplet acceleration. In particular, the small-scale reaction apparatus has limited material feed rates, making it difficult to achieve good reproducibility of the reaction rate and conversion process in each batch. This means that the reaction endpoint cannot generally be determined by time alone; otherwise, significant differences in conversion rates would occur, hindering effective systematic experimental verification. Currently, the industry typically determines the reaction endpoint by visually observing the amount of foam generated during the decomposition of excess raw materials at the end of the reaction. However, this method is not quantifiable and is highly subjective, thus hindering the effective conduct and data analysis of peroxide initiator synthesis experiments.

[0004] Therefore, there is an urgent need to design a reaction system for organic peroxidation reactions to achieve accurate determination of the reaction endpoint. Summary of the Invention

[0005] 1. The problem to be solved

[0006] The purpose of this invention is to provide a reaction system for organic peroxidation reactions, which aims to accurately determine the reaction endpoint.

[0007] 2. Technical Solution

[0008] To solve the above problems, the technical solution adopted by this utility model is as follows:

[0009] A reaction system for an organic peroxidation reaction includes a reaction unit and a stirring unit. The reaction unit includes a reaction chamber for containing reactants. The stirring unit is inserted into the reaction chamber to stir the reactants. The system also includes a foam collection unit, which comprises a foam collection chamber, a foam guide pipe, and a foam trapping tank. The foam collection chamber is fixed to the inner wall of the reaction chamber. One end of the foam guide pipe connects to the interior of the foam collection chamber, and the other end connects to the foam trapping tank. The outlet of the foam guide pipe faces the outlet of the foam trapping tank. A reaction endpoint line is provided on the foam collection chamber. In operation, foam enters the foam collection chamber from the foam trapping tank via the foam guide pipe through an airflow.

[0010] A foam collection unit is installed at the bottom of the end cap on the inner wall of the reaction chamber. During the final stage of the organic peroxidation reaction, the foam generated will mainly concentrate at the stirring pump (stirring center) due to stirring inertia. At this time, the foam is continuously collected. The foam collection tank is funnel-shaped, and the foam drainage pipe is at a 60° angle to the bottom of the foam collection chamber, connecting the foam collection tank and the foam collection chamber. Due to the rotational inertia of the foam in the reaction chamber, after being collected by the foam collection tank, the foam enters the foam collection chamber through the foam drainage pipe. There is a verified foam liquid level line at the reaction endpoint in the foam collection chamber. During the experiment, it is only necessary to observe the foam liquid level in the foam collection chamber to determine whether the reaction has reached the endpoint, so as to achieve quantitative control of the reaction endpoint.

[0011] In one possible embodiment of this invention, the ratio of the volume of the foam collection chamber to the volume of the reaction chamber is 1:(4~6); preferably, the ratio is 1:5. The reaction endpoint is located at one-third of the volume of the foam collection chamber.

[0012] In one possible embodiment of this utility model, the stirring unit includes a stirring motor, a stirring shaft, and at least one dispersion disk. The stirring motor is located outside the reaction unit, the stirring shaft is inserted into the reaction chamber, and the stirring motor is electrically connected to the stirring shaft to control the rotation of the stirring shaft. The dispersion disk is fixed on the stirring shaft and is used to disperse the reactants.

[0013] In one possible embodiment of this utility model, the shortest distance between the outer surface of the foam collecting tank and the outer surface of the stirring shaft is 'a', and the distance between the outer surface of the foam collecting tank and the initial liquid level of the reactants in the reaction chamber is 'b', where a:b = (1~3):1. Preferably, a:b = 2:1. The initial liquid level of the reactants in the reaction chamber refers to the liquid level before heating for the peroxidation reaction begins after the reactants are added.

[0014] As one possible embodiment of this utility model, the shortest distance between the outer surface of the foam collection tank and the outer surface of the stirring shaft is at least 2 cm.

[0015] As one possible implementation of this utility model, the shortest distance between the outer surface of the foam collection tank and the outer surface of the stirring shaft is controlled within 3 cm.

[0016] In one possible embodiment of this utility model, at least two dispersion discs are provided, each with a different diameter, and they are concentrically fixed on the stirring shaft. The diameter of each dispersion disc increases sequentially from top to bottom along the stirring shaft. This double-layer dispersion disc structure significantly improves material flowability, reduces dead zones in the stirring process, and, combined with the heat exchange of the jacketed circulation channel, makes the temperature distribution of the reaction system more uniform.

[0017] In one possible implementation of this invention, several guide holes are provided around the periphery of the dispersion disk near its edge. The combination of the upper and lower dispersion disks with different diameters and the guide hole design enhances the material shear force and turbulence intensity, accelerates heat transfer, and avoids uneven local temperatures.

[0018] In one possible embodiment of this invention, the reaction unit is composed of an outer layer and an inner layer nested together, with a circulation channel formed between the outer and inner layers. The inner layer space forms a reaction chamber, wherein a circulating liquid is introduced into the circulation channel to heat or cool the reactants in the reaction chamber. Preferably, the inner and outer layers are made of high-borosilicate glass, which is resistant to high temperatures and corrosion, and facilitates observation of the experimental process. The circulation channel prevents direct contact between the coolant and the materials, improving experimental safety.

[0019] As one possible embodiment of this utility model, it also includes a temperature control unit, which includes several temperature electrodes and a temperature adjustment device. Temperature electrodes are inserted into the circulation channel and the reaction chamber respectively, and the temperature signals generated by the temperature electrodes are transmitted to the temperature adjustment device. The temperature adjustment device is a high and low temperature integrated machine, which is used to heat or cool the temperature-controlled liquid and transport it into the circulation channel to form a circulation loop.

[0020] As one possible implementation of this utility model, the temperature electrode uses a platinum resistance temperature sensor with an accuracy of ±0.1℃ to collect temperature data in real time at high frequency.

[0021] As one possible implementation of this utility model, the temperature control device delivers the temperature-controlled liquid to the pipe of the circulation channel, sets up a temperature electrode, and transmits the temperature signal to the temperature control device.

[0022] 3. Beneficial effects

[0023] Compared with the prior art, the beneficial effects of this utility model are as follows:

[0024] This invention relates to a reaction system for organic peroxidation reactions that can quantitatively determine the reaction endpoint, solving the problem of subjective determination of the reaction endpoint in existing devices and achieving a high degree of consistency in repeated experimental results under the same formula. Simultaneously, it features rapid temperature control, high temperature control accuracy, and excellent stirring effect. Attached Figure Description

[0025] Figure 1 This is a schematic diagram of the reaction system used in the organic peroxidation reaction of this utility model;

[0026] Figure 2 This is a schematic diagram of the foam collection unit in the reaction system for organic peroxidation reaction of this utility model;

[0027] In the picture:

[0028] 1. Reaction unit; 11. Outer layer; 12. Circulation channel; 13. Inner layer; 14. Reaction chamber; 21. Stirring motor; 22. Stirring shaft; 23. Dispersion disc; 231. First dispersion disc; 232. Second dispersion disc; 3. Foam collection unit; 31. Foam collection chamber; 32. Foam drainage pipe; 33. Foam collection tank; 4. Temperature control unit; 41. Temperature electrode; 42. Temperature adjustment device. Detailed Implementation

[0029] To make the objectives, technical solutions, and advantages of the embodiments of this utility model clearer, the technical solutions of the embodiments of this utility model will be clearly described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this utility model, not all embodiments. Based on the embodiments of this utility model, all other embodiments obtained by those skilled in the art without creative effort are within the protection scope of this utility model.

[0030] Example

[0031] like Figure 1 As shown, a reaction system for an organic peroxidation reaction according to this embodiment includes a reaction unit 1, a stirring unit, a foam collection unit 3, and a temperature control unit 4. The reaction unit 1 is used to contain reactants for an organic reaction, such as a peroxidation reaction. The stirring unit provides stirring force to the reactants within the reaction unit 1, ensuring sufficient contact between the reactants and increasing reaction efficiency. The foam collection unit 3 is fixed inside the reaction unit 1 and is used to collect bubbles generated on the surface of the organic reaction liquid, determining whether the reaction has reached its endpoint based on the amount of bubbles collected. The temperature control unit 4 provides a heat source and cooling for the reaction in the reaction unit 1.

[0032] Specifically, the reaction unit 1 is composed of an outer layer 11 and an inner layer 13 made of high borosilicate glass. The outer layer 11 and the inner layer 13 form a circulation channel 12, and the space of the inner layer 13 forms a reaction chamber 14. An inlet is provided at the top, and an outlet and a discharge valve are provided at the bottom. Cold and hot circulating liquids are introduced into the circulation channel 12 to cool or heat the reaction materials in the reaction chamber 14.

[0033] The stirring unit includes a stirring motor 21, a stirring shaft 22, and at least one dispersion disk 23. The stirring motor 21 is located outside the reaction unit 1, and the stirring shaft 22 is inserted into the reaction chamber 14. The stirring motor 21 is electrically connected to the stirring shaft 22 to drive its rotation. The dispersion disk 23 is fixed on the stirring shaft 22 and is used to disperse the reactants. At least two dispersion disks 23 are provided. In this embodiment, a first dispersion disk 231 and a second dispersion disk 232 are concentrically fixed on the stirring shaft 22. The vertical distance between the first dispersion disk 231 and the second dispersion disk 232 is 5-10 cm. The diameter of the first dispersion disk 231 is 1 / 2-3 / 4 of the diameter of the second dispersion disk 232, and the diameter of the second dispersion disk 232 is 1 / 2-2 / 3 of the inner diameter of the reaction chamber 14. To improve the shear force of the dispersion disk on the material, accelerate heat transfer, and avoid uneven local temperature, several guide holes (not shown in the attached drawings) are provided around the periphery of each dispersion disk 23 near the edge.

[0034] Foam collection unit 3, such as Figure 2 As shown, the system includes a foam collection chamber 31, a foam drainage pipe 32, and a foam collection tank 33. In operation, the foam generated by the reaction enters the foam collection chamber 31 from the foam collection tank 33 via the foam drainage pipe 32 through an airflow. The specific structure is as follows:

[0035] The foam collection chamber 31 is fixed to the inner wall of the reaction chamber 14, and the volume ratio of the foam collection chamber 31 to the volume of the reaction chamber 14 is 1:(4~6); in this embodiment, the volume ratio of the foam collection chamber 31 to the volume of the reaction chamber 14 is set to 1:5. The reaction endpoint line is located at one-third of the volume of the foam collection chamber 31.

[0036] One end of the foam drainage tube 32 is connected to the inside of the foam collection chamber 31, and the other end of the foam drainage tube 32 is connected to the foam trapping tank 33. The opening of the foam drainage tube 32 faces the opening of the foam trapping tank 33, and a reaction endpoint line is set on the foam collection chamber 31.

[0037] The shortest distance between the outer surface of the foam trap 33 and the outer surface of the stirring shaft 22 is 'a', and the distance between the outer surface of the foam trap 33 and the initial liquid level of the reactants in the reaction chamber 14 is 'b', where a:b = (1~3):1. In this embodiment, the shortest distance between the outer surface of the foam trap 33 and the outer surface of the stirring shaft 22 is set to 2 cm, and the distance between the outer surface of the foam trap 33 and the initial liquid level of the reactants in the reaction chamber 14 is set to 1 cm. The initial liquid level of the reactants in the reaction chamber 14 refers to the liquid level before heating for peroxidation reaction begins after the reactants are added.

[0038] The temperature control unit 4 includes several temperature electrodes 41 and a temperature regulating device 42. The circulation channel 12 has an inlet and an outlet, which are respectively connected to the temperature regulating device 42 to form a circulation loop. The temperature regulating device 42 is a commercially available high and low temperature integrated machine, such as the high and low temperature integrated machine produced by Maipu, used to heat or cool the circulating fluid and transport it into the circulation channel 12. Temperature electrodes 41 are inserted into the circulation channel 12, the reaction chamber 14, and the pipes of the circulation loop, and the temperature signals generated by the temperature electrodes 41 are transmitted to the high and low temperature integrated machine. Temperature electrodes 41 are also installed in the circulating fluid in the high and low temperature integrated machine for temperature measurement as needed. In this embodiment, the temperature electrodes 41 are selected from platinum resistance temperature sensors with an accuracy of ±0.1℃.

[0039] The present invention and its embodiments have been described above illustratively. This description is not restrictive, and the figures shown are only one embodiment of the present invention; the actual structure is not limited thereto. Therefore, if those skilled in the art are inspired by this description and design similar structures and embodiments without departing from the inventive spirit of the present invention, such designs should fall within the protection scope of the present invention.

Claims

1. A reaction system for an organic peroxidation reaction, comprising a reaction unit (1) and a stirring unit, wherein the reaction unit (1) includes a reaction chamber (14) for containing reactants, and the stirring unit is inserted into the reaction chamber (14) to stir the reactants within the reaction chamber (14), characterized in that: It also includes a foam collection unit (3), which includes a foam collection chamber (31), a foam drainage pipe (32), and a foam trapping tank (33). The foam collection chamber (31) is fixed to the inner wall of the reaction chamber (14). One end of the foam drainage pipe (32) is connected to the inside of the foam collection chamber (31), and the other end of the foam drainage pipe (32) is connected to the foam trapping tank (33). The opening of the foam drainage pipe (32) faces the opening of the foam trapping tank (33). A reaction endpoint line is set on the foam collection chamber (31).

2. The reaction system for an organic peroxidation reaction according to claim 1, characterized in that: The ratio of the volume of the foam collection chamber (31) to the volume of the reaction chamber (14) is 1:(4~6), and the reaction endpoint is located at one-third of the volume of the foam collection chamber (31).

3. The reaction system for an organic peroxidation reaction according to claim 2, characterized in that: The stirring unit includes a stirring motor (21), a stirring shaft (22), and at least one dispersion disk (23). The stirring motor (21) is located outside the reaction unit (1), the stirring shaft (22) is inserted into the reaction chamber (14), and the stirring motor (21) is electrically connected to the stirring shaft (22) to control the rotation of the stirring shaft (22). The dispersion disk (23) is fixed on the stirring shaft (22) and is used to disperse the reactants.

4. The reaction system for an organic peroxidation reaction according to claim 3, characterized in that: The shortest distance between the outer surface of the foam collecting tank (33) and the outer surface of the stirring shaft (22) is a, and the distance between the outer surface of the foam collecting tank (33) and the initial liquid surface of the reactants in the reaction chamber (14) is b, where a:b=(1~3):

1.

5. The reaction system for an organic peroxidation reaction according to claim 4, characterized in that: The ratio of the volume of the foam collection chamber (31) to the volume of the reaction chamber (14) is 1:5; a:b=2:

1.

6. The reaction system for an organic peroxidation reaction according to claim 3, characterized in that: The dispersion disk (23) is provided in at least two, and the diameters of the dispersion disks (23) are different. They are concentrically fixed on the stirring shaft (22). The diameters of the dispersion disks (23) increase sequentially from top to bottom along the stirring shaft (22).

7. The reaction system for an organic peroxidation reaction according to claim 6, characterized in that: The dispersion disk (23) has several guide holes arranged around its periphery near the edge.

8. A reaction system for an organic peroxidation reaction according to any one of claims 1 to 7, characterized in that: The reaction unit (1) is formed by connecting an outer layer (11) and an inner layer (13). The outer layer (11) and the inner layer (13) form a circulation channel (12), and the space of the inner layer (13) forms a reaction chamber (14). The circulation channel (12) is filled with circulating liquid to heat or cool the reactants in the reaction chamber (14).

9. The reaction system for an organic peroxidation reaction according to claim 8, characterized in that: It also includes a temperature control unit (4), which includes several temperature electrodes (41) and a temperature adjustment device (42). Temperature electrodes (41) are inserted into the circulation channel (12) and the reaction chamber (14) respectively, and the temperature signal generated by the temperature electrodes (41) is transmitted to the temperature adjustment device (42). The temperature adjustment device (42) is a high and low temperature integrated machine, used to heat or cool the temperature-controlled liquid and transport it to the circulation channel (12) to form a circulation loop.

10. The reaction system for an organic peroxidation reaction according to claim 9, characterized in that: The temperature control device (42) delivers the temperature-controlled liquid to the pipe of the circulation channel (12) and also provides a temperature electrode (41) and transmits the temperature signal to the temperature control device (42).

Images