Grignard reactor
By using a sectional temperature-controlled heating mechanism and a stirring mechanism in the Grignard reactor, the problem of insufficient temperature control accuracy of traditional Grignard reactors is solved, and more stable reaction progress and higher safety are achieved.
Patent Information
- Application Number
- CN202421285458.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-06-06
- Publication Date
- 2025-02-21
- Estimated Expiration
- 2034-06-06
AI Technical Summary
Traditional Grignard reactors have insufficient accuracy in temperature control, and they have the risk of explosion, which cannot meet the strict temperature control needs.
A Grignard reactor is designed, adopting a sectional temperature-controlled heating mechanism, including a first heater, a second heater and a third heater, which is sequentially connected along the height of the reaction tube, and is passed through a stirring mechanism and heat exchange The channel realizes uniform heating and temperature control of the reaction liquid.
The accuracy of temperature control is improved, energy accumulation caused by uninitiated reactions and rapid exothermic heat after severe initiation are avoided, and the stable progress of the reaction is ensured.
Smart Images
Figure CN222510954U_ABST
Abstract
Description
Technical Field
[0001] The utility model belongs to the technical field of chemical equipment, in particular to a Grignard reactor. Background Art
[0002] Grignard reactor refers to equipment for preparing Grignard reagents, which are generally prepared by chemical reactions between organic halogen compounds and magnesium metal. Its chemical principle is that magnesium atoms and carbon chains are directly connected, and carbon atoms exhibit negative electrical properties under the effect of polarization. The reaction process needs to be kept free of water and oxygen, and the initiation temperature and reaction temperature must be precisely controlled.
[0003] In order to reach the temperature required for the reaction, the traditional Grignard reactor usually has a heating device installed on the periphery of the reactor, such as winding a heating tube around the periphery of the reactor and using the heating tube to heat the reactor. Since the preparation of Grignard reagents requires strict temperature control accuracy, there is a risk of explosion once strong heat occurs. Therefore, the traditional Grignard reactor obviously cannot meet the demand for precise temperature control. Therefore, it is particularly important to further improve the structure of the Grignard reactor. Utility Model Content
[0004] Based on the above background, the purpose of the utility model is to provide a Grignard reactor to improve the accuracy of temperature control and ensure stable reaction.
[0005] In order to achieve the above objectives, the utility model adopts the following technical solutions:
[0006] A Grignard reactor comprises: a reaction tube, with a first inlet and a second inlet and a discharge port respectively provided at both ends; a feeding mechanism connected with the first inlet and used for feeding magnesium powder into the reaction tube, and the second inlet is used for introducing raw material liquid; a heating mechanism comprising a first heater, a second heater and a third heater, the first heater, the second heater and the third heater are sequentially sleeved outside the reaction tube along the height direction of the reaction tube, the first heater is close to the first inlet, the third heater is close to the second inlet, and the heating temperature of the third heater is higher than the heating temperature of the second heater; a stirring mechanism, at least partially located in the reaction tube, and used for stirring the raw material liquid and magnesium powder in the reaction tube.
[0007] Furthermore, the stirring mechanism includes a motor, a stirring component and a bearing. The stirring component is located in the reaction tube, and two ends of the stirring component are respectively installed on two ends of the reaction tube through the bearings. The motor is used to drive the stirring component to rotate.
[0008] Furthermore, the stirring assembly includes a rotating shaft and a plurality of stirring structures arranged on the rotating shaft, the two ends of the rotating shaft are respectively installed on the two ends of the reaction tube through the bearings, the rotating shaft has an axially penetrating heat exchange channel, the stirring structure has a diversion channel, and each of the diversion channels is connected to the heat exchange channel.
[0009] Furthermore, the stirring structure includes an upper stirring tube, a lower stirring tube and a connecting tube connected between the upper stirring tube and the lower stirring tube, the upper stirring tube, the connecting tube and the lower stirring tube define the diversion channel, the upper stirring tube and the lower stirring tube are both connected to the rotating shaft and are both connected to the heat exchange channel.
[0010] Furthermore, the lower stirring tube is located below the upper stirring tube, the upper stirring tube is inclined relative to the horizontal direction, and the end of the upper stirring tube away from the rotating shaft is set downward; the lower stirring tube is inclined relative to the horizontal direction, and the end of the lower stirring tube away from the rotating shaft is set upward.
[0011] Furthermore, the stirring mechanism also includes a first rotating joint and a second rotating joint, and the first rotating joint and the second rotating joint are respectively connected to two ends of the rotating shaft.
[0012] Furthermore, the stirring mechanism also includes a roller and a belt, one end of the stirring component extends out of the reaction tube, the roller is arranged on the part of the stirring component extending out of the reaction tube, and the belt is sleeved on the roller and the output shaft of the motor.
[0013] Furthermore, the first heater, the second heater and the third heater each include a heat exchange shell, an input pipe and an output pipe, the heat exchange shell is sleeved outside the reaction tube and forms a heat exchange cavity between the shell and the outer wall of the reaction tube, and the input pipe and the output pipe are both connected to the heat exchange cavity.
[0014] Furthermore, the feeding mechanism includes a hopper, a pushing assembly and a feeding pipe. The feeding pipe is connected between the hopper and the first inlet. At least part of the pushing assembly is located in the hopper for pushing the magnesium powder into the feeding pipe. The hopper is also used to connect to a nitrogen tank.
[0015] The utility model has the following beneficial effects:
[0016] (1) During the preparation of the Grignard reagent, magnesium powder is fed into the first inlet through the feeding mechanism, so that the magnesium powder enters the reaction tube and settles downward and disperses; at the same time, the raw material liquid is introduced into the second inlet, so that the raw material liquid is in a plug flow from bottom to top in the reaction tube, so that the reaction liquid gradually triggers the reaction from bottom to top. Since the first heater, the second heater and the third heater are sequentially arranged along the height direction of the outer side of the reaction tube, the heating mechanism can implement segmented temperature control according to the temperature requirements of different heights of the reaction tube, meet the precise control of different temperatures required for the reaction at different sections, improve the accuracy of temperature control, and ensure the stable reaction. Since the temperature of the third heater is higher than that of the second heater, the energy accumulation caused by the failure of the reaction to be initiated can be avoided, and the rapid heat release caused by the violent initiation can be avoided.
[0017] (2) The two ends of the stirring assembly are fixed to the two ends of the reaction tube through bearings to ensure that the stirring assembly can rotate smoothly in the reaction tube, thereby improving the stability of the reaction stirring.
[0018] (3) A heat exchange channel is provided in the rotating shaft, and a shunt channel is provided in the stirring structure, so that during the reaction process, heat transfer oil can be introduced into the heat exchange channel, so that the heat transfer oil can enter the shunt channel when flowing in the heat exchange channel, ensuring that the heat transfer oil is evenly distributed in the stirring component, so that the inside of the reaction liquid can also be effectively heated. At the same time, the rotation of the stirring component makes the internal heating more uniform. In addition, the channel is provided inside the stirring component, and the external heating mechanism is used, which not only makes the reaction liquid evenly heated, but also helps to further accurately control the reaction temperature and improve the stability of the reaction.
[0019] (4) The upper stirring tube and the lower stirring tube are designed to be inclined relative to the horizontal direction, and one end of the upper stirring tube is set downward, and one end of the lower stirring tube is set upward, so that the heat transfer oil in the heat exchange channel can easily enter the upper stirring tube, and then flow into the lower stirring tube through the connecting tube; finally, it flows back to the heat exchange channel from the lower stirring tube. This design ensures that the flow of heat transfer oil is smoother and avoids congestion of heat transfer oil flow and poor heat transfer. BRIEF DESCRIPTION OF THE DRAWINGS
[0020] In order to more clearly illustrate the embodiments of the utility model or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the utility model. For ordinary technicians in this field, other drawings can be obtained based on the structures shown in these drawings without paying creative work.
[0021] Figure 1 is a structural diagram of a Grignard reactor shown in one embodiment;
[0022] Figure 2 A structural diagram showing the coordination between a reaction tube and a stirring mechanism in one embodiment;
[0023] Figure 3 for Figure 2 A magnified view of the structure at the center circle A;
[0024] Figure 4 for Figure 2 A magnified view of the structure at the center circle B;
[0025] Figure 5 for Figure 2 Enlarged view of the structure at point C in the middle circle.
[0026] Description of Figure Numbers:
[0027] 100 is a Grignard reactor; 10 is a reaction tube; 11 is a first inlet; 12 is a second inlet; 13 is a discharge port; 20 is a feeding mechanism; 21 is a pushing assembly; 22 is a hopper; 23 is a feeding pipe; 30 is a heating mechanism; 31 is a first heater; 32 is a second heater; 33 is a third heater; 34 is a heat exchange shell; 35 is an input pipe; 36 is an output pipe; 37 is a heat exchange chamber; 40 is a stirring mechanism; 41 is a motor; 42 is a stirring assembly; 43 is a rotating shaft; 431 is a heat exchange channel; 44 is a stirring structure; 441 is a diversion channel; 442 is an upper stirring tube; 443 is a lower stirring tube; 444 is a connecting pipe; 45 is a roller; 46 is a belt; 47 is a bearing; 48 is a first rotary joint; 49 is a second rotary joint; 200 is a nitrogen tank.
[0028] The realization of the purpose, functional features and advantages of the utility model will be further explained in conjunction with embodiments and with reference to the accompanying drawings. DETAILED DESCRIPTION
[0029] The following will be combined with the drawings in the embodiments of the utility model to clearly and completely describe the technical solutions in the embodiments of the utility model. Obviously, the described embodiments are only part of the embodiments of the utility model, not all of the embodiments. Based on the embodiments of the utility model, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the utility model.
[0030] It should be noted that all directional indications in the embodiments of the present invention (such as up, down, left, right, front, back...) are only used to explain the relative position relationship, movement status, etc. between the components under a certain specific posture (as shown in the accompanying drawings). If the specific posture changes, the directional indication will also change accordingly.
[0031] In addition, in the present utility model, descriptions such as "first", "second", etc. are only used for descriptive purposes and cannot be understood as indicating or implying their relative importance or implicitly indicating the number of the indicated technical features. Therefore, the features defined as "first" and "second" may explicitly or implicitly include at least one of the features. In addition, the technical solutions between the various embodiments can be combined with each other, but they must be based on the ability of ordinary technicians in the field to implement them. When the combination of technical solutions is contradictory or cannot be implemented, it should be deemed that such a combination of technical solutions does not exist and is not within the scope of protection required by the present utility model.
[0032] In one embodiment, please refer to Figures 1 to 5 The present application provides a Grignard reactor 100, comprising: a reaction tube 10, a feeding mechanism 20, a heating mechanism 30 and a stirring mechanism 40. The reaction tube 10 has a first inlet 11 and a second inlet 12 and a discharge port 13 at both ends thereof. The feeding mechanism 20 is connected to the first inlet 11 for feeding magnesium powder into the reaction tube 10, and the second inlet 12 is used for passing raw material liquid. The heating mechanism 30 comprises a first heater 31, a second heater 32 and a third heater 33, which are sequentially sleeved outside the reaction tube 10 along the height direction of the reaction tube 10, the first heater 31 is close to the first inlet 11, the third heater 33 is close to the second inlet 12, and the heating temperature of the third heater 33 is higher than the heating temperature of the second heater 32. The stirring mechanism 40 is at least partially located in the reaction tube 10, and is used to stir the raw material liquid and magnesium powder in the reaction tube 10.
[0033] In the Grignard reactor 100, during the preparation of the Grignard reagent, magnesium powder is fed into the first inlet 11 through the feeding mechanism 20, so that the magnesium powder enters the reaction tube 10 and settles downward and disperses; at the same time, the raw material liquid is introduced into the second inlet 12, so that the raw material liquid is in a plug flow from bottom to top in the reaction tube 10, so that the reaction liquid gradually triggers the reaction from bottom to top. Since the first heater 31, the second heater 32 and the third heater 33 are sequentially arranged along the height direction of the outside of the reaction tube 10, the heating mechanism 30 can implement segmented temperature control according to the temperature requirements of different heights of the reaction tube 10, meet the precise control of different temperatures required for the reaction at different sections, improve the accuracy of temperature control, and ensure the stable reaction. Since the temperature of the third heater 33 is higher than that of the second heater 32, the energy accumulation caused by the failure of the reaction to be triggered can be avoided, and the rapid heat release caused by the violent triggering can be avoided.
[0034] It should be explained that, in order to achieve temperature control of the first heater 31 , the second heater 32 and the third heater 33 , temperature measuring devices, such as thermocouples, etc., may be respectively provided on the first heater 31 , the second heater 32 and the third heater 33 .
[0035] For further information, please refer to Figure 2 and Figure 3 The stirring mechanism 40 includes a motor 41, a stirring assembly 42 and a bearing 47. The stirring assembly 42 is located in the reaction tube 10, and the two ends of the stirring assembly 42 are respectively mounted on the two ends of the reaction tube 10 through the bearings 47. The motor 41 is used to drive the stirring assembly 42 to rotate. It can be seen that the two ends of the stirring assembly 42 are respectively fixed to the two ends of the reaction tube 10 through the bearings 47 to ensure that the stirring assembly 42 can rotate smoothly in the reaction tube 10, thereby improving the stability of the reaction stirring.
[0036] In one embodiment, please refer to Figure 2 , the stirring assembly 42 includes a rotating shaft 43 and a plurality of stirring structures 44 arranged on the rotating shaft 43, the two ends of the rotating shaft 43 are respectively installed at the two ends of the reaction tube 10 through bearings 47, the rotating shaft 43 has an axially penetrating heat exchange channel 431, the stirring structure 44 has a shunt channel 441, and each shunt channel 441 is connected to the heat exchange channel 431. It can be seen that the heat exchange channel 431 is arranged in the rotating shaft 43, and the shunt channel 441 is arranged in the stirring structure 44, so that during the reaction process, heat transfer oil can be introduced into the heat exchange channel 431, so that the heat transfer oil can enter the shunt channel 441 when flowing in the heat exchange channel 431, ensuring that the heat transfer oil is evenly distributed in the stirring assembly 42, so that the inside of the reaction liquid can also be effectively heated. At the same time, the rotation of the stirring assembly 42 is coordinated to make the internal heating more uniform. In addition, the channel is arranged inside the stirring assembly 42, and the external heating mechanism 30 is coordinated to not only make the reaction liquid evenly heated, but also facilitate further accurate control of the reaction temperature and improve the stability of the reaction.
[0037] For further information, please refer to Figure 4 The stirring structure 44 includes an upper stirring tube 442, a lower stirring tube 443 and a connecting tube 444 connecting the upper stirring tube 442 and the lower stirring tube 443. The upper stirring tube 442, the connecting tube 444 and the lower stirring tube 443 define a diversion channel 441. The upper stirring tube 442 and the lower stirring tube 443 are both connected to the rotating shaft 43 and are both connected to the heat exchange channel 431.
[0038] Specifically, the upper stirring tube 442 , the lower stirring tube 443 , the connecting tube 444 and the rotating shaft 43 are an integrated structure.
[0039] In one embodiment, please refer to Figure 4 The lower stirring tube 443 is located below the upper stirring tube 442, the upper stirring tube 442 is inclined relative to the horizontal direction, and the end of the upper stirring tube 442 away from the rotating shaft 43 is set downward. The lower stirring tube 443 is inclined relative to the horizontal direction, and the end of the lower stirring tube 443 away from the rotating shaft 43 is set upward.
[0040] It can be seen that the upper stirring tube 442 and the lower stirring tube 443 are both designed to be inclined relative to the horizontal direction, and one end of the upper stirring tube 442 is set downward, and one end of the lower stirring tube 443 is set upward, so that the heat transfer oil in the heat exchange channel 431 can easily enter the upper stirring tube 442, and then flow into the lower stirring tube 443 through the connecting tube; finally, it flows back from the lower stirring tube 443 to the heat exchange channel 431. Such a design ensures that the flow of the heat transfer oil is smoother and avoids the congestion of the heat transfer oil flow and causes poor heat conduction.
[0041] In one embodiment, please refer to Figure 3 and Figure 5 The stirring mechanism 40 further includes a first rotating joint 48 and a second rotating joint 49 , and the first rotating joint 48 and the second rotating joint 49 are respectively connected to two ends of the rotating shaft 43 .
[0042] The rotary joint refers to a pipe connection device, and the connected pipes can rotate relatively and can be used to transport various media such as gas, liquid, oil, etc. The compact design structure. In this embodiment, the first rotary joint 48 and the second rotary joint 49 are connected to the rotating shaft 43 respectively, which can ensure the entry and discharge of the heat transfer oil in the rotating shaft 43, and ensure that the pipes will not be entangled during the rotation of the rotating shaft 43, so as to ensure the stable reaction.
[0043] In one embodiment, the stirring mechanism 40 further includes a roller 45 and a belt 46. One end of the stirring component 42 extends out of the reaction tube 10. The roller 45 is disposed on the portion of the stirring component 42 extending out of the reaction tube 10. The belt 46 is sleeved on the roller 45 and the output shaft of the motor 41. It can be seen that the roller 45 and the belt 46 ensure that the stirring component 42 rotates stably.
[0044] In one embodiment, please refer to Figure 2 The first heater 31, the second heater 32 and the third heater 33 all include a heat exchange shell 34, an input pipe 35 and an output pipe 36. The heat exchange shell 34 is sleeved outside the reaction tube 10 and forms a heat exchange cavity 37 with the outer wall of the reaction tube 10. The input pipe 35 and the output pipe 36 are both connected to the heat exchange cavity 37. It can be seen that directly forming the heat exchange cavity 37 with the outer wall of the reaction tube 10 can increase the specific surface area of the reaction tube 10, improve the heat exchange efficiency, realize precise temperature control, and avoid the risk of loss of control caused by manual operation.
[0045] For further information, please refer to Figure 1 The feeding mechanism 20 includes a hopper 22, a pushing assembly 21 and a feeding pipe 23. The feeding pipe 23 is connected between the hopper 22 and the first inlet 11. At least part of the pushing assembly 21 is located in the hopper 22, which is used to push magnesium powder into the feeding pipe 23. The hopper 22 is also used to communicate with the nitrogen tank 200.
[0046] It should be explained that the hopper 22 is connected to the nitrogen tank 200. The purpose is that since magnesium powder has a relatively active chemical property, the magnesium powder can be protected by nitrogen to prevent the risk of combustion and explosion.
[0047] Meanwhile, the pushing component 21 refers to a device capable of pushing magnesium powder into the feeding tube 23. For example, the pushing component 21 can be a cylinder, a hydraulic cylinder or other device, and uses a telescopic function to push magnesium powder from the hopper 22 into the feeding tube 23. Among them, the feeding tube 23 can be tilted for the convenience of feeding. Of course, the magnesium powder can also smoothly enter the reaction tube 10 under the blowing of nitrogen.
[0048] Of course, the above description is not a limitation of the present invention, and the present invention is not limited to the above examples. Changes, modifications, additions or substitutions made by technicians in this technical field within the essential scope of the present invention should also fall within the protection scope of the present invention.
Claims
1. A Grignard reactor, characterized in that: include: A reaction tube (10) having a first inlet (11) and a second inlet (12) and a discharge port (13) located below the first inlet (11) at both ends; a feeding mechanism (20) connected to the first inlet (11) and used for feeding magnesium powder into the reaction tube (10); and a second inlet (12) for introducing raw material liquid; The heating mechanism (30) comprises a first heater (31), a second heater (32) and a third heater (33), wherein the first heater (31), the second heater (32) and the third heater (33) are sequentially sleeved outside the reaction tube (10) along the height direction of the reaction tube (10), the first heater (31) is close to the first inlet (11), the third heater (33) is close to the second inlet (12), and the heating temperature of the third heater (33) is higher than the heating temperature of the second heater (32); The stirring mechanism (40) is at least partially located in the reaction tube (10) and is used to stir the raw material liquid and magnesium powder in the reaction tube (10).
2. A Grignard reactor according to claim 1, characterized in that: The stirring mechanism (40) comprises a motor (41), a stirring component (42) and a bearing (47); the stirring component (42) is located in the reaction tube (10), and two ends of the stirring component (42) are respectively mounted on two ends of the reaction tube (10) via the bearings (47); the motor (41) is used to drive the stirring component (42) to rotate.
3. A Grignard reactor according to claim 2, characterized in that: The stirring assembly (42) comprises a rotating shaft (43) and a plurality of stirring structures (44) arranged on the rotating shaft (43); the two ends of the rotating shaft (43) are respectively mounted on the two ends of the reaction tube (10) through the bearings (47); the rotating shaft (43) has an axially penetrating heat exchange channel (431); the stirring structure (44) has a diversion channel (441); and each of the diversion channels (441) is connected to the heat exchange channel (431).
4. A Grignard reactor according to claim 3, characterized in that: The stirring structure (44) comprises an upper stirring tube (442), a lower stirring tube (443) and a connecting tube (444) connecting the upper stirring tube (442) and the lower stirring tube (443); the upper stirring tube (442), the connecting tube (444) and the lower stirring tube (443) define the diversion channel (441); the upper stirring tube (442) and the lower stirring tube (443) are both connected to the rotating shaft (43) and are both connected to the heat exchange channel (431).
5. A Grignard reactor according to claim 4, characterized in that: The lower stirring tube (443) is located below the upper stirring tube (442); the upper stirring tube (442) is inclined relative to the horizontal direction, and one end of the upper stirring tube (442) away from the rotating shaft (43) is arranged downward; the lower stirring tube (443) is inclined relative to the horizontal direction, and one end of the lower stirring tube (443) away from the rotating shaft (43) is arranged upward.
6. A Grignard reactor according to claim 3, characterized in that: The stirring mechanism (40) further comprises a first rotating joint (48) and a second rotating joint (49), wherein the first rotating joint (48) and the second rotating joint (49) are respectively connected to two ends of the rotating shaft (43).
7. A Grignard reactor according to claim 2, characterized in that: The stirring mechanism (40) further comprises a roller (45) and a belt (46); one end of the stirring component (42) extends out of the reaction tube (10); the roller (45) is arranged on the portion of the stirring component (42) extending out of the reaction tube (10); and the belt (46) is sleeved on the roller (45) and the output shaft of the motor (41).
8. A Grignard reactor according to any one of claims 1 to 7, characterized in that: The first heater (31), the second heater (32) and the third heater (33) all comprise a heat exchange shell (34), an input pipe (35) and an output pipe (36); the heat exchange shell (34) is sleeved on the outside of the reaction tube (10) and forms a heat exchange cavity (37) with the outer wall of the reaction tube (10); the input pipe (35) and the output pipe (36) are both connected to the heat exchange cavity (37).
9. A Grignard reactor according to any one of claims 1 to 7, characterized in that: The feeding mechanism (20) comprises a hopper (22), a pushing assembly (21) and a feeding pipe (23); the feeding pipe (23) is connected between the hopper (22) and the first inlet (11); at least a portion of the pushing assembly (21) is located in the hopper (22) and is used to push the magnesium powder into the feeding pipe (23); the hopper (22) is also used to communicate with a nitrogen tank (200).