Solid-liquid reactor
By designing a vertical solid-liquid reactor, the problems of low production efficiency and spillage risk in batch reactor processes were solved, enabling efficient continuous production of Grignard reagents and improved reaction rates.
Patent Information
- Application Number
- CN202423247427.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-27
- Publication Date
- 2025-12-05
- Estimated Expiration
- 2034-12-27
AI Technical Summary
Existing batch reactor processes for preparing Grignard reagents suffer from problems such as low production efficiency, high risk of reaction liquid overflow, and doping of unreacted magnesium metal into the product.
A vertical solid-liquid reactor is adopted, designed with an upper buffer chamber and a lower reaction chamber for continuous feeding and discharging. A stirring assembly and baffles are set up to control the contact area and heat transfer effect of the solid and liquid phases and prevent overflow.
It achieves efficient and continuous production, avoids overflow of reaction liquid, improves reaction rate and heat transfer efficiency, and reduces subsequent filtration steps.
Smart Images
Figure CN223628632U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model relates to chemical reactor technical field, concretely relates to a solid liquid reactor. BACKGROUND
[0002] Grignard reagent is generally prepared by reaction of magnesium powder, magnesium chips and halogenated hydrocarbon, which belongs to solid-liquid reaction, and at present, batch tank process is mostly used. The main problems of preparing Grignard reagent by using batch tank process are as follows: (1) Grignard reaction needs to be initiated, and when using batch process, initiation is needed every time of feeding, so the production efficiency is low; (2) In order to ensure the stirring effect, the amount of materials in the tank is large, and the filling coefficient is high, but the Grignard reaction releases heat violently when initiated, and violent boiling may occur, and when the reaction liquid violently boils, the materials are easy to overflow; (3) In the production by using batch tank process, in order to ensure the reaction rate, the magnesium metal is generally slightly excessive, and usually the reaction product flows out from the discharge port at the bottom of the tank body after the reaction is completed, and the magnesium metal which is not completely reacted is mixed in the reaction product, so it needs to be removed by filtration in the subsequent process steps, which makes the production process more complicated. SUMMARY
[0003] In order to solve the above technical problems, the utility model provides a solid liquid reactor, which only needs to be initiated once during production, and can realize continuous feeding and continuous production after initiation, so the production efficiency is high, and the reaction liquid will not overflow during violent boiling in the production process, and the reaction product does not need to be filtered.
[0004] In order to achieve the above purpose, the utility model adopts the technical solving scheme of:
[0005] A solid liquid reactor is vertically placed, and comprises a reactor cylinder and a stirring assembly arranged in the reactor cylinder.
[0006] The inner cavity of the reactor cylinder is divided into an upper buffer cavity and a lower reaction cavity which are in communication, a solid phase feeding port is arranged on the upper part of the outer wall of the reactor cylinder and communicates with the upper buffer cavity, an overflow discharge port is arranged on the middle part of the outer wall of the reactor cylinder and communicates with the upper part of the lower reaction cavity, and a liquid phase feeding port is arranged on the lower part of the outer wall of the reactor cylinder and communicates with the lower part of the lower reaction cavity.
[0007] The stirring assembly comprises a rotating shaft and a plurality of stirring blades arranged in the lower part of the rotating shaft in the axial direction, the upper end of the rotating shaft extends out of the reactor cylinder, the stirring blades are arranged in the lower reaction cavity of the reactor cylinder, and the uppermost stirring blade is located below the overflow discharge port.
[0008] Preferably, the volume of the upper buffer cavity of the reactor cylinder is 2-3 times that of the lower reaction cavity.
[0009] Preferably, the length-diameter ratio of the lower reaction cavity of the reactor cylinder is 2-3.
[0010] Preferably, a plurality of baffles are arranged in the lower reaction cavity of the reactor cylinder in a circumferential direction, gaps are arranged between the baffles and the inner wall of the reactor cylinder, and the upper end of the baffles is fixedly connected to the inner wall of the reactor cylinder.
[0011] Preferably, the outer wall of the reactor cylinder is further provided with a gas inlet communicating with the upper buffer cavity, and the bottom of the outer wall of the reactor cylinder is provided with a discharge port communicating with the bottom of the lower reaction cavity.
[0012] Preferably, the outer wall of the reactor cylinder is further provided with a pressure gauge interface communicating with the upper buffer cavity, and the lower part of the outer wall of the reactor cylinder is further provided with a thermometer interface communicating with the lower reaction cavity.
[0013] Preferably, a jacket is further arranged outside the corresponding part of the reactor cylinder of the lower reaction cavity, a heat exchange cavity is formed between the jacket and the reactor cylinder, the jacket is provided with a heat exchange medium inlet and a heat exchange medium outlet communicating with the heat exchange cavity, and baffles are arranged in the heat exchange cavity between the jacket and the reactor cylinder, and the baffles are fixed to the outer wall of the reactor cylinder or the inner wall of the jacket.
[0014] Preferably, the rotating shaft comprises a connected and fastened upper transmission shaft and a lower stirring shaft, the upper end of the upper transmission shaft extends out of the reactor cylinder and is connected to a driving motor, and the stirring blades are arranged on the lower stirring shaft.
[0015] Preferably, a bearing chamber is fixedly arranged above the reactor cylinder, at least one bearing with a seat is fixedly arranged in the bearing chamber, and the upper transmission shaft of the rotating shaft is sleeved in the bearing with a seat.
[0016] Preferably, a sealing element is arranged at the top of the reactor cylinder, and the rotating shaft is rotationally connected to the sealing element.
[0017] The beneficial effects of the utility model are as follows:
[0018] (1) The solid-liquid reactor provided by the utility model only needs to be initiated once when used for preparing Grignard reagent, the subsequent liquid-phase reactants are continuously fed, the solid-phase reactants are fed at intervals, the overflow discharge port continuously discharges, and the reaction continuously proceeds without multiple initiations.
[0019] (2) The solid-liquid reactor provided by the utility model is provided with a buffer cavity at the upper part of the reactor cylinder, if violent boiling occurs in the reaction process, the upper buffer cavity can store the violently boiling materials, and then immediately flow back into the lower reaction cavity, so that the reactants are prevented from overflowing the reactor.
[0020] (3) The solid-liquid reactor provided by the utility model, liquid phase feeds from the lower part of the lower reaction cavity, solid phase feeds from the upper part of the lower reaction cavity, liquid phase moves from bottom to top and solid phase moves from top to bottom in the lower reaction cavity, which increases the contact area of solid-liquid phase and improves the reaction rate; moreover, the length-diameter ratio of the lower reaction cavity of the reactor cylinder is large, and a plurality of baffle plates are arranged in the lower reaction cavity, which can reduce the circumferential flow of reaction materials during stirring, improve axial circulation, make excessive solid phase in a completely off-bottom suspension state, reduce the aggregation of solid phase and promote the progress of reaction;
[0021] (4) The solid-liquid reactor provided by the utility model controls the setting area of the stirring blade and the position of the overflow discharge port, so that solid phase is uniformly dispersed in the area below the overflow discharge port in the lower reaction cavity during stirring, that is, the overflow discharge port is located above the solid phase dispersion area, so that solid phase is prevented from flowing out of the overflow discharge port with reaction products;
[0022] (5) The solid-liquid reactor provided by the utility model has a large length-diameter ratio, a larger specific surface area, a high heat transfer coefficient and strong heat exchange capacity compared with a kettle-type reactor. BRIEF DESCRIPTION OF DRAWINGS
[0023] In order to clearly illustrate the technical solutions in the embodiments of the utility model or the prior art, the following will briefly introduce the drawings needed to be used in the embodiments or prior art description. Obviously, the drawings in the following description are some embodiments of the utility model, and for those skilled in the art, other drawings can also be obtained from these drawings without creative labor.
[0024] Figure 1 It is the overall structure schematic diagram of the reactor of the utility model;
[0025] Figure 2 It is the structure schematic diagram of the reactor cylinder of the utility model;
[0026] Figure 3 It is the structure schematic diagram of the stirring assembly of the utility model;
[0027] Figure 4 It is the structure schematic diagram of the bearing chamber of the utility model.
[0028] In the figure, 1 is a reactor barrel, 101 is an upper buffer cavity, 102 is a lower reaction cavity, 103 is a solid phase feeding port, 104 is a liquid phase feeding port, 105 is an overflow discharge port, 106 is an air inlet, 107 is a discharge port, 108 is a solid phase feeding pipe, 109 is a baffle, 110 is a pressure gauge interface, 111 is a thermometer interface, 2 is a jacket, 201 is a heat exchange medium inlet, 202 is a heat exchange medium outlet, 203 is a baffle, 3 is a stirring assembly, 301 is a stirring blade, 302 is an upper transmission shaft, 303 is a lower stirring shaft, 4 is a driving motor, 5 is a bearing chamber, 501 is a bearing with a seat, and 6 is a sealing element. DETAILED DESCRIPTION
[0029] The utility model provides a solid -liquid reactor, for the purpose, technical scheme and effect of the utility model more clearly, explicitly, the following to the utility model further detailed explanation. It should be understood that the specific embodiments described here are only used to explain the utility model, and are not used to limit the utility model.
[0030] In the description of the utility model, it should be understood that the terms "upper", "lower", "top", "bottom", "inner", "outer" and the like indicate the orientation or positional relationship shown in the drawings, which is only for the convenience of describing the utility model and simplifying the description, and does not indicate or imply that the indicated device or element must have a particular orientation, be constructed and operated in a particular orientation, therefore it can not be understood as a limitation on the utility model.
[0031] The utility model will be described in detail below in combination with the drawings:
[0032] Embodiment 1
[0033] Referring to Figure 1 , the embodiment provides a solid -liquid reactor, is placed vertically, is used for the production process of solid phase and liquid phase reaction, such as the production of grignard reagent. The reactor specifically includes: reactor barrel 1, jacket 2 and stirring assembly 3, the jacket 2 is arranged outside the reactor barrel 1, the stirring assembly 3 is arranged inside the reactor barrel 1, and the upper end of the stirring assembly 3 is out of the reactor barrel 1 and is connected with driving motor 4.
[0034] Specifically, referring to Figure 2 The inner cavity of the above-mentioned reactor barrel 1 is divided into two parts of the upper buffer cavity 101 and the lower reaction cavity 102 in communication, wherein the volume of the upper buffer cavity 101 is greater than the volume of the lower reaction cavity 102, and the volume of the upper buffer cavity 101 is preferably 2-3 times that of the lower reaction cavity 102, for the buffer of violent boiling initiation, to prevent the overflow of reaction liquid when violent boiling.
[0035] The outer wall of the reactor cylinder 1 is provided with a solid phase feeding port 103, a liquid phase feeding port 104, an overflow discharge port 105, an air inlet 106 and a discharge port 107. The solid phase feeding port 103 is arranged on the upper portion of the outer wall of the reactor cylinder 1 and communicates with the upper buffer chamber 101. The solid phase feeding port 103 is used for feeding solid phase. The solid phase feeding port 103 is connected with a solid phase feeding pipe 108. The solid phase feeding pipe 108 is arranged obliquely downward. The solid phase can enter the lower reaction chamber 102 through the upper buffer chamber 101 under the action of gravity. The liquid phase feeding port 104 is arranged on the lower portion of the outer wall of the reactor cylinder 1 and communicates with the lower portion of the lower reaction chamber 102. The liquid phase feeding port 104 is used for feeding liquid phase. The liquid phase is fed from the lower portion of the lower reaction chamber 102. The solid phase is fed from the upper portion of the lower reaction chamber 102. The liquid phase moves upward from the lower portion in the lower reaction chamber 102. The solid phase moves downward from the upper portion in the lower reaction chamber 102. The contact area of the solid-liquid phase is increased. The overflow discharge port 105 is arranged on the middle portion of the outer wall of the reactor cylinder 1 and communicates with the upper portion of the lower reaction chamber 102. The liquid phase product after reaction is discharged from the overflow discharge port 105. The air inlet 106 is arranged on the upper portion of the outer wall of the reactor cylinder 1 and communicates with the upper buffer chamber 101. The air inlet 106 is used for introducing inert gas such as nitrogen. The reaction is carried out in a protective atmosphere. The reaction of the reactants with oxygen and water in the air is prevented. The discharge port 107 is arranged on the bottom of the outer wall of the reactor cylinder 1 and communicates with the bottom of the lower reaction chamber 102. The material in the reactor cylinder 1 is discharged after production.
[0036] In addition, the length-diameter ratio of the lower reaction chamber 102 of the reactor cylinder 1 is 2-3. A plurality of baffles 109 are arranged in the lower reaction chamber 102 of the reactor cylinder 1 in a circumferential direction. A gap is arranged between the baffle 109 and the inner wall of the reactor cylinder 1. The length direction of the baffle 109 is parallel to the axial direction of the reactor cylinder 1. The upper end of the baffle 109 is fixedly connected to the inner wall of the reactor cylinder 1 by welding. The lower end of the baffle 109 is located above the liquid phase feeding port 104. By controlling the length-diameter ratio of the lower reaction chamber 102 and arranging the baffles 109 in the lower reaction chamber 102, the circumferential flow of the reaction material can be reduced during stirring. The axial circulation is improved. The solid phase is in a completely off-bottom suspension state.
[0037] Specifically, referring to Figure 2 The jacket 2 is sleeved on the outer portion of the corresponding portion of the reactor cylinder 1 of the lower reaction chamber 102. A heat exchange chamber is formed between the jacket 2 and the reactor cylinder 1. The jacket 2 is provided with a heat exchange medium inlet 201 and a heat exchange medium outlet 202 which communicate with the heat exchange chamber. High-temperature heat exchange medium or low-temperature heat exchange medium is introduced into the heat exchange chamber according to the reaction requirement. The lower reaction chamber 102 reaches the required reaction temperature.
[0038] In addition, baffles 203 are arranged in the heat exchange cavity between the jacket 2 and the reactor cylinder 1, the baffles 203 are fixed to the outer wall of the reactor cylinder 1 or the inner wall of the jacket 2, and the baffles 203 can be in a spiral shape. By arranging the baffles 203 in the heat exchange cavity, the flow rate of the heat exchange medium in the jacket 2 can be increased, the heat transfer coefficient can be increased, and the heat transfer capacity can be enhanced.
[0039] Specifically, referring to Figure 1 and Figure 3 The stirring assembly 3 includes a rotating shaft and a plurality of stirring blades 301 arranged in the lower part of the rotating shaft in the axial direction. In order to ensure that the rotating shaft maintains a high critical speed when it is in a long cantilever state, the rotating shaft in the embodiment includes a connected and fixed upper transmission shaft 302 and a lower stirring shaft 303, wherein the upper transmission shaft 302 is arranged in the upper buffer cavity 102 of the reactor cylinder 1 and the upper end thereof extends out of the reactor cylinder 1 and is connected with the driving motor 4, the lower stirring shaft 303 is arranged in the lower reaction cavity 102 of the reactor cylinder 1, and the stirring blades 301 are arranged on the lower stirring shaft 303 to stir the liquid phase and solid phase reactants in the lower reaction cavity 102. In addition, the uppermost stirring blade 301 needs to be controlled below the overflow discharge port 105, and a certain distance is left between the uppermost stirring blade 301 and the overflow discharge port 105. During the stirring process, the solid phase is uniformly dispersed in the area below the overflow discharge port 105 in the lower reaction cavity 102 as much as possible, so as to prevent the solid phase from flowing out of the overflow discharge port 105 with the reaction product; in addition, a filter screen can also be arranged on the overflow discharge port 105 to further prevent the solid phase from flowing out of the overflow discharge port 105 with the reaction product.
[0040] In order to facilitate the replacement of the stirring part according to different needs, the upper transmission shaft 302 and the lower stirring shaft 303 can be connected by thermal shrinkage interference or rigid shaft coupling; if replacement is not required, the upper transmission shaft 302 and the lower stirring shaft 303 can be fixed as a whole by welding.
[0041] In order to facilitate the adjustment of the stirring speed, the driving motor 4 can be a motor that can accurately adjust the speed, such as a servo motor. By controlling the stirring speed, the solid phase suspended material in the reactor cylinder 1 is in a completely off-bottom suspended state, and the contact area of the liquid phase and the solid phase is increased.
[0042] Specifically, referring to Figure 4 In the embodiment, a bearing chamber 5 is also fixedly arranged above the reactor cylinder 1, two bearing seats 501 are fixedly arranged in the bearing chamber 5, the upper transmission shaft 302 of the rotating shaft is sleeved in the bearing seat 501, and the upper end of the upper transmission shaft 302 extends out of the bearing seat 501 during installation, so as to be connected with the driving motor 4. The bearing chamber and the bearing seat are used to support the rotating shaft and ensure the rotation accuracy and stability of the rotating shaft.
[0043] In addition, in the embodiment, the top of the reactor cylinder 1 is further provided with a sealing element 6, and the rotating shaft is rotationally connected with the sealing element 6. The sealing element 6 is used to seal the top of the reactor cylinder 1 and to seal the rotationally connected part of the reactor cylinder 1 and the rotating shaft. The sealing element 6 is specifically a mechanical seal, which has high reliability, small power loss, and high sealing pressure, or other sealing forms such as magnetic sealing and packing sealing can also be selected according to requirements.
[0044] In the embodiment, the Grignard reagent is prepared by using the solid-liquid reactor. The specific process is as follows:
[0045] First, the reactor cylinder is replaced by nitrogen to discharge air, then the magnesium chips are added into the lower reaction cavity of the reactor cylinder from the solid-phase feeding port, the halogenated hydrocarbon and the solvent tetrahydrofuran are added into the lower reaction cavity of the reactor cylinder from the liquid-phase feeding port, after the feeding is completed, the Grignard reaction is initiated by heating the reactor cylinder by introducing a heat exchange medium with a higher temperature into the heat exchange cavity between the jacket and the reactor cylinder, after the initiation, the heating is stopped, and a heat exchange medium with a lower temperature such as cold water is introduced into the heat exchange cavity between the jacket and the reactor cylinder, the heat exchange medium in the heat exchange cavity exchanges heat with the heat generated during the reaction to ensure that the heat generated during the preparation of the Grignard reagent is promptly discharged, after the first initiation, the feeding speed of the liquid-phase reactants halogenated hydrocarbon and solvent tetrahydrofuran is set to continuously feed the liquid phase, and the solid-phase reactant magnesium is intermittently fed according to the actual reaction condition, the reaction is continuously carried out, and the reaction product is continuously discharged from the overflow discharge port.
[0046] In addition, when the solid-phase reactant magnesium is fed, the discharge port can be closed, and after the magnesium is uniformly stirred, the discharge port is opened to prevent the magnesium from contacting the upper surface of the reaction product on the liquid surface and flowing out of the overflow discharge port with the reaction product.
[0047] Embodiment 2
[0048] The difference between the embodiment 2 and the embodiment 1 is that in the embodiment 2, the outer wall of the reactor cylinder 1 is further provided with a pressure gauge interface 110 and a thermometer interface 111. The pressure gauge interface 110 is arranged on the upper part of the outer wall of one side of the reactor cylinder 1 and communicates with the upper buffer cavity 101, and the thermometer interface 111 is arranged on the lower part of the outer wall of one side of the reactor cylinder 1 and communicates with the lower reaction cavity 102.
[0049] The pressure gauge interface 110 and the thermometer interface 111 are respectively used to connect a pressure sensor and a temperature sensor to monitor the real-time reaction pressure and reaction temperature during the reaction, and the operator can adjust according to the monitored reaction pressure and reaction temperature to ensure that the pressure and temperature in the reactor meet the reaction requirements, for example, when the temperature is too high, the flow of the heat exchange medium can be increased to reduce the temperature.
[0050] It should be noted that the parts not described in the utility model can be realized by using or referring to the existing technology.
[0051] Of course, the above description is not a limitation of the utility model, and the utility model is not limited to the above examples. Changes, modifications, additions or replacements made by those skilled in the art within the essential scope of the utility model should also be within the protection scope of the utility model.
Claims
1. A solid-liquid reactor, placed vertically, characterized in that, The utility model relates to a reactor, which comprises: a reactor cylinder (1) and a stirring assembly (3) arranged in the reactor cylinder (1); the inner cavity of the reactor cylinder (1) is divided into an upper buffer cavity (101) and a lower reaction cavity (102) in communication, the outer wall of the reactor cylinder (1) is provided with a solid-phase feeding port (103) in communication with the upper buffer cavity (101) at the upper part, the outer wall of the reactor cylinder (1) is provided with an overflow discharge port (105) in communication with the upper part of the lower reaction cavity (102) at the middle part, and the outer wall of the reactor cylinder (1) is provided with a liquid-phase feeding port (104) in communication with the lower part of the lower reaction cavity (102) at the lower part; the stirring assembly (3) comprises a rotating shaft and a plurality of stirring blades (301) arranged in the lower part of the rotating shaft in the axial direction, the upper end of the rotating shaft extends out of the reactor cylinder (1), the stirring blades (301) are arranged in the lower reaction cavity (102) of the reactor cylinder (1), and the uppermost stirring blade (301) is located below the overflow discharge port (105).
2. The solid-liquid reactor of claim 1, wherein The volume of the upper buffer cavity (101) of the reactor cylinder (1) is 2-3 times that of the lower reaction cavity (102).
3. The solid-liquid reactor of claim 1, wherein The length-diameter ratio of the lower reaction cavity (102) of the reactor cylinder (1) is 2-3.
4. The solid-liquid reactor of claim 1, wherein A plurality of baffles (109) are arranged in the lower reaction cavity (102) of the reactor cylinder (1) in the circumferential direction, gaps are arranged between the baffles (109) and the inner wall of the reactor cylinder (1), and the upper end of each baffle (109) is fixedly connected to the inner wall of the reactor cylinder (1).
5. The solid-liquid reactor of claim 1, wherein The outer wall of the reactor cylinder (1) is provided with an air inlet (106) in communication with the upper buffer cavity (101) at the upper part, and the bottom of the outer wall of the reactor cylinder (1) is provided with a discharge port (107) in communication with the bottom of the lower reaction cavity (102).
6. The solid-liquid reactor of claim 1, wherein The outer wall of the reactor cylinder (1) is further provided with a pressure gauge interface (110) in communication with the upper buffer cavity (101) at the upper part, and the lower part of the outer wall of the reactor cylinder (1) is further provided with a thermometer interface (111) in communication with the lower reaction cavity (102).
7. The solid-liquid reactor of claim 1, wherein The utility model further comprises a jacket (2), the jacket (2) is arranged outside the corresponding part of the reactor cylinder (1) of the lower reaction cavity (102), a heat exchange cavity is formed between the jacket (2) and the reactor cylinder (1), the jacket (2) is provided with a heat exchange medium inlet (201) and a heat exchange medium outlet (202) in communication with the heat exchange cavity, and baffles are arranged in the heat exchange cavity between the jacket (2) and the reactor cylinder (1), the baffles are fixed to the outer wall of the reactor cylinder (1) or the inner wall of the jacket (2).
8. The solid-liquid reactor of claim 1, wherein The rotating shaft comprises an upper transmission shaft (302) and a lower stirring shaft (303) connected and fixed, the upper end of the upper transmission shaft (302) extends out of the reactor cylinder (1) and is connected to a driving motor (4), and the stirring blades (301) are arranged on the lower stirring shaft (303).
9. A solid-liquid reactor according to claim 8, wherein The reactor cylinder (1) is fixedly provided with a bearing chamber (5) above, at least one bearing with seat (501) is fixedly arranged in the bearing chamber (5), and the upper transmission shaft (302) of the rotating shaft is sleeved in the bearing with seat (501).
10. The solid-liquid reactor of claim 1, wherein The reactor cylinder (1) is provided with a sealing piece (6) at the top, and the rotating shaft is rotationally connected with the sealing piece (6).